WO2013149572A1 - 规模化连续制备二维纳米薄膜的装备 - Google Patents
规模化连续制备二维纳米薄膜的装备 Download PDFInfo
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- WO2013149572A1 WO2013149572A1 PCT/CN2013/073573 CN2013073573W WO2013149572A1 WO 2013149572 A1 WO2013149572 A1 WO 2013149572A1 CN 2013073573 W CN2013073573 W CN 2013073573W WO 2013149572 A1 WO2013149572 A1 WO 2013149572A1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/568—Transferring the substrates through a series of coating stations
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
- C23C14/0647—Boron nitride
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/48—Ion implantation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/54—Apparatus specially adapted for continuous coating
Definitions
- the present invention relates to a new material preparation apparatus, and more particularly to an apparatus for large-scale continuous preparation of novel two-dimensional nanomaterials such as graphene, metal chalcogenide, silene, terpene, and boron nitride. Background technique
- Graphene is a honeycomb-like single carbon atom layer with a thickness of 0.334 nm. It has excellent two-dimensional electrical, optical, thermal, mechanical properties and chemical stability. Graphene is in ultrafast optoelectronic devices, clean energy, Sensors and other aspects have broad application prospects.
- the transmission speed of electrons in graphene is 150 times that of silicon. IBM and other famous companies have already prepared ultra-fast optoelectronic devices with speeds up to terahertz.
- the University of California uses graphene to develop optical modems, which is expected to increase the network speed by 10,000 times.
- the global demand for semiconductor crystalline silicon is about 2,500 tons per year.
- graphene replaces one-tenth of crystalline silicon to make high-end integrated circuits such as RF circuits, the market capacity is at least 500 billion yuan. Because graphene has only 2.3% light absorption, this makes graphene useful for the preparation of flexible transparent electrodes for optoelectronic devices such as display devices, solar cells, touch panels, etc., thereby replacing expensive, resource-intensive, non-freely foldable indium-based components.
- ITO transparent conductive film According to reports, the global demand for ITO conductive glass in 2011 is between 85 and 95 million pieces, so that the replacement space for graphene is huge.
- New two-dimensional graphene-based material comprising a layered metal chalcogenide (metal chalcogenides), silicon-ene (sili Cene), germanium-ene (germanene), BN (boron nitride) and the like.
- metal chalcogenides metal chalcogenides
- silicon-ene silicon-ene
- germanium-ene germanium-ene
- BN boron nitride
- the apparatus for preparing two-dimensional nanofilms is basically a quartz tube high temperature furnace [Science 324, 1312-1314 (2009); Nature Nanotechnology 5, 574 (2010); Nano Lett. 11, 297-303 (2011)].
- the high temperature furnace based on quartz tube only has the single function of synthesizing two-dimensional nano-film on the existing metal catalyst layer, that is, the surface of the substrate cannot be processed successively, and the catalysis required for preparing the two-dimensional nano-film on the substrate is prepared.
- the two-dimensional nano-film synthesized by quartz tube furnace has many structural defects, which leads to poor electron transport performance of the prepared film.
- the quartz tube furnace has severely restricted the application of two-dimensional nano-films such as graphene films, which is not suitable for scale.
- a two-dimensional nanofilm such as graphene is continuously prepared.
- each chamber should be proprietary in the preparation process of the two-dimensional nano film. Unique functional role.
- the present invention provides an apparatus capable of large-scale continuous preparation of two-dimensional nano-films such as graphene, metal chalcogenide, silene, terpene or boron nitride.
- the apparatus is provided with a high temperature resistant sample transport device; in order to achieve balance and stability during continuous preparation, it is preferred to provide a transition between a specific chamber and the chamber.
- the balance chamber and the balance chamber have a stabilizing effect on the whole preparation process of the two-dimensional nano film; the functions of the film preparation chamber and the chemical vapor deposition chamber are mainly used for preparing the film and appropriately processing the prepared film,
- the film includes a catalytic layer, a precursor of a two-dimensional film, a two-dimensional film, and the like; the function of the processing chamber is mainly used to optimize the structure of the substrate, the catalytic layer, the precursor of the two-dimensional film, and the two-dimensional film, thereby being able to prepare
- the high-quality two-dimensional film; the device has the characteristics of simple structure, simple operation, good safety, etc.
- the process for preparing the two-dimensional nano film by the device is simple, the cost is low, and the prepared film has excellent structure and performance.
- the physical vapor deposition system includes any one or a combination of two or more of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system.
- the chemical vapor deposition system comprises a chemical vapor deposition system composed of a chamber, a gas and a heater (ie, a thermal chemical vapor deposition system), a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, and an aerosol assist. Any one or a combination of two or more of a chemical vapor deposition system, an inductively coupled plasma chemical vapor deposition system.
- continuous preparation of the two-dimensional film can be realized by selecting different device combinations or equipments.
- a scaled-up apparatus for continuously preparing a two-dimensional nanofilm comprising a feed chamber, a first film preparation chamber, and a discharge chamber.
- the first film preparation chamber may also be referred to as a sample preparation chamber.
- the feed chamber, the first film preparation chamber and the discharge chamber are each provided with a sample transfer device, and the sample can be transferred from the feed chamber to the first film preparation chamber through the sample transfer device, from the first
- the film preparation chamber is transported to the discharge chamber for continuous preparation of the two-dimensional nanofilm;
- the sample transfer device includes any one or a combination of two or more of a roller, a pulley and a conveyor belt.
- the feeding chamber is provided with a valve communicating with the atmosphere, a valve is arranged between the feeding chamber and the first film preparing chamber, and a valve is arranged between the first film preparing chamber and the discharging chamber.
- the material chamber is provided with a valve that communicates with the atmosphere.
- At least one of the feeding chamber, the first film preparation chamber and the discharge chamber is provided with a heating device; the heating device may be a resistance wire heating device, an infrared heating device, a laser heating device or the like.
- the feeding chamber, the first film preparing chamber and the discharging chamber are respectively provided with independent vacuuming devices, and each vacuuming device comprises various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc.
- the vacuum device can maintain the vacuum of each chamber at a normal pressure to between 1.0 x 10 - 1 Q Pa.
- At least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided with one or more gas connection ports, and the gas connection port may be a gas connection port, a gas connection port It can also be connected to the gas mixing box, and the gas connection port is connected to the gas path; at least two or more gas paths are connected in parallel at the inlet of the gas mixing box, so that two or more gases can enter the gas mixing box at the same time; each gas path is It is equipped with a mass flow meter and an electromagnetic shut-off valve, so that the flow rate of the gas can be independently and precisely controlled; the gas to be introduced can be selected from an inert gas such as argon or nitrogen, a reducing gas such as hydrogen, an oxidizing gas such as oxygen, and a two-dimensional synthesis.
- the gaseous precursors required for the nanofilm are, for example, CH 4 , C 2 H 4 , C 2 H 2 , NH 3 , B 3 N 3 H 6 or steam of ethanol.
- At least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided with a chemical vapor deposition system, including a plasma enhanced chemical vapor deposition system and a microwave plasma chemical vapor deposition system; Any one of the material chamber, the first film preparation chamber or the discharge chamber may form a chemical vapor deposition system with the heating device and the gas connection port, and the chemical vapor deposition system may be generally referred to as thermal chemical vapor deposition. system.
- At least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided with a physical vapor deposition system, and the physical vapor deposition system is a sputtering target thin film deposition system, an electron gun deposition system Any one or a combination of two or more of an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system.
- Either one of the feed chamber, the first membrane preparation chamber or the discharge chamber may include both a chemical vapor deposition system and a physical vapor deposition system.
- the temperature of at least one of the feed chamber, the first film preparation chamber or the discharge chamber is controlled at 20 to 1600 ° C;
- the chamber wall of at least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided Have a heat shielding system;
- the chamber wall of at least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided with a cooling system, and the cooling system may be double-layer water-cooled system.
- the chamber is provided with a chamber of the heat shield system, while the chamber wall of the chamber is provided with a cooling system.
- the apparatus for large-scale continuous preparation of the two-dimensional nano-film of the present invention may further be provided with a control system including a sample transmission control system, a gas path control system, a vacuum control system, a valve control system or a temperature control system. Any one or a combination of two or more.
- the apparatus of the present invention can be used for growing a two-dimensional nano-film including graphene, metal chalcogenide, silicon dip, decene or boron nitride.
- the desired solid can be appropriately prepared. , precursors such as liquids or gases.
- the feed chamber serves as a surface treatment chamber
- the first film preparation chamber serves as a preparation chamber for the substrate, the catalytic layer and the two-dimensional nano-film
- the discharge chamber serves as a cooling chamber or a two-dimensional nano-film.
- Processing chamber the feed chamber is provided with a plasma surface processor
- the first film preparation chamber is provided with a thin film deposition system.
- the basic process of large-scale continuous preparation of two-dimensional nano-films includes: placing a substrate material or a catalytic layer required for synthesizing a two-dimensional nano film on a carrier gantry, and transferring the sample transfer device to the first film through the feed chamber
- the chamber is prepared, and a two-dimensional nano-film is prepared by physical vapor deposition or chemical vapor deposition in the first film preparation chamber, and then the prepared two-dimensional nano film is sent from the sample transfer device to the discharge chamber.
- the basic process of continuously preparing a two-dimensional nano film further includes: placing a substrate or a catalytic layer required for synthesizing a two-dimensional nano film on a loading gantry
- the sample transfer device is transferred to the feed chamber. Under a certain atmosphere, the substrate material or the catalytic layer is pretreated in the feed chamber, and then the substrate or catalytic layer is transferred to the first film by the sample transfer device.
- a catalytic layer, a carbon film or a two-dimensional nano-film is prepared by a physical vapor deposition or a chemical vapor deposition method in a first film preparation chamber; the film may be sent to a discharge chamber for heat treatment or processing by a sample transfer device. Surface optimization processing.
- the technical solution adopted by the invention can also be as follows:
- a scaled-up apparatus for continuously preparing a two-dimensional nanofilm includes a feed chamber, a first film preparation chamber, a first balance chamber, and a chemical vapor deposition chamber.
- the film preparation chamber is referred to as the first film preparation chamber
- the balance chamber is referred to as the first balance chamber.
- the balance chamber can serve as a transition, stable, and balanced sample during sample transfer.
- the chemical vapor deposition chamber is also referred to as a thin film preparation chamber.
- a sample transfer device is disposed between each of the feed chamber, the first thin film preparation chamber, the first balance chamber, and the chemical vapor deposition chamber, and the sample can be moved through the sample transfer device.
- the material chamber is continuously transferred to the first film preparation chamber, continuously transferred from the first film preparation chamber to the first balance chamber, and continuously transferred from the first balance chamber to the chemical vapor deposition chamber to realize the two-dimensional nano film Continuous preparation of the sample;
- the sample transfer device includes any one or a combination of two or more of a roller, a pulley, a conveyor belt, and the like.
- the feed chamber is provided with a valve that communicates with the atmosphere, a valve is disposed between the feed chamber and the first film preparation chamber, and a valve is disposed between the first film preparation chamber and the first balance chamber.
- a valve is disposed between the first balance chamber and the chemical vapor deposition chamber, and the chemical vapor deposition chamber is provided with a valve that communicates with the atmosphere.
- the feed chamber, the first film preparation chamber, the first balance chamber, and the chemical vapor deposition chamber are connected in one piece by a sample transfer device and a valve.
- the first thin film preparation chamber is provided with a physical vapor deposition system including an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system. Any one or a combination of two or more of the systems.
- the chemical vapor deposition chamber is provided with a heating device and a gas connection port;
- the chemical vapor deposition chamber, the heating device and the gas connection port can constitute a simple chemical vapor deposition system
- the chemical vapor deposition chamber is further provided with any one or a combination of two or more of a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, an aerosol assisted chemical vapor deposition system, and the like;
- the deposition chamber is provided with a valve that is open to the atmosphere, so the chemical vapor deposition chamber also functions as a discharge chamber.
- At least one of the feed chamber, the first film preparation chamber and the first balance chamber is provided with a gas connection port; preferably, the feed chamber, the first film preparation chamber and the first balance The chambers are each provided with a gas connection port;
- the gas connection port may be a gas connection port or a gas mixture box, and at least two or more gas paths may be connected in parallel to the inlet of the gas mixture box, so that two or more gases may be used.
- the gas mixing box is entered; preferably, each gas path is independently connected with a metering and flow regulating device such as a mass flow meter and an electromagnetic shut-off valve, so that the flow rate of each gas can be independently and accurately controlled.
- the feeding chamber, the first film preparing chamber, the first balancing chamber, and the chemical vapor deposition chamber are all provided with a vacuuming device, and each vacuuming device comprises various vacuum pumps, vacuum pipes, vacuum valves, vacuum By the vacuuming device, the vacuum of each chamber can be maintained at a normal pressure to between 1.0 x 10 - 1 () Pa.
- At least one of the feed chamber and the first film preparation chamber is provided with a sample processing device; preferably, the feed chamber and the first film preparation chamber are each provided with a sample processing device;
- the sample processing device adopts a plasma surface processor, a wire ionizing or heating device for gas ionization, and the like, and the device for modifying the sample can be used under vacuum high frequency conditions.
- the ionization of the gas is realized; the heating device uses a resistance heating device, an infrared heating device, a laser heating device, and the like to realize heating of the sample.
- the temperature in the feed chamber, the first film preparation chamber and the chemical vapor deposition chamber can be controlled at 20 to 2000 ° C;
- At least one of the feed chamber, the first film preparation chamber and the chemical vapor deposition chamber is provided with an insulation shielding system; Only in the chamber where high temperature (such as higher than 40CTC) exists, there is an insulation shielding system.
- a cooling system is provided in the chamber wall of at least one of the feeding chamber, the first film preparation chamber and the chemical vapor deposition chamber, and the cooling system may be a double water cooling system or the like.
- the cooling system may be a double water cooling system or the like.
- a high temperature e.g. 40 CTC
- the apparatus for large-scale continuous preparation of two-dimensional nano-films of the present invention is further provided with a control system, and the control system comprises a sample transmission control system, a gas path control system, a vacuum control system, a valve control system or a temperature control system. Any one or a combination of two or more.
- the feed chamber serves as a substrate and/or a chamber for processing the catalytic layer
- the first film preparation chamber serves as a chamber for preparing a film of a two-dimensional nano film or a catalytic layer
- the chemical vapor deposition chamber serves as a cooling chamber.
- the device of the invention can be used for growing various two-dimensional nano-films including graphene, metal chalcogenide, silicon thinner, germanium or boron nitride, and can be appropriately selected according to the difference of the two-dimensional nano film synthesized. Prepare the desired precursors such as solids, liquids or gases.
- the basic process for continuously preparing a two-dimensional nano film comprises: placing a substrate and/or a catalytic layer required for synthesizing a two-dimensional nano film on a carrier gantry and transferring it from a sample transfer device to a feed chamber, in a certain atmosphere environment Substituting the substrate material and/or the catalytic layer in the feed chamber, and then transferring the substrate and/or the catalytic layer to the first thin film preparation chamber by the sample transfer device; utilizing in the first thin film preparation chamber
- the physical vapor deposition system prepares a two-dimensional nano-film or a catalytic layer film; the two-dimensional film preparation can also be prepared in a chemical vapor deposition chamber and then transferred to the atmosphere to complete the preparation.
- the technical solution adopted by the invention can also be as follows:
- An apparatus for continuously preparing a two-dimensional nano film by scale characterized in that: a feeding chamber, a first processing chamber, a first balance chamber, a first film preparation chamber, and a second balance are sequentially disposed on a production line a chamber, a second processing chamber, and a discharge chamber.
- the film preparation chamber is referred to herein as the first film preparation chamber.
- the feeding chamber is provided with a valve communicating with the atmosphere, a valve is arranged between the feeding chamber and the first processing chamber, and a valve is arranged between the first processing chamber and the first balancing chamber, the first balance a valve is disposed between the chamber and the first film preparation chamber, a valve is disposed between the first film preparation chamber and the second balance chamber, and a valve is disposed between the second balance chamber and the second processing chamber.
- a valve is disposed between the second processing chamber and the discharge chamber, and the discharge chamber is provided with a valve that is open to the atmosphere;
- a sample transfer device a sample
- a sample is provided between the feed chamber, the first processing chamber, the first balance chamber, the first thin film preparation chamber, the second balance chamber, the second processing chamber, and the discharge chamber Transfer from the atmosphere to the feed chamber by the sample transfer device, from the feed chamber to the first processing chamber, from the first processing chamber to the first balancing chamber, from the first balancing chamber to the first
- the film preparation chamber is transferred from the first film preparation chamber to the second balance chamber, from the second balance chamber to the second processing chamber, from the second processing chamber to the discharge chamber, and from the discharge
- the chamber is delivered to the atmosphere to effect continuous preparation of the two-dimensional nanofilm;
- the sample transport device includes any one or a combination of two or more of a roller, a pulley, and a conveyor belt.
- the balance chamber functions as a transition, stable, and balanced sample during sample transfer.
- At least one of the feed chamber, the first processing chamber, the first membrane preparation chamber, the second processing chamber, and the discharge chamber is provided with a heating device to reach a certain temperature, such as 20 to 2000°. C ;
- the heating device may be a resistance heating device, an infrared heating device, a laser heating device, or the like.
- At least one of the feed chamber, the first processing chamber, the first balancing chamber, the first membrane preparation chamber, the second balance chamber, the second processing chamber, and the discharge chamber is provided with one or a plurality of gas connection ports;
- the gas connection port may be a gas connection port, and the gas connection port may also be connected to the gas mixing box;
- the inlet of the gas mixture box has at least two or more gas paths connected in parallel, which may be two or The above gas enters the gas mixing box at the same time; the mass flow meter and the electromagnetic cut-off valve are used, so that each gas path can precisely control the flow rate of the gas;
- the gas to be introduced can be selected from inert gases such as Ar and N 2 , reducing gas
- H 2 an oxidizing gas such as 0 2
- a gas required for synthesizing a two-dimensional nano film such as CH 4 , C 2 H 4 , C 2 H 2 , NH 3 , B 3 N 3 H 6 or a vapor of ethanol or the like.
- the feed chamber, the first processing chamber, the first balance chamber, the first film preparation chamber, the second balance chamber, the second processing chamber, and the discharge chamber are respectively connected to independent vacuuming devices, each The vacuuming device includes various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be made to be between normal pressure and 1.0 ⁇ 10 10 10 Pa by vacuuming.
- At least one of the first processing chamber, the first thin film preparation chamber, and the second processing chamber is provided with a physical vapor deposition system, the physical vapor deposition system Any one or a combination of two or more of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system is included.
- At least one of the first processing chamber, the first thin film preparation chamber, and the second processing chamber is provided with a chemical vapor deposition system including plasma enhanced chemical vapor deposition.
- a chemical vapor deposition system including plasma enhanced chemical vapor deposition.
- System aerosol-assisted chemical vapor deposition system, microwave plasma chemical vapor deposition system, etc.; any chamber (including first processing chamber, first membrane preparation chamber or second processing chamber), heating device and gas connection port
- any chamber including first processing chamber, first membrane preparation chamber or second processing chamber
- heating device and gas connection port Both can form a chemical vapor deposition system, which can be generally referred to as a thermal chemical vapor deposition system.
- Various films can be prepared in the first film preparation chamber or the second processing chamber, such as a substrate material for synthesizing a two-dimensional nano film such as a graphene film, a catalytic layer material, a carbon film, and a two-dimensional nano film.
- a substrate material for synthesizing a two-dimensional nano film such as a graphene film, a catalytic layer material, a carbon film, and a two-dimensional nano film.
- the required precursors as well as two-dimensional nanofilms.
- At least one of the first processing chamber, the first film preparation chamber, and the second processing chamber is provided with a heat shielding system
- the cavity wall of at least one of the first processing chamber, the first film preparation chamber and the second processing chamber is provided with a cooling system, and the cooling system may be double Layer water cooling system.
- the chamber is provided with a chamber of the heat shield system, while the chamber wall of the chamber is provided with a cooling system.
- the first processing chamber is provided with a sample surface processor, and the surface processor may be a plasma surface processor, a thermal processor or the like.
- the apparatus for continuously preparing a two-dimensional nano film of the present invention may further be provided with a control system, and the control system includes sample transmission control Any one or a combination of two or more of a system, a pneumatic control system, a vacuum control system, a valve control system, or a temperature control system.
- the apparatus of the present invention can be used to prepare two-dimensional nanofilms including graphene, metal chalcogenides, silenes, terpenes or boron nitride.
- the first processing chamber is used as a substrate surface processing chamber
- the first thin film preparation chamber is used as a catalytic layer or a preparation chamber for a two-dimensional nano-film
- the second processing chamber is used as a cooling chamber for preparing a two-dimensional nano-film. Or a two-dimensional nanofilm reprocessing chamber.
- the basic processes for preparing two-dimensional nano-films such as graphene films include, but are not limited to:
- the substrate material or catalytic layer material required to synthesize a two-dimensional nanofilm such as a graphene film is placed on a carrier gantry, and from the feed chamber through the sample transfer device through the feed chamber and a valve of the processing chamber enters the first processing chamber; under a certain atmosphere, the substrate material or the catalytic layer material is first surface treated in the first processing chamber, and then passed through the first balancing chamber by the sample transfer device Transferring the substrate or catalytic layer material to the first thin film preparation chamber; preparing a catalytic layer, a carbon film, etc.
- the transfer device is sent to the second balance chamber and then transferred to the second processing chamber.
- the two-dimensional nano film is prepared in the second processing chamber; finally, the prepared two-dimensional nano film is sent by the sample transfer device.
- Discharge chamber Depending on the function of each chamber, the two-dimensional nanofilm is either prepared in the first film preparation chamber or formed in the second processing chamber.
- the technical solution adopted by the invention can also be as follows:
- An apparatus for continuously preparing a two-dimensional nano film by scale characterized in that: a feeding chamber, a first processing chamber, a first balance chamber, a first film preparation chamber, a second balance chamber, and a second film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a discharge chamber; in order to harmonize the terminology, the processing chamber is referred to herein as a first processing chamber; functionally, chemical vapor deposition
- the chamber may also be referred to as a thin film preparation chamber.
- the feeding chamber is provided with a valve communicating with the atmosphere
- a valve is arranged between the feeding chamber and the first processing chamber, and a valve is arranged between the first processing chamber and the first balancing chamber
- the first balance a valve is disposed between the chamber and the first film preparation chamber
- a valve is disposed between the first film preparation chamber and the second balance chamber
- a valve is disposed between the second balance chamber and the second film preparation chamber.
- a valve is disposed between the second film preparation chamber and the third balance chamber
- a valve is disposed between the third balance chamber and the chemical vapor deposition chamber
- a chemical vapor deposition chamber is disposed between the discharge chamber and the discharge chamber
- the valve, the discharge chamber is provided with a valve that communicates with the atmosphere.
- a feed chamber a first processing chamber, a first balance chamber, a first thin film preparation chamber, a second balance chamber, a second thin film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a a sample transfer device is disposed in the chamber of the material chamber; the sample is transferred to the feed chamber through the sample transfer device, transferred from the feed chamber to the first processing chamber, and transferred from the first processing chamber to the first balance chamber Transfer from the first balance chamber to the first film preparation chamber, from the first film preparation chamber to the second balance chamber, from the second balance chamber to the second film preparation chamber, from the second The film preparation chamber is transferred to the third balance chamber, from the third balance chamber to the chemical vapor deposition chamber, and from the chemical vapor deposition chamber to the discharge chamber for continuous preparation of the two-dimensional nanofilm.
- the basic function of the feed chamber is to prepare the sample and enter the preparation device of the two-dimensional nano film, the first processing chamber realizes the pretreatment of the substrate or the catalytic layer, the first film preparation chamber and the second film preparation chamber It can be used to prepare substrates, catalytic layers, precursors of two-dimensional nano-films or two-dimensional nano-films required for the synthesis of two-dimensional nanomaterials.
- the chemical vapor deposition chamber can be used to prepare two-dimensional nano-films, and the equilibrium chamber is in the sample. It can function as a transition, stable, and balanced sample during transfer.
- the sample transfer device includes any one or a combination of two or more of a roller, a pulley, a belt, and the like.
- the entire apparatus passes the sample transfer device and the valve to the feed chamber, the first processing chamber, the first balance chamber, the first thin film preparation chamber, the second balance chamber, the second thin film preparation chamber, and the third balance chamber
- the chamber, the chemical vapor deposition chamber and the discharge chamber are connected in one piece.
- a feed chamber a first processing chamber, a first balance chamber, a first thin film preparation chamber, a second balance chamber, a second thin film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a At least one chamber in the material chamber is provided with a vacuuming device, and the vacuuming device comprises various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be made to a normal pressure to 1.0 by a vacuuming device. Between x 10 - 1Q Pa.
- the feed chamber, the first processing chamber, the first balance chamber, the first thin film preparation chamber, the second balance chamber, the second thin film preparation chamber, the third balance chamber, the chemical vapor deposition chamber The chamber and the discharge chamber are provided with independent vacuuming devices.
- Each vacuuming device includes various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be made at atmospheric pressure by the vacuuming device. To 1.0x l0 - 1Q Pa.
- a physical vapor deposition system is provided in a chamber of at least one of the first film preparation chamber and the second film preparation chamber for preparing a substrate, a catalytic layer, and a precursor of the two-dimensional nano film required for synthesizing the two-dimensional nano material
- the physical vapor deposition system includes any one or two of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system. More than one combination.
- Chamber of a chemical vapor deposition chamber is provided with heating means in order to reach a certain temperature, for example 20 ⁇ 2000 ° C; heating means may be resistance heating means, infrared heating means, laser heating means and the like.
- a feed chamber a first processing chamber, a first balance chamber, a first thin film preparation chamber, a second balance chamber, a second thin film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a At least one of the chambers is provided with one or more gas connections.
- the gas connection port may be a gas connection port, and the gas connection port may also be connected to the gas mixing box; the inlet of the gas mixture box is connected at least in parallel
- Two or more gas paths allow two or more gases to enter the gas mixing chamber at the same time; preferably, each gas path is independently connected with a metering and flow regulating device such as a mass flow meter and an electromagnetic shut-off valve. In order to achieve independent and precise control of the flow rate of each gas.
- the gas to be introduced may be selected from inert gases such as Ar and N 2 , reducing gases such as H 2 , oxidizing gases such as 02 , and gases required to synthesize two-dimensional nanofilms such as CH 4 , C 2 H 4 , C 2 H 2 , NH 3 , B 3 N 3 H 6 or steam of ethanol, etc., depending on the two-dimensional film to be synthesized, different gases can be appropriately selected.
- inert gases such as Ar and N 2
- reducing gases such as H 2
- oxidizing gases such as 02
- gases required to synthesize two-dimensional nanofilms such as CH 4 , C 2 H 4 , C 2 H 2 , NH 3 , B 3 N 3 H 6 or steam of ethanol, etc.
- the chemical vapor deposition chamber, the heating device and the gas connection port may constitute a chemical vapor deposition system; a chemical vapor deposition system may also be disposed in the chemical vapor deposition chamber, and the chemical vapor deposition system is plasma enhanced chemical vapor deposition Any one or a combination of two systems, a microwave plasma chemical vapor deposition system, an aerosol assisted chemical vapor deposition system, and an inductively coupled plasma chemical vapor deposition system.
- the first film preparation chamber, the second film preparation chamber or the first treatment chamber may be combined with the heating device and the gas connection port respectively to form a chemical vapor deposition system
- both the chemical vapor deposition system and the physical vapor deposition system are provided in the first film preparation chamber, the second film preparation chamber, the first processing chamber or the chemical vapor deposition chamber.
- At least one of the first processing chamber, the first film preparation chamber and the second film preparation chamber is provided with heating means to reach a certain temperature, such as 20 to 2000 ° C; It may be a resistance heating device, an infrared heating device, a laser heating device, or the like.
- the first processing chamber is provided with a sample processing device
- the sample processing device is a plasma sample processing device, a wire enthalpy or a heating device for gas ionization, and the like, which can modify the sample.
- the wire enthalpy for gas ionization can realize ionization of gas under vacuum high-frequency conditions;
- the heating device is a device capable of heating the sample, such as a resistance heating device, an infrared heating device, and a laser heating device.
- the first processing chamber, the first film preparation chamber, the second film preparation chamber, and the chemical vapor deposition chamber At least one chamber in the chamber is provided with a heat shield system; preferably, only a heat shield system is provided in the chamber where high temperature (e.g., above 400 °C) is present.
- the chamber walls of at least one of the first processing chamber, the first thin film preparation chamber, the second thin film preparation chamber and the chemical vapor deposition chamber are cooled.
- System preferably, only the wall of the chamber in which a high temperature (e.g., above 40 CTC) is present is provided with a cooling system.
- the chamber of at least one of the first processing chamber, the first thin film preparation chamber, the second thin film preparation chamber and the chemical vapor deposition chamber is provided with a cavity of the heat shielding system.
- the chamber wall is also equipped with a cooling system.
- the complete set of equipment is further provided with a control system for controlling the equipment or the process, and the control system includes any one of a sample transfer control system, a gas path control system, a vacuum control system, a valve control system or a temperature control system.
- the control system includes any one of a sample transfer control system, a gas path control system, a vacuum control system, a valve control system or a temperature control system.
- a sample transfer control system for controlling the equipment or the process
- the control system includes any one of a sample transfer control system, a gas path control system, a vacuum control system, a valve control system or a temperature control system.
- the device of the invention can continuously prepare a two-dimensional nano film by scale, and the two-dimensional nano film comprises graphene, metal chalcogenide, silicon thinner, germanium or boron nitride film.
- the first processing chamber serves as a surface treatment chamber for the substrate and/or the catalytic layer
- the first thin film preparation chamber serves as a preparation chamber for the catalytic layer
- the second thin film preparation chamber serves as a substrate and/or catalyst
- a chemical vapor deposition chamber as a chamber for processing the precursor to form a two-dimensional nano-film.
- the functions of the chambers of the present invention vary depending on the preparation process conditions due to differences in the selected substrate, catalytic layer, and process, etc., in different preparation processes. Conditions may assume multiple functions at the same time, or may not assume specific functions.
- Components disposed in or connected to the chambers such as valves, gas ports, sample processors, heaters, physical vapor deposition systems, chemical vapor deposition systems, thermal barrier systems, cooling systems, etc. may be prepared according to The specific process of the nano-film is set at different positions of each chamber, and the relevant components can be selectively selected according to a specific process.
- a precursor of a two-dimensional nanomaterial refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, for preparing a graphene, the precursor includes an amorphous carbon, an amorphous carbon film, and a carbon target. Materials, carbon-containing polymers, etc.; for the synthesis of MoS 2 as an example, the precursor includes a MoS 2 target, a Mo target, a sulfur powder, and the like.
- the basic processes for large-scale continuous preparation of two-dimensional nano-films include, but are not limited to:
- the substrate and/or catalytic layer required for synthesizing the two-dimensional nanofilm is placed on the loading rack and transferred from the feeding chamber to the first processing chamber by the sample conveying device; under certain atmosphere, the lining
- the bottom and/or catalytic layer is processed in the first processing chamber, and then the substrate and/or catalytic layer is transported by the sample transfer device to the first thin film preparation chamber through the first balancing chamber; in the first thin film preparation chamber
- the catalytic layer required for the growth of the two-dimensional nano-film is prepared by a physical vapor deposition method or a chemical vapor deposition method; and then sent to the second thin film preparation chamber through the second balance chamber through the sample transfer device under a certain atmosphere Preparing a two-dimensional nanofilm on the substrate and/or the catalytic layer.
- the basic process for preparing a two-dimensional nano film may also be: placing a substrate and/or a catalytic layer required for synthesizing a two-dimensional nano film on a carrier gantry and transferring it from the feed chamber to the first by a sample transfer device Processing the chamber; under a certain atmosphere, the substrate and/or the catalytic layer are processed in the processing chamber, and then the substrate and/or the catalytic layer are transported to the first film by the sample transfer device through the first balancing chamber.
- a chamber for preparing a catalytic layer required for growth of a two-dimensional nano-film by a physical vapor deposition method or a chemical vapor deposition method in a first film preparation chamber and then passing through a second balance chamber and being sent to a second by a sample transfer device a thin film preparation chamber for preparing a precursor for growth of a two-dimensional nano-film on a substrate and/or a catalytic layer under a certain atmosphere; after the precursor is prepared, the sample transfer device is transported to the chemical through the third equilibrium chamber
- a two-dimensional nano-film is prepared by a vapor deposition chamber; after the preparation of the two-dimensional nano-film, a two-dimensional nano-film preparation device is transported through the discharge chamber.
- control system which includes a sample transfer control system, a pneumatic control system, a vacuum control system, a valve control system or a temperature control system. Any one or a combination of two or more.
- the device of the invention is suitable for large-scale continuous preparation of all two-dimensional nano-films, including the graphene, the metal chalcogenide, the silene, the terpene or the boron nitride film, etc., according to the prepared Different from the nano-film, the solid, liquid or gas required for preparing the two-dimensional nano film can be appropriately selected.
- Preparation of two-dimensional film must meet certain conditions: For example, a higher temperature, such as 400 ° C, is required.
- a certain catalytic layer, such as a graphene film is required to use a transition metal such as Ni or Cu as a catalyst and a crystal structure of the catalytic layer.
- it is necessary to control the atmosphere and vacuum degree of the preparation chamber; equipment for continuously preparing a two-dimensional film must satisfy these conditions or achieve these functions, and is an integrated device.
- the existing process equipment cannot meet these basic conditions, and therefore cannot be used to continuously prepare a high-quality two-dimensional film; the combination of each chamber and device in the equipment of the present invention can satisfy the continuous preparation of a two-dimensional film.
- Different process technology requirements enable continuous production of high quality 2D films.
- the whole equipment is provided with a sample transfer device capable of withstanding high temperature, and has the characteristics of large-scale continuous preparation of two-dimensional nano-films, and each chamber is in the whole process of preparing the two-dimensional nano-film.
- the basic function of the feed chamber is to prepare the sample and enter the preparation device of the two-dimensional nano-film.
- the processing chamber is used to pre-treat the substrate or the catalytic layer.
- the thin film preparation chamber can be used to prepare the synthetic two-dimensional nano material.
- the required substrate, catalytic layer, precursor of two-dimensional nano-film or two-dimensional nano-film, chemical vapor deposition chamber can be used to prepare two-dimensional nano-film, balance chamber can be transition and stable during sample transfer , balance the function of the sample.
- the device of the invention can continuously prepare a two-dimensional nano film such as graphene, metal chalcogenide, silylene, decene or boron nitride film in a large area and large scale, and is suitable for industrial application, and is beneficial to realize two-dimensional nano film. Industrialization of technology.
- FIG. 1 is a schematic view showing the overall structure of a large-scale continuous preparation of a two-dimensional nano-film apparatus according to the present invention, wherein a first film preparation chamber is provided with a heating device;
- FIG. 2 is a schematic view showing the overall structure of a large-scale continuous preparation of a two-dimensional nano-film apparatus according to the present invention, wherein the first film preparation chamber and the discharge chamber are each provided with a heating device, and the discharge chamber is provided with a heat shielding system. And a cooling system, the discharge chamber is provided with a gas mixing box connection;
- FIG. 3 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor, and the first film preparation chamber is provided with a vapor deposition system, a heating device, and a heat The shielding system and the cooling system, the discharge chamber is provided with a heating device;
- FIG. 4 is a schematic view of the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor and heating The first thin film preparation chamber is provided with a vapor deposition system, a heating device, a heat shielding system and a cooling system, and the discharge chamber is provided with a heating device;
- FIG. 5 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor and a heating device, and the first film preparation chamber is provided with a vapor deposition system and heating.
- the device, the heat shield system and the cooling system, the discharge chamber is provided with a surface processor, a heating device and a cooling system.
- FIG. 6 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention.
- FIG. 7 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feed chamber is provided with a sample processing device, and the first film preparation chamber is provided with a sample processing device and a cooling system, and chemistry
- the vapor deposition chamber is provided with a chemical vapor deposition system, an insulation shielding system and a cooling system;
- FIG. 8 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a sample processing device and a heat shielding system, and the first film preparation chamber is provided with heat shielding.
- the system, the cooling system, the gas mixing box connection port and the sample processing device, the chemical vapor deposition chamber is provided with a chemical vapor deposition system, an insulation shielding system and a gas mixing box connection port.
- FIG. 9 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor and a heating device, and the first processing chamber is provided with a heating device and a gas mixture. a box interface, the first film preparation chamber is provided with a heating device and a heat shielding device, and the second processing chamber is provided with a heating device, a heat shielding device, a cooling device and a gas mixing box interface;
- FIG. 10 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor, and the first processing chamber is provided with a heating device, a heat shielding device and cooling Device, the first film preparation chamber is provided with a physical vapor deposition system, heating a device and a gas mixing box connection port, the second processing chamber is provided with a heating device, a heat shielding shielding device, a cooling device and a gas mixing box connection port, and the chamber is provided with a surface processor;
- FIG. 11 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor, and the first processing chamber is provided with a heating device, a heat shielding device and cooling
- the first film preparation chamber is provided with a physical vapor deposition system, a heating device, a heat shielding device, a cooling device and a gas mixing box connection port
- the second processing chamber is provided with a heating device, a heat shielding device, and a cooling device.
- a gas mixing box connection ;
- FIG. 12 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor, the first processing chamber is provided with a heating device, and the first film preparation chamber is provided.
- a physical vapor deposition system, a heating device and a gas mixing box connection port are provided, and the second processing chamber is provided with a heating device, a heat shielding device, a cooling device and a gas mixing box connection port, and the discharge chamber is provided with a surface treatment
- Figure 13 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment of the present invention, wherein the feeding chamber is provided with a surface processor, the first processing chamber is provided with a heating device, and the first film is prepared.
- the chamber is provided with a physical vapor deposition system, a heating device, a heat shielding device, a cooling device and a gas mixing box connection port, and the second processing chamber is provided with a heating device and a gas mixing box connection port.
- FIG. 14 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the first processing chamber is provided with a heating device, a heat shielding system and a cooling system, and the first film preparation chamber is provided a heating device and a physical vapor deposition system, the second film preparation chamber is provided with a heating device and a physical vapor deposition system, the chemical vapor deposition chamber is provided with a sample processing device, a heating device, a heat shielding system, a cooling system and a gas mixing box Interface
- FIG. 15 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the first processing chamber is provided with a heating device and a sample processing device, and the first film preparation chamber is provided with a physical vapor deposition system.
- the heating device, the heat shielding system and the gas mixing box connection port, the second film preparation chamber is provided with a heating device and a physical vapor deposition system, and the chemical vapor deposition chamber is provided with a chemical vapor deposition system, a heating device, and an insulation shielding system. , cooling system and air box interface;
- FIG. 16 is a schematic view showing the overall structure of a large-scale continuous preparation of a two-dimensional nano-film apparatus according to the present invention, wherein a first processing chamber is provided with a sample processing device, and a first thin film preparation chamber is provided with a physical vapor deposition system and a heating device.
- the second film preparation chamber is provided with a heating device, a heat shielding system, a cooling system and a physical vapor deposition system
- the chemical vapor deposition chamber is provided with a sample processing device, a heating device, a heat shielding system, a cooling system and a gas mixing box.
- the discharge chamber is provided with a sample processing device;
- the figure shows:
- Feed chamber 1 first processing chamber 2, first balance chamber 3, first film preparation chamber 4, second balance chamber 5, second film preparation chamber 6, third balance chamber 7, a chemical vapor deposition chamber 8, a second processing chamber 201, a discharge chamber 9;
- Vapor deposition system 101, 102 Vapor deposition system 101, 102.
- a scaled continuous preparation of a two-dimensional nanofilm apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a roller 30 for conveying a sample; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, between the feed chamber 1 and the first film preparation chamber 4 A valve 11 is disposed, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 that communicates with the atmosphere; the feed chamber is passed through the roller and the valve.
- the first film preparation chamber 4 and the discharge chamber 9 are connected in one piece.
- a second heating device 40 is disposed in the first film preparation chamber 4.
- the feed chamber 1 is provided with a vacuuming device 20, the first film preparation chamber 4 is provided with a vacuuming device 21, and the discharge chamber 9 is provided with a vacuuming device 22.
- the feed chamber 1 is provided with a gas connection port 60
- the first film preparation chamber 4 is provided with two gas connection ports 61, 62
- the discharge chamber 9 is provided with a gas connection port 63.
- each gas connection port is connected with a mass flow meter to control the flow rate of each gas
- each of the mass flow meters is provided with an electromagnetic cut-off valve at both ends thereof, and the electromagnetic cut-off valve and the mass flow meter pass through the pipeline. Connected to the gas connection.
- the first film preparation chamber 4, the second heating means 40 and the gas connection ports 61, 62 constitute a chemical vapor deposition system which is generally referred to as a thermal chemical vapor deposition system.
- the basic process for continuously preparing a two-dimensional nano film is: placing a substrate material and/or a catalytic layer material required for synthesizing a two-dimensional nano film on a carrier gantry 29, and transferring the roller 30 through the feeding chamber 1 to the first
- a film preparation chamber 4 is prepared in the first film preparation chamber 4 by a chemical vapor deposition method, and the sample is prepared and sent to the discharge chamber 9 by the roller 30.
- a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a pulley 30 for conveying a sample; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, between the feed chamber 1 and the first film preparation chamber 4 a valve 11 is provided, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 which is open to the atmosphere; the feed chamber 1 is passed through the pulley and the valve, The first film preparation chamber 4 and the discharge chamber 9 are connected in one piece.
- a second heating device 40 is disposed in the first film preparation chamber 4, and a third heating device 41 is disposed in the discharge chamber 9.
- a heat shielding system 96 is provided in the chamber, and a cooling system 90 is provided in the chamber wall to prevent the chamber wall from being overheated.
- the feeding chamber 1 is provided with a vacuuming device 20, the first film preparing chamber 4 is provided with a vacuuming device 21, and the discharging chamber 9 is provided with a vacuuming device 22.
- the feed chamber 1 is provided with a gas connection port 60, the first film preparation chamber 4 is provided with a gas connection port 61, and the discharge chamber 9 is provided with a gas connection port 68 connected to an air mixing box 85, the air mixing box
- the inlet of 85 is connected in parallel with two gas connection ports 66, 67; each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each end of each mass flow meter is provided with an electromagnetic shut-off valve, an electromagnetic cut-off valve and The mass flow meter is connected to the gas mixing box or the gas connection port through the pipeline, so that the flow rate of the gas can be precisely controlled.
- the discharge chamber 9, the third heating means 41 and the gas connection port 63, and the gas mixture tank 85 constitute a chemical vapor deposition system which is generally referred to as a thermal chemical vapor deposition system.
- the basic process for continuously preparing a two-dimensional nano film is: placing a substrate material and/or a catalytic layer material required for synthesizing a two-dimensional nano film on a carrier gantry 29, and transferring it from the pulley 30 through the feeding chamber 1 a film preparation chamber 4, the substrate/catalyst layer is heat-treated in the first film preparation chamber 4, and then transported by the pulley 30 to the discharge chamber 9, and a two-dimensional nano film is prepared by chemical vapor deposition, and a two-dimensional nano film is prepared. After preparation, it is conveyed by the pulley sample conveying device to the outside of the discharge chamber 9.
- a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a roller 30 for conveying a sample; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, between the feed chamber 1 and the first film preparation chamber 4 a valve 11 is provided, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 that communicates with the atmosphere; the feed chamber 1 is fed through the roller and the valve, The first film preparation chamber 4 and the discharge chamber 9 are connected in one piece.
- a first surface processor 50 is disposed in the feed chamber 1, a second heating device 40 is disposed in the first film preparation chamber 4, and a third heating device 41 is disposed in the discharge chamber 9.
- the first film preparation chamber 4 is provided with two vapor deposition systems: a first vapor deposition system 101 and a second vapor deposition system 102, which may be any combination of a physical gas phase system and a chemical vapor deposition system.
- the first vapor deposition system or the second vapor deposition system is a physical vapor deposition system, including any one of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system. Or a combination of two or more; the first vapor deposition system or the second vapor deposition system may also be a chemical vapor deposition system, including any one or two of a plasma enhanced chemical vapor deposition system and a microwave plasma chemical vapor deposition system. The combination above.
- the first film preparation chamber 4 Since the temperature of the first film preparation chamber 4 may be as high as several hundred degrees or even thousands of degrees, in order to concentrate the heat in a desired place and reduce the transfer to a place where heat is not required, the first film preparation chamber is provided with heat.
- the system 96 is shielded while the chamber wall is provided with a cooling system 90, which may be a dual layer water cooling system.
- the feed chamber 1 is provided with a vacuuming device 20, the first film preparation chamber 4 is provided with a vacuuming device 21, and the discharge chamber 9 is provided with a vacuuming device 22.
- the feed chamber 1 is provided with a gas connection port 60, and the discharge chamber 9 is provided with a gas connection port 63; the first film preparation chamber 4 is provided with two gas connection ports, one of which has a connection port of 61, the other
- the connection port 68 is connected to the air mixing box 85, and the inlet of the air mixing box 85 is connected in parallel with three gas connections.
- each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each end of each mass flow meter is provided with an electromagnetic cut-off valve, an electromagnetic cut-off valve And the mass flow meter is connected to the gas mixing box or the gas connection port through a pipeline.
- the basic process for continuously preparing a two-dimensional nano film is: placing the substrate material required for synthesizing the two-dimensional nano film on the loading stage 29 and transferring it to the feeding chamber 1 by the roller 30, under a certain atmosphere, lining
- the bottom material is pretreated in the feed chamber 1, and then the substrate material is transferred by the roller 30 to the first film preparation chamber 4; the physical vapor phase is utilized in the first vapor deposition system 101 in the first film preparation chamber 4.
- the deposition method is prepared by electron gun deposition to prepare a catalytic layer, and then a second physical vapor deposition method such as ion implantation is used in the second vapor deposition system 102 to inject a precursor of the two-dimensional nano material into the catalytic layer, and then transferred to the discharge chamber.
- Chamber 9 In the discharge chamber 9, a sample implanted with a precursor of a two-dimensional nanomaterial is processed to form a two-dimensional nanofilm.
- a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a roller 30 for conveying a sample; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, between the feed chamber 1 and the first film preparation chamber 4 a valve 11 is provided, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 that communicates with the atmosphere; the feed chamber 1 is fed through the roller and the valve, The first film preparation chamber 4 and the discharge chamber 9 are connected in one piece.
- a first surface processor 50 and a first heating device 42 are disposed in the feed chamber 1, a second heating device 40 is disposed in the first film preparation chamber 4, and a third heating device 41 is disposed in the discharge chamber 9.
- the first film preparation chamber 4 is provided with a first vapor deposition system 101, which is a physical vapor deposition system or/and a chemical vapor deposition system, and the physical vapor deposition system includes a sputtering target film deposition. Any one or a combination of two or more of a system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system; the chemical vapor deposition system including a plasma enhanced chemical vapor deposition system and microwave plasma A chemical vapor deposition system or the like; a physical vapor deposition system and a chemical vapor deposition system can be arbitrarily combined.
- a first vapor deposition system 101 is a physical vapor deposition system or/and a chemical vapor deposition system
- the physical vapor deposition system includes a sputtering target film deposition. Any one or a combination of two or more of a system, an electron gun deposition system, an ion gun deposition system, an
- the first film preparation chamber 4 Since the temperature of the first film preparation chamber 4 may be as high as several hundred degrees or even thousands of degrees, in order to concentrate the heat in a desired place and reduce the transfer to a place where heat is not required, the first film preparation chamber is provided with heat.
- the system 96 is shielded while the chamber wall is provided with a cooling system 90, which may be a dual layer water cooling system.
- the feeding chamber 1 is provided with a vacuuming device 20, the first film preparing chamber 4 is provided with a vacuuming device 21, and the discharging chamber 9 is provided with a vacuuming device 22.
- the feed chamber 1 is provided with a gas connection port 60, the discharge chamber 9 is provided with a gas connection port 63, and the first film preparation chamber 4 is provided with two gas connection ports 61, 62, each of which is connected to the gas connection port.
- There is a mass flow meter to control the flow rate of each gas and each end of each mass flow meter is provided with an electromagnetic cut-off valve, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through the pipeline.
- the discharge chamber 9, the discharge chamber heating device 41, and the gas connection port 63 constitute a chemical vapor deposition system.
- the basic process for continuously preparing a two-dimensional nano film is: placing the substrate material required for synthesizing the two-dimensional nano film on the loading stage 29 and transporting it by the roller 30 to the feeding chamber 1, under a certain atmosphere and temperature Next, the substrate material is pretreated in the feed chamber 1, and then the substrate material is transferred by the roller 30 to the first film preparation chamber 4; in the first film preparation chamber 4, a physical vapor deposition method or/and The catalytic layer is prepared by a chemical vapor deposition method and then transferred to a discharge chamber 9, where a two-dimensional nanofilm is prepared by chemical vapor deposition.
- a scaled continuous preparation of a two-dimensional nanofilm apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a sample conveyor belt 30; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, and between the feed chamber 1 and the first film preparation chamber 4 is provided. a valve 11, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 that communicates with the atmosphere; the feed chamber 1 is fed through the conveyor belt and the valve, first The film preparation chamber 4 and the discharge chamber 9 are connected in one piece.
- a first surface processor 50 and a first heating device 42 are disposed in the feed chamber 1, a second heating device 40 is disposed in the first film preparation chamber 4, and a second surface processor 51 is disposed in the discharge chamber 9. And a third heating device 41.
- the first thin film preparation chamber 4 is provided with a first vapor deposition system 101, which is a physical vapor deposition system or/and a chemical vapor deposition system, and the physical vapor deposition system includes a sputtering target thin film deposition. Any one or a combination of two or more of a system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system; the chemical vapor deposition system including a plasma enhanced chemical vapor deposition system and microwave plasma A chemical vapor deposition system or the like; a physical vapor deposition system and a chemical vapor deposition system can be arbitrarily combined.
- a first vapor deposition system 101 is a physical vapor deposition system or/and a chemical vapor deposition system
- the physical vapor deposition system includes a sputtering target thin film deposition. Any one or a combination of two or more of a system, an electron gun deposition system, an ion gun deposition
- a heat shield system 96 is provided in the first film preparation chamber 4 to reduce heat transfer to an undesired place, and the chamber wall is provided with a cooling system 90 to prevent overheating of the chamber wall.
- the discharge chamber 9 is provided with a cooling system 90 due to the presence of high temperatures.
- the feed chamber 1 is provided with a vacuuming device 20, the first film preparation chamber 4 is provided with a vacuuming device 21, and the discharge chamber 9 is provided with a vacuuming device 22.
- the feed chamber 1 is provided with a gas connection port 60, and the discharge chamber 9 is provided with a gas connection port 63;
- the first film preparation chamber 4 is provided with two a gas connection port, one of the connection ports is 61, the other connection port 68 is connected to the air mixing box 85, and the inlet of the air mixture box 85 is connected in parallel with three gas connection ports 62, 64 and 65; in order to precisely control the flow of the gas, each The gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each end of each mass flow meter is provided with an electromagnetic shut-off valve, and the electromagnetic cut-off valve and the mass flow meter pass through the pipeline and the gas mixing box or the gas connection port. connection.
- the feed chamber 1, the heating device 42 and the gas connection port 60 constitute a chemical vapor deposition system; the discharge chamber 9, the heating device 41 and the gas connection port 63 constitute a chemical vapor deposition system.
- the basic process for continuously preparing a two-dimensional nano film is to place the substrate material required for synthesizing the two-dimensional nano film on the carrier gantry 29 and transport it to the feed chamber 1 by the conveyor belt 30, under a certain atmosphere and temperature.
- the substrate material is pretreated in the feed chamber 1, and then the substrate material is transferred by the conveyor belt 30 to the first film preparation chamber 4; the physical vapor deposition method or/and the chemistry is utilized in the first film preparation chamber 4.
- the catalytic layer is prepared by a vapor deposition method, and then a two-dimensional nano film is prepared by a chemical vapor deposition method; the prepared two-dimensional nano film is transported by a sample transfer device to a discharge chamber 9, which can be surface-treated in the discharge chamber 9. .
- a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feeding chamber 1, a first film preparing chamber 4, a first balancing chamber 3, a chemical vapor deposition chamber 8, and a whole set of equipment.
- a sample transfer device 30 is disposed between each of the chambers of the feed chamber 1, the first thin film preparation chamber 4, the first balance chamber 3, and the chemical vapor deposition chamber 8 and the chamber;
- the device comprises any one or a combination of two or more of a roller, a pulley and a conveyor belt;
- the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, and between the feed chamber 1 and the first film preparation chamber 4 is provided a valve 12 is disposed between the first film preparation chamber 4 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the chemical vapor deposition chamber 8.
- the chemical vapor deposition chamber 8 is provided.
- a valve 14 is provided which is open to the atmosphere; the feed chamber 1, the first film preparation chamber 4, the first balance chamber 3 and the
- the feeding chamber 1 is provided with a vacuuming device 21, the first film preparing chamber 4 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the chemical vapor deposition chamber 8 is provided with a vacuuming device 24;
- Each vacuuming device includes various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be maintained at a normal pressure to 1.0 x 10 - 1 Q Pa by a vacuuming device.
- a sample processor device 51 is disposed in the first film preparation chamber 4, and the sample processing device may be a plasma surface processor, a wire ionizing device for gas ionization or a heating device, etc., capable of realizing modification of the sample.
- the sample processor device 51 is a heating device, and the heating device uses a resistance heater, an infrared heater, and a laser heater to implement a device for heating the sample; the first film preparation chamber 4 is further provided with a physical vapor deposition system. 33.
- the physical vapor deposition system comprises any one or a combination of two or more of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system.
- the chemical vapor deposition chamber 8 is provided with a heating device 40 which is a device which can heat the sample by using an electric resistance heater, an infrared heater and a laser heater.
- the feed chamber 1 is provided with a gas connection port 60
- the first film preparation chamber 4 is provided with gas connection ports 61 and 62
- the first balance chamber 3 is provided with a gas connection port 63
- the chemical vapor deposition chamber 8 is provided with a gas.
- the connecting ports 64 and 75, the gas connecting port 75 are connected to the air mixing box 85, and the air mixing box 85 is connected to the two gas connecting ports 66 and 67; each gas path is independently provided with a metering and flow regulating device such as a mass flow meter and an electromagnetic cut-off valve. Therefore, the flow rate of the gas is precisely controlled.
- each gas connection port is connected with a mass flow meter to control the flow rate of each gas.
- Each of the mass flow meters is provided with an electromagnetic shut-off valve at both ends, and the electromagnetic cut-off valve and the mass flow meter pass The line is connected to the gas connection.
- the chemical vapor deposition chamber 8, the heating device 40 and the gas connection ports 64 and/or 75 constitute a chemical vapor deposition system.
- the first film preparation chamber 4, the sample processing device 51 and the gas connection ports 61 and/or 62 may also constitute a chemical vapor deposition system.
- the basic process for continuously preparing a two-dimensional nanofilm is: placing the substrate required for synthesizing the two-dimensional nanofilm and/or placing it on the carrier gantry 29, transferring it from the sample transfer device 30 to the feed chamber 1, and then transferring it to a first film preparation chamber 4; at a certain temperature, a catalytic layer is prepared on the substrate and/or the catalytic layer in the first film preparation chamber 4 by a physical vapor deposition system such as an electron beam deposition system 33, and then passes through the first
- the chamber 3 is transferred to the chemical vapor deposition chamber 8; a two-dimensional nano-film is prepared by a chemical vapor deposition system in the chemical vapor deposition chamber 8, and the two-dimensional film is prepared, and then passed through the valve 14 to the atmosphere to complete the two-dimensional film.
- a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feeding chamber 1, a first film preparation chamber 4, a first balance chamber 3, a chemical vapor deposition chamber 8, and a whole set of equipment.
- a sample transfer device 30 is disposed between each of the chambers of the feed chamber 1, the first thin film preparation chamber 4, the first balance chamber 3, and the chemical vapor deposition chamber 8 and the chamber;
- the device comprises any one or a combination of two or more of a roller, a pulley and a conveyor belt;
- the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, and between the feed chamber 1 and the first film preparation chamber 4 is provided a valve 12 is disposed between the first film preparation chamber 4 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the chemical vapor deposition chamber 8.
- the chemical vapor deposition chamber 8 is provided.
- a valve 14 is provided which is open to the atmosphere; the feed chamber 1, the first film preparation chamber 4, the first balance chamber 3 and the chemical vapor
- the feeding chamber 1 is provided with a vacuuming device 21, the first film preparing chamber 4 is provided with a vacuuming device 22, and the first balancing chamber 3 is provided with a vacuuming device 23, the chemical vapor deposition chamber 8 is provided with a vacuuming device 24; each vacuuming device comprises various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be kept constant by the vacuuming device Press between 1.0x 10 - 1Q Pa.
- the feeding chamber 1 is provided with a sample processing device 50, which may be a plasma surface processor, a surface processor composed of a gas ionization coil, and a heating device capable of modifying the sample, and the heating device adopts a resistor.
- a device that can heat a sample such as a heater, an infrared heater, and a laser heater.
- a sample processor device 51 is disposed in the first film preparation chamber 4.
- the sample processing device may be a plasma surface processor, a device for modifying a sample such as a gas ionization coil or a heating device, where the sample is
- the processor device 51 is a heating device, and the heating device uses a device capable of heating the sample, such as a resistance heater, an infrared heater, and a laser heater;
- the first film preparation chamber 4 is further provided with physical vapor deposition systems 33 and 34,
- the physical vapor deposition system includes any one or a combination of two or more of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system;
- a cooling system 90 is also provided in the film preparation chamber 4.
- the chemical vapor deposition chamber 8 is provided with a heating device 40, which is a device capable of heating a sample, such as a resistance heater, an infrared heater and a laser heater; the chemical vapor deposition chamber 8 is further provided with a chemical vapor deposition system 38,
- the chemical vapor deposition system includes any one or a combination of two or more of a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, and an aerosol assisted chemical vapor deposition system; the chemical vapor deposition chamber 8 further An insulation shielding system 96 and a cooling system 91 are provided, and the cooling system may be a double water cooling system or the like.
- the feed chamber 1 is provided with a gas connection port 60
- the first film preparation chamber 4 is provided with gas connection ports 61 and 62
- the first balance chamber 3 is provided with a gas connection port 63
- the chemical vapor deposition chamber 8 is provided with a gas.
- the connecting ports 64 and 75, the gas connecting port 75 are connected to the air mixing box 85, and the air mixing box 85 is connected to the two gas connecting ports 66 and 67; each gas path is independently provided with a metering and flow regulating device such as a mass flow meter and an electromagnetic cut-off valve. Therefore, the flow rate of the gas is precisely controlled.
- each gas connection port is connected with a mass flow meter to control the flow rate of each gas.
- Each of the mass flow meters is provided with an electromagnetic shut-off valve at both ends, and the electromagnetic cut-off valve and the mass flow meter pass The line is connected to the gas connection.
- the chemical vapor deposition chamber 8 may also constitute a simple chemical vapor deposition system.
- the first film preparation chamber 4, the sample processing device 51 and the gas connection ports 61 and/or 62 may also constitute a chemical vapor deposition system.
- the basic process for continuously preparing a two-dimensional nano film is: placing a substrate and/or a catalytic layer required for synthesizing a two-dimensional nano film on a carrier gantry 29, and transferring it from the sample transfer device 30 to the feed chamber 1;
- the feed chamber 1 processes the surface of the sample by the sample processing device 50, and after surface treatment, transfers to the first film preparation chamber 4; at a certain temperature, the first film preparation chamber 4 utilizes a physical vapor deposition system such as
- the thermal evaporation deposition system 33 prepares a catalytic layer on the substrate and/or the catalytic layer, and then injects a precursor required for preparing the two-dimensional nano film into the catalytic layer by a physical vapor deposition system such as an ion implantation deposition system 34, and then passes through
- the first balance chamber 3 is transferred to the chemical
- the precursor of the two-dimensional nano material is a compound containing an element constituting the two-dimensional nano material, and the synthesis of graphene includes, for example, an amorphous carbon, an amorphous carbon film, a carbon-containing polymer, etc.; to synthesize MoS 2
- the precursor includes MoS 2 powder, Mo powder, and the like.
- the basic process of continuously preparing the two-dimensional nano film may also be: placing the substrate and/or the catalytic layer required for synthesizing the two-dimensional nano film on the loading stage 29, and transferring it from the sample conveying device 30 to the feeding chamber 1
- the surface of the sample is processed in the feed chamber 1 by the sample processing device 50, and then surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, physical vapor deposition is performed in the first film preparation chamber 4.
- a system such as laser deposition system 33 prepares a catalytic layer on the substrate and/or catalytic layer, which is then passed through first diffusion chamber 3 to chemical vapor deposition chamber 8; in chemical vapor deposition chamber 8, a chemical vapor deposition system is employed.
- a two-dimensional nanofilm is prepared by a microwave plasma chemical vapor deposition technique. After the two-dimensional film is prepared, it is passed through the valve 14 to the atmosphere to complete a process for continuous preparation of the two-dimensional film.
- the basic process for continuously preparing a two-dimensional nano film may also be: placing a substrate required for synthesizing a two-dimensional nano film on a carrier gantry 29, transferring it from the sample transfer device 30 to the feed chamber 1; in the feed chamber
- the chamber 1 processes the surface of the sample by the sample processing device 50, and is surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, the first film preparation chamber 4 is deposited by a physical vapor deposition system such as sputtering.
- Systems 33 and 34 prepare a catalytic layer on the substrate and/or catalytic layer, which is then passed through a first balancing chamber 3 to a chemical vapor deposition chamber 8; in a chemical vapor deposition chamber 8, a chemical vapor deposition system such as an aerosol is employed.
- a two-dimensional nanofilm is prepared by an auxiliary chemical vapor deposition technique. After the two-dimensional film is prepared, it is passed through the valve 14 to the atmosphere to complete a process of continuous preparation of the two-dimensional film.
- a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feeding chamber 1, a first film preparing chamber 4, a first balancing chamber 3, a chemical vapor deposition chamber 8, and a whole set of equipment.
- a sample transfer device 30 is disposed between each of the chambers of the feed chamber 1, the first thin film preparation chamber 4, the first balance chamber 3, and the chemical vapor deposition chamber 8 and the chamber;
- the device comprises any one or a combination of two or more of a roller, a pulley and a conveyor belt;
- the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, and between the feed chamber 1 and the first film preparation chamber 4 is provided a valve 11, a first valve preparation chamber 4 and a first balance chamber 3 are provided with a valve 12, a first balance chamber 3 and a chemical vapor deposition chamber
- the chemical vapor deposition chamber 8 is provided with a valve 14 which is open to the atmosphere;
- the feed chamber 1, the first film preparation chamber 4, and the first balance chamber 3 are
- the feeding chamber 1 is provided with a vacuuming device 21, the first film preparing chamber 4 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the chemical vapor deposition chamber 8 is provided with a vacuuming device 24;
- Each vacuuming device includes various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be maintained at a normal pressure to 1.0 x 10 - 1 Q Pa by a vacuuming device.
- the feeding chamber 1 is provided with a sample processing device 50 and a heat insulating shielding system 98, and the sample processing device may be a plasma surface processor, a gas ionization wire surface processor and a heating device, etc., which can modify the sample.
- the heating device uses a resistance heater, an infrared heater, and a laser heater to heat the sample.
- a sample processor device 51 is disposed in the first film preparation chamber 4, and the sample processing device may be a plasma surface processor, a device for gas ionization, or a heating device, such as a device capable of modifying a sample.
- the sample processor device 51 is a heating device using a resistance heater, an infrared heater, a laser heater or the like to enable heating of the sample; the first film preparation chamber 4 is provided with physical vapor deposition systems 33 and 34.
- the physical vapor deposition system includes any one or a combination of two or more of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system;
- a film preparation chamber 4 is provided with a cooling system 90 and an insulation shielding system 97.
- the chemical vapor deposition chamber 8 is provided with a heating device 40, which is a device capable of heating a sample by using an electric resistance heater, an infrared heater and a laser heater; and a chemical vapor deposition system 38 is disposed in the chemical vapor deposition chamber 8.
- the chemical vapor deposition system comprises any one or a combination of two or more of an ion-enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, and an aerosol-assisted chemical vapor deposition system; a chemical vapor deposition chamber There is an insulation shielding system 96 in the 8th.
- the feeding chamber 1 is provided with a gas connection port 60
- the first film preparation chamber 4 is provided with gas connection ports 61 and 76
- 76 is connected to the air mixing box 86
- the air mixing box 86 is connected to the two gas connection ports 69 and 70
- a balance chamber 3 is provided with a gas connection port 63
- a chemical vapor deposition chamber 8 is provided with gas connection ports 64 and 75
- a gas connection port 75 is connected to the gas mixture box 85
- a gas mixing box 85 is connected to the three gas connection ports 66, 67.
- each gas path is independently equipped with a metering and flow regulating device such as a mass flow meter and an electromagnetic shut-off valve, so as to accurately control the flow rate of the gas, for example, each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each Each of the mass flowmeters is provided with an electromagnetic shut-off valve at both ends, and the electromagnetic shut-off valve and the mass flowmeter are connected to the gas connection port through the pipeline.
- a metering and flow regulating device such as a mass flow meter and an electromagnetic shut-off valve
- the chemical vapor deposition chamber 8, the heating device 40 and the gas connection ports 64 and/or 75 may also constitute a chemical vapor deposition system.
- the first film preparation chamber 4, the sample processing device 51 and the gas connection ports 61 and/or 76 may also constitute a chemical vapor deposition system.
- the basic process for continuously preparing a two-dimensional nanofilm is: placing a substrate required for synthesizing a two-dimensional nanofilm on a carrier gantry 29, transferring it from the sample transfer device 30 to the feed chamber 1; in the feed chamber 1
- the surface of the sample is processed by the sample processing device 50, and then surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, a physical deposition system such as a thermal evaporation deposition system is utilized in the first film preparation chamber 4.
- the deposition chamber 8 uses a chemical vapor deposition system 38 and 39 to prepare a two-dimensional nanofilm. After the two-dimensional film is prepared, it is passed through the valve 14 to the atmosphere to complete a process for continuous preparation of the two-dimensional film.
- the first catalytic layer and the second catalytic layer may also be deposited simultaneously to achieve blending.
- the basic process for continuously preparing the two-dimensional nano film may also be: placing the substrate required for synthesizing the two-dimensional nano film and/or placing it on the loading stage 29, and transferring it to the feeding chamber 1 by the sample conveying device 30;
- the feed chamber 1 processes the surface of the sample by the sample processing device 50, and is surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, a physical deposition system such as a laser is used in the first film preparation chamber 4.
- the deposition system 33 prepares a catalytic layer on the substrate and/or the catalytic layer, and then deposits a precursor required for synthesizing the two-dimensional nano-film on the catalytic layer by a physical deposition system such as an ion beam deposition system 34; after deposition, after the first
- a physical deposition system such as an ion beam deposition system 34
- the precursor of the two-dimensional nano-film is converted into a two-dimensional nano-film in the chemical vapor deposition chamber 8.
- the valve is passed through the valve. 14 is passed to the atmosphere to complete a process for the continuous preparation of a two-dimensional film.
- the precursor of the two-dimensional nanomaterial is a compound containing an element constituting the two-dimensional nano material, and the synthetic precursor includes a carbonaceous polymer such as methane, ethylene or ethanol.
- the basic process for continuously preparing a two-dimensional nano film may also be: placing a substrate required for synthesizing a two-dimensional nano film on a carrier gantry 29, transferring it from the sample transfer device 30 to the feed chamber 1; in the feed chamber The chamber 1 processes the surface of the sample by the sample processing device 50, and is surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, a physical deposition system such as a sputter deposition system is used in the first film preparation chamber 4.
- a two-dimensional nanofilm is prepared by chemical vapor deposition technology. After the two-dimensional film is prepared, it is passed through the valve 14 to the atmosphere to complete a process for continuous preparation of the two-dimensional film.
- a scaled continuous preparation of two-dimensional nano-film equipment of the present invention includes sequentially providing a feeding chamber 1 on a production line, the first place a chamber 2, a first balance chamber 3, a first membrane preparation chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with an atmosphere a valve 10 is disposed between the feed chamber 1 and the first processing chamber 2, and a valve 12 is disposed between the first processing chamber 2 and the first balancing chamber 3, and the first balancing chamber 3 is A valve 13 is disposed between the first film preparation chambers 4, and a valve 14 is disposed between the first film preparation chamber 4 and the second balance chamber 5, and between the second balance chamber 5 and the second processing chamber 201.
- a valve 15 is disposed, a valve 16 is disposed between the second processing chamber 201 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 17 that communicates with the atmosphere;
- the entire device is in the feeding chamber 1, the first treatment
- the chamber 2, the first balance chamber 3, the first film preparation chamber 4, the second balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are each provided with a roller conveyor 30 for conveying samples;
- the device will feed the chamber 1 through the roller conveyor and the valve, the first processing chamber 2, the first balancing chamber 3, the first film preparation chamber 4, the second balancing chamber 5,
- the processing chamber 201 and a discharge chamber 9 is connected into a whole.
- the feeding chamber 1 is provided with a vacuuming device 21, the first processing chamber 2 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the first film preparation chamber 4 is provided with a vacuuming device 24, the second balancing chamber 5 is provided with a vacuuming device 25, the second processing chamber 201 is provided with a vacuuming device 26, and the discharging chamber 9 is provided with a vacuuming device 27.
- the feeding chamber 1 is provided with a gas connection port 61
- the first processing chamber 2 is provided with two gas connection ports 62 and 80
- the gas connection port 80 is connected to the air mixing box 86
- the air mixing box 86 is connected to the two gas connection ports 76.
- the first balance chamber 3 is provided with a gas connection port 64
- the first film preparation chamber 4 is provided with a gas connection port 78
- the second balance chamber 5 is provided with a gas connection port 68
- the second process chamber 201 is provided.
- gas connection ports 69 and 79 There are two gas connection ports 69 and 79, a gas connection port 79 is connected to the air mixing box 85, a gas mixing box 85 is connected to the three gas connection ports 71, 72 and 73, and the discharge chamber 9 is provided with a gas connection port 74;
- the road can precisely control the flow of gas.
- the mass flow meter and the electromagnetic cut-off valve are included.
- Each gas connection port is connected with a mass flow meter to control the flow rate of the gas.
- Each mass flow meter has one end at each end.
- the electromagnetic shut-off valve, the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.
- the feeding chamber 1 is provided with a surface processor 50 and a heating device 40.
- the first processing chamber 2 is provided with a heating device 41, and the first film preparation chamber 4 is provided with a heating device 42 and a heat insulating shielding device 97, and the second processing
- the chamber 201 is provided with heating means 43 and 44, a cooling means 90 and a heat insulating shield 96.
- the first processing chamber 2, the heating device 41 and the gas connection ports 62 and/or 80 constitute a chemical vapor deposition system.
- the first film preparation chamber 4, the heating device 42 and the gas connection port 78 constitute a chemical vapor deposition system.
- the second processing chamber 201, the heating means 43 and/or 44, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system.
- the basic process for continuously preparing a two-dimensional nano film is: placing a substrate material/catalyst layer required for preparing a two-dimensional nano film on a carrier gantry 29, and transporting it by a roller conveyor 30 to a feed chamber 1; At a certain temperature, the substrate material/catalyst layer is surface-treated in the feed chamber 1 by the surface processor 50, and then transferred to the first film preparation chamber through the first processing chamber 2 and the first balance chamber 3.
- the substrate/catalyst layer is heat-treated in the first film preparation chamber 4, and then transferred to the second processing chamber 201 via the second balance chamber 5; in the second processing chamber 201 uses a microwave plasma chemical vapor deposition system to prepare a two-dimensional nano-film on the substrate/catalyst layer.
- the two-dimensional nano-film is prepared and transported out of the device through the discharge chamber 9 to complete the preparation of the two-dimensional nano-film.
- a scaled continuous preparation of a two-dimensional nano-film apparatus of the present invention includes sequentially providing a feed chamber 1, a first processing chamber 2, a first balance chamber 3, and a first film preparation chamber on a production line. a chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, the feed chamber 1 and the first processing chamber 2 A valve 11 is disposed between the first processing chamber 2 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the first film preparation chamber 4, and the first film is disposed.
- a valve 14 is disposed between the preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second processing chamber 201.
- the second processing chamber 201 and the discharge chamber 9 are provided. Between the valve 16 is provided, the discharge chamber 9 is provided with a valve 17 which is open to the atmosphere; the whole set of equipment is in the feed chamber 1, the first processing chamber 2, the first balance chamber 3, the first film preparation chamber 4.
- the second balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are each provided with a roller for conveying samples.
- the feeding device 30 the whole device passes through the roller conveying device and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparing chamber 4, the second balancing chamber 5, the second The processing chamber 201 and the discharge chamber 9 are connected in one piece.
- the feeding chamber 1 is provided with a vacuuming device 21, the first processing chamber 2 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the first film preparation chamber 4 is provided with a vacuuming device 24, the second balancing chamber 5 is provided with a vacuuming device 25, the second processing chamber 201 is provided with a vacuuming device 26, and the discharging chamber 9 is provided with a vacuuming device 27.
- the feed chamber 1 is provided with a gas connection port 61
- the first process chamber 2 is provided with two gas connection ports 62 and 63
- the first balance chamber 3 is provided with a gas connection port 64
- the first film preparation chamber 4 is provided.
- the gas connection port 80, the gas connection port 80 is connected to the air mixing box 86, the air mixing box 86 is connected to the two gas connection ports 66 and 67, the second balance chamber 5 is provided with a gas connection port 68, and the second processing chamber 201 is provided.
- the gas connection port is connected to the gas path, and each gas path can precisely control the flow rate of the gas.
- a mass flow meter and an electromagnetic cut-off valve are included, and each gas connection port is connected with a mass flow meter to control the flow rate of each gas.
- Each of the mass flowmeters is provided with an electromagnetic shut-off valve at both ends, and the electromagnetic shut-off valve and the mass flowmeter are connected to the gas connection port through the pipeline.
- the feeding chamber 1 is provided with a surface processor 50.
- the first processing chamber 2 is provided with a heating device 41, a cooling device 91 and a heat insulating shielding device 98.
- the first film preparing chamber 4 is provided with a heating device 42 and physical vapor deposition.
- Systems 33 and 34, second processing chamber 201 are provided with heating means 43 and 44, cooling means 90 and thermal barrier means 96, and discharge chamber 9 is provided with a surface processor 51.
- the first processing chamber 2, the heating device 41 and the gas connection ports 62 and/or 63 constitute a chemical vapor deposition system.
- the first film preparation chamber 4, the heating device 42 and the gas connection port 80 constitute a chemical vapor deposition system.
- the second processing chamber 201, the heating means 43 and/or 44, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system.
- the physical vapor deposition system includes any one or a combination of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system; a chemical vapor deposition system, Including plasma enhanced chemical vapor deposition systems, aerosol assisted chemical vapor deposition systems and microwave plasma chemical vapor deposition systems.
- the basic process for continuously preparing a two-dimensional nano film is: placing a substrate material required for synthesizing a two-dimensional nano film on a carrier gantry 29, which is transported by a roller conveyor 30 to a feed chamber 1; The surface of the feed chamber 1 is surface treated by the surface processor 50, then transferred to the first processing chamber 2 for heat treatment, and then transferred to the first film preparation chamber 4 via the first balance chamber 3; A catalytic layer film is prepared on the surface of the substrate by a physical vapor deposition system such as a sputtering target thin film deposition system 33 and 34 in an atmosphere environment and temperature; after the catalytic layer is prepared, it is transferred to the second processing chamber through the second balance chamber 5.
- a physical vapor deposition system such as a sputtering target thin film deposition system 33 and 34 in an atmosphere environment and temperature
- a large-scale continuous preparation of two-dimensional nano-film equipment of the present invention includes sequentially providing a feeding chamber 1, a first processing chamber 2, a first balancing chamber 3, and a first film preparation chamber on a production line. a chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, the feed chamber 1 and the first processing chamber 2 A valve 11 is disposed between the first processing chamber 2 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the first film preparation chamber 4, and the first film is disposed.
- a valve 14 is disposed between the preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second processing chamber 201.
- the second processing chamber 201 and the discharge chamber 9 are provided. Between the valve 16 is provided, the discharge chamber 9 is provided with a valve 17 which is open to the atmosphere; the whole set of equipment is in the feed chamber 1, the first processing chamber 2, the first balance chamber 3, the first film preparation chamber 4.
- the second balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are each provided with a roller for conveying samples.
- the feeding device 30 the whole device passes through the roller conveying device and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparing chamber 4, the second balancing chamber 5, the second The processing chamber 201 and the discharge chamber 9 are connected in one piece.
- the feeding chamber 1 is provided with a vacuuming device 21, the first processing chamber 2 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the first film preparation chamber 4 is provided with a vacuuming device 24, the second balancing chamber 5 is provided with a vacuuming device 25, the second processing chamber 201 is provided with a vacuuming device 26, and the discharging chamber 9 is provided with a vacuuming device 27.
- the feed chamber 1 is provided with a gas connection port 61
- the first process chamber 2 is provided with a gas connection port 62
- the first balance chamber 3 is provided with a gas connection port 64
- the first film preparation chamber 4 is provided with two gases.
- the connecting ports 80 and 78, the gas connecting port 80 are connected to the air mixing box 86
- the air mixing box 86 is connected to the two gas connecting ports 66 and 67
- the second balancing chamber 5 is provided with a gas connecting port 68
- the second processing chamber 201 is provided.
- each gas path can precisely control the flow of gas, including mass flow meters and electromagnetic shut-off valves, etc.
- Each gas connection port is connected with a mass flow meter to control the flow rate of each gas, two of each mass flow meter
- Each end is provided with an electromagnetic shut-off valve, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.
- the feeding chamber 1 is provided with a surface processor 50.
- the first processing chamber 2 is provided with a heating device 41, a cooling device 91 and a heat insulating shielding device 98.
- the first film preparing chamber 4 is provided with a heating device 42 and physical vapor deposition.
- the systems 33 and 34, the cooling device 92 and the thermal shield 96, the second processing chamber 201 are provided with a heating device 43, a cooling device 90 and a thermal barrier 96.
- the first processing chamber 2, the heating device 41 and the gas connection port 62 constitute a chemical vapor deposition system.
- the first film preparation chamber 4, the heating device 42 and the gas connection ports 80 and/or 78 constitute a chemical vapor deposition system.
- the second processing chamber 201, the heating means 43, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system.
- the physical vapor deposition system includes any one or a combination of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system; a chemical vapor deposition system, Including plasma enhanced chemical vapor deposition systems, aerosol assisted chemical vapor deposition systems and microwave plasma chemical vapor deposition systems.
- the basic process for continuously preparing a two-dimensional nano film is: placing a substrate material required for synthesizing a two-dimensional nano film on a carrier gantry 29, which is transported by a roller conveyor 30 to a feed chamber 1;
- the surface of the feed chamber 1 is surface treated by the surface processor 50, then transferred to the first processing chamber 2 for heat treatment, and then transferred to the first film preparation chamber 4 via the first balance chamber 3;
- the catalytic layer is prepared on the substrate by a physical vapor deposition system such as an electron gun deposition system 33 in an atmosphere environment and temperature, and then a precursor of the two-dimensional nanomaterial is injected into the catalytic layer by a physical vapor deposition system such as an ion implanter 34, after which Passing through the second balance chamber 5 to the second processing chamber 201;
- the processing chamber 201 processes a sample in which a precursor of a two-dimensional nanomaterial is injected into the catalytic layer. After the heat treatment, the sample is transferred to the discharge chamber 9 for cooling to complete the preparation
- a scaled continuous preparation of two-dimensional nano-film equipment of the present invention includes sequentially providing a feed chamber 1, a first processing chamber 2, a first balance chamber 3, and a first film preparation chamber on a production line. a chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, the feed chamber 1 and the first processing chamber 2 A valve 11 is disposed between the first processing chamber 2 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the first film preparation chamber 4, and the first film is disposed.
- a valve 14 is disposed between the preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second processing chamber 201.
- the second processing chamber 201 and the discharge chamber 9 are provided. Between the valve 16 is provided, the discharge chamber 9 is provided with a valve 17 which is open to the atmosphere; the whole set of equipment is in the feed chamber 1, the first processing chamber 2, the first balance chamber 3, the first film preparation chamber 4.
- the second balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are each provided with a transfer of the transport sample.
- Conveying device 30 the entire device passes through the conveyor belt and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparation chamber 4, the second balancing chamber 5, the second The processing chamber 201 and the discharge chamber 9 are connected in one piece.
- the feeding chamber 1 is provided with a vacuuming device 21, the first processing chamber 2 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the first film preparation chamber 4 is provided with a vacuuming device 24, the second balancing chamber 5 is provided with a vacuuming device 25, the second processing chamber 201 is provided with a vacuuming device 26, and the discharging chamber 9 is provided with a vacuuming device 27.
- the feed chamber 1 is provided with a gas connection port 61
- the first process chamber 2 is provided with two gas connection ports 62 and 63
- the first balance chamber 3 is provided with a gas connection port 64
- the first film preparation chamber 4 is provided.
- a gas connection port 80 a gas connection port 80 is connected to the air mixing box 86
- the air mixing box 86 is provided with two gas connection ports 66 and 67
- the second balance chamber 5 is provided with a gas connection port 68
- the second processing chamber is provided.
- a gas connection port 79 is connected to the gas mixing box 85
- the gas mixing box 85 is connected to three gas connection ports 71, 72 and 73
- the discharge chamber 9 is provided with a gas connection port 74;
- Each gas path can precisely control the flow rate of the gas.
- a mass flow meter and an electromagnetic shut-off valve are included.
- Each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each end of each mass flow meter is provided.
- There is an electromagnetic shut-off valve, and the electromagnetic shut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.
- the feeding chamber 1 is provided with a surface processor 50
- the first processing chamber 2 is provided with a heating device 41
- the first film preparation chamber 4 is provided with a physical vapor deposition system 33 and a heating device 42
- the second processing chamber 201 is provided
- heating means 43 and 44 there are heating means 43 and 44, a cooling means 90 and a heat insulating shield 96
- the discharge chamber 9 is provided with a surface processor 51.
- the first processing chamber 2, the heating device 41 and the gas connection ports 62 and/or 63 constitute a chemical vapor deposition system.
- the first film preparation chamber 4, the heating device 42 and the gas connection port 80 constitute a chemical vapor deposition system.
- the second processing chamber 201, the heating means 43 and/or 44, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system.
- the physical vapor deposition system includes any one or a combination of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implanter deposition system, and a thermal evaporation system; a chemical vapor deposition system Including plasma enhanced chemical vapor deposition systems, aerosol assisted chemical vapor deposition systems, and microwave plasma chemical vapor deposition systems.
- the basic process for continuously preparing a two-dimensional nano film is: placing the substrate material required for synthesizing the two-dimensional nano film on the carrier gantry 29, and transferring it to the feeding chamber 1 by the conveyor belt conveying device 30;
- the material chamber 1 is surface-treated by the surface processor 50, and then transferred to the first film preparation chamber 4 through the first processing chamber 2 and the first balance chamber 3; under a certain atmosphere, the substrate is
- the first film preparation chamber 4 is subjected to heat treatment, and then transferred to the second processing chamber 201 via the second balance chamber 5; a two-dimensional nano-film is prepared on the substrate by using a chemical vapor deposition system in the second processing chamber 201, After the two-dimensional nano film is prepared, it is conveyed to the discharge chamber 9; in the discharge chamber 9, the prepared two-dimensional nano film is subjected to surface modification treatment, and then processed and transferred to the device to complete the preparation of the two-dimensional nano film.
- a scaled continuous preparation of two-dimensional nano-film equipment comprises a feeding chamber 1, a first processing chamber 2, a first balancing chamber 3, and a first film preparation chamber. a chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, the feed chamber 1 and the first processing chamber 2 A valve 11 is disposed between the first processing chamber 2 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the first film preparation chamber 4, and the first film is disposed.
- a valve 14 is disposed between the preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second processing chamber 201.
- the second processing chamber 201 and the discharge chamber 9 are provided. Between the valve 16 is provided, the discharge chamber 9 is provided with a valve 17 which is open to the atmosphere; the whole set of equipment is in the feed chamber 1, the first balance chamber 3, the second balance chamber 5 and the discharge chamber 9 a pulley conveying device 30 for conveying a sample; a first processing chamber 2, a first film preparation chamber 4 and a second
- the processing chamber 201 is provided with a roller conveying device 30; the entire device passes through the sample conveying device and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparation chamber 4, the second The balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are connected in one piece.
- the feeding chamber 1 is provided with a vacuuming device 21, the first processing chamber 2 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the first film preparation chamber 4 is provided with a vacuuming device 24, the second balance chamber 5 is provided with a vacuuming device 25, and the second processing chamber 201 is provided with a vacuum At 26, the discharge chamber 9 is provided with a vacuuming device 27.
- the feed chamber 1 is provided with a gas connection port 61
- the first process chamber 2 is provided with gas connection ports 62 and 63
- the first balance chamber 3 is provided with a gas connection port 64
- the first film preparation chamber 4 is provided with two
- the gas connection ports 80 and 78, the gas connection port 80 are connected to the air mixing box 86
- the air mixing box 86 is connected to the two gas connection ports 66 and 67
- the second balance chamber 5 is provided with a gas connection port 68
- the second processing chamber 201 is provided with two gas connection ports 69 and 79
- a gas connection port 79 is connected to the air mixing box 85
- a gas mixing box 85 is connected to the two gas connection ports 71 and 72
- the discharge chamber 9 is provided with two gas connection ports 74 and 75;
- Each gas path can precisely control the flow of gas, including mass flow meters and electromagnetic shut-off valves, etc.
- Each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and both ends of each mass flow meter
- Each has an electromagnetic shut-off valve, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.
- the feeding chamber 1 is provided with a surface processor 50
- the first processing chamber 2 is provided with a heating device 41
- the first film preparation chamber 4 is provided with heating means 42 and physical vapor deposition systems 33 and 34, cooling means 92 and partition
- the heat shielding device 97, the second processing chamber 201 is provided with a heating device 44.
- the first processing chamber 2, the heating device 41, and the gas connection ports 62 and/or 63 constitute a chemical vapor deposition system.
- the first film preparation chamber 4, the heating means 42, and the gas connection ports 80 and/or 78 constitute a chemical vapor deposition system.
- the second processing chamber 201, the heating device 44, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system.
- the physical vapor deposition system includes any one or a combination of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system; a chemical vapor deposition system, Including plasma enhanced chemical vapor deposition systems, aerosol assisted chemical vapor deposition systems and microwave plasma chemical vapor deposition systems.
- the basic process for continuously preparing the two-dimensional nano film is: placing the substrate material required for synthesizing the two-dimensional nano film on the loading stage 29, and transferring it to the feeding chamber 1 by the transfer pulley conveying device 30;
- the surface treatment is performed in the feed chamber 1 by the surface processor 50, and then transferred to the first processing chamber 2 for heat treatment. After the heat treatment, it is transferred to the first balance chamber 3 by the roller conveyor 30, and then, A balance chamber 3 is transferred to the first film preparation chamber 4; a catalytic layer is prepared on the substrate by a physical vapor deposition system such as a thermal evaporation system 33 under a certain atmosphere and temperature, and then physical vapor deposition is employed.
- a system such as ion gun deposition system 34 ionizes the precursor of the two-dimensional nanomaterial onto the catalytic layer, and thereafter, is transported to the second processing chamber 201 via the second balancing chamber 5;
- a sample of a precursor of a two-dimensional nanomaterial deposited on the catalytic layer is processed, and after the heat treatment, the sample is transferred to the discharge chamber 9 for cooling to complete the preparation of the two-dimensional nanofilm.
- a large-scale continuous preparation two-dimensional nano film device of the present invention is sequentially provided with a feeding chamber 1, a first processing chamber 2, a first balancing chamber 3, a first film preparing chamber 4, and a first a second balance chamber 5, a second thin film preparation chamber 6, a third balance chamber 7, a chemical vapor deposition chamber 8 and a discharge chamber 9;
- the feed chamber 1 is provided with a valve 10 connected to the atmosphere, feeding A valve 11 is disposed between the chamber 1 and the first processing chamber 2, and a valve 12 is disposed between the first processing chamber 2 and the first balancing chamber 3, and the first balancing chamber 3 and the first thin film preparation chamber
- a valve 13 is disposed between the first film preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second film preparation chamber 6.
- a valve 16 is disposed between the second film preparation chamber 6 and the third balance chamber 7, and a valve 17 is disposed between the third balance chamber 7 and the chemical vapor deposition chamber 8, and the chemical vapor deposition chamber 8 and the discharge are provided.
- a valve 18 is arranged between the chambers 9, and the discharge chamber 9 is provided with a valve 19 which is open to the atmosphere; Material chamber 1, first processing chamber 2, first balance chamber 3, first thin film preparation chamber 4, second balance chamber 5, second thin film preparation chamber 6, third balance chamber 7, chemistry
- the sample delivery device 30 is disposed in the chambers of the vapor deposition chamber 8 and the discharge chamber 9; the sample delivery device 30 includes any one or a combination of two or more of a roller, a pulley, and a conveyor belt;
- the apparatus will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first thin film preparation chamber 4, the second balance chamber 5, and the second thin film preparation chamber 6 through the sample transfer device and the valve
- the third balance chamber 7, the chemical vapor deposition chamber 8 and the discharge chamber 9 are connected
- the first processing chamber 2 is provided with a heating device 40, and the heating device may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be adjusted between 20 and 2000 ° C; Cooling system 90.
- the heating device may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be adjusted between 20 and 2000 ° C; Cooling system 90.
- the first processing chamber 2, the heating device 40 and the gas connection port 61 or 62 may constitute a thermal chemical vapor deposition system.
- the first film preparation chamber 4 is provided with a physical vapor deposition system 33 and a heating device 41;
- the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion Any one or a combination of two or more of the injection systems;
- the heating device may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be adjusted between 20 and 2000 °C.
- the first film preparation chamber 4, the heating means 41 and the gas connection port 64 may constitute a thermal chemical vapor deposition system.
- the second thin film preparation chamber 6 is provided with a physical vapor deposition system 34 and a heating device 42;
- the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion Any one or a combination of two or more of the injection systems;
- the heating device may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be adjusted between 20 and 2000 °C.
- the second film preparation chamber 6, the heating device 42, and the gas connection port 66 may constitute a thermal chemical vapor deposition system.
- the chemical vapor deposition chamber 8 is provided with a sample processing device 51, a heating device 43, a cooling system 91 and a heat insulating shielding system 97;
- the sample processing device 51 may be a plasma sample processing device, a wire enthalpy or heating for gas ionization.
- a device capable of modifying a sample such as a device,
- the wire enthalpy for gas ionization can realize ionization of gas under high-frequency conditions of vacuum;
- the heating device can be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature can be adjusted between 20 and 2000 ° C. .
- the feed chamber 1 is provided with a gas connection port 60
- the first process chamber 2 is provided with two gas connection ports 61 and 62
- the first balance chamber 3 is provided with a gas connection port 63
- the first film preparation chamber 4 is provided.
- a second balance chamber 5 is provided with a gas connection port 65
- a second film preparation chamber 6 is provided with a gas connection port 66
- a third balance chamber 7 is provided with a gas connection port 67
- a chemical vapor deposition chamber The chamber is provided with gas connection ports 68 and 69
- the gas connection port 69 is connected to the air mixing box 87
- the air mixing box 87 is connected to the three gas connection ports 76, 77 and 78
- the discharge chamber is connected with two gas connection ports 70 and 71.
- Each gas path can precisely control the flow of gas, and can include metering and flow regulating devices such as mass flow meters and electromagnetic shut-off valves.
- Each gas connection port is connected with a mass flow meter to control the flow rate of each gas.
- Each mass flow meter Each end of the two ends is provided with an electromagnetic shut-off valve, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through the pipeline.
- the chemical vapor deposition chamber 8, the heating device 43 and the gas connection ports 68 and/or 69 may constitute a thermal chemical vapor deposition system.
- the chemical vapor deposition chamber 8 may also be provided with any one or two of a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, an aerosol assisted chemical vapor deposition system, and an inductively coupled plasma chemical vapor deposition system. The combination above.
- the feeding chamber 1 is provided with a vacuuming device 20, the first processing chamber 2 is provided with a vacuuming device 21, the first balancing chamber 3 is provided with a vacuuming device 22, and the first film preparation chamber 4 is provided with a vacuuming device 23, the second balance chamber 5 is provided with a vacuuming device 24, the second film preparation chamber 6 is provided with a vacuuming device 25, the third balancing chamber 7 is provided with a vacuuming device 26, and the chemical vapor deposition chamber 8 is provided The vacuuming device 27, the discharge chamber 9 is provided with a vacuuming device 28.
- Each individual evacuating device include various vacuum pumps, vacuum lines, vacuum valves, vacuum meter, etc., can make the degree of vacuum in the chambers between 1.0x l0- 1Q Pa to atmospheric pressure by the evacuating device.
- the basic process for the continuous preparation of a two-dimensional nanofilm on a large scale may be: placing a substrate/catalyst layer required for preparing a two-dimensional nanofilm on a carrier gantry 29, which is conveyed by the sample transfer device 30 through the feed chamber 1
- the first processing chamber 2; the substrate/catalytic layer is heat treated in the first processing chamber 2 by the heating device 40, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3;
- the preparation chamber 4 deposits a precursor of the two-dimensional nano-film on the substrate/catalyst layer by means of a physical vapor deposition system 33 such as a sputter deposition system, and then passes through the second balance chamber 5 by the sample transfer device 30,
- the two thin film deposition chambers 6 and the third balance chamber 7 are transferred to the chemical vapor deposition chamber 8; the precursor of the two-dimensional nano material is chemically vapor deposited in the chemical vapor deposition chamber 8 under a certain atmosphere. Conversion into a two-dimensional
- a precursor of a two-dimensional nanomaterial refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, preparing a graphene including an amorphous carbon, an amorphous carbon film, and a carbon-containing material.
- the basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate/catalyst layer required for preparing a two-dimensional nano film on a carrier gantry 29, and transporting it through the sample chamber 30 through the feed chamber 1 Arriving at the first processing chamber 2 ⁇ '
- the substrate/catalyst layer is heat treated by the heating device 40 in the first processing chamber 2, and then passed through the second balancing chamber 5 and the second thin film deposition chamber 6 from the sample transport device 30.
- the third balance chamber 7 is transferred to the chemical vapor deposition chamber 8; the two-dimensional nano-film is prepared by using a chemical vapor deposition system in the chemical vapor deposition chamber 8; finally, the prepared two-dimensional nano-film is transported through the discharge chamber 9.
- the preparation device is prepared to complete the continuous preparation of the two-dimensional nano film.
- a large-scale continuous preparation two-dimensional nano film device of the present invention is sequentially provided with a feeding chamber 1, a first processing chamber 2, a first balancing chamber 3, a first film preparing chamber 4, and a first a second balance chamber 5, a second thin film preparation chamber 6, a third balance chamber 7, a chemical vapor deposition chamber 8 and a discharge chamber 9;
- the feed chamber 1 is provided with a valve 10 connected to the atmosphere, feeding A valve 11 is disposed between the chamber 1 and the first processing chamber 2, and a valve 12 is disposed between the first processing chamber 2 and the first balancing chamber 3, and the first balancing chamber 3 and the first thin film preparation chamber
- a valve 13 is disposed between the first film preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second film preparation chamber 6.
- a valve 16 is disposed between the second film preparation chamber 6 and the third balance chamber 7, and a valve 17 is disposed between the third balance chamber 7 and the chemical vapor deposition chamber 8, and the chemical vapor deposition chamber 8 and the discharge are provided.
- a valve 18 is arranged between the chambers 9, and the discharge chamber 9 is provided with a valve 19 which is open to the atmosphere; Material chamber 1, first processing chamber 2, first balance chamber 3, first thin film preparation chamber 4, second balance chamber 5, second thin film preparation chamber 6, third balance chamber 7, chemistry a sample transfer device 30 is disposed in the chambers of the vapor deposition chamber 8 and the discharge chamber 9; the sample transfer device 30 includes any one or a combination of two or more of a roller, a pulley, and a conveyor belt; The feed chamber 1, the first processing chamber 2, the first balance chamber 3, the first film preparation chamber 4, the second balance chamber 5, and the second film preparation chamber 6 are passed through the sample transfer device and the valve.
- the third balance chamber 7, the chemical vapor deposition chamber 8 and the discharge chamber 9 are connected in one piece.
- the first processing chamber 2 is provided with a sample processing device 50 and a heating device 40;
- the sample processing device may be a plasma processor, a wire enthalpy for gas ionization, a heating device, etc.;
- the heating device may be a resistance heating device, an infrared heating device, For laser heating devices, etc., the temperature can be adjusted between 20 and 2000 °C.
- the first processing chamber 2, the heating device 40 and the gas connection port 61 or 62 may constitute a thermal chemical vapor deposition system.
- the first film preparation chamber 4 is provided with physical vapor deposition systems 33 and 35, a heating device 41 and an insulation shielding system 98;
- the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, Any one or a combination of two or more of a thermal evaporation deposition system, a laser deposition system, and an ion implantation system;
- the heating device 41 may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be 20 to 2000°. Adjust between C.
- the first film preparation chamber 4, the heating means 41 and the gas connection port 64 may constitute a thermal chemical vapor deposition system.
- the second thin film preparation chamber 6 is provided with a physical vapor deposition system device 34 and a heating device 42;
- the physical vapor deposition system 34 includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, and a laser deposition system. Any one or a combination of two or more of the ion implantation systems;
- the heating device 42 may be a resistance heating device, an infrared heating device, a laser heating device, or the like, and the temperature may be adjusted between 20 and 2000 °C.
- the second film preparation chamber 6, heating means 42 and gas connection port 66 may constitute a thermal chemical vapor deposition system.
- the chemical vapor deposition chamber 8 is provided with a chemical vapor deposition system 38, a heating device 43, a cooling system 91 and an insulation shielding system 97; the chemical vapor deposition system 38 comprises a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor phase Any one or a combination of two or more of a deposition system, an aerosol-assisted chemical vapor deposition system, and an inductively coupled plasma chemical vapor deposition system.
- the discharge chamber 9 is provided with a sample processing device 52, which may be a plasma processor, a coil for gas ionization, a heating device, and the like.
- the feed chamber 1 is provided with a gas connection port 60
- the first process chamber 2 is provided with two gas connection ports 61 and 62
- the first balance chamber 3 is provided with a gas connection port 63
- the first film preparation chamber 4 is provided.
- There is a gas connection port 64 a gas connection port 64 is connected to the air mixing box 85
- a gas mixing box 85 is connected to the two gas connection ports 72 and 73
- a second balance chamber 5 is provided with a gas connection port 65
- a second film preparation chamber 6 is provided.
- the gas connection port 66 is provided, the gas connection port 66 is connected to the air mixing box 86, the air mixing box 86 is connected to the two gas connection ports 74 and 75, and the third balance chamber 7 is provided with a gas connection port 67, and the chemical vapor deposition chamber is provided.
- a gas path can precisely control the flow of gas, and can include metering and flow regulating devices such as mass flow meters and electromagnetic shut-off valves.
- Each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and two of each mass flow meter.
- One at each end The electromagnetic shut-off valve, the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.
- the chemical vapor deposition chamber 8, the heating device 43 and the gas connection ports 68 and/or 69 may constitute a chemical vapor deposition system.
- the feeding chamber 1 is provided with a vacuuming device 20, the first processing chamber 2 is provided with a vacuuming device 21, the first balancing chamber 3 is provided with a vacuuming device 22, and the first film preparation chamber 4 is provided with a vacuuming device 23, the second balance chamber 5 is provided with a vacuuming device 24, the second film preparation chamber 6 is provided with a vacuuming device 25, the third balancing chamber 7 is provided with a vacuuming device 26, and the chemical vapor deposition chamber 8 is provided The vacuuming device 27, the discharge chamber 9 is provided with a vacuuming device 28.
- Each of the independent vacuuming devices includes various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum of each chamber can be made to be between normal pressure and 1.0x 10- 1Q Pa by vacuuming.
- the basic process for the continuous preparation of the two-dimensional nano-film on a large scale may be: placing the substrate required for preparing the two-dimensional nano film on the carrier gantry 29, and the substrate is transported by the sample transfer device 30 through the feed chamber 1 to reach the first a processing chamber 2; at a certain temperature, the substrate is pretreated in the first processing chamber 2, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3; in the first thin film preparation chamber
- the chamber 4 is prepared on the substrate by physical vapor deposition systems 33 and 35, such as an electron beam deposition system, and then passed through the second balancing chamber 5, to the second thin film deposition chamber 6; in the second thin film preparation chamber a chamber 6, using a physical vapor deposition system 34 such as an ion beam deposition system to ionize the precursor of the two-dimensional nano-film onto the catalytic layer, and then through the third balance chamber 7, is transferred to the chemical vapor deposition chamber 8;
- the vapor deposition chamber 8 processes the sample to form a two
- the precursor of the two-dimensional nano material refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, preparing graphene, the precursor includes methane, ethanol, etc.; taking MoS 2 as an example
- the precursor includes H 2 S and the like.
- the basic process for the continuous preparation of a two-dimensional nanofilm on a large scale may also be: placing a substrate required for preparing a two-dimensional nanofilm on a carrier gantry 29, which is conveyed by the sample transfer device 30 through the feed chamber 1 First processing chamber 2; at a certain temperature, the substrate is pretreated in the first processing chamber 2, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3; in the first film preparation
- the chamber 4 simultaneously deposits two different catalytic layer materials on the substrate by physical vapor deposition systems 33 and 35, such as an electron beam deposition system and a sputter deposition system, and then passes through the second balance chamber 5, and is transferred to the first a second thin film deposition chamber 6; in the second thin film preparation chamber 6, a precursor of the two-dimensional nano-film is deposited onto the catalytic layer by a physical vapor deposition system 34 such as a thermal evaporation deposition system, and then passes through the third balance chamber 7 , is transferred to the chemical vapor deposition chamber
- the precursor of the two-dimensional nano material refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, preparing a graphene, the precursor including graphite powder, carbon black, etc.; to prepare MoS 2 As an example, the precursor includes MoS 2 powder and the like.
- the basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate required for preparing a two-dimensional nano film on a loading stage 29, which is conveyed by the sample conveying device 30 through the feeding chamber 1 First processing chamber 2; at a certain temperature, the substrate is in the first processing chamber 2 Pre-processing is carried out, and then transferred to the first film preparation chamber 4 through the first balance chamber 3; on the substrate is prepared in the first film preparation chamber 4 by using physical vapor deposition systems 33 and 35 such as an electron beam deposition system.
- the first catalytic layer is then passed through the second balancing chamber 5 to the second thin film deposition chamber 6; in the second thin film preparation chamber 6, the second is formed by a physical vapor deposition system 34 such as a sputter deposition system
- the catalytic layer is deposited on the first catalytic layer and then passed through the third equilibrium chamber 7 to be transferred to the chemical vapor deposition chamber 8; in the chemical vapor deposition chamber 8, the chemical vapor deposition system 38 is used to enhance the chemical vapor phase.
- the deposition system prepares a two-dimensional nano film on the catalytic layer; finally, the prepared two-dimensional nano film is transported out of the preparation device through the discharge chamber 9, thereby completing the continuous preparation of the two-dimensional nano film.
- the basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate/catalyst layer required for preparing a two-dimensional nano film on a carrier gantry 29, which is transported by the sample transfer device 30 through the feed chamber. 1.
- the first processing chamber 2 and the first balancing chamber 3 reach the first film preparation chamber 4; the substrate/catalyst layer is surface treated in the first film preparation chamber 4, and then passes through the second balance chamber 5
- the second thin film deposition chamber 6 and the third balance chamber 7 are transferred from the sample transfer device 30 to the chemical vapor deposition chamber 8; in the chemical vapor deposition chamber 8, using a chemical vapor deposition system 38 such as microwave plasma chemical vapor deposition
- the system prepares a two-dimensional nano film; finally, the prepared two-dimensional nano film is transferred to the atmosphere through the discharge chamber 9, thereby completing the continuous preparation of the two-dimensional nano film.
- a large-scale continuous preparation two-dimensional nano film device of the present invention is sequentially provided with a feeding chamber 1, a first processing chamber 2, a first balance chamber 3, a first film preparation chamber 4, and a first a second balance chamber 5, a second thin film preparation chamber 6, a third balance chamber 7, a chemical vapor deposition chamber 8 and a discharge chamber 9;
- the feed chamber 1 is provided with a valve 10 connected to the atmosphere, feeding A valve 11 is disposed between the chamber 1 and the processing chamber 2, and a valve 12 is disposed between the first processing chamber 2 and the first balancing chamber 3, and the first balancing chamber 3 and the first thin film preparation chamber 4
- a valve 13 is disposed between the first film preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second film preparation chamber 6.
- a valve 16 is disposed between the film preparation chamber 6 and the third balance chamber 7, and a valve 17, a chemical vapor deposition chamber 8 and a discharge chamber are disposed between the third balance chamber 7 and the chemical vapor deposition chamber 8. Between 9 is provided a valve 18, the discharge chamber 9 is provided with a valve 19 which is open to the atmosphere; the whole set of equipment is in the feed chamber Room 1, first processing chamber 2, first balancing chamber 3, first film preparation chamber 4, second balance chamber 5, second film preparation chamber 6, third balance chamber 7, chemical vapor deposition
- a sample transfer device 30 is disposed in the chamber of the chamber 8 and the discharge chamber 9; the sample transfer device 30 includes any one or a combination of two or more of a roller, a pulley, a conveyor belt, and the like; The conveying device and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparation chamber 4, the second balance chamber 5, the second film preparation chamber 6, and the third The balance chamber 7, the chemical vapor deposition chamber 8 and the discharge chamber 9 are connected in one piece.
- the first processing chamber 2 is provided with a sample processing device 50; the sample processing device may be a plasma processor, a wire enthalpy for gas ionization, and a heating device.
- the sample processing device may be a plasma processor, a wire enthalpy for gas ionization, and a heating device.
- the first processing chamber 2, the sample processing unit 50 and the gas connection port 61 or 62 may constitute a thermal chemical vapor deposition system.
- the first film preparation chamber 4 is provided with a physical vapor deposition system device 33 and a heating device 41;
- the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, Any one or a combination of two or more of the ion implantation systems;
- the heating device may be a resistance heating device, an infrared heating device, a laser heating device, or the like, and the temperature may be adjusted between 20 and 2000 °C.
- the first film preparation chamber 4, the heating means 41 and the gas connection port 64 may constitute a thermal chemical vapor deposition system.
- the second film preparation chamber 6 is provided with physical vapor deposition system devices 34 and 36, a heating device 42, a cooling system 92, and a heat shield system 99;
- the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, and electron beam deposition. Any one or a combination of two or more of a system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system;
- the heating device may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be 20 to 2000. Adjust between °C.
- the second film preparation chamber 6, the heating means 42 and the gas connection port 74 or 75 may constitute a thermal chemical vapor deposition system.
- the chemical vapor deposition chamber 8 is provided with a sample processing device 51, a heating device 43, a cooling system 91 and a heat shield system 97; the chemical vapor deposition chamber 8, the heating device 43, and the gas connection port 68 or 69 constitute a thermal chemical vapor deposition
- the chemical vapor deposition chamber 8 may also be provided with any one of a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, an aerosol assisted chemical vapor deposition system, an inductively coupled plasma chemical vapor deposition system, or Two or more combinations.
- the discharge chamber 9 is provided with a sample processing device 52, which may be a plasma processor, a wire enthalpy for gas ionization, a heating device, and the like.
- the feed chamber 1 is provided with a gas connection port 60
- the first process chamber 2 is provided with two gas connection ports 61 and 62
- the first balance chamber 3 is provided with a gas connection port 63
- the first film preparation chamber 4 is provided.
- a gas connection port 64 There is a gas connection port 64, a second balance chamber 5 is provided with a gas connection port 65, a second film preparation chamber 6 is provided with gas connection ports 74 and 75, and a third balance chamber 7 is provided with a gas connection port 67, a chemical vapor phase
- the deposition chamber is provided with gas connection ports 68 and 69, the gas connection port 69 is connected to the gas mixing box 87, the gas mixing box 87 is connected to the three gas connection ports 76, 77 and 78, and the discharge chamber is connected with two gas connection ports 70.
- each gas path can precisely control the flow of gas, including metering and flow regulating devices such as mass flow meters and electromagnetic shut-off valves, each gas connection port is connected with a mass flow meter to control the flow of each gas, each mass An electromagnetic shut-off valve is arranged at each end of the flow meter, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through the pipeline.
- the chemical vapor deposition chamber 8, the heating device 43 and the gas connection ports 68 and/or 69 may constitute a chemical vapor deposition system.
- the feeding chamber 1 is provided with a vacuuming device 20, the first processing chamber 2 is provided with a vacuuming device 21, the first balancing chamber 3 is provided with a vacuuming device 22, and the first film preparation chamber 4 is provided with a vacuuming device 23, the second balance chamber 5 is provided with a vacuuming device 24, the second film preparation chamber 6 is provided with a vacuuming device 25, the third balancing chamber 7 is provided with a vacuuming device 26, and the chemical vapor deposition chamber 8 is provided The vacuuming device 27, the discharge chamber 9 is provided with a vacuuming device 28.
- Each individual evacuating device include various vacuum pumps, vacuum lines, vacuum valves, vacuum meter, etc., can make the degree of vacuum in the chambers between 1.0x l0- 1Q Pa to atmospheric pressure by the evacuating device.
- the basic process for the continuous preparation of the two-dimensional nano-film can be: placing the substrate required for preparing the two-dimensional nano film on the loading stage 29, passing through the feeding chamber 1, and transferring the substrate to the first processing chamber 2; the substrate is pretreated in the first processing chamber 2, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3; in the first thin film preparation chamber 4 using the physical vapor deposition system 33 such as The electron beam deposition system prepares the catalytic layer on the substrate and then passes through the second balancing chamber 5 to be transferred to the second thin film deposition chamber 6; in the second thin film preparation chamber 6, using the physical vapor deposition systems 34 and 36 A precursor of the two-dimensional nano-film is deposited on the catalytic layer by a sputter deposition system, and then transferred to the chemical vapor deposition chamber 8 through the third balance chamber 7, and chemical vapor deposition is performed in the chemical vapor deposition chamber 8.
- the method comprises preparing a two-dimensional nano film; finally, the prepared two-dimensional nano film is sent
- the precursor of the two-dimensional nano material refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, preparing a graphene, the precursor including graphite powder, carbon black, etc.; to prepare MoS 2 As an example, the precursor includes MoS 2 powder and the like.
- the basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate and/or a catalytic layer required for preparing a two-dimensional nano film on a loading stage 29, passing through a feeding chamber 1, a substrate, and / or the catalytic layer is transported to the first processing chamber 2; the substrate and / or catalytic layer is pretreated in the first processing chamber 2, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3 Depositing a precursor of the two-dimensional nanomaterial on the substrate and/or the catalytic layer in the first thin film preparation chamber 4 using a physical vapor deposition system 33 such as an electron beam deposition system, and then passing through the second balance chamber 5, Is transferred to the second thin film deposition chamber 6; in the second thin film preparation chamber 6, a precursor of another two-dimensional nano-film is deposited onto the substrate by physical vapor deposition systems 34 and 36 such as a thermal evaporation deposition system and And / or on the catalytic layer, then through the
- the precursor of the two-dimensional nano material refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, preparing a graphene, the precursor including graphite powder, carbon black, etc.; to prepare MoS 2 As an example, the precursor includes MoS 2 powder and the like.
- the basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate and/or a catalytic layer required for preparing a two-dimensional nano film on a loading stage 29, passing through a feeding chamber 1, a substrate, and / or the catalytic layer is transported to the first processing chamber 2; the substrate and / or the catalytic layer is pretreated in the first processing chamber 2, and then passes through the first balancing chamber 3, the first thin film preparation chamber 4, The second balance chamber 5 is transferred to the second thin film deposition chamber 6; in the second thin film preparation chamber 6, the precursor deposition of the two-dimensional nano-film is implanted by the physical vapor deposition systems 34 and 36, such as an ion implantation deposition system.
- the sample is processed to form a two-dimensional nano-film;
- the prepared two-dimensional nano film is transferred to the atmosphere through the discharge chamber 9, thereby completing the continuous preparation of the two-dimensional nano film.
- the precursor of the two-dimensional nano material refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, preparing a graphene, the precursor including graphite powder, carbon black, etc.; to prepare MoS 2 As an example, the precursor includes MoS 2 powder and the like.
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Abstract
本发明公开了一种规模化连续制备二维纳米薄膜装备,包括进料腔室、薄膜制备腔室、平衡腔室、化学气相沉积腔室、出料腔室等;各腔室之间设有阀门,样品通过设置于整套系统内的传送装置而实现在各腔室之间的连续传输;腔室内设有样品处理装置、加热装置、物理气相沉积系统和/或化学气相沉积系统等;各腔室和气体连接口相连,与真空系统相连;整套装备设有自动化控制系统以控制腔室之间的阀门的开关、样品的传输、气体流量的控制、抽真空等。利用本设备,可以采用化学气相沉积等方法制备石墨烯、过镀金属硫化物、硅烯、锗烯或氮化硼等二维纳米薄膜。本装备结构简单、工作可靠,可规模化连续制备均匀的高质量的石墨烯、金属硫族化合物、硅烯、锗烯或氮化硼等二维纳米薄膜,适合于二维纳米薄膜的产业化制备。
Description
规模化连续制备二维纳米薄膜的装备 技术领域
本发明涉及一种新材料的制备装备, 特别是涉及规模化连续制备石墨烯、 金属硫族化物、 硅烯、 锗烯、 氮 化硼等新型二维纳米材料的装备。 背景技术
石墨烯 (graphene)是如蜂窝状的单一碳原子层, 其厚度为 0.334 nm, 具有卓越的二维电学、 光学、 热学、 力 学性能以及化学稳定性, 石墨烯在超快光电子器件、 洁净能源、 传感器等方面具有广泛的应用前景。 电子在石 墨烯中传输速度是硅的 150倍, IBM等著名公司已经制备速度可达太赫兹的超快速光电子器件, 美国加州大学 利用石墨烯研制成光学调制解调器, 有望将网速提高 1万倍; 全球每年半导体晶硅的需求量在 2500吨左右, 石 墨烯如果替代十分之一的晶硅制成高端集成电路如射频电路, 市场容量至少在 5000亿元以上。 因为石墨烯只有 2.3%光吸收, 这使石墨烯可用于制备光电子器件如显示器件、 太阳能电池、 触摸面板等的柔性透明电极, 从而 取代成本昂贵、 资源稀少、 不可自由折叠的由铟为主要成分的 ITO透明导电膜; 据报道, 2011年全球 ITO导电 玻璃的需求量在 8500万 -9500万片, 这样, 石墨烯的替代空间巨大。 由于石墨烯独特的电子传输特性, 作为传 感器, 它具有单分子的敏感性; 如果基于石墨烯的基因电子测序技术能够实现, 人类全基因谱图测定的测序成 本将由目前的约 10万美元 /人而大大降低到约 1000美元 /人, 从而有助于生物医学的创新, 有助于实现个性化的 医疗保健。 经过这几年的快速发展, 石墨烯产品已经出现在触摸屏应用上。 因此, 石墨烯良好的商业价值和广 阔的市场已经展现曙光, 石墨烯材料的产业化将是对材料、 信息、 能源工业的一次革命性变革!
除了石墨烯外, 类石墨烯 (graphene-like)的新型二维纳米材料也具有其独特的光电子性能, 具有广泛的应用 前景。 类石墨烯的新型二维纳米材料包括层状的金属硫族化物 (metal chalcogenides ) , 硅烯 (siliCene)、 锗烯 (germanene)、 氮化硼 (boron nitride)等。
然而,目前还没有规模化连续制备石墨烯等二维纳米薄膜的装置,化学气相沉积法 (CVD)以及碳偏析 (surface segregation)法是大面积制备二维纳米薄膜的技术方法, 采用这两种方法制备二维纳米薄膜的设备基本上都是石 英管高温炉 [Science 324, 1312-1314 (2009); Nature Nanotechnology 5, 574 (2010); Nano Lett. 11, 297-303 (2011)]。 基于石英管的高温炉仅具备在已有金属催化层上合成二维纳米薄膜的单一功能, 即不能先后连续对衬底的表面 进行处理, 在衬底上制备合成二维纳米薄膜所需的催化层和之后的二维纳米薄膜的合成。 并且, 采用石英管式 炉合成的二维纳米薄膜存在许多结构缺陷, 导致制备薄膜的电子传输性能较差, 石英管式炉已经严重制约了二 维纳米薄膜如石墨烯薄膜的应用, 不适合规模化连续制备如石墨烯等二维纳米薄膜。
为了实现二维纳米薄膜的规模化连续制备, 即包括衬底的处理、 催化层的制备、 二维薄膜的制备等连续过 程, 各腔室在二维纳米薄膜的制备过程中应该承担专有的独特的功能角色。 由于石墨烯等二维薄膜的结构特征 以及制备工艺技术的要求, 传统的其它行业的设备不能胜任高质量石墨烯薄膜的连续化可控制备; 比如由于高 温对合成石墨烯等薄膜所需的衬底 /催化层的机械性能等的影响, 卷-对-卷 (roll-to-roll)的设备不可能制备高品质 的石墨烯薄膜 [Applied Physics Letters 98, 133106 (2011)]; 由于生产工艺技术的差别, 目前用于制备 ITO导电玻 璃的生产工艺设备不适合制备石墨烯等二维薄膜; 至今, 国际上还没有为高质量的石墨烯薄膜的规模化连续制 备的研制过专项装备。 发明内容
针对现有技术的不足, 本发明提供一种能够规模化连续制备二维纳米薄膜如石墨烯、 金属硫族化合物、 硅 烯、 锗烯或氮化硼等的装备。 为了能够实现二维纳米薄膜的连续化制备, 该装备设有耐高温的样品传送装置; 为了达到连续制备过程中的平衡与稳定, 作为优选在特定的腔室与腔室之间设有过渡的平衡腔室, 平衡腔室对 二维纳米薄膜的整个制备过程具有稳定作用; 薄膜制备腔室和化学气相沉积腔室的功能主要用于制备薄膜以及 对制备的薄膜进行适当的处理, 所述的薄膜包括催化层、 二维薄膜的前驱体以及二维薄膜等; 处理腔室的功能 主要用于优化衬底、 催化层、 二维薄膜的前驱体以及二维薄膜等的结构, 从而能够制备出高质量的二维薄膜; 该装备具有结构简单、 操作简单、 安全性好等特点, 采用该设备制备二维纳米薄膜的工艺简单、 成本较低、 制 备出的薄膜具有优良的结构和性能。
所述的物理气相沉积系统包括离子束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光 沉积系统、 离子注入系统中的任意一种或二种以上的组合。
所述的化学气相沉积系统包括由腔室、 气体和加热器构成的化学气相沉积系统(即热化学气相沉积系统) 、 等离子体增强化学气相沉积系统、 微波等离子体化学气相沉积系统、 气溶胶辅助化学气相沉积系统、 电感耦合 等离子体化学气相沉积系统中的任意一种或二种以上的组合。
根据制备二维薄膜的工艺的不同, 比如衬底、 催化层以及合成二维薄膜的源材料的不同, 可以选择不同的 装置组合方式或者装备而实现二维薄膜的连续制备。
为了各个实施例的简单、 清楚的说明, 本说明书对各种名称术语进行了统一化。
依据二维薄膜的制备工艺条件的不同, 本发明采用的技术方案如下:
一种规模化连续制备二维纳米薄膜的装备, 包括进料腔室、 第一薄膜制备腔室和出料腔室。 第一薄膜制备 腔室也可称为样品制备腔室。
所述的进料腔室、第一薄膜制备腔室和出料腔室均设有样品传送装置, 样品通过样品传送装置可以从进料 腔室传传输到第一薄膜制备腔室, 从第一薄膜制备腔室传输到出料腔室, 以便实现二维纳米薄膜的连续制备; 所述的样品传送装置包括滚轮、 皮带轮和传送带中的任意一种或二种以上的组合。
所述的进料腔室设有与大气相通的阀门, 进料腔室与第一薄膜制备腔室之间设有阀门, 第一薄膜制备腔室 与出料腔室之间设有阀门, 出料腔室设有与大气相通的阀门。
所述的进料腔室、 第一薄膜制备腔室和出料腔室中至少有一个腔室设有加热装置; 加热装置可以是电阻丝 加热装置、 红外加热装置、 激光加热装置等。
所述的进料腔室、 第一薄膜制备腔室和出料腔室分别设有独立的抽真空装置, 每一抽真空装置包括各种真 空泵、真空管道、真空阀门、真空计等,通过抽真空装置可以使各腔室的真空度保持在常压至 1.0x 10— 1Q Pa之间。
所述的进料腔室、 第一薄膜制备腔室和出料腔室中的至少一个腔室设有一个或多个气体连接口, 气体连接 口可以是一种气体的连接口, 气体连接口也可以与混气盒连接, 气体连接口连接气路; 混气盒的入口至少并联 有两个或以上的气路, 可使两种或以上的气体同时进入混气盒; 每一个气路都设有质量流量计和电磁截止阀等, 从而可以独立精确控制气体的流量; 通入的气体可以选自惰性气体如氩气或氮气, 还原性气体如氢气, 氧化性 气体如氧气, 合成二维纳米薄膜所需的气态的前驱体如 CH4, C2H4, C2H2, NH3, B3N3H6或乙醇的蒸汽等。
所述的进料腔室、 第一薄膜制备腔室和出料腔室中的至少一个腔室设有化学气相沉积系统, 包括等离子体 增强化学气相沉积系统和微波等离子化学气相沉积系统等; 进料腔室、 第一薄膜制备腔室或出料腔室中的任何 一个腔室均可以与加热装置和气体连接口构成化学气相沉积系统, 这种化学气相沉积系统一般可以称为热化学 气相沉积系统。
所述的进料腔室、 第一薄膜制备腔室和出料腔室中的至少一个腔室设有物理气相沉积系统, 所述的物理气 相沉积系统为溅射靶薄膜沉积系统、 电子枪沉积系统、 离子枪沉积系统、 离子注入沉积系统和热蒸镀系统中的 任意一种或二种以上的组合。
进料腔室、 第一薄膜制备腔室或出料腔室中的任何一个腔室都可以既包括化学气相沉积系统, 又包括物理 气相沉积系统。
所述的进料腔室、 第一薄膜制备腔室或出料腔室中的至少一个腔室的温度控制在 20〜1600°C ;
作为优选, 为了将热量集中在样品处, 并减少向不需要热的地方传递, 所述的进料腔室、 第一薄膜制备腔 室和出料腔室中的至少一个腔室的腔壁设有热屏蔽系统;
作为优选, 为了使设备安全稳定运转, 所述的进料腔室、 第一薄膜制备腔室和出料腔室中的至少一个腔室 的腔壁设有冷却系统, 冷却系统可以是双层水冷系统。
作为优选, 腔室内设有热屏蔽系统的腔室, 同时此腔室的腔壁设有冷却系统。
作为优选, 本发明的规模化连续制备二维纳米薄膜的装备还可以设有控制系统, 所述的控制系统包括样品 传输控制系统、 气路控制系统、 真空控制系统、 阀门控制系统或温度控制系统中的任意一种或二种以上的组合。
本发明的设备可用于生长包括石墨烯、 金属硫族化合物、 硅稀、 锗烯或氮化硼等二维纳米薄膜, 依据所合 成的二维纳米薄膜的不同, 可以适当选择制备所需的固体、 液体或气体等前驱体。
作为优选, 进料腔室作为表面处理腔室, 第一薄膜制备腔室作为衬底、 催化层和二维纳米薄膜的制备腔室, 出料腔室作为降温腔室或二维纳米薄膜的再处理腔室; 进料腔室设有等离子表面处理器, 第一薄膜制备腔室设 有薄膜沉积系统。
规模化连续制备二维纳米薄膜的基本过程包括: 将合成二维纳米薄膜所需的衬底材料或催化层放置在载料 台架上, 由样品传送装置经进料腔室传输到第一薄膜制备腔室, 在第一薄膜制备腔室利用物理气相沉积或化学 气相沉积方法制备二维纳米薄膜, 然后将制备好的二维纳米薄膜由样品传送装置送到出料腔室。
连续制备二维纳米薄膜的基本过程还包括: 将合成二维纳米薄膜所需的衬底或催化层放置在载料台架上由
样品传送装置传输到进料腔室, 在一定的气氛环境下, 衬底材料或催化层先在进料腔室进行预处理, 然后由样 品传送装置将衬底或催化层传输到第一薄膜制备腔室; 在第一薄膜制备腔室里利用物理气相沉积或化学气相沉 积方法制备催化层、 碳膜或者二维纳米薄膜; 薄膜制备后可以由样品传送装置送到出料腔室进行热处理或进行 表面优化处理。
依据二维薄膜的制备工艺条件的不同, 本发明采用的技术方案还可以如下:
一种规模化连续制备二维纳米薄膜的装备, 包括进料腔室、 第一薄膜制备腔室、 第一平衡腔室和化学气相 沉积腔室。 为了统一名称术语, 薄膜制备腔室被称之为第一薄膜制备腔室, 平衡腔室被称之为第一平衡腔室, 平衡腔室在样品传送过程中可以起到过渡、 稳定、 平衡样品的功能; 在功能上, 化学气相沉积腔室也可称之为 薄膜制备腔室。
所述的进料腔室、第一薄膜制备腔室、第一平衡腔室和化学气相沉积腔室的各腔室内和腔室之间均设有样 品传送装置, 样品通过样品传送装置可以从进料腔室连续传输到第一薄膜制备腔室, 从第一薄膜制备腔室连续 传输到第一平衡腔室, 从第一平衡腔室连续传输到化学气相沉积腔室, 以便实现二维纳米薄膜的连续制备; 所 述的样品传送装置包括滚轮、 皮带轮和传送带等中的任意一种或二种以上的组合。
所述的进料腔室设有与大气相通的阀门, 进料腔室与第一薄膜制备腔室之间设有阀门, 第一薄膜制备腔室 与第一平衡腔室之间设有阀门, 第一平衡腔室与化学气相沉积腔室之间设有阀门, 化学气相沉积腔室设有与大 气相通的阀门。
通过样品传送装置与阀门将进料腔室、 第一薄膜制备腔室、 第一平衡腔室和化学气相沉积腔室连接成一个 整体。
所述第一薄膜制备腔室设有物理气相沉积系统, 所述的物理气相沉积系统包括离子束沉积系统、 溅射沉积 系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系统等中的任意一种或二种以上的组合。
所述的化学气相沉积腔室设有加热装置和气体连接口;
所述的化学气相沉积腔室、 加热装置与气体连接口可以构成一个简单的化学气相沉积系统;
作为优选, 化学气相沉积腔室还设有等离子体增强化学气相沉积系统、 微波等离子体化学气相沉积系统、 气溶胶辅助化学气相沉积系统等中的任意一种或二种以上的组合; 由于化学气相沉积腔室设有与大气相通的阀 门, 因此化学气相沉积腔室也具有出料腔室的功能。
所述的进料腔室、 第一薄膜制备腔室和第一平衡腔室中的至少一个腔室设有气体连接口; 作为优选, 进料 腔室、 第一薄膜制备腔室和第一平衡腔室均设有气体连接口;
所述的气体连接口可以是一种气体的连接口, 也可以连接混气盒, 混气盒的入口至少并联有两个或两个以 上的气路, 可使两种或两种以上的气体同时进入混气盒; 作为优选, 每一个气路独立连接有质量流量计、 电磁 截止阀等计量和流量调节装置, 从而可以独立精确控制每一种气体的流量。
所述的进料腔室、 第一薄膜制备腔室、 第一平衡腔室、 化学气相沉积腔室均设有抽真空装置, 每一抽真空 装置包括各种真空泵、 真空管道、 真空阀门、 真空计等, 通过抽真空装置可以使各腔室的真空度保持在常压至 1.0x 10— 1() Pa之间。
所述的进料腔室和第一薄膜制备腔室中的至少一个腔室设有样品处理装置; 作为优选, 进料腔室和第一薄 膜制备腔室均设有样品处理装置;
所述的样品处理装置采用等离子表面处理器、 对气体离子化的线圏或加热装置等能够实现对样品进行改性 的装置, 所述的对气体离子化的线圏可在真空高频条件下实现气体的离子化; 加热装置采用电阻加热装置、 红 外加热装置、 激光加热装置等能实现对样品加热的装置。
作为优选, 进料腔室、 第一薄膜制备腔室和化学气相沉积腔室内的温度可以控制在 20〜2000°C ;
为了将热量集中在样品处, 减少不必要的热传递, 所述的进料腔室、 第一薄膜制备腔室和化学气相沉积腔 室中的至少一个腔室内设有隔热屏蔽系统; 作为优选, 只有当有高温 (如高于 40CTC ) 存在的腔室内设有隔热 屏蔽系统。
为了使设备安全稳定运行, 所述的进料腔室、 第一薄膜制备腔室和化学气相沉积腔室中的至少一个腔室的 腔壁设有冷却系统, 冷却系统可以是双层水冷系统等; 作为优选, 只有当有高温 (如高 40CTC ) 存在的腔室的 腔壁设有冷却系统。
作为优选, 本发明的规模化连续制备二维纳米薄膜的装备还设有控制系统, 所述的控制系统包括样品传输 控制系统、 气路控制系统、 真空控制系统、 阀门控制系统或温度控制系统中的任意一种或二种以上的组合。
作为优选, 进料腔室作为衬底和 /或催化层处理的腔室, 第一薄膜制备腔室作为制备二维纳米薄膜或催化层 等薄膜的腔室, 化学气相沉积腔室作为降温腔室或制备二维纳米薄膜或二维纳米薄膜再处理的腔室。
本发明的设备可用于生长包括石墨烯、 金属硫族化合物、 硅稀、 锗烯或氮化硼等在内的各种二维纳米薄膜, 依据所合成的二维纳米薄膜的不同, 可以适当选择制备所需的固体、 液体或气体等前驱体。
连续制备二维纳米薄膜的基本过程包括: 将合成二维纳米薄膜所需的衬底和 /或催化层放置在载料台架上由 样品传送装置传输到进料腔室, 在一定的气氛环境下, 衬底材料和 /或催化层在进料腔室进行预处理, 然后由样 品传送装置将衬底和 /或催化层传输到第一薄膜制备腔室; 在第一薄膜制备腔室里利用物理气相沉积系统制备二 维纳米薄膜或催化层薄膜; 二维薄膜制备也可以在化学气相沉积腔室中制备, 然后传到大气中而完成制备。
依据二维薄膜的制备工艺条件的不同, 本发明采用的技术方案还可以如下:
一种规模化连续制备二维纳米薄膜的装备, 其特征在于: 在生产线上依次设置有进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二处理腔室和出料腔室。 为了统一名称术语, 在这将薄 膜制备腔室称为第一薄膜制备腔室。
其中: 进料腔室设有与大气相通的阀门, 进料腔室与第一处理腔室之间设有阀门, 第一处理腔室与第一平 衡腔室之间设有阀门, 第一平衡腔室与第一薄膜制备腔室之间设有阀门, 第一薄膜制备腔室与第二平衡腔室之 间设有阀门, 第二平衡腔室与第二处理腔室之间设有阀门, 第二处理腔室与出料腔室之间设有阀门, 出料腔室 设有与大气相通的阀门;
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二处理腔室和出料腔室 之间均设有样品传送装置, 样品通过样品传送装置从大气传送到进料腔室, 从进料腔室传送到第一处理腔室, 从第一处理腔室传送到第一平衡腔室, 从第一平衡腔室传送到第一薄膜制备腔室, 从第一薄膜制备腔室传送到 第二平衡腔室, 从第二平衡腔室传送到第二处理腔室, 从第二处理腔室传送到出料腔室, 从出料腔室传送到大 气, 以便实现二维纳米薄膜的连续制备; 所述的样品传送装置包括滚轮、 皮带轮和传送带中的任意一种或二种 以上的组合。 平衡腔室在样品传送过程中可以起到过渡、 稳定、 平衡样品的功能。
进料腔室、 第一处理腔室、 第一薄膜制备腔室、 第二处理腔室和出料腔室中的至少一个腔室的设有加热装 置, 以便达到一定的温度如 20〜2000°C ; 加热装置可以是电阻加热装置、 红外加热装置、 激光加热装置等。
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二处理腔室和出料腔室 中的至少一个腔室设有一个或多个气体连接口; 气体连接口可以是一种气体的连接口, 气体连接口也可以与混 气盒连接; 混气盒的入口至少并联有两个或以上的气路, 可使两种或以上的气体同时进入混气盒; 采用质量流 量计和电磁截止阀等, 使每一个气路都可以精确控制气体的流量; 通入的气体可以选自惰性气体如 Ar和 N2, 还原性气体如 H2,氧化性气体如 02,合成二维纳米薄膜所需的气体如 CH4, C2H4, C2H2, NH3, B3N3H6或乙醇的蒸 汽等。
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二处理腔室和出料腔室 分别连接独立的抽真空装置, 每一抽真空装置包括各种真空泵、 真空管道、 真空阀门、 真空计等, 通过抽真空 装置可以使各腔室的真空度在常压至 l.Ox 10-10 Pa之间。
为更好地实现本发明的目的, 所述第一处理腔室、 第一薄膜制备腔室和第二处理腔室中的至少一个腔室设 有物理气相沉积系统, 所述的物理气相沉积系统包括溅射靶薄膜沉积系统、 电子枪沉积系统、 离子枪沉积系统、 离子注入沉积系统和热蒸镀系统中的任意一种或二种以上的组合。
为更好地实现本发明的目的, 所述第一处理腔室、 第一薄膜制备腔室和第二处理腔室中的至少一个腔室设 有化学气相沉积系统, 包括等离子体增强化学气相沉积系统、 气溶胶辅助化学气相沉积系统和微波等离子化学 气相沉积系统等; 任何一个腔室 (包括第一处理腔室、第一薄膜制备腔室或第二处理腔室)、加热装置和气体连接 口均可以构成一种化学气相沉积系统, 这种化学气相沉积系统一般可以称为热化学气相沉积系统。
也可以在同一个腔室 (第一薄膜制备腔室或第二处理腔室)中既包括有化学气相沉积系统又包括有物理气相 沉积系统。
在第一薄膜制备腔室或第二处理腔室可以制备各种薄膜, 比如用于合成二维纳米薄膜如石墨烯薄膜所需的 衬底材料、 催化层材料、 碳薄膜、 制备二维纳米薄膜所需的前驱体以及二维纳米薄膜等。
作为优选, 为了将热量集中在样品处, 并减少向不需要热的地方的热传递, 所述的第一处理腔室、 第一薄 膜制备腔室和第二处理腔室中的至少一个腔室的腔壁设有热屏蔽系统;
作为优选, 为了使设备安全稳定运转, 所述的第一处理腔室、 第一薄膜制备腔室和第二处理腔室中的至少 一个腔室的腔壁设有冷却系统, 冷却系统可以是双层水冷系统。
作为优选, 腔室内设有热屏蔽系统的腔室, 同时此腔室的腔壁设有冷却系统。
作为优选, 第一处理腔室内设有样品表面处理器, 表面处理器可以是等离子体表面处理器、 热处理器等。 作为优选, 本发明的连续制备二维纳米薄膜的装备还可以设有控制系统, 所述的控制系统包括样品传输控
制系统、 气路控制系统、 真空控制系统、 阀门控制系统或温度控制系统中的任意一种或二种以上的组合。 本发明的设备可用于制备包括石墨烯、 金属硫族化合物、 硅烯、 锗烯或氮化硼等二维纳米薄膜。
作为优选, 第一处理腔室作为衬底表面处理腔室, 第一薄膜制备腔室作为催化层或二维纳米薄膜的制备腔 室, 第二处理腔室作为降温腔室、 二维纳米薄膜制备或二维纳米薄膜再处理腔室。
制备二维纳米薄膜如石墨烯薄膜的基本过程包括但不局限于此:
利用自动化控制系统,将合成二维纳米薄膜如石墨烯薄膜所需的衬底材料或催化层材料放置在载料台架上, 并从进料腔室由样品传送装置通过进料腔室与第一处理腔室的阀门进入第一处理腔室; 在一定的气氛环境下, 衬底材料或催化层材料先在第一处理腔室进行表面处理, 然后通过第一平衡腔室由样品传送装置将衬底或催化 层材料传输到第一薄膜制备腔室; 在第一薄膜制备腔室里利用物理沉积方法或化学气相沉积方法制备二维纳米 薄膜所需的催化层、 碳膜等; 然后由样品传送装置送到第二平衡腔室再传送到第二处理腔室, 在一定的气氛下, 二维纳米薄膜在第二处理腔室制备; 最后, 制备的二维纳米薄膜由样品传送装置送到出料腔室。 依据各腔室的 功能, 二维纳米薄膜或在第一薄膜制备腔室中制备, 或在第二处理腔室内形成。
依据二维薄膜的制备工艺条件的不同, 本发明采用的技术方案还可以如下:
一种规模化连续制备二维纳米薄膜的装备, 其特征在于: 依次设有进料腔室、 第一处理腔室、 第一平衡腔 室、 第一薄膜制备腔室、 第二平衡腔室、 第二薄膜制备腔室、 第三平衡腔室、 化学气相沉积腔室和出料腔室; 为了统一名称术语, 在这将处理腔室称为第一处理腔室; 在功能上, 化学气相沉积腔室也可称之为薄膜制备腔 室。
其中: 进料腔室设有与大气相通的阀门, 进料腔室与第一处理腔室之间设有阀门, 第一处理腔室与第一平 衡腔室之间设有阀门, 第一平衡腔室与第一薄膜制备腔室之间设有阀门, 第一薄膜制备腔室与第二平衡腔室之 间设有阀门, 第二平衡腔室与第二薄膜制备腔室之间设有阀门, 第二薄膜制备腔室与第三平衡腔室之间设有阀 门, 第三平衡腔室与化学气相沉积腔室之间设有阀门, 化学气相沉积腔室与出料腔室之间设有阀门, 出料腔室 设有与大气相通的阀门。
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二薄膜制备腔室、 第三 平衡腔室、 化学气相沉积腔室和出料腔室的腔室内均设有样品传送装置; 样品通过样品传送装置传送到进料腔 室, 从进料腔室传送到第一处理腔室, 从第一处理腔室传送到第一平衡腔室, 从第一平衡腔室传送到第一薄膜 制备腔室, 从第一薄膜制备腔室传送到第二平衡腔室, 从第二平衡腔室传送到第二薄膜制备腔室, 从第二薄膜 制备腔室传送到第三平衡腔室, 从第三平衡腔室传送到化学气相沉积腔室, 从化学气相沉积腔室传送到出料腔 室, 以便实现二维纳米薄膜的连续制备。进料腔室的基本功能是实现样品装载并进入二维纳米薄膜的制备装置, 第一处理腔室实现对衬底或催化层的预处理, 第一薄膜制备腔室和第二薄膜制备腔室可以用于制备合成二维纳 米材料所需的衬底、 催化层、 二维纳米薄膜的前驱体或者二维纳米薄膜, 化学气相沉积腔室可以用来制备二维 纳米薄膜, 平衡腔室在样品传送过程中可以起到过渡、 稳定、 平衡样品的功能。
所述的样品传送装置包括滚轮、 皮带轮和传送带等中的任意一种或二种以上的组合。
整套设备通过样品传送装置与阀门将进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二 平衡腔室、 第二薄膜制备腔室、 第三平衡腔室、 化学气相沉积腔室和出料腔室连接成一个整体。
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二薄膜制备腔室、 第三 平衡腔室、 化学气相沉积腔室和出料腔室中的至少一个腔室设有抽真空装置, 抽真空装置包括各种真空泵、 真 空管道、 真空阀门、 真空计等, 通过抽真空装置可以使各腔室的真空度在常压至 1.0x 10— 1Q Pa之间。
作为优选, 进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二薄膜制备 腔室、 第三平衡腔室、 化学气相沉积腔室和出料腔室都设有独立的抽真空装置, 每一抽真空装置包括各种真空 泵、 真空管道、 真空阀门、 真空计等, 通过抽真空装置可以使各腔室的真空度在常压至 1.0x l0—1QPa之间。
第一薄膜制备腔室和第二薄膜制备腔室中的至少一个的腔室内设有物理气相沉积系统, 用于制备合成二维 纳米材料所需的衬底、 催化层、 二维纳米薄膜的前驱体或者二维纳米薄膜; 所述的物理气相沉积系统包括离子 束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系统中的任意一种 或二种以上的组合。
化学气相沉积腔室的腔室内设有加热装置, 以便达到一定的温度如 20~2000°C ; 加热装置可以是电阻加热 装置、 红外加热装置、 激光加热装置等。
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二薄膜制备腔室、 第三 平衡腔室、 化学气相沉积腔室和出料腔室中的至少一个腔室设有一个或二个以上的气体连接口。
所述的气体连接口可以是一种气体的连接口, 气体连接口也可以与混气盒连接; 混气盒的入口至少并联有
两个或两个以上的气路, 可使两种或两种以上的气体同时进入混气盒; 作为优选, 每一个气路独立连接有质量 流量计、 电磁截止阀等计量和流量调节装置, 以便达到独立精确控制每一种气体的流量。
通入的气体可以选自惰性气体如 Ar和 N2, 还原性气体如 H2, 氧化性气体如 02, 合成二维纳米薄膜所需的 气体如 CH4, C2H4, C2H2, NH3, B3N3H6或乙醇的蒸汽等, 依据所合成的二维薄膜的不同, 可以适当选择不同的气 体。
化学气相沉积腔室、 加热装置与气体连接口可构成一个化学气相沉积系统; 还可以在化学气相沉积腔室中 设有化学气相沉积系统, 所述的化学气相沉积系统为等离子体增强化学气相沉积系统、 微波等离子体化学气相 沉积系统、 气溶胶辅助化学气相沉积系统、 电感耦合等离子体化学气相沉积系统中的任意一种或二种以上的组 合.
第一薄膜制备腔室、 第二薄膜制备腔室或第一处理腔室可分别与加热装置和气体连接口结合构成一种化学 气相沉积系统;
作为优选, 在第一薄膜制备腔室、 第二薄膜制备腔室、 第一处理腔室或化学气相沉积腔室中既设有化学气 相沉积系统又设有物理气相沉积系统。
作为优选, 所述的第一处理腔室、 第一薄膜制备腔室和第二薄膜制备腔室中的至少一个腔室内设有加热装 置, 以便达到一定的温度如 20〜2000°C ; 加热装置可以是电阻加热装置、 红外加热装置、 激光加热装置等。
作为优选, 所述第一处理腔室设有样品处理装置, 所述的样品处理装置为等离子样品处理装置、 对气体离 子化的线圏或加热装置等能够实现对样品进行改性的装置, 所述的对气体离子化的线圏可在真空高频条件下实 现气体的离子化; 加热装置为电阻加热装置、 红外加热装置、 激光加热装置等能实现对样品加热的装置。
作为优选, 为了将热量集中在样品处, 并减少向不需要热的地方的热传递, 所述的第一处理腔室、 第一薄 膜制备腔室、 第二薄膜制备腔室和化学气相沉积腔室中的至少一个腔室内设有隔热屏蔽系统; 作为优选, 只有 当有高温 (如高于 400 °C ) 存在的腔室内设有隔热屏蔽系统。
作为优选, 为了使设备安全稳定运转, 所述的第一处理腔室、 第一薄膜制备腔室、 第二薄膜制备腔室和化 学气相沉积腔室中的至少一个腔室的腔壁设有冷却系统; 作为优选, 只有当有高温 (如高于 40CTC ) 存在的腔 室的腔壁设有冷却系统。
作为优选, 所述的第一处理腔室、 第一薄膜制备腔室、 第二薄膜制备腔室和化学气相沉积腔室的中的至少 一个腔室的腔室内既设有隔热屏蔽系统的腔室, 腔壁也设有冷却系统。
作为优选, 整套装备还设有控制系统, 以实现对设备或工艺的控制, 所述的控制系统包括样品传送控制系 统、 气路控制系统、 真空控制系统、 阀门控制系统或温度控制系统中的任意一种或二种以上的组合。
本发明的装置可规模化连续制备二维纳米薄膜, 所述的二维纳米薄膜包括石墨烯、 金属硫族化物、 硅稀、 锗烯或氮化硼薄膜等。
作为优选,第一处理腔室作为衬底和 /或催化层的表面处理腔室,第一薄膜制备腔室作为催化层的制备腔室, 第二薄膜制备腔室作为在衬底和 /或催化层上制备二维纳米薄膜所需的前驱体的制备腔室, 化学气相沉积腔室作 为将前驱体进行处理而形成二维纳米薄膜的腔室。
在制备二维纳米薄膜时, 由于所选用的衬底、 催化层以及工艺等方面的差异, 本发明装备的各腔室承担的 功能随制备工艺条件的不同而有所变化, 在不同的制备工艺条件中可能同时承担多种功能, 也可能不承担特定 的功能。
设置于各腔室内或与各腔室相连接的部件如阀门、 气体连接口、 样品处理器、 加热器、 物理气相沉积系统、 化学气相沉积系统、 隔热屏蔽系统、 冷却系统等可以依据制备二维纳米薄膜的具体工艺的不同而设置于各腔室 的不同位置, 并且可以根据具体工艺的有选择性地选取相关部件。
二维纳米材料的前驱体是指含有组成二维纳米材料的元素或含有组成二维纳米材料的元素的化合物, 以制 备石墨烯为例, 前驱体包括无定型碳、 非晶碳膜、 碳靶材、 含碳元素的聚合物等; 以合成 MoS2为例, 前驱体包 括 MoS2靶材、 Mo靶材、 硫粉等。
规模化连续制备二维纳米薄膜的基本过程包括但不局限于此:
将合成二维纳米薄膜所需的衬底和 /或催化层放置在载料台架上, 并从进料腔室由样品传送装置传送到第一 处理腔室; 在一定的气氛环境下, 衬底和 /或催化层在第一处理腔室进行处理, 然后通过第一平衡腔室由样品传 送装置将衬底和 /或催化层传输到第一薄膜制备腔室; 在第一薄膜制备腔室里利用物理气相沉积方法或化学气相 沉积方法制备二维纳米薄膜生长所需的催化层等; 然后经过第二平衡腔室, 由样品传送装置送到第二薄膜制备 腔室, 在一定的气氛下, 在衬底和 /或催化层上制备二维纳米薄膜。 二维纳米薄膜在第二薄膜制备腔室制备后, 经第三平衡腔室、 化学气相沉积腔室以及出料腔室而传送出二维纳米薄膜制备装置。
制备二维纳米薄膜的基本过程也可以是: 将合成二维纳米薄膜所需的衬底和 /或催化层放置在载料台架上, 并从进料腔室由样品传送装置传送到第一处理腔室; 在一定的气氛环境下, 衬底和 /或催化层在处理腔室进行处 理, 然后通过第一平衡腔室由样品传送装置将衬底和 /或催化层传输到第一薄膜制备腔室; 在第一薄膜制备腔室 里利用物理气相沉积方法或化学气相沉积方法制备二维纳米薄膜生长所需的催化层等;然后经过第二平衡腔室, 由样品传送装置送到第二薄膜制备腔室, 在一定的气氛下, 在衬底和 /或催化层上制备二维纳米薄膜生长所需的 前驱体; 前驱体制备后, 由样品传送装置经第三平衡腔室传送到化学气相沉积腔室制备二维纳米薄膜; 二维纳 米薄膜制备后经出料腔室传送出二维纳米薄膜制备装置。
为了实现对各腔室的设备或工艺的控制, 整套装备还设有控制系统, 所述的控制系统包括样品传送控制系 统、 气路控制系统、 真空控制系统、 阀门控制系统或温度控制系统中的任意一种或二种以上的组合。
本发明的装置适合于所有二维纳米薄膜的规模化连续制备, 所述的二维纳米薄膜包括石墨烯、 金属硫族化 物、 硅烯、 锗烯或氮化硼薄膜等, 依据所制备的二维纳米薄膜的不同, 可以适当选择制备二维纳米薄膜所需的 固体、 液体或气体等。
制备二维薄膜必须满足一定的条件: 比如需要较高的温度如 400° C以上, 必须一定的催化层如制备石墨烯 薄膜是需要如 Ni, Cu等过渡金属作为催化剂及对催化层的晶体结构进行优化,必须控制制备腔室的气氛与真空 度等; 连续化制备二维薄膜的装备必须满足这些条件或者达到这些功能, 是一种一体化的装备。 而现有的工艺 设备不能够满足这些基本条件, 因此不能够用来连续化制备高质量的二维薄膜; 本发明的装备中的各腔室与装 置的组合能够满足连续化制备二维薄膜的不同的工艺技术要求, 能够实现高质量的二维薄膜的连续化制备。
与现有技术相比, 本发明的有益效果是: 整个装备设有可耐高温的样品传送装置, 具有规模化连续制备二 维纳米薄膜的特点, 各个腔室在整个二维纳米薄膜制备过程中承担其独特的功能。 比如: 进料腔室的基本功能 是实现样品装载并进入二维纳米薄膜的制备装置, 处理腔室实现对衬底或催化层的预处理, 薄膜制备腔室可以 用于制备合成二维纳米材料所需的衬底、 催化层、 二维纳米薄膜的前驱体或者二维纳米薄膜, 化学气相沉积腔 室可以用来制备二维纳米薄膜, 平衡腔室在样品传送过程中可以起到过渡、 稳定、 平衡样品的功能。 本发明的 装置可以大面积、 规模化连续制备如石墨烯、 金属硫族化物、 硅烯、 锗烯或氮化硼薄膜等二维纳米薄膜, 适合 于工业化应用, 有助于实现二维纳米薄膜技术的产业化。
附图说明:
图 1是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 第一薄膜制备腔室设有 加热装置;
图 2是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 第一薄膜制备腔室和出 料腔室均设有加热装置, 出料腔室设有热屏蔽系统和冷却系统, 出料腔室设有一个混气盒连接口;
图 3是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有表面处理 器, 第一薄膜制备腔室设有气相沉积系统、 加热装置、 热屏蔽系统和冷却系统, 出料腔室设有加热装置; 图 4是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有表面处理 器和加热装置, 第一薄膜制备腔室设有气相沉积系统、 加热装置、 热屏蔽系统和冷却系统, 出料腔室设有加热 装置;
图 5是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有表面处理 器和加热装置, 第一薄膜制备腔室设有气相沉积系统、 加热装置、 热屏蔽系统和冷却系统, 出料腔室设有表面 处理器、 加热装置和冷却系统。
图 6是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图;
图 7是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有样品处理 装置, 第一薄膜制备腔室设有样品处理装置和冷却系统, 化学气相沉积腔室设有化学气相沉积系统、 隔热屏蔽 系统和冷却系统;
图 8是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有样品处理 装置和隔热屏蔽系统, 第一薄膜制备腔室设有隔热屏蔽系统、 冷却系统、 混气盒连接口和样品处理装置, 化学 气相沉积腔室设有化学气相沉积系统、 隔热屏蔽系统和混气盒连接口。
图 9是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有表面处理 器和加热装置, 第一处理腔室设有加热装置和气体混气盒接口, 第一薄膜制备腔室设有加热装置和隔热屏蔽装 置, 第二处理腔室设有加热装置、 隔热屏蔽装置、 冷却装置和气体混气盒接口;
图 10是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有表面处理 器, 第一处理腔室设有加热装置、 隔热屏蔽装置和冷却装置, 第一薄膜制备腔室设有物理气相沉积系统、 加热
装置和气体混气盒连接口, 第二处理腔室设有加热装置、 隔热屏蔽装置、 冷却装置和气体混气盒连接口, 出了 腔室设有表面处理器;
图 11是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有表面处理 器, 第一处理腔室设有加热装置、 隔热屏蔽装置和冷却装置, 第一薄膜制备腔室设有物理气相沉积系统、 加热 装置、 隔热屏蔽装置、 冷却装置和气体混气盒连接口, 第二处理腔室设有加热装置、 隔热屏蔽装置、 冷却装置 和气体混气盒连接口;
图 12是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有表面处理 器, 第一处理腔室设有加热装置, 第一薄膜制备腔室设有物理气相沉积系统、 加热装置和气体混气盒连接口, 第二处理腔室设有加热装置、 隔热屏蔽装置、 冷却装置和气体混气盒连接口, 出料腔室设有表面处理器; 图 13是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 进料腔室设有表面处理 器, 第一处理腔室设有加热装置, 第一薄膜制备腔室设有物理气相沉积系统、 加热装置、 隔热屏蔽装置、 冷却 装置和气体混气盒连接口, 第二处理腔室设有加热装置和气体混气盒连接口。
图 14是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 第一处理腔室设有加热 装置、 隔热屏蔽系统和冷却系统, 第一薄膜制备腔室设有加热装置和物理气相沉积系统, 第二薄膜制备腔室设 有加热装置和物理气相沉积系统, 化学气相沉积腔室设有样品处理装置、 加热装置、 隔热屏蔽系统、 冷却系统 和气体混气盒接口;
图 15是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 第一处理腔室设有加热 装置和样品处理装置, 第一薄膜制备腔室设有物理气相沉积系统、 加热装置、 隔热屏蔽系统和混气盒连接口, 第二薄膜制备腔室设有加热装置和物理气相沉积系统, 化学气相沉积腔室设有化学气相沉积系统、 加热装置、 隔热屏蔽系统、 冷却系统和混气盒接口;
图 16是本发明的一种规模化连续制备二维纳米薄膜装备的整体结构示意图, 其中, 第一处理腔室设有样品 处理装置, 第一薄膜制备腔室设有物理气相沉积系统和加热装置, 第二薄膜制备腔室设有加热装置、 隔热屏蔽 系统、 冷却系统和物理气相沉积系统, 化学气相沉积腔室设有样品处理装置、 加热装置、 隔热屏蔽系统、 冷却 系统和混气盒接口, 出料腔室设有样品处理装置;
图中所示:
进料腔室 1、 第一处理腔室 2、 第一平衡腔室 3、 第一薄膜制备腔室 4、 第二平衡腔室 5、 第二薄膜制备腔 室 6、 第三平衡腔室 7、 化学气相沉积腔室 8、 第二处理腔室 201、 出料腔室 9;
阀门 10、 11、 12、 13、 14、 15、 16、 17、 18、 19;
抽真空装置 20、 21、 22、 23、 24、 25、 26、 27、 28;
载料台架 29;
样品传送装置 30;
物理气相沉积系统 33、 34、 35、 36;
化学气相沉积系统 38、 39;
加热装置 40、 41、 42、 43、 44;
样品处理装置 50、 51、 52;
气体连接口 60、 61、 62、 63、 64、 65、 66、 67、 68、 69、 70、 71、 72、 73、 74、 75、 76、 78、 79、 80; 混气盒 85、 86、 87;
冷却系统 90、 91、 92;
隔热屏蔽系统 96、 97、 98、 99;
气相沉积系统 101、 102。
具体实施方式
为了更清楚地理解本发明和本发明所产生的技术效果, 下面结合附图对本发明作进一步详细说明。
实施例 1
参见图 1, 本发明的一种规模化连续制备二维纳米薄膜装备包括: 进料腔室 1, 第一薄膜制备腔室 4, 出 料腔室 9; 整套设备在进料腔室 1、 第一薄膜制备腔室 4和出料腔室 9均设有传送样品的滚轮 30; 进料腔室 1 设有与大气相通的阀门 10, 进料腔室 1与第一薄膜制备腔室 4之间设有阀门 11, 第一薄膜制备腔室 4与出料腔 室 9之间设有阀门 12, 出料腔室 9设有与大气相通的阀门 13 ; 通过滚轮与阀门将进料腔室 1、 第一薄膜制备腔 室 4和出料腔室 9连接成一个整体。
第一薄膜制备腔室 4内设有第二加热装置 40。
进料腔室 1设有抽真空装置 20, 第一薄膜制备腔室 4设有抽真空装置 21, 出料腔室 9设有抽真空装置 22。 进料腔室 1设有一个气体连接口 60, 第一薄膜制备腔室 4设有两个气体连接口 61、 62, 出料腔室 9设有一 个气体连接口 63。 为了精确控制气体的流量, 每个气体连接口连有质量流量计而控制各气体的流量, 每个质量 流量计的两端各设有一个电磁截止阀, 电磁截止阀和质量流量计通过管路与气体连接口相连接。
第一薄膜制备腔室 4、 第二加热装置 40和气体连接口 61、 62构成了一个化学气相沉积系统, 这种化学气 相沉积系统一般可称为热化学气相沉积系统。
连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底材料和 /或催化层材料放置在载料台 架 29上, 由滚轮 30经进料腔室 1传输到第一薄膜制备腔室 4, 在第一薄膜制备腔室 4利用化学气相沉积方法 制备二维纳米薄膜, 样品制备后由滚轮 30送到出料腔室 9。
实施例 2
参见图 2, 本发明的一种规模化连续制备二维纳米薄膜装备包括: 进料腔室 1, 第一薄膜制备腔室 4, 出料 腔室 9; 整套设备在进料腔室 1、 第一薄膜制备腔室 4和出料腔室 9均设有传送样品的皮带轮 30; 进料腔室 1 设有与大气相通的阀门 10, 进料腔室 1与第一薄膜制备腔室 4之间设有阀门 11, 第一薄膜制备腔室 4与出料腔 室 9之间设有阀门 12, 出料腔室 9设有与大气相通的阀门 13; 通过皮带轮与阀门将进料腔室 1, 第一薄膜制备 腔室 4和出料腔室 9连接成一个整体。
第一薄膜制备腔室 4内设有第二加热装置 40, 出料腔室 9设有第三加热装置 41。
由于出料腔室 9的腔室的温度可能会高达数百度甚至上千度, 为了提高对热量的利用, 腔室内设有热屏蔽 系统 96、 并且腔壁设有冷却系统 90以防腔壁过热。
进料腔室 1设有抽真空装置 20, 第一薄膜制备腔室 4设有抽真空装置 21, 出料腔室 9设有抽真空装置 22。 进料腔室 1设有一个气体连接口 60, 第一薄膜制备腔室 4设有一个气体连接口 61, 出料腔室 9设有一个 气体连接口 68连接一个混气盒 85, 混气盒 85的入口并联两个气体连接口 66、 67; 每个气体连接口连有质量流 量计而控制各气体的流量, 每个质量流量计的两端各设有一个电磁截止阀, 电磁截止阀和质量流量计通过管路 与混气盒或气体连接口相连接, 从而可以精确控制气体的流量。
出料腔室 9、第三加热装置 41和气体连接口 63以及混气盒 85构成一个化学气相沉积系统,这种化学气相 沉积系统一般可称为热化学气相沉积系统。
连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底材料和 /或催化层材料放置在载料台 架 29上, 由皮带轮 30经进料腔室 1传输到第一薄膜制备腔室 4, 衬底 /催化层在第一薄膜制备腔室 4进行热处 理, 然后由皮带轮 30传送到出料腔室 9, 利用化学气相沉积方法制备二维纳米薄膜, 二维纳米薄膜制备后由皮 带轮样品传送装置传送到出料腔室 9外。
实施例 3
参见图 3, 本发明的一种规模化连续制备二维纳米薄膜装备包括: 进料腔室 1, 第一薄膜制备腔室 4, 出料 腔室 9; 整套设备在进料腔室 1、 第一薄膜制备腔室 4和出料腔室 9均设有传送样品的滚轮 30; 进料腔室 1设 有与大气相通的阀门 10, 进料腔室 1与第一薄膜制备腔室 4之间设有阀门 11, 第一薄膜制备腔室 4与出料腔室 9之间设有阀门 12, 出料腔室 9设有与大气相通的阀门 13; 通过滚轮与阀门将进料腔室 1, 第一薄膜制备腔室 4和出料腔室 9连接成一个整体。
进料腔室 1内设有第一表面处理器 50, 第一薄膜制备腔室 4内设有第二加热装置 40, 出料腔室 9设有第三 加热装置 41。
第一薄膜制备腔室 4设有两个气相沉积系统: 第一气相沉积系统 101和第二气相沉积系统 102, 可以是物理 气相系统和化学气相沉积系统的任意组合。
所述的第一气相沉积系统或第二气相沉积系统为物理气相沉积系统, 包括溅射靶薄膜沉积系统、 电子枪沉积 系统、 离子枪沉积系统、 离子注入沉积系统和热蒸镀系统中的任意一种或二种以上的组合; 第一气相沉积系统 或第二气相沉积系统也可以是化学气相沉积系统, 包括等离子体增强化学气相沉积系统和微波等离子化学气相 沉积系统中的任意一种或二种以上的组合。
由于第一薄膜制备腔室 4的温度可能会高达数百度甚至上千度, 这样为了将热量集中在所需的地方, 并减 少向不需要热的地方传递, 第一薄膜制备腔室内设有热屏蔽系统 96, 同时腔壁设有冷却系统 90, 冷却系统可以 是双层水冷系统。
进料腔室 1设有抽真空装置 20, 第一薄膜制备腔室 4设有抽真空装置 21, 出料腔室 9设有抽真空装置 22。 进料腔室 1设有一个气体连接口 60, 出料腔室 9设有一个气体连接口 63; 第一薄膜制备腔室 4设有两个 气体连接口, 其中一个连接口为 61, 另一个连接口 68与混气盒 85相连, 混气盒 85的入口并联三个气体连接
口 62、 64和 65; 为了精确控制气体的流量, 每个气体连接口连有质量流量计而控制各气体的流量, 每个质量 流量计的两端各设有一个电磁截止阀, 电磁截止阀和质量流量计通过管路与混气盒或气体连接口相连接。
连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底材料放置在载料台架 29 上由滚轮 30传输到进料腔室 1, 在一定的气氛环境下, 衬底材料在进料腔室 1进行预处理, 然后由滚轮 30将衬底材料传 输到第一薄膜制备腔室 4; 在第一薄膜制备腔室 4内的第一气相沉积系统 101 中利用物理气相沉积方法如电子 枪沉积制备催化层, 然后在第二气相沉积系统 102中利用另一种物理气相沉积方法如离子注入法往催化层中注 入二维纳米材料的前驱体, 之后被传送到出料腔室 9; 在出料腔室 9, 对注入有二维纳米材料的前驱体的样品进 行处理而形成二维纳米薄膜。
实施例 4
参见图 4, 本发明的一种规模化连续制备二维纳米薄膜装备包括: 进料腔室 1, 第一薄膜制备腔室 4, 出料 腔室 9; 整套设备在进料腔室 1、 第一薄膜制备腔室 4和出料腔室 9均设有传送样品的滚轮 30; 进料腔室 1设 有与大气相通的阀门 10, 进料腔室 1与第一薄膜制备腔室 4之间设有阀门 11, 第一薄膜制备腔室 4与出料腔室 9之间设有阀门 12, 出料腔室 9设有与大气相通的阀门 13; 通过滚轮与阀门将进料腔室 1, 第一薄膜制备腔室 4和出料腔室 9连接成一个整体。
进料腔室 1内设有第一表面处理器 50和第一加热装置 42, 第一薄膜制备腔室 4内设有第二加热装置 40, 出 料腔室 9设有第三加热装置 41。
第一薄膜制备腔室 4设有第一气相沉积系统 101,所述的第一气相沉积系统为物理气相沉积系统或 /和化学气 相沉积系统, 所述的物理气相沉积系统包括溅射靶薄膜沉积系统、 电子枪沉积系统、 离子枪沉积系统、 离子注 入沉积系统和热蒸镀系统中的任意一种或二种以上的组合; 所述的化学气相沉积系统包括等离子体增强化学气 相沉积系统和微波等离子化学气相沉积系统等; 物理气相沉积系统与化学气相沉积系统可以任意组合。
由于第一薄膜制备腔室 4的温度可能会高达数百度甚至上千度, 这样为了将热量集中在所需的地方, 并减 少向不需要热的地方传递, 第一薄膜制备腔室内设有热屏蔽系统 96, 同时腔壁设有冷却系统 90, 冷却系统可以 是双层水冷系统。
进料腔室 1设有抽真空装置 20, 第一薄膜制备腔室 4设有抽真空装置 21, 出料腔室 9设有抽真空装置 22。 进料腔室 1设有一个气体连接口 60, 出料腔室 9设有一个气体连接口 63, 第一薄膜制备腔室 4设有两个 气体连接口 61、 62, 每个气体连接口连有质量流量计而控制各气体的流量, 每个质量流量计的两端各设有一个 电磁截止阀, 电磁截止阀和质量流量计通过管路与气体连接口相连接。
出料腔室 9、 出料腔室加热装置 41以及气体连接口 63构成化学气相沉积系统。
连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底材料放置在载料台架 29 上由滚轮 30传输到进料腔室 1, 在一定的气氛环境下与温度下, 衬底材料在进料腔室 1进行预处理, 然后由滚轮 30将衬 底材料传输到第一薄膜制备腔室 4; 在第一薄膜制备腔室 4内利用物理气相沉积方法或 /和化学气相沉积方法制 备催化层, 然后传送到出料腔室 9, 在出料腔室 9采用化学气相沉积方法制备二维纳米薄膜。
实施例 5
参见图 5, 本发明的一种规模化连续制备二维纳米薄膜装备包括: 进料腔室 1, 第一薄膜制备腔室 4, 出料 腔室 9; 整套设备在进料腔室 1、 第一薄膜制备腔室 4和出料腔室 9均设有样品传送带 30; 进料腔室 1设有与 大气相通的阀门 10, 进料腔室 1与第一薄膜制备腔室 4之间设有阀门 11, 第一薄膜制备腔室 4与出料腔室 9之 间设有阀门 12, 出料腔室 9设有与大气相通的阀门 13; 通过传送带与阀门将进料腔室 1, 第一薄膜制备腔室 4 和出料腔室 9连接成一个整体。
进料腔室 1内设有第一表面处理器 50和第一加热装置 42, 第一薄膜制备腔室 4内设有第二加热装置 40, 出料腔室 9设有第二表面处理器 51和第三加热装置 41。
第一薄膜制备腔室 4设有第一气相沉积系统 101, 所述的第一气相沉积系统为物理气相沉积系统或 /和化学 气相沉积系统, 所述的物理气相沉积系统包括溅射靶薄膜沉积系统、 电子枪沉积系统、 离子枪沉积系统、 离子 注入沉积系统和热蒸镀系统中的任意一种或二种以上的组合; 所述的化学气相沉积系统包括等离子体增强化学 气相沉积系统和微波等离子化学气相沉积系统等; 物理气相沉积系统与化学气相沉积系统可以任意组合。
第一薄膜制备腔室 4内设有热屏蔽系统 96以减少热量向不需要的地方传递, 腔壁设有冷却系统 90以免腔 壁过热。
由于高温的存在, 出料腔室 9设有冷却系统 90。
进料腔室 1设有抽真空装置 20, 第一薄膜制备腔室 4设有抽真空装置 21, 出料腔室 9设有抽真空装置 22。 进料腔室 1设有一个气体连接口 60, 出料腔室 9设有一个气体连接口 63; 第一薄膜制备腔室 4设有两个
气体连接口, 其中一个连接口为 61, 另一个连接口 68与混气盒 85相连, 混气盒 85的入口并联三个气体连接 口 62、 64和 65; 为了精确控制气体的流量, 每个气体连接口连有质量流量计而控制各气体的流量, 每个质量 流量计的两端各设有一个电磁截止阀, 电磁截止阀和质量流量计通过管路与混气盒或气体连接口相连接。
进料腔室 1、 加热装置 42与气体连接口 60构成化学气相沉积系统; 出料腔室 9、 加热装置 41与气体连接 口 63构成化学气相沉积系统。
连续制备二维纳米薄膜的基本过程是:将合成二维纳米薄膜所需的衬底材料放置在载料台架 29上由传送带 30传输到进料腔室 1, 在一定的气氛环境与温度下, 衬底材料在进料腔室 1进行预处理, 然后由传送带 30将衬 底材料传输到第一薄膜制备腔室 4; 在第一薄膜制备腔室 4内利用物理气相沉积方法或 /和化学气相沉积方法制 备催化层, 然后采用化学气相沉积方法制备二维纳米薄膜; 制备好的二维纳米薄膜被样品传送装置传送到出料 腔室 9, 在出料腔室 9可以对其进行表面处理。
实施例 6
参见图 6, 本发明的一种规模化连续制备二维纳米薄膜装备包括: 进料腔室 1, 第一薄膜制备腔室 4, 第 一平衡腔室 3, 化学气相沉积腔室 8; 整套设备在进料腔室 1、 第一薄膜制备腔室 4、 第一平衡腔室 3和化学气 相沉积腔室 8的各腔室内和腔室之间均设有样品传送装置 30; 所述的样品传送装置包括滚轮、 皮带轮和传送带 中的任意一种或二种以上的组合; 进料腔室 1设有与大气相通的阀门 10, 进料腔室 1与第一薄膜制备腔室 4之 间设有阀门 11, 第一薄膜制备腔室 4与第一平衡腔室 3之间设有阀门 12, 第一平衡腔室 3与化学气相沉积腔室 8之间设有阀门 13, 化学气相沉积腔室 8设有与大气相通的阀门 14; 通过样品传送装置与阀门将进料腔室 1、 第一薄膜制备腔室 4、 第一平衡腔室 3和化学气相沉积腔室 8连接成一个整体。
进料腔室 1设有抽真空装置 21, 第一薄膜制备腔室 4设有抽真空装置 22, 第一平衡腔室 3设有抽真空装置 23, 化学气相沉积腔室 8设有抽真空装置 24; 每一抽真空装置包括各种真空泵、 真空管道、 真空阀门、 真空计 等, 通过抽真空装置可以使各腔室的真空度保持在常压至 1.0x 10— 1Q Pa之间。
第一薄膜制备腔室 4内设有样品处理器装置 51, 样品处理装置可以为等离子体表面处理器、 对气体离子化 的线圏或加热装置等能够实现对样品进行改性的装置, 在本例中样品处理器装置 51为加热装置, 加热装置采用 电阻加热器、 红外加热器和激光加热器等能够实现对样品进行加热的装置; 第一薄膜制备腔室 4内还设有物理 气相沉积系统 33, 所述的物理气相沉积系统包括离子束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉 积系统、 激光沉积系统、 离子注入系统中的任意一种或二种以上的组合。
化学气相沉积腔室 8设有加热装置 40, 加热装置采用电阻加热器、 红外加热器和激光加热器等能够实现对 样品进行加热的装置。
进料腔室 1设有气体连接口 60, 第一薄膜制备腔室 4设有气体连接口 61和 62, 第一平衡腔室 3设有气体 连接口 63, 化学气相沉积腔室 8设有气体连接口 64和 75、 气体连接口 75连接混气盒 85、 混气盒 85连接两个 气体连接口 66和 67; 每一气路都独立设有质量流量计、 电磁截止阀等计量和流量调节装置, 从而精确控制气 体的流量, 比如每一气体连接口联有质量流量计而控制各气体的流量, 每个质量流量计的两端各设有一个电磁 截止阀, 电磁截止阀和质量流量计通过管路与气体连接口相连接。
化学气相沉积腔室 8、 加热装置 40与气体连接口 64和 /或 75构成了一个化学气相沉积系统。
第一薄膜制备腔室 4、 样品处理装置 51与气体连接口 61和 /或 62也可以构成一个化学气相沉积系统。 连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底和 /或放置在载料台架 29上, 由样 品传送装置 30传送到进料腔室 1, 然后传输到第一薄膜制备腔室 4; 在一定的温度下, 在第一薄膜制备腔室 4 利用物理气相沉积系统如电子束沉积系统 33在衬底和 /或催化层上制备催化层, 之后经过第一平衡腔室 3而传 送到化学气相沉积腔室 8; 在化学气相沉积腔室 8采用化学气相沉积系统制备二维纳米薄膜, 二维薄膜制备后, 通过阀门 14传到大气而完成二维薄膜的连续制备的一个流程。
实施例 7
参见图 7, 本发明的一种规模化连续制备二维纳米薄膜装备包括: 进料腔室 1, 第一薄膜制备腔室 4, 第 一平衡腔室 3, 化学气相沉积腔室 8; 整套设备在进料腔室 1、 第一薄膜制备腔室 4、 第一平衡腔室 3和化学气 相沉积腔室 8的各腔室内和腔室之间均设有样品传送装置 30; 所述的样品传送装置包括滚轮、 皮带轮和传送带 中的任意一种或二种以上的组合; 进料腔室 1设有与大气相通的阀门 10, 进料腔室 1与第一薄膜制备腔室 4之 间设有阀门 11, 第一薄膜制备腔室 4与第一平衡腔室 3之间设有阀门 12, 第一平衡腔室 3与化学气相沉积腔室 8之间设有阀门 13, 化学气相沉积腔室 8设有与大气相通的阀门 14; 通过样品传送装置与阀门将进料腔室 1、 第一薄膜制备腔室 4、 第一平衡腔室 3和化学气相沉积腔室 8连接成一个整体。
进料腔室 1设有抽真空装置 21, 第一薄膜制备腔室 4设有抽真空装置 22, 第一平衡腔室 3设有抽真空装置
23, 化学气相沉积腔室 8设有抽真空装置 24; 每一抽真空装置包括各种真空泵、 真空管道、 真空阀门、 真空计 等, 通过抽真空装置可以使各腔室的真空度保持在常压至 1.0x 10— 1Q Pa之间。
进料腔室 1设有样品处理装置 50, 样品处理装置可以为等离子体表面处理器、 气体离子化线圏构成的表面 处理器和加热装置等能够对样品进行改性的装置, 加热装置采用电阻加热器、 红外加热器和激光加热器等能够 对样品进行加热的装置。
第一薄膜制备腔室 4内设有样品处理器装置 51, 样品处理装置可以为等离子体表面处理器、 对气体离子化 的线圏或加热装置等能够对样品进行改性的装置, 在此样品处理器装置 51为加热装置, 加热装置采用电阻加热 器、 红外加热器和激光加热器等能够对样品进行加热的装置; 第一薄膜制备腔室 4内还设有物理气相沉积系统 33和 34, 所述的物理气相沉积系统包括离子束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系统中的任意一种或二种以上的组合; 第一薄膜制备腔室 4内还设有冷却系统 90。
化学气相沉积腔室 8设有加热装置 40, 加热装置采用电阻加热器、 红外加热器和激光加热器等能够对样品 进行加热的装置; 化学气相沉积腔室 8还设有化学气相沉积系统 38, 所述的化学气相沉积系统包括等离子体增 强化学气相沉积系统、 微波等离子体化学气相沉积系统、 气溶胶辅助化学气相沉积系统中的任意一种或二种以 上的组合; 化学气相沉积腔室 8还设有隔热屏蔽系统 96和冷却系统 91, 冷却系统可以是双层水冷系统等。
进料腔室 1设有气体连接口 60, 第一薄膜制备腔室 4设有气体连接口 61和 62, 第一平衡腔室 3设有气体 连接口 63, 化学气相沉积腔室 8设有气体连接口 64和 75、 气体连接口 75连接混气盒 85、 混气盒 85连接两个 气体连接口 66和 67; 每一气路都独立设有质量流量计、 电磁截止阀等计量和流量调节装置, 从而精确控制气 体的流量, 比如每一气体连接口联有质量流量计而控制各气体的流量, 每个质量流量计的两端各设有一个电磁 截止阀, 电磁截止阀和质量流量计通过管路与气体连接口相连接。
除了另设的化学气相沉积系统 38以外, 化学气相沉积腔室 8、 加热装置 40与气体连接口 64和 /或 75也可 以构成一个简单的化学气相沉积系统。
第一薄膜制备腔室 4、 样品处理装置 51与气体连接口 61和 /或 62也可以构成一个化学气相沉积系统。 连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底和 /或催化层放置在载料台架 29上, 由样品传送装置 30传送到进料腔室 1 ; 在进料腔室 1利用样品处理装置 50对样品的表面进行处理, 表面处理 后传输到第一薄膜制备腔室 4; 在一定的温度下, 在第一薄膜制备腔室 4利用物理气相沉积系统如热蒸镀沉积 系统 33在衬底和 /或催化层上制备催化层, 之后采用物理气相沉积系统如离子注入沉积系统 34将制备二维纳米 薄膜所需的前驱体注入到催化层中, 然后经过第一平衡腔室 3而传送到化学气相沉积腔室 8; 在化学气相沉积 腔室 8采用热处理将二维纳米薄膜的前驱体转化为二维纳米薄膜, 二维薄膜制备后, 通过阀门 14传到大气而完 成二维薄膜的连续制备的一个流程。 二维纳米材料的前驱体为含有组成二维纳米材料的元素的化合物, 以合成 石墨烯为例, 前驱体包括无定型碳、 非晶碳膜、 含碳元素的聚合物等; 以合成 MoS2为例, 前驱体包括 MoS2粉 末、 Mo粉末等。
连续制备二维纳米薄膜的基本过程还可以是: 将合成二维纳米薄膜所需的衬底和 /或催化层放置在载料台架 29上, 由样品传送装置 30传送到进料腔室 1 ; 在进料腔室 1利用样品处理装置 50对样品的表面进行处理, 表 面处理后传输到第一薄膜制备腔室 4; 在一定的温度下, 在第一薄膜制备腔室 4利用物理气相沉积系统如激光 沉积系统 33在衬底和 /或催化层上制备催化层, 然后经过第一平衡腔室 3而传送到化学气相沉积腔室 8; 在化学 气相沉积腔室 8采用化学气相沉积系统如微波等离子化学气相沉积技术制备二维纳米薄膜, 二维薄膜制备后, 通过阀门 14传到大气而完成二维薄膜的连续制备的一个流程。
连续制备二维纳米薄膜的基本过程也可以是: 将合成二维纳米薄膜所需的衬底放置在载料台架 29上, 由 样品传送装置 30传送到进料腔室 1 ; 在进料腔室 1利用样品处理装置 50对样品的表面进行处理, 表面处理后 传输到第一薄膜制备腔室 4; 在一定的温度下, 在第一薄膜制备腔室 4利用物理气相沉积系统如溅射沉积系统 33和 34在衬底和 /或催化层上制备催化层, 然后经过第一平衡腔室 3而传送到化学气相沉积腔室 8; 在化学气 相沉积腔室 8采用化学气相沉积系统如气溶胶辅助化学气相沉积技术制备二维纳米薄膜, 二维薄膜制备后, 通 过阀门 14传到大气而完成二维薄膜的连续制备的一个流程。
实施例 8
参见图 8, 本发明的一种规模化连续制备二维纳米薄膜装备包括: 进料腔室 1, 第一薄膜制备腔室 4, 第 一平衡腔室 3, 化学气相沉积腔室 8; 整套设备在进料腔室 1、 第一薄膜制备腔室 4、 第一平衡腔室 3和化学气 相沉积腔室 8的各腔室内和腔室之间均设有样品传送装置 30; 所述的样品传送装置包括滚轮、 皮带轮和传送带 中的任意一种或二种以上的组合; 进料腔室 1设有与大气相通的阀门 10, 进料腔室 1与第一薄膜制备腔室 4之 间设有阀门 11, 第一薄膜制备腔室 4与第一平衡腔室 3之间设有阀门 12, 第一平衡腔室 3与化学气相沉积腔室
8之间设有阀门 13, 化学气相沉积腔室 8设有与大气相通的阀门 14; 通过样品传送装置与阀门将进料腔室 1、 第一薄膜制备腔室 4、 第一平衡腔室 3和化学气相沉积腔室 8连接成一个整体。
进料腔室 1设有抽真空装置 21, 第一薄膜制备腔室 4设有抽真空装置 22, 第一平衡腔室 3设有抽真空装置 23 , 化学气相沉积腔室 8设有抽真空装置 24; 每一抽真空装置包括各种真空泵、 真空管道、 真空阀门、 真空计 等, 通过抽真空装置可以使各腔室的真空度保持在常压至 1.0x 10— 1Q Pa之间。
进料腔室 1设有样品处理装置 50和隔热屏蔽系统 98, 样品处理装置可以为等离子体表面处理器、 气体离 子化线圏表面处理器和加热装置等能够实现对样品进行改性的装置, 加热装置采用电阻加热器、 红外加热器和 激光加热器等能够实现对样品进行加热的装置。
第一薄膜制备腔室 4内设有样品处理器装置 51, 样品处理装置可以为等离子体表面处理器、 对气体离子化 的线圏或加热装置等能够实现对样品进行改性的装置, 在此样品处理器装置 51为加热装置, 加热装置采用电阻 加热器、 红外加热器和激光加热器等能够实现对样品进行加热的装置; 第一薄膜制备腔室 4内设有物理气相沉 积系统 33和 34, 所述的物理气相沉积系统包括离子束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉 积系统、 激光沉积系统、 离子注入系统中的任意一种或二种以上的组合; 第一薄膜制备腔室 4内设有冷却系统 90和隔热屏蔽系统 97。
化学气相沉积腔室 8设有加热装置 40, 加热装置采用电阻加热器、 红外加热器和激光加热器等能够实现对 样品进行加热的装置; 化学气相沉积腔室 8内设有化学气相沉积系统 38和 39, 所述的化学气相沉积系统包括 离子增强化学气相沉积系统、 微波等离子体化学气相沉积系统、 气溶胶辅助化学气相沉积系统中的任意一种或 二种以上的组合; 化学气相沉积腔室 8内设有隔热屏蔽系统 96。
进料腔室 1设有气体连接口 60, 第一薄膜制备腔室 4设有气体连接口 61和 76、 76连接混气盒 86、 混气盒 86连接两个气体连接口 69和 70, 第一平衡腔室 3设有气体连接口 63, 化学气相沉积腔室 8设有气体连接口 64 和 75、 气体连接口 75连接混气盒 85、 混气盒 85连接三个气体连接口 66、 67和 68 ; 每一气路都独立设有质量 流量计、 电磁截止阀等计量和流量调节装置, 从而精确控制气体的流量, 比如每一气体连接口联有质量流量计 而控制各气体的流量, 每个质量流量计的两端各设有一个电磁截止阀, 电磁截止阀和质量流量计通过管路与气 体连接口相连接。
化学气相沉积腔室 8、 加热装置 40与气体连接口 64和 /或 75也可以构成一个化学气相沉积系统。
第一薄膜制备腔室 4、 样品处理装置 51与气体连接口 61和 /或 76也可以构成一个化学气相沉积系统。 连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底放置在载料台架 29上, 由样品传送 装置 30传送到进料腔室 1 ; 在进料腔室 1利用样品处理装置 50对样品的表面进行处理, 表面处理后传输到第 一薄膜制备腔室 4; 在一定的温度下, 在第一薄膜制备腔室 4利用物理沉积系统如热蒸镀沉积系统 33在衬底上 制备第一种催化层, 之后采用物理沉积系统如溅射沉积系统 34制备第二种催化层, 然后经过第一平衡腔室 3而 传送到化学气相沉积腔室 8; 在化学气相沉积腔室 8采用化学气相沉积系统 38和 39制备二维纳米薄膜, 二维 薄膜制备后, 通过阀门 14传到大气而完成二维薄膜的连续制备的一个流程。 在此实施例中, 第一种催化层和第 二种催化层也可以同时沉积而达到共混。
连续制备二维纳米薄膜的基本过程还可以是: 将合成二维纳米薄膜所需的衬底和 /或放置在载料台架 29上, 由样品传送装置 30传送到进料腔室 1 ; 在进料腔室 1利用样品处理装置 50对样品的表面进行处理, 表面处理 后传输到第一薄膜制备腔室 4; 在一定的温度下, 在第一薄膜制备腔室 4利用物理沉积系统如激光沉积系统 33 在衬底和 /或催化层上制备催化层, 然后采用物理沉积系统如离子束沉积系统 34将合成二维纳米薄膜所需的前 驱体沉积在催化层上; 沉积后, 经过第一平衡腔室 3而传送到化学气相沉积腔室 8, 在一定的环境下, 在化学 气相沉积腔室 8将二维纳米薄膜的前驱体转化为二维纳米薄膜, 二维薄膜制备后, 通过阀门 14传到大气而完成 二维薄膜的连续制备的一个流程。 二维纳米材料的前驱体为含有组成二维纳米材料的元素的化合物, 以合成石 墨烯为例, 前驱体包括甲烷、 乙烯、 乙醇等含碳元素的聚合物等。
连续制备二维纳米薄膜的基本过程也可以是: 将合成二维纳米薄膜所需的衬底放置在载料台架 29上, 由 样品传送装置 30传送到进料腔室 1 ; 在进料腔室 1利用样品处理装置 50对样品的表面进行处理, 表面处理后 传输到第一薄膜制备腔室 4; 在一定的温度下, 在第一薄膜制备腔室 4利用物理沉积系统如溅射沉积系统 33和 34在衬底和 /或催化层上制备催化层, 然后经过第一平衡腔室 3而传送到化学气相沉积腔室 8 ; 在化学气相沉积 腔室 8采用化学气相沉积系统如气溶胶辅助化学气相沉积技术制备二维纳米薄膜, 二维薄膜制备后, 通过阀门 14传到大气而完成二维薄膜的连续制备的一个流程。
实施例 9
参见图 9, 本发明的一种规模化连续制备二维纳米薄膜装备包括在生产线上依次设置有进料腔室 1, 第一处
理腔室 2, 第一平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9; 进料腔 室 1设有与大气相通的阀门 10, 进料腔室 1与第一处理腔室 2之间设有阀门 11, 第一处理腔室 2与第一平衡腔 室 3之间设有阀门 12, 第一平衡腔室 3与第一薄膜制备腔室 4之间设有阀门 13, 第一薄膜制备腔室 4与第二平 衡腔室 5之间设有阀门 14, 第二平衡腔室 5与第二处理腔室 201之间设有阀门 15, 第二处理腔室 201与出料腔 室 9之间设有阀门 16, 出料腔室 9设有与大气相通的阀门 17; 整套设备在进料腔室 1, 第一处理腔室 2, 第一 平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9均设有传送样品的滚轮传 送装置 30; 整套设备通过滚轮传送装置与阀门将进料腔室 1, 第一处理腔室 2, 第一平衡腔室 3, 第一薄膜制备 腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9连接成一个整体。
进料腔室 1设有抽真空装置 21, 第一处理腔室 2设有抽真空装置 22, 第一平衡腔室 3设有抽真空装置 23, 第一薄膜制备腔室 4设有抽真空装置 24, 第二平衡腔室 5设有抽真空装置 25, 第二处理腔室 201设有抽真空装 置 26, 出料腔室 9设有抽真空装置 27。
进料腔室 1设有气体连接口 61, 第一处理腔室 2设有两个气体连接口 62和 80、气体连接口 80连接混气盒 86、 混气盒 86连接两个气体连接口 76和 77, 第一平衡腔室 3设有气体连接口 64, 第一薄膜制备腔室 4设有气 体连接口 78, 第二平衡腔室 5设有气体连接口 68, 第二处理腔室 201设有两个气体连接口 69和 79、 气体连接 口 79连接混气盒 85、 混气盒 85连接三个气体连接口 71、 72和 73, 出料腔室 9设有气体连接口 74; 每一气路 都可以精确控制气体的流量, 为此包括质量流量计和电磁截止阀等, 每一气体连接口联有质量流量计而控制个 气体的流量, 每个质量流量计的两端各设有一个电磁截止阀, 电磁截止阀和质量流量计通过管路与气体连接口 相连接。
进料腔室 1设有表面处理器 50和加热装置 40, 第一处理腔室 2设有加热装置 41, 第一薄膜制备腔室 4设 有加热装置 42和隔热屏蔽装置 97,第二处理腔室 201设有加热装置 43和 44、冷却装置 90和隔热屏蔽装置 96。
第一处理腔室 2、 加热装置 41与气体连接口 62和 /或 80构成了一个化学气相沉积系统。
第一薄膜制备腔室 4、 加热装置 42与气体连接口 78构成了一个化学气相沉积系统。
第二处理腔室 201、 加热装置 43和 /或 44、 与气体连接口 69和 /或 79构成了一个化学气相沉积系统。 连续制备二维纳米薄膜的基本过程是: 将制备二维纳米薄膜所需的衬底材料 /催化层放置在载料台架 29上, 由滚轮传送装置 30传送到经进料腔室 1 ; 在一定的温度下, 衬底材料 /催化层在进料腔室 1 内采用表面处理器 50进行表面处理, 之后经过第一处理腔室 2和第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在一定的气氛环 境下, 衬底 /催化层在第一薄膜制备腔室 4进行热处理, 之后经第二平衡腔室 5被传送到第二处理腔室 201 ; 于 第二处理腔室 201采用微波等离子化学气相沉积系统在衬底 /催化层上制备二维纳米薄膜, 二维纳米薄膜制备后 经出料腔室 9被传送出设备, 完成二维纳米薄膜的制备。
实施例 10
参见图 10, 本发明的一种规模化连续制备二维纳米薄膜装备包括在生产线上依次设置有进料腔室 1, 第一 处理腔室 2, 第一平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9; 进料 腔室 1设有与大气相通的阀门 10, 进料腔室 1与第一处理腔室 2之间设有阀门 11, 第一处理腔室 2与第一平衡 腔室 3之间设有阀门 12, 第一平衡腔室 3与第一薄膜制备腔室 4之间设有阀门 13, 第一薄膜制备腔室 4与第二 平衡腔室 5之间设有阀门 14, 第二平衡腔室 5与第二处理腔室 201之间设有阀门 15, 第二处理腔室 201与出料 腔室 9之间设有阀门 16, 出料腔室 9设有与大气相通的阀门 17; 整套设备在进料腔室 1, 第一处理腔室 2, 第 一平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9均设有传送样品的滚轮 传送装置 30; 整套设备通过滚轮传送装置与阀门将进料腔室 1, 第一处理腔室 2, 第一平衡腔室 3, 第一薄膜制 备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9连接成一个整体。
进料腔室 1设有抽真空装置 21, 第一处理腔室 2设有抽真空装置 22, 第一平衡腔室 3设有抽真空装置 23, 第一薄膜制备腔室 4设有抽真空装置 24, 第二平衡腔室 5设有抽真空装置 25, 第二处理腔室 201设有抽真空装 置 26, 出料腔室 9设有抽真空装置 27。
进料腔室 1设有气体连接口 61, 第一处理腔室 2设有两个气体连接口 62和 63, 第一平衡腔室 3设有气体 连接口 64, 第一薄膜制备腔室 4设有气体连接口 80、 气体连接口 80连接混气盒 86、 混气盒 86连接两个气体 连接口 66和 67, 第二平衡腔室 5设有气体连接口 68, 第二处理腔室 201设有两个气体连接口 69和 79、 气体 连接口 79连接混气盒 85、 混气盒 85连接三个气体连接口 71、 72和 73, 出料腔室 9设有两个气体连接口 74和 75; 气体连接口连接气路, 每一气路都可以精确控制气体的流量, 为此包括质量流量计和电磁截止阀等, 每一 气体连接口联有质量流量计而控制个气体的流量, 每个质量流量计的两端各设有一个电磁截止阀, 电磁截止阀 和质量流量计通过管路与气体连接口相连接。
进料腔室 1设有表面处理器 50, 第一处理腔室 2设有加热装置 41、 冷却装置 91和隔热屏蔽装置 98, 第一 薄膜制备腔室 4设有加热装置 42和物理气相沉积系统 33和 34, 第二处理腔室 201设有加热装置 43和 44、 冷 却装置 90和隔热屏蔽装置 96, 出料腔室 9设有表面处理器 51。
第一处理腔室 2、 加热装置 41与气体连接口 62和 /或 63构成了一个化学气相沉积系统。
第一薄膜制备腔室 4、 加热装置 42与气体连接口 80构成了一个化学气相沉积系统。
第二处理腔室 201、 加热装置 43和 /或 44、 与气体连接口 69和 /或 79构成了一个化学气相沉积系统。 所述的物理气相沉积系统包括溅射靶薄膜沉积系统、 电子枪沉积系统、 离子枪沉积系统、 离子注入沉积系 统和热蒸镀系统中的任意一种或二种以上的组合; 化学气相沉积系统, 包括等离子体增强化学气相沉积系统、 气溶胶辅助化学气相沉积系统和微波等离子化学气相沉积系统等。
连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底材料放置在载料台架 29上, 由滚轮 传送装置 30传送到经进料腔室 1 ; 衬底材料在进料腔室 1 内采用表面处理器 50进行表面处理, 之后被传送到 第一处理腔室 2进行热处理, 然后经第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在一定的气氛环境和温度 下, 采用物理气相沉积系统如溅射靶薄膜沉积系统 33和 34在衬底表面制备催化层薄膜; 催化层制备后, 经第 二平衡腔室 5被传送到第二处理腔室 201 ; 于第二处理腔室 201采用等离子增强化学气相沉积系统在衬底 /催化 层上制备二维纳米薄膜, 二维纳米薄膜制备后经出料腔室 9被传送出设备, 完成二维纳米薄膜的制备。
实施例 11
参见图 11, 本发明的一种规模化连续制备二维纳米薄膜装备包括在生产线上依次设置有进料腔室 1, 第一 处理腔室 2, 第一平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9; 进料 腔室 1设有与大气相通的阀门 10, 进料腔室 1与第一处理腔室 2之间设有阀门 11, 第一处理腔室 2与第一平衡 腔室 3之间设有阀门 12, 第一平衡腔室 3与第一薄膜制备腔室 4之间设有阀门 13, 第一薄膜制备腔室 4与第二 平衡腔室 5之间设有阀门 14, 第二平衡腔室 5与第二处理腔室 201之间设有阀门 15, 第二处理腔室 201与出料 腔室 9之间设有阀门 16, 出料腔室 9设有与大气相通的阀门 17; 整套设备在进料腔室 1, 第一处理腔室 2, 第 一平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9均设有传送样品的滚轮 传送装置 30; 整套设备通过滚轮传送装置与阀门将进料腔室 1, 第一处理腔室 2, 第一平衡腔室 3, 第一薄膜制 备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9连接成一个整体。
进料腔室 1设有抽真空装置 21, 第一处理腔室 2设有抽真空装置 22, 第一平衡腔室 3设有抽真空装置 23, 第一薄膜制备腔室 4设有抽真空装置 24, 第二平衡腔室 5设有抽真空装置 25, 第二处理腔室 201设有抽真空装 置 26, 出料腔室 9设有抽真空装置 27。
进料腔室 1设有气体连接口 61, 第一处理腔室 2设有气体连接口 62, 第一平衡腔室 3设有气体连接口 64, 第一薄膜制备腔室 4设有两个气体连接口 80和 78、 气体连接口 80连接混气盒 86、 混气盒 86连接两个气体连 接口 66和 67, 第二平衡腔室 5设有气体连接口 68, 第二处理腔室 201设有两个气体连接口 69和 79、 气体连 接口 79连接混气盒 85、 混气盒 85连接两个气体连接口 71和 72, 出料腔室 9设有气体连接口 74; 气体连接口 连接气路, 每一气路都可以精确控制气体的流量, 为此包括质量流量计和电磁截止阀等, 每一气体连接口联有 质量流量计而控制个气体的流量, 每个质量流量计的两端各设有一个电磁截止阀, 电磁截止阀和质量流量计通 过管路与气体连接口相连接。
进料腔室 1设有表面处理器 50, 第一处理腔室 2设有加热装置 41、 冷却装置 91和隔热屏蔽装置 98, 第一 薄膜制备腔室 4设有加热装置 42和物理气相沉积系统 33和 34、 冷却装置 92和隔热屏蔽装置 97, 第二处理腔 室 201设有加热装置 43、 冷却装置 90和隔热屏蔽装置 96。
第一处理腔室 2、 加热装置 41与气体连接口 62构成了一个化学气相沉积系统。
第一薄膜制备腔室 4、 加热装置 42与气体连接口 80和 /或 78构成了一个化学气相沉积系统。
第二处理腔室 201、 加热装置 43、 与气体连接口 69和 /或 79构成了一个化学气相沉积系统。
所述的物理气相沉积系统包括溅射靶薄膜沉积系统、 电子枪沉积系统、 离子枪沉积系统、 离子注入沉积系 统和热蒸镀系统中的任意一种或二种以上的组合; 化学气相沉积系统, 包括等离子体增强化学气相沉积系统、 气溶胶辅助化学气相沉积系统和微波等离子化学气相沉积系统等。
连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底材料放置在载料台架 29上, 由滚轮 传送装置 30传送到经进料腔室 1 ; 衬底材料在进料腔室 1 内采用表面处理器 50进行表面处理, 之后被传送到 第一处理腔室 2进行热处理, 然后经第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在一定的气氛环境和温度 下, 采用物理气相沉积系统如电子枪沉积系统 33在衬底上制备催化层, 然后再采用物理气相沉积系统如离子注 入器 34将二维纳米材料的前驱体注入到催化层, 之后, 经第二平衡腔室 5被传送到第二处理腔室 201 ; 于第二
处理腔室 201对在催化层中注入有二维纳米材料的前驱体的样品进行处理, 热处理后, 将样品传送到出料腔室 9进行冷却而完成二维纳米薄膜的制备。
实施例 12
参见图 12, 本发明的一种规模化连续制备二维纳米薄膜装备包括在生产线上依次设置有进料腔室 1, 第一 处理腔室 2, 第一平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9; 进料 腔室 1设有与大气相通的阀门 10, 进料腔室 1与第一处理腔室 2之间设有阀门 11, 第一处理腔室 2与第一平衡 腔室 3之间设有阀门 12, 第一平衡腔室 3与第一薄膜制备腔室 4之间设有阀门 13, 第一薄膜制备腔室 4与第二 平衡腔室 5之间设有阀门 14, 第二平衡腔室 5与第二处理腔室 201之间设有阀门 15, 第二处理腔室 201与出料 腔室 9之间设有阀门 16, 出料腔室 9设有与大气相通的阀门 17; 整套设备在进料腔室 1, 第一处理腔室 2, 第 一平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9均设有传送样品的传送 带传送装置 30; 整套设备通过传送带传送装置与阀门将进料腔室 1, 第一处理腔室 2, 第一平衡腔室 3, 第一薄 膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9连接成一个整体。
进料腔室 1设有抽真空装置 21, 第一处理腔室 2设有抽真空装置 22, 第一平衡腔室 3设有抽真空装置 23, 第一薄膜制备腔室 4设有抽真空装置 24, 第二平衡腔室 5设有抽真空装置 25, 第二处理腔室 201设有抽真空装 置 26, 出料腔室 9设有抽真空装置 27。
进料腔室 1设有气体连接口 61, 第一处理腔室 2设有两个气体连接口 62和 63, 第一平衡腔室 3设有气体 连接口 64, 第一薄膜制备腔室 4设有气体连接口 80、 气体连接口 80连接有混气盒 86、 混气盒 86设有两个气 体连接口 66和 67, 第二平衡腔室 5设有气体连接口 68, 第二处理腔室 201设有两个气体连接口 69和 79、 气 体连接口 79连接混气盒 85、 混气盒 85连接三个气体连接口 71、 72和 73, 出料腔室 9设有气体连接口 74; 每 一气路都可以精确控制气体的流量, 为此包括质量流量计和电磁截止阀等, 每一气体连接口联有质量流量计而 控制个气体的流量, 每个质量流量计的两端各设有一个电磁截止阀, 电磁截止阀和质量流量计通过管路与气体 连接口相连接。
进料腔室 1设有表面处理器 50, 第一处理腔室 2设有加热装置 41, 第一薄膜制备腔室 4设有物理气相沉积 系统 33和加热装置 42, 第二处理腔室 201设有加热装置 43和 44、 冷却装置 90和隔热屏蔽装置 96, 出料腔室 9设有表面处理器 51。
第一处理腔室 2、 加热装置 41与气体连接口 62和 /或 63构成了一个化学气相沉积系统。
第一薄膜制备腔室 4、 加热装置 42与气体连接口 80构成了一个化学气相沉积系统。
第二处理腔室 201、 加热装置 43和 /或 44、 与气体连接口 69和 /或 79构成了一个化学气相沉积系统。 所述的物理气相沉积系统包括溅射靶薄膜沉积系统、 电子枪沉积系统、 离子枪沉积系统、 离子注入器沉积 系统和热蒸镀系统中的任意一种或二种以上的组合; 化学气相沉积系统, 包括等离子体增强化学气相沉积系统、 气溶胶辅助化学气相沉积系统和微波等离子化学气相沉积系统等。
连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底材料放置在载料台架 29上, 由传送 带传送装置 30传送到进料腔室 1 ; 衬底材料在进料腔室 1 内采用表面处理器 50进行表面处理, 之后经过第一 处理腔室 2和第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在一定的气氛环境下, 衬底在第一薄膜制备腔室 4 进行热处理, 之后经第二平衡腔室 5被传送到第二处理腔室 201 ; 于第二处理腔室 201采用化学气相沉积系统 在衬底上制备二维纳米薄膜, 二维纳米薄膜制备后被传送带出料腔室 9; 在出料腔室 9, 再对制备的二维纳米薄 膜进行表面改性处理, 处理后被传送出设备, 完成二维纳米薄膜的制备。
实施例 13
参见图 13, 本发明的一种规模化连续制备二维纳米薄膜装备包括在生产线上依次设置有进料腔室 1, 第一 处理腔室 2, 第一平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9; 进料 腔室 1设有与大气相通的阀门 10, 进料腔室 1与第一处理腔室 2之间设有阀门 11, 第一处理腔室 2与第一平衡 腔室 3之间设有阀门 12, 第一平衡腔室 3与第一薄膜制备腔室 4之间设有阀门 13, 第一薄膜制备腔室 4与第二 平衡腔室 5之间设有阀门 14, 第二平衡腔室 5与第二处理腔室 201之间设有阀门 15, 第二处理腔室 201与出料 腔室 9之间设有阀门 16, 出料腔室 9设有与大气相通的阀门 17; 整套设备在进料腔室 1, 第一平衡腔室 3, 第 二平衡腔室 5和出料腔室 9均设有传送样品的皮带轮传送装置 30; 第一处理腔室 2, 第一薄膜制备腔室 4和第 二处理腔室 201设有滚轮传送装置 30; 整套设备通过样品传送装置与阀门将进料腔室 1, 第一处理腔室 2, 第 一平衡腔室 3, 第一薄膜制备腔室 4, 第二平衡腔室 5, 第二处理腔室 201和出料腔室 9连接成一个整体。
进料腔室 1设有抽真空装置 21, 第一处理腔室 2设有抽真空装置 22, 第一平衡腔室 3设有抽真空装置 23, 第一薄膜制备腔室 4设有抽真空装置 24, 第二平衡腔室 5设有抽真空装置 25, 第二处理腔室 201设有抽真空装
置 26, 出料腔室 9设有抽真空装置 27。
进料腔室 1设有气体连接口 61, 第一处理腔室 2设有气体连接口 62和 63, 第一平衡腔室 3设有气体连接 口 64, 第一薄膜制备腔室 4设有两个气体连接口 80和 78、 气体连接口 80连接混气盒 86、 混气盒 86连接两个 气体连接口 66和 67, 第二平衡腔室 5设有气体连接口 68, 第二处理腔室 201设有两个气体连接口 69和 79、 气体连接口 79连接混气盒 85、混气盒 85连接两个气体连接口 71和 72, 出料腔室 9设有两个气体连接口 74和 75; 每一气路都可以精确控制气体的流量, 为此包括质量流量计和电磁截止阀等, 每一气体连接口联有质量流 量计而控制个气体的流量, 每个质量流量计的两端各设有一个电磁截止阀, 电磁截止阀和质量流量计通过管路 与气体连接口相连接。
进料腔室 1设有表面处理器 50, 第一处理腔室 2设有加热装置 41, 第一薄膜制备腔室 4设有加热装置 42 和物理气相沉积系统 33和 34、 冷却装置 92和隔热屏蔽装置 97, 第二处理腔室 201设有加热装置 44。
第一处理腔室 2、 加热装置 41、 与气体连接口 62和 /或 63构成了一个化学气相沉积系统。
第一薄膜制备腔室 4、 加热装置 42、 与气体连接口 80和 /或 78构成了一个化学气相沉积系统。
第二处理腔室 201、 加热装置 44、 与气体连接口 69和 /或 79构成了一个化学气相沉积系统。
所述的物理气相沉积系统包括溅射靶薄膜沉积系统、 电子枪沉积系统、 离子枪沉积系统、 离子注入沉积系 统和热蒸镀系统中的任意一种或二种以上的组合; 化学气相沉积系统, 包括等离子体增强化学气相沉积系统、 气溶胶辅助化学气相沉积系统和微波等离子化学气相沉积系统等。
连续制备二维纳米薄膜的基本过程是: 将合成二维纳米薄膜所需的衬底材料放置在载料台架 29上, 由传皮 带轮传送装置 30传送到经进料腔室 1 ; 衬底材料在进料腔室 1 内采用表面处理器 50进行表面处理, 之后被传 送到第一处理腔室 2进行热处理, 热处理后, 由滚轮传送装置 30传送到第一平衡腔室 3, 之后, 经第一平衡腔 室 3被传送到第一薄膜制备腔室 4; 在一定的气氛环境和温度下, 采用物理气相沉积系统如热蒸镀系统 33在衬 底上制备催化层, 然后再采用物理气相沉积系统如离子枪沉积系统 34 将二维纳米材料的前驱体离化在催化层 上, 之后, 经第二平衡腔室 5被传送到第二处理腔室 201 ; 于第二处理腔室 201对在催化层上沉积有二维纳米 材料的前驱体的样品进行处理, 热处理后, 将样品传送到出料腔室 9进行冷却而完成二维纳米薄膜的制备。 实施例 14
参见图 14, 本发明的一种规模化连续制备二维纳米薄膜装备依次设有进料腔室 1, 第一处理腔室 2, 第一 平衡腔室 3, 第一薄膜制备腔室 4、 第二平衡腔室 5、 第二薄膜制备腔室 6、 第三平衡腔室 7、 化学气相沉积腔 室 8和出料腔室 9; 进料腔室 1设有与大气相通的阀门 10, 进料腔室 1与第一处理腔室 2之间设有阀门 11, 第 一处理腔室 2与第一平衡腔室 3之间设有阀门 12, 第一平衡腔室 3与第一薄膜制备腔室 4之间设有阀门 13, 第 一薄膜制备腔室 4与第二平衡腔室 5之间设有阀门 14,第二平衡腔室 5与第二薄膜制备腔室 6之间设有阀门 15, 第二薄膜制备腔室 6与第三平衡腔室 7之间设有阀门 16, 第三平衡腔室 7与化学气相沉积腔室 8之间设有阀门 17, 化学气相沉积腔室 8与出料腔室 9之间设有阀门 18, 出料腔室 9设有与大气相通的阀门 19; 整套设备在进 料腔室 1、 第一处理腔室 2、 第一平衡腔室 3、 第一薄膜制备腔室 4、 第二平衡腔室 5、 第二薄膜制备腔室 6、 第 三平衡腔室 7、 化学气相沉积腔室 8和出料腔室 9的腔室内均设有传送样品送装置 30; 所述的样品传送装置 30 包括滚轮、 皮带轮和传送带等中的任意一种或二种以上的组合; 整套设备通过样品传送装置与阀门将进料腔室 1、 第一处理腔室 2、 第一平衡腔室 3, 第一薄膜制备腔室 4、 第二平衡腔室 5、 第二薄膜制备腔室 6、 第三平衡 腔室 7、 化学气相沉积腔室 8和出料腔室 9连接成一个整体。
第一处理腔室 2设有加热装置 40, 加热装置可以是电阻加热装置、 红外加热装置、 激光加热装置等, 温度 可以在 20〜2000°C之间调节; 还设有隔热屏蔽系统 96和冷却系统 90。
第一处理腔室 2、 加热装置 40与气体连接口 61或 62可以构成一个热化学气相沉积系统。
第一薄膜制备腔室 4设有物理气相沉积系统 33和加热装置 41 ; 物理气相沉积系统包括离子束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系统中的任意一种或二种以上的 组合; 加热装置可以是电阻加热装置、 红外加热装置、 激光加热装置等, 温度可以在 20〜2000°C之间调节。 第 一薄膜制备腔室 4、 加热装置 41和气体连接口 64可以构成一个热化学气相沉积系统。
第二薄膜制备腔室 6设有物理气相沉积系统 34和加热装置 42; 物理气相沉积系统包括离子束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系统中的任意一种或二种以上的 组合; 加热装置可以是电阻加热装置、 红外加热装置、 激光加热装置等, 温度可以在 20〜2000°C之间调节。 第 二薄膜制备腔室 6、 加热装置 42和气体连接口 66可以构成一个热化学气相沉积系统。
化学气相沉积腔室 8设有样品处理装置 51、 加热装置 43、 冷却系统 91和隔热屏蔽系统 97; 所述的样品处 理装置 51可以为等离子样品处理装置、对气体离子化的线圏或加热装置等能够实现对样品进行改性的装置, 所
述的对气体离子化的线圏可在真空高频条件下实现气体的离子化; 加热装置可以是电阻加热装置、 红外加热装 置、 激光加热装置等, 温度可以在 20〜2000°C之间调节。
进料腔室 1设有气体连接口 60, 第一处理腔室 2设有两个气体连接口 61和 62, 第一平衡腔室 3设有气体 连接口 63, 第一薄膜制备腔室 4设有气体连接口 64, 第二平衡腔室 5设有气体连接口 65, 第二薄膜制备腔室 6 设有气体连接口 66, 第三平衡腔室 7设有气体连接口 67, 化学气相沉积腔室设有气体连接口 68和 69、 气体连 接口 69连接混气盒 87、 混气盒 87连接三个气体连接口 76、 77和 78, 出料腔室连接有两个气体连接口 70和 71; 每一气路都可以精确控制气体的流量, 可包括质量流量计和电磁截止阀等计量和流量调节装置, 每一气体 连接口联有质量流量计而控制各气体的流量, 每个质量流量计的两端各设有一个电磁截止阀, 电磁截止阀和质 量流量计通过管路与气体连接口相连接。
化学气相沉积腔室 8、 加热装置 43与气体连接口 68和 /或 69可以构成一个热化学气相沉积系统。
化学气相沉积腔室 8还可以设有等离子体增强化学气相沉积系统、 微波等离子体化学气相沉积系统、 气溶 胶辅助化学气相沉积系统、 电感耦合等离子体化学气相沉积系统中的任意一种或二种以上的组合。
进料腔室 1设有抽真空装置 20, 第一处理腔室 2设有抽真空装置 21, 第一平衡腔室 3设有抽真空装置 22, 第一薄膜制备腔室 4设有抽真空装置 23, 第二平衡腔室 5设有抽真空装置 24, 第二薄膜制备腔室 6设有抽真空 装置 25, 第三平衡腔室 7设有抽真空装置 26, 化学气相沉积腔室 8设有抽真空装置 27, 出料腔室 9设有抽真 空装置 28。 每一独立的抽真空装置包括各种真空泵、 真空管道、 真空阀门、 真空计等, 通过抽真空装置可以使 各腔室的真空度在常压至 1.0x l0—1Q Pa之间。
规模化连续制备二维纳米薄膜的基本过程可以是: 将制备二维纳米薄膜所需的衬底 /催化层放置在载料台架 29上, 由样品传送装置 30传送经过进料腔室 1到达第一处理腔室 2; 衬底 /催化层在第一处理腔室 2内采用加 热装置 40进行热处理, 之后经过第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在第一薄膜制备腔室 4利用物 理气相沉积系统 33如溅射沉积系统将二维纳米薄膜的前驱体 (precursor)沉积在衬底 /催化层上, 然后由样品传送 装置 30经第二平衡腔室 5、 第二薄膜沉积腔室 6和第三平衡腔室 7传送到化学气相沉积腔室 8; 在化学气相沉 积腔室 8内于一定的气氛环境下, 采用化学气相沉积系统将二维纳米材料的前驱体转化为二维纳米薄膜; 最后, 制备的二维纳米薄膜经由出料腔室 9传送出制备装置, 从而完成二维纳米薄膜的连续制备。
二维纳米材料的前驱体是指含有组成二维纳米材料的元素或含有组成二维纳米材料的元素的化合物, 以制 备石墨烯为例, 前驱体包括无定型碳、 非晶碳膜、 含碳元素的聚合物等; 以制备 MoS2为例, 前驱体包括 MoS2 靶材、 Mo靶材等。
规模化连续制备二维纳米薄膜的基本过程也可以是: 将制备二维纳米薄膜所需的衬底 /催化层放置在载料台 架 29上, 由样品传送装置 30传送经过进料腔室 1到达第一处理腔室 2·' 衬底 /催化层在第一处理腔室 2内采用 加热装置 40进行热处理后, 由样品传送装置 30经第二平衡腔室 5、 第二薄膜沉积腔室 6和第三平衡腔室 7传 送到化学气相沉积腔室 8 ; 在化学气相沉积腔室 8 内采用化学气相沉积系统制备二维纳米薄膜; 最后, 制备的 二维纳米薄膜经由出料腔室 9传送出制备装置, 从而完成二维纳米薄膜的连续制备。
实施例 15
参见图 15, 本发明的一种规模化连续制备二维纳米薄膜装备依次设有进料腔室 1, 第一处理腔室 2, 第一 平衡腔室 3, 第一薄膜制备腔室 4、 第二平衡腔室 5、 第二薄膜制备腔室 6、 第三平衡腔室 7、 化学气相沉积腔 室 8和出料腔室 9; 进料腔室 1设有与大气相通的阀门 10, 进料腔室 1与第一处理腔室 2之间设有阀门 11, 第 一处理腔室 2与第一平衡腔室 3之间设有阀门 12, 第一平衡腔室 3与第一薄膜制备腔室 4之间设有阀门 13, 第 一薄膜制备腔室 4与第二平衡腔室 5之间设有阀门 14,第二平衡腔室 5与第二薄膜制备腔室 6之间设有阀门 15, 第二薄膜制备腔室 6与第三平衡腔室 7之间设有阀门 16, 第三平衡腔室 7与化学气相沉积腔室 8之间设有阀门 17, 化学气相沉积腔室 8与出料腔室 9之间设有阀门 18, 出料腔室 9设有与大气相通的阀门 19; 整套设备在进 料腔室 1、 第一处理腔室 2、 第一平衡腔室 3、 第一薄膜制备腔室 4、 第二平衡腔室 5、 第二薄膜制备腔室 6、 第 三平衡腔室 7、化学气相沉积腔室 8和出料腔室 9的腔室内均设有样品传送装置 30; 所述的样品传送装置 30包 括滚轮、 皮带轮和传送带等中的任意一种或二种以上的组合; 整套设备通过样品传送装置与阀门将进料腔室 1、 第一处理腔室 2、 第一平衡腔室 3, 第一薄膜制备腔室 4、 第二平衡腔室 5、 第二薄膜制备腔室 6、 第三平衡腔 室 7、 化学气相沉积腔室 8和出料腔室 9连接成一个整体。
第一处理腔室 2设有样品处理装置 50和加热装置 40; 样品处理装置可以是等离子处理器、 对气体离子化 的线圏和加热装置等; 加热装置可以是电阻加热装置、 红外加热装置、 激光加热装置等, 温度可以在 20〜2000 °C之间调节。
第一处理腔室 2、 加热装置 40与气体连接口 61或 62可以构成一个热化学气相沉积系统。
第一薄膜制备腔室 4设有物理气相沉积系统 33和 35、加热装置 41和隔热屏蔽系统 98; 所述的物理气相沉 积系统包括离子束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系 统中的任意一种或二种以上的组合; 加热装置 41可以是电阻加热装置、 红外加热装置、 激光加热装置等, 温度 可以在 20〜2000°C之间调节。 第一薄膜制备腔室 4、 加热装置 41和气体连接口 64可以构成一个热化学气相沉 积系统。
第二薄膜制备腔室 6设有物理气相沉积系统装置 34和加热装置 42; 物理气相沉积系统 34包括离子束沉积 系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系统中的任意一种或二种 以上的组合; 加热装置 42可以是电阻加热装置、 红外加热装置、 激光加热装置等, 温度可以在 20〜2000°C之 间调节。 第二薄膜制备腔室 6、 加热装置 42和气体连接口 66可以构成一个热化学气相沉积系统。
化学气相沉积腔室 8设有化学气相沉积系统 38、 加热装置 43、 冷却系统 91和隔热屏蔽系统 97; 所述的化 学气相沉积系统 38包括等离子体增强化学气相沉积系统、微波等离子体化学气相沉积系统、气溶胶辅助化学气 相沉积系统、 电感耦合等离子体化学气相沉积系统中的任意一种或二种以上的组合。
出料腔室 9设有样品处理装置 52, 样品处理装置可以是等离子处理器、 对气体离化的线圏和加热装置等。 进料腔室 1设有气体连接口 60, 第一处理腔室 2设有两个气体连接口 61和 62, 第一平衡腔室 3设有气体 连接口 63, 第一薄膜制备腔室 4设有气体连接口 64、 气体连接口 64连接混气盒 85、 混气盒 85连接两个气体 连接口 72和 73, 第二平衡腔室 5设有气体连接口 65, 第二薄膜制备腔室 6设有气体连接口 66、 气体连接口 66 连接混气盒 86、 混气盒 86连接两个气体连接口 74和 75, 第三平衡腔室 7设有气体连接口 67, 化学气相沉积 腔室设有气体连接口 68和 69、 气体连接口 69连接混气盒 87、 混气盒 87连接三个气体连接口 76、 77和 78, 出料腔室连接有两个气体连接口 70和 71 ; 每一气路都可以精确控制气体的流量, 可包括质量流量计和电磁截 止阀等计量和流量调节装置, 每一气体连接口联有质量流量计而控制各气体的流量, 每个质量流量计的两端各 设有一个电磁截止阀, 电磁截止阀和质量流量计通过管路与气体连接口相连接。
化学气相沉积腔室 8、 加热装置 43与气体连接口 68和 /或 69可以构成一个化学气相沉积系统。
进料腔室 1设有抽真空装置 20, 第一处理腔室 2设有抽真空装置 21, 第一平衡腔室 3设有抽真空装置 22, 第一薄膜制备腔室 4设有抽真空装置 23, 第二平衡腔室 5设有抽真空装置 24, 第二薄膜制备腔室 6设有抽真空 装置 25, 第三平衡腔室 7设有抽真空装置 26, 化学气相沉积腔室 8设有抽真空装置 27, 出料腔室 9设有抽真 空装置 28。 每一独立的抽真空装置包括各种真空泵、 真空管道、 真空阀门、 真空计等, 通过抽真空装置可以使 各腔室的真空度在常压至 1.0x 10- 1Q Pa之间。
规模化连续制备二维纳米薄膜的基本过程可以是: 将制备二维纳米薄膜所需的衬底放置在载料台架 29上, 衬底由样品传送装置 30传送经过进料腔室 1到达第一处理腔室 2; 在一定温度下, 衬底在第一处理腔室 2内进 行预处理, 之后经过第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在第一薄膜制备腔室 4利用物理气相沉积 系统 33和 35如电子束沉积系统将催化层制备在衬底上, 然后经过第二平衡腔室 5, 被传送到第二薄膜沉积腔 室 6; 在第二薄膜制备腔室 6, 利用物理气相沉积系统 34如离子束沉积系统将二维纳米薄膜的前驱体离化在催 化层上, 然后经过第三平衡腔室 7, 被传送到化学气相沉积腔室 8; 在化学气相沉积腔室 8, 对样品进行处理而 形成二维纳米薄膜; 最后, 制备的二维纳米薄膜经由出料腔室 9传送出制备装置, 从而完成二维纳米薄膜的连 续制备。
二维纳米材料的前驱体是指含有组成二维纳米材料的元素或含有组成二维纳米材料的元素的化合物, 以制 备石墨烯为例, 前驱体包括甲烷、 乙醇等; 以制备 MoS2为例, 前驱体包括 H2S等。
规模化连续制备二维纳米薄膜的基本过程也可以是: 将制备二维纳米薄膜所需的衬底放置在载料台架 29 上, 衬底由样品传送装置 30传送经过进料腔室 1到达第一处理腔室 2; 在一定温度下, 衬底在第一处理腔室 2 内进行预处理, 之后经过第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在第一薄膜制备腔室 4分别利用物理 气相沉积系统 33和 35如电子束沉积系统和溅射沉积系统将两种不同的催化层材料同时沉积在衬底上, 然后经 过第二平衡腔室 5, 被传送到第二薄膜沉积腔室 6; 在第二薄膜制备腔室 6, 利用物理气相沉积系统 34如热蒸 镀沉积系统将二维纳米薄膜的前驱体沉积到催化层上,然后经过第三平衡腔室 7,被传送到化学气相沉积腔室 8; 在化学气相沉积腔室 8, 对样品进行处理而形成二维纳米薄膜; 最后, 制备的二维纳米薄膜经由出料腔室 9传 送出制备装置, 从而完成二维纳米薄膜的连续制备。
二维纳米材料的前驱体是指含有组成二维纳米材料的元素或含有组成二维纳米材料的元素的化合物, 以制 备石墨烯为例, 前驱体包括石墨粉、 炭黑等; 以制备 MoS2为例, 前驱体包括 MoS2粉等。
规模化连续制备二维纳米薄膜的基本过程还可以是: 将制备二维纳米薄膜所需的衬底放置在载料台架 29 上, 衬底由样品传送装置 30传送经过进料腔室 1到达第一处理腔室 2; 在一定温度下, 衬底在第一处理腔室 2
内进行预处理, 之后经过第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在第一薄膜制备腔室 4利用物理气相 沉积系统 33和 35 如电子束沉积系统在衬底上制备第一种催化层, 然后经过第二平衡腔室 5, 被传送到第二薄 膜沉积腔室 6; 在第二薄膜制备腔室 6, 利用物理气相沉积系统 34如溅射沉积系统将第二种催化层沉积在第一 种催化层之上, 然后经过第三平衡腔室 7, 被传送到化学气相沉积腔室 8; 在化学气相沉积腔室 8, 利用化学气 相沉积系统 38如等离子增强化学气相沉积系统在催化层上制备二维纳米薄膜; 最后, 制备的二维纳米薄膜经由 出料腔室 9传送出制备装置, 从而完成二维纳米薄膜的连续制备。
规模化连续制备二维纳米薄膜的基本过程还可以是: 将制备二维纳米薄膜所需的衬底 /催化层放置在载料台 架 29上, 由样品传送装置 30传送先后经过进料腔室 1、 第一处理腔室 2和第一平衡腔室 3到达第一薄膜制备 腔室 4; 在第一薄膜制备腔室 4对衬底 /催化层进行表面处理, 然后经过第二平衡腔室 5、 第二薄膜沉积腔室 6 和第三平衡腔室 7, 由样品传送装置 30传送到化学气相沉积腔室 8; 在化学气相沉积腔室 8, 利用化学气相沉 积系统 38如微波等离子化学气相沉积系统制备二维纳米薄膜; 最后, 制备的二维纳米薄膜经由出料腔室 9传到 大气, 从而完成二维纳米薄膜的连续制备。
实施例 16
参见图 16, 本发明的一种规模化连续制备二维纳米薄膜装备依次设有进料腔室 1, 第一处理腔室 2, 第一 平衡腔室 3, 第一薄膜制备腔室 4、 第二平衡腔室 5、 第二薄膜制备腔室 6、 第三平衡腔室 7、 化学气相沉积腔 室 8和出料腔室 9; 进料腔室 1设有与大气相通的阀门 10, 进料腔室 1与处理腔室 2之间设有阀门 11, 第一处 理腔室 2与第一平衡腔室 3之间设有阀门 12, 第一平衡腔室 3与第一薄膜制备腔室 4之间设有阀门 13, 第一薄 膜制备腔室 4与第二平衡腔室 5之间设有阀门 14, 第二平衡腔室 5与第二薄膜制备腔室 6之间设有阀门 15, 第 二薄膜制备腔室 6与第三平衡腔室 7之间设有阀门 16,第三平衡腔室 7与化学气相沉积腔室 8之间设有阀门 17, 化学气相沉积腔室 8与出料腔室 9之间设有阀门 18, 出料腔室 9设有与大气相通的阀门 19; 整套设备在进料腔 室 1、 第一处理腔室 2、 第一平衡腔室 3、 第一薄膜制备腔室 4、 第二平衡腔室 5、 第二薄膜制备腔室 6、 第三平 衡腔室 7、化学气相沉积腔室 8和出料腔室 9的腔室内均设有样品传送装置 30; 所述的样品传送装置 30包括滚 轮、 皮带轮和传送带等中的任意一种或二种以上的组合; 整套设备通过样品传送装置与阀门将进料腔室 1、 第 一处理腔室 2、第一平衡腔室 3, 第一薄膜制备腔室 4、第二平衡腔室 5、第二薄膜制备腔室 6、第三平衡腔室 7、 化学气相沉积腔室 8和出料腔室 9连接成一个整体。
第一处理腔室 2设有样品处理装置 50; 样品处理装置可以是等离子处理器、 对气体离子化的线圏和加热装 置等。
第一处理腔室 2、 样品处理装置 50与气体连接口 61或 62可以构成一个热化学气相沉积系统。
第一薄膜制备腔室 4设有物理气相沉积系统装置 33和加热装置 41 ; 物理气相沉积系统包括离子束沉积系 统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系统中的任意一种或二种以 上的组合; 加热装置可以是电阻加热装置、 红外加热装置、激光加热装置等, 温度可以在 20〜2000°C之间调节。 第一薄膜制备腔室 4、 加热装置 41和气体连接口 64可以构成一个热化学气相沉积系统。
第二薄膜制备腔室 6设有物理气相沉积系统装置 34和 36、 加热装置 42、 冷却系统 92和隔热屏蔽系统 99; 物理气相沉积系统包括离子束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系统中的任意一种或二种以上的组合; 加热装置可以是电阻加热装置、 红外加热装置、 激光加热装置 等, 温度可以在 20〜2000°C之间调节。 第二薄膜制备腔室 6、 加热装置 42和气体连接口 74或 75可以构成一个 热化学气相沉积系统。
化学气相沉积腔室 8设有样品处理装置 51、 加热装置 43、 冷却系统 91和隔热屏蔽系统 97; 化学气相沉积 腔室 8、 加热装置 43和气体连接口 68或 69构成一个热化学气相沉积系统; 化学气相沉积腔室 8还可以设有等 离子体增强化学气相沉积系统、 微波等离子体化学气相沉积系统、 气溶胶辅助化学气相沉积系统、 电感耦合等 离子体化学气相沉积系统中的任意一种或二种以上的组合。
出料腔室 9设有样品处理装置 52,样品处理装置可以是等离子处理器、对气体离子化的线圏和加热装置等。 进料腔室 1设有气体连接口 60, 第一处理腔室 2设有两个气体连接口 61和 62, 第一平衡腔室 3设有气体 连接口 63, 第一薄膜制备腔室 4设有气体连接口 64, 第二平衡腔室 5设有气体连接口 65, 第二薄膜制备腔室 6 设有气体连接口 74和 75, 第三平衡腔室 7设有气体连接口 67, 化学气相沉积腔室设有气体连接口 68和 69、 气体连接口 69连接混气盒 87、 混气盒 87连接三个气体连接口 76、 77和 78, 出料腔室连接有两个气体连接口 70和 71 ; 每一气路都可以精确控制气体的流量, 可包括质量流量计和电磁截止阀等计量和流量调节装置, 每一 气体连接口联有质量流量计而控制各气体的流量, 每个质量流量计的两端各设有一个电磁截止阀, 电磁截止阀 和质量流量计通过管路与气体连接口相连接。
化学气相沉积腔室 8、 加热装置 43与气体连接口 68和 /或 69可以构成一个化学气相沉积系统。 进料腔室 1设有抽真空装置 20, 第一处理腔室 2设有抽真空装置 21, 第一平衡腔室 3设有抽真空装置 22, 第一薄膜制备腔室 4设有抽真空装置 23, 第二平衡腔室 5设有抽真空装置 24, 第二薄膜制备腔室 6设有抽真空 装置 25, 第三平衡腔室 7设有抽真空装置 26, 化学气相沉积腔室 8设有抽真空装置 27, 出料腔室 9设有抽真 空装置 28。 每一独立的抽真空装置包括各种真空泵、 真空管道、 真空阀门、 真空计等, 通过抽真空装置可以使 各腔室的真空度在常压至 1.0x l0—1Q Pa之间。
规模化连续制备二维纳米薄膜的基本过程可以是: 将制备二维纳米薄膜所需的衬底放置在载料台架 29上, 经过进料腔室 1, 衬底传送到达第一处理腔室 2; 衬底在第一处理腔室 2内进行预处理, 之后经过第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在第一薄膜制备腔室 4利用物理气相沉积系统 33如电子束沉积系统将催化层 制备在衬底上, 然后经过第二平衡腔室 5, 被传送到第二薄膜沉积腔室 6; 在第二薄膜制备腔室 6, 利用物理气 相沉积系统 34和 36如溅射沉积系统将二维纳米薄膜的前驱体沉积在催化层上, 然后经过第三平衡腔室 7, 被 传送到化学气相沉积腔室 8; 在化学气相沉积腔室 8, 采用化学气相沉积方法制备二维纳米薄膜; 最后, 制备的 二维纳米薄膜经由出料腔室 9传送出制备装置, 从而完成二维纳米薄膜的连续制备。
二维纳米材料的前驱体是指含有组成二维纳米材料的元素或含有组成二维纳米材料的元素的化合物, 以制 备石墨烯为例, 前驱体包括石墨粉、 炭黑等; 以制备 MoS2为例, 前驱体包括 MoS2粉等。
规模化连续制备二维纳米薄膜的基本过程也可以是: 将制备二维纳米薄膜所需的衬底和 /或催化层放置在载 料台架 29上, 经过进料腔室 1, 衬底和 /或催化层传送到达第一处理腔室 2; 衬底和 /或催化层在第一处理腔室 2 内进行预处理, 之后经过第一平衡腔室 3被传送到第一薄膜制备腔室 4; 在第一薄膜制备腔室 4利用物理气相 沉积系统 33 如电子束沉积系统将二维纳米材料的一种前驱体沉积在衬底和 /或催化层上, 然后经过第二平衡腔 室 5, 被传送到第二薄膜沉积腔室 6; 在第二薄膜制备腔室 6, 利用物理气相沉积系统 34和 36如热蒸镀沉积系 统将另一种二维纳米薄膜的前驱体沉积到衬底和 /或催化层上, 然后经过第三平衡腔室 7, 被传送到化学气相沉 积腔室 8; 在化学气相沉积腔室 8, 对样品进行处理而形成二维纳米薄膜; 最后, 制备的二维纳米薄膜经由出料 腔室 9传送出制备装置, 从而完成二维纳米薄膜的连续制备。
二维纳米材料的前驱体是指含有组成二维纳米材料的元素或含有组成二维纳米材料的元素的化合物, 以制 备石墨烯为例, 前驱体包括石墨粉、 炭黑等; 以制备 MoS2为例, 前驱体包括 MoS2粉等。
规模化连续制备二维纳米薄膜的基本过程还可以是: 将制备二维纳米薄膜所需的衬底和 /或催化层放置在载 料台架 29上, 经过进料腔室 1, 衬底和 /或催化层传送到达第一处理腔室 2; 衬底和 /或催化层在第一处理腔室 2 内进行预处理, 之后先后经过第一平衡腔室 3、 第一薄膜制备腔室 4、 第二平衡腔室 5, 被传送到第二薄膜沉积 腔室 6; 在第二薄膜制备腔室 6, 利用物理气相沉积系统 34和 36如离子注入沉积系统将二维纳米薄膜的前驱体 沉积注入到衬底和 /或催化层中, 然后经过第三平衡腔室 7, 被传送到化学气相沉积腔室 8; 在化学气相沉积腔 室 8, 对样品进行处理而形成二维纳米薄膜; 最后, 制备的二维纳米薄膜经由出料腔室 9传到大气, 从而完成 二维纳米薄膜的连续制备。
二维纳米材料的前驱体是指含有组成二维纳米材料的元素或含有组成二维纳米材料的元素的化合物, 以制 备石墨烯为例, 前驱体包括石墨粉、 炭黑等; 以制备 MoS2为例, 前驱体包括 MoS2粉等。
虽然已经明确展示且参考本发明的示范性实施例描述了本发明, 但所属领域的技术人员将了解, 可在不脱 离有所附权利要求书界定的本发明的精神和范围的情况下, 对本文作各种形式上和细节上的改变。
Claims
1. 规模化连续制备二维纳米薄膜的装备, 包括进料腔室 、 第一薄膜制备腔室和出料腔室, 其特征 在于:
所述的进料腔室、 第一薄膜制备腔室和出料腔室均设有样品传送装置;
所述的进料腔室设有与大气相通的阀门, 进料腔室与第一薄膜制备腔室之间设有阀门, 第 一薄膜制备腔室与出料腔室之间设有阀门, 出料腔室设有与大气相通的阀门;
所述的进料腔室、 第一薄膜制备腔室和出料腔室中至少有一个腔室设有加热装置; 所述的进料腔室、 第一薄膜制备腔室和出料腔室分别连接独立的抽真空装置; 所述的进料腔室、 第一薄膜制备腔室和出料腔室中的至少一个腔室设有一个或多个气体连 接口。
2. 根据权利要求 1所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的进料腔室、 第一薄膜制备腔室和出料腔室中的至少一个腔室设有化学气相沉积系统。
3. 根据权利要求 1所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的进料腔室、 第一薄膜制备腔室和出料腔室中的至少一个腔室设有物理气相沉积系统。
4. 根据权利要求 1所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的进料腔室、 第一薄膜制制备腔室和出料腔室中的至少一个腔室的温度控制在 20〜1600°C。
5. 规模化连续制备二维纳米薄膜的装备, 包括进料腔室、 第一薄膜制备腔室、 第一平衡腔室和化 学气相沉积腔室, 其特征在于:
所述的进料腔室、 第一薄膜制备腔室、 第一平衡腔室和化学气相沉积腔室均设有样品传送 装置;
所述的进料腔室设有与大气相通的阀门, 进料腔室与第一薄膜制备腔室之间设有阀门, 第 一薄膜制备腔室与第一平衡腔室之间设有阀门, 第一平衡腔室与化学气相沉积腔室之间设有阀 门, 化学气相沉积腔室设有与大气相通的阀门;
所述的第一薄膜制备腔室设有物理气相沉积系统;
所述的化学气相沉积腔室设有加热装置和气体连接口;
所述的进料腔室、 第一薄膜制备腔室、 第一平衡腔室、 化学气相沉积腔室均设有抽真空装 置。
6. 根据权利要求 5所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的进料腔室、 第一薄膜制备腔室和第一平衡腔室中的至少一个腔室设有气体连接口。
7. 根据权利要求 5所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的进料腔室和 第一薄膜制备腔室中的至少一个腔室设有样品处理装置。
8. 规模化连续制备二维纳米薄膜的装备, 包括在生产线上依次设置有进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二处理腔室和出料腔室, 其特征在于: 进料腔室设有与大气相通的阀门, 进料腔室与第一处理腔室之间设有阀门, 第一处理腔室 与第一平衡腔室之间设有阀门, 第一平衡腔室与第一薄膜制备腔室之间设有阀门, 第一薄膜制 备腔室与第二平衡腔室之间设有阀门, 第二平衡腔室与第二处理腔室之间设有阀门, 第二处理 腔室与出料腔室之间设有阀门, 出料腔室设有与大气相通的阀门;
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二处理 腔室和出料腔室均设有样品传送装置;
进料腔室、 第一处理腔室、 第一薄膜制备腔室、 第二处理腔室和出料腔室中的至少一个腔 室设有加热装置;
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二处理 腔室和出料腔室中的至少一个腔室设有一个或多个气体连接口;
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二处理 腔室和出料腔室分别连接独立的抽真空装置。
9. 根据权利要求 8所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的第一处理腔 室、 第一薄膜制备腔室和第二处理腔室中的至少一个腔室设有化学气相沉积系统。
10. 根据权利要求 8所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的第一处理腔 室、 第一薄膜制备腔室和第二处理腔室中的至少一个腔室设有物理气相沉积系统。
11. 规模化连续制备二维纳米薄膜的装备, 其特征在于: 依次设有进料腔室、 第一处理腔室、 第一 平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二薄膜制备腔室、 第三平衡腔室、 化学气相 沉积腔室和出料腔室, 其中:
进料腔室设有与大气相通的阀门,进料腔室与第一处理腔室之间设有阀门,第一处理腔室与 第一平衡腔室之间设有阀门, 第一平衡腔室与第一薄膜制备腔室 之间设有阀门, 第一薄膜制备 腔室与第二平衡腔室之间设有阀门, 第二平衡腔室 与第二薄膜制备腔室之间设有阀门, 第二薄 膜制备腔室与第三平衡腔室之间设有阀门, 第三平衡腔室与化学气相沉积腔室之间设有阀门, 化学气相沉积腔室与出料腔室之间设有阀门, 出料腔室设有与大气相通的阀门;
进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二薄膜 制备腔室、 第三平衡腔室、 化学气相沉积腔室和出料腔室的腔室内均设有样品传送装置; 进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二薄膜 制备腔室、 第三平衡腔室、 化学气相沉积腔室和出料腔室中的至少一个的腔室设有抽真空装置; 第一薄膜制备腔室和第二薄膜制备腔室的至少一个的腔室内设有物理气相沉积系统; 进料腔室、 第一处理腔室、 第一平衡腔室、 第一薄膜制备腔室、 第二平衡腔室、 第二薄膜制备 腔室、 第三平衡腔室、 化学气相沉积腔室和出料腔室中的至少一个腔室设有一个或二个以上的 气体连接口;
化学气相沉积腔室的腔室内设有加热装置。
12. 根据权利要求 11所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的第一处理腔 室、 第一薄膜制备腔室和第二薄膜制备腔室中的至少一个腔室内设有加热装置。
13. 根据权利要求 11所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的第一处理腔 室内设有样品处理装置。
14. 根据权利要求 5或 11所述的规模化连续制备二维纳米薄膜的装备,所述的化学气相沉积腔室中 还设有等离子体增强化学气相沉积系统、 微波等离子体化学气相沉积系统、 气溶胶辅助化学气 相沉积系统、 电感耦合等离子体化学气相沉积系统中的任意一种或二种以上的组合。
15. 根据权利要求 3、 5、 10或 11所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述 的物理气相沉积系统包括离子束沉积系统、 溅射沉积系统、 电子束沉积系统、 热蒸镀沉积系统、 激光沉积系统、 离子注入系统中的任意一种或二种以上的组合。
16. 根据权利要求 1-15任一项所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 组成所述 装备的各腔室中的至少一个腔室的腔壁设有冷却系统; 作为优选, 所述的进料腔室、 第一处理 腔室、 第一薄膜制备腔室、 第二薄膜制备腔室、 第三平衡腔室、 化学气相沉积腔室中的至少一 个腔室的腔壁设有冷却系统。
17. 根据权利要求 1-15任一项所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 组成所述 装备的各腔室中的的至少一个腔室内设有热屏蔽系统; 作为优选, 所述的所述的进料腔室、 第 一处理腔室、 第一薄膜制备腔室、 第二薄膜制备腔室、 第三平衡腔室、 化学气相沉积腔室中的 至少一个腔室内设有热屏蔽系统。
18. 根据权利要求 1-15任一项所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的装 备还设有控制系统, 所述的控制系统包括样品传送控制系统、 气路控制系统、 真空控制系统、 阀门控制系统或温度控制系统中的任意一种或二种以上的组合。
19. 根据权利要求 1-15任一项所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的样 品传送装置包括滚轮、 传送带和皮带轮中的任意一种或二种以上的组合。
20. 根据权利要求 1-15任一项所述的规模化连续制备二维纳米薄膜的装备, 其特征在于: 所述的二 维纳米薄膜包括石墨烯、 金属硫族化合物、 硅稀、 锗稀或氮化硼。
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CN114703466A (zh) * | 2022-02-07 | 2022-07-05 | 常州第六元素半导体有限公司 | 连续式cvd薄膜制造设备及方法 |
CN114703466B (zh) * | 2022-02-07 | 2024-04-09 | 常州第六元素半导体有限公司 | 连续式cvd薄膜制造设备及方法 |
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