CN115992346B - Multifunctional ion deposition film preparation device and film deposition method - Google Patents
Multifunctional ion deposition film preparation device and film deposition method Download PDFInfo
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- CN115992346B CN115992346B CN202310121914.2A CN202310121914A CN115992346B CN 115992346 B CN115992346 B CN 115992346B CN 202310121914 A CN202310121914 A CN 202310121914A CN 115992346 B CN115992346 B CN 115992346B
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- 230000007246 mechanism Effects 0.000 claims abstract description 161
- 239000010408 film Substances 0.000 claims abstract description 110
- 150000002500 ions Chemical class 0.000 claims abstract description 88
- 239000010409 thin film Substances 0.000 claims abstract description 26
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 25
- 238000001451 molecular beam epitaxy Methods 0.000 claims abstract description 24
- 238000012216 screening Methods 0.000 claims abstract description 6
- 238000002207 thermal evaporation Methods 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 28
- 238000002347 injection Methods 0.000 claims description 20
- 239000007924 injection Substances 0.000 claims description 20
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
本发明实施例公开了一种多功能的离子沉积薄膜制备装置及薄膜沉积方法，包括薄膜生长机构，进样承载机构，离子源提供机构、分子束外延机构和化学气相沉积机构；进样承载机构用于向薄膜生长机构中提供样品；离子源提供机构提供经过筛分后的待沉积离子，用于离子沉积；分子束外延机构产生分子束流，用于分子束外延生长；化学气相沉积机构产生气态物质，用于化学气相沉积。通过离子源提供机构、分子束外延机构和化学气相沉积机构的协同配合，一次操作过程中可完成分子束外延、化学气相沉积、离子沉积等多种薄膜制备功能，实现电中性分子和带电离子的共沉积，可用于氧化物、氮化物、硒化物以及金刚石等薄膜材料及其异质结的原位制备，提高制备效率。
The embodiment of the present invention discloses a multifunctional ion deposition film preparation device and a film deposition method, including a film growth mechanism, a sample feeding and carrying mechanism, an ion source providing mechanism, a molecular beam epitaxy mechanism and a chemical vapor deposition mechanism; the sample feeding and carrying mechanism is used to provide samples to the film growth mechanism; the ion source providing mechanism provides ions to be deposited after screening for ion deposition; the molecular beam epitaxy mechanism generates a molecular beam for molecular beam epitaxy growth; and the chemical vapor deposition mechanism generates a gaseous substance for chemical vapor deposition. Through the coordinated cooperation of the ion source providing mechanism, the molecular beam epitaxy mechanism and the chemical vapor deposition mechanism, multiple film preparation functions such as molecular beam epitaxy, chemical vapor deposition, and ion deposition can be completed in one operation, and the co-deposition of electrically neutral molecules and charged ions can be achieved. It can be used for the in-situ preparation of thin film materials such as oxides, nitrides, selenides, and diamonds and their heterojunctions, thereby improving the preparation efficiency.
Description
Technical Field
The embodiment of the invention relates to the technical field of film preparation, in particular to a multifunctional ion deposition film preparation device and a film deposition method.
Background
Thin film growth technology is an important technology in semiconductor manufacturing processes. The existing film growth methods mainly comprise chemical vapor deposition, molecular beam epitaxy, physical vapor deposition and the like. Along with the development of the electronic industry, development of novel electronic devices requires construction of various films with specific structures, and high-precision control of chemical proportions on the surfaces of the films, such as film preparation operations of oxidation, nitridation, selenization and the like. In order to achieve these thin film preparation operations more efficiently, ion and atom deposition are required in some cases, which requires that the thin film growth apparatus can achieve co-deposition of electrically neutral molecules and charged ions, but the existing apparatus generally has only one function of molecular beam epitaxy or chemical vapor deposition, and cannot achieve the above functions. In addition, existing thin film growth equipment cannot effectively screen out target ions when ion deposition is performed, and non-target ions are often deposited on a sample to cause pollution. Therefore, the requirement of precursor isotope-level purity of certain materials in the preparation process cannot be met, so that the growth of the film materials is limited. In view of this, it is a need to improve ion sources and design a set of multifunctional ion deposition thin film manufacturing apparatus.
Disclosure of Invention
Therefore, the embodiment of the invention provides a multifunctional ion deposition film preparation device and a film deposition method, which can finish various film preparation functions such as molecular beam epitaxy, chemical vapor deposition, ion deposition and the like in one operation process by the cooperative cooperation of an ion source providing mechanism, a molecular beam epitaxy mechanism and a chemical vapor deposition mechanism, and effectively realize the co-deposition of neutral molecules and charged ions. The method can be used for in-situ preparation of oxide, nitride, selenide, diamond and other film materials and heterojunctions thereof, greatly simplifies the preparation process and improves the preparation efficiency.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions:
In one aspect of the embodiment of the invention, a multifunctional ion deposition film preparation device is provided, which comprises a film growth mechanism, a sample loading bearing mechanism capable of being connected with the film growth mechanism in an open or closed mode, an ion source providing mechanism, a molecular beam epitaxy mechanism and a chemical vapor deposition mechanism, wherein the ion source providing mechanism, the molecular beam epitaxy mechanism and the chemical vapor deposition mechanism are connected to the film growth mechanism in a communicating mode; wherein,
The sample injection bearing mechanism can be at least partially positioned in the film growth mechanism and is used for providing a sample into the film growth mechanism;
the ion source providing mechanism provides screened ions to be deposited for ion deposition of a sample to the film growing mechanism;
the molecular beam epitaxy mechanism generates molecular beam current for molecular beam epitaxy growth of the sample;
the chemical vapor deposition mechanism generates gaseous substances for chemical vapor deposition of a sample.
As a preferable mode of the invention, the film growth mechanism is formed into a double-layer cavity, and the cavity comprises a preparation cavity and an interlayer which are sequentially arranged from inside to outside; wherein,
The preparation cavity is used for depositing a film;
And the interlayer is communicated with a cooling medium supply structure.
As a preferable scheme of the invention, the sample injection bearing mechanism comprises a sample injection structure and a sample bearing heating structure which are respectively communicated with the film growth mechanism;
the sample injection structure comprises an injection cavity which is connected with the film growth mechanism in an opening or closing way through a gate valve, and a magnetic sample transmission rod which is arranged in the injection cavity and can extend into the film growth mechanism;
The sample bearing heating structure comprises a sample heating table which can be extended and positioned in the film growing mechanism, and the sample heating table is used for bearing a sample and controlling the placing position and the temperature of the sample;
The magnetic force sample transmission rod can transmit a sample to the sample heating table.
As a preferred embodiment of the present invention, the molecular beam epitaxy mechanism includes at least one thermal evaporation source, each of which is selected from a K-cell evaporation source or an electron beam evaporation source.
As a preferred embodiment of the present invention, the element types of the molecular beam generated by each of the thermal evaporation sources are not exactly the same.
As a preferred embodiment of the present invention, the element of each of the molecular beams is at least one selected from Se, V and Te.
As a preferred scheme of the invention, the ion source providing mechanism comprises a CF three-way cavity and a mass spectrometer which are sequentially communicated with the film growing mechanism, and the mass spectrometer is also respectively and communicably connected with an ion source and an ion beam focusing structure;
The mass spectrometer is used for screening ions provided by the ion body source.
As a preferred embodiment of the present invention, the chemical vapor deposition mechanism includes at least one gas supply unit connected to the thin film growth mechanism.
As a preferable mode of the present invention, the ion source providing mechanism further includes a rotary introducer connected to the film growing mechanism, and the rotary introducer and the mass spectrometer are both connected to the film growing mechanism through a reducing flange.
As a preferable scheme of the invention, the film growing mechanism, the sample loading bearing mechanism and the ion source providing mechanism are also communicated with a vacuum providing system;
The ion source providing mechanism and the chemical vapor deposition mechanism at least further comprise a high purity gas source;
the vacuum providing system is used for adjusting and monitoring the vacuum degree of the film growing mechanism, the sample loading mechanism and the ion source providing mechanism;
The high purity gas source is for providing a high purity gas.
As a preferable scheme of the invention, the CF three-way cavity and the mass spectrometer are respectively communicated with a vacuum providing system, and the film growing mechanism, the CF three-way cavity and the vacuum providing system on the mass spectrometer are matched to manufacture a triple differential vacuum environment so as to remove non-target ions screened out by the mass spectrometer step by step.
As a preferred aspect of the present invention, the vacuum supply system includes at least one of a secondary vacuum pump and a cryopump, and a vacuum degree measuring apparatus;
the secondary vacuum pump includes a mechanical pump for obtaining a rough vacuum state and a molecular pump for obtaining a high vacuum state.
As a preferred embodiment of the present invention, the apparatus further comprises a support frame, and at least one of the thin film growth mechanism, the sample loading mechanism, the ion source providing mechanism, the molecular beam epitaxy mechanism, and the chemical vapor deposition mechanism is mounted on the support frame.
In another aspect of the embodiment of the present invention, there is also provided a thin film deposition method, using the ion deposition thin film preparation apparatus according to the above, the thin film deposition method including:
S100, vacuumizing the film growing mechanism, the sample injection bearing mechanism and the ion source providing mechanism to a preset value;
S200, moving a sample into the film growth mechanism through the sample injection bearing mechanism;
s300, opening at least one of the ion source providing mechanism, the molecular beam epitaxy mechanism and the chemical vapor deposition mechanism to deposit a thin film on a sample;
s400, taking out the sample after film deposition.
Embodiments of the present invention have the following advantages:
The invention is based on the same film growth mechanism, integrates the ion source providing mechanism, the molecular beam epitaxy mechanism and the chemical vapor deposition mechanism pertinently, and controllably realizes the preparation of various films through the cooperative coordination thereof, thereby greatly reducing the operation difficulty and the operation cost for simultaneously preparing various films; on the basis, the co-deposition of the neutral molecules and the charged ions can be further realized through the cooperation of the structures, and a wider application range is provided for the deposition of the film through simple deposition operation. And the pollution of non-target ions to the sample in the ion deposition process can be effectively solved based on screening of ions to be deposited, so that the preparation of the sample with isotope-level purity is realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It will be apparent to those of ordinary skill in the art that the drawings in the following description are exemplary only and that other implementations can be obtained from the extensions of the drawings provided without inventive effort.
The structures, proportions, sizes, etc. shown in the present specification are shown only for the purposes of illustration and description, and are not intended to limit the scope of the invention, which is defined by the claims, so that any structural modifications, changes in proportions, or adjustments of sizes, which do not affect the efficacy or the achievement of the present invention, should fall within the ambit of the technical disclosure.
FIG. 1 is a schematic view showing a partial structure of an ion-deposited film forming apparatus according to an embodiment of the present invention in one direction;
FIG. 2 is a schematic view of a part of an ion-deposited film forming apparatus according to another embodiment of the present invention;
FIG. 3 is an exploded view of an ion deposited film manufacturing apparatus according to an embodiment of the present invention;
Fig. 4 is a schematic structural diagram of an ion source providing mechanism according to an embodiment of the present invention;
FIG. 5 is a schematic structural diagram of an apparatus for preparing an ion-deposited film according to an embodiment of the present invention;
fig. 6 is a partial cross-sectional view of an ion deposition thin film formation apparatus according to an embodiment of the present invention.
In the figure:
01-a film growth mechanism; 02-sample injection structure; 03-CF three-way cavity; 04-supporting frame;
1-a first CF150 flange; 2-first CF63 flange, 3-second CF63 flange, 4-third CF63 flange, 5-fourth CF63 flange; 6-a first CF100 flange; 7-fourth CF100 flange; 8-a fifth CF35 flange; 9-a fifth CF100 flange; 10-a sixth CF100 flange; 11-seventh CF100 flange; 12-eighth CF100 flange; 13-a second CF100 flange; 14-a second CF150 flange; 15-a first CF35 flange; 16-a second CF35 flange; 17-a third CF150 flange; 18-a third CF100 flange; 19-a fourth CF150 flange; 20-a fifth CF150 flange; 21-a sixth CF35 flange; 22-seventh CF35 flange; 23-ninth CF100 flange; 24-a third CF35 flange; 25-a fifth CF63 flange; 26-sixth CF63 flange; 27-a seventh CF63 flange; 28-eighth CF63 flange; 29-a ninth CF63 flange; 30-tenth CF63 flange; 31-reducing flanges; 32-seventh CF150 flange; 33-fourth CF35 flange; 34-eighth CF150 flange; 35-sample carrying heating structure; 36-a magnetic sample transmission rod; 37-a first molecular pump; 38-a cryogenic adsorption pump; 39-a second full-range vacuum gauge; 40-a first full-range vacuum gauge; 41-a support; 42-a third molecular pump; 43-a first thermal evaporation source; 44-a second thermal evaporation source; 45-a third thermal evaporation source; 46-a fourth thermal evaporation source; 47-a fifth thermal evaporation source; 48-a sixth thermal evaporation source; 49-a second molecular pump; a 50-ion source; 51-sample holder; 52-sample; 53-a first micro drain valve; 54-a second micro drain valve; 55-a third micro drain valve; 56-a first connection flange; 57-a second connection flange; 58-Wien mass spectrometry; 59-a third connecting flange; 60-ion beam focusing structure; 61-fourth connecting flange; 62-a fourth molecular pump; 63-a first mechanical pump; 64-a second mechanical pump; 65-a third mechanical pump; 66-rotating introducer.
Detailed Description
Other advantages and advantages of the present invention will become apparent to those skilled in the art from the following detailed description, which, by way of illustration, is to be read in connection with certain specific embodiments, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in fig. 1 to 6, the invention provides a multifunctional ion deposition film preparation device, which specifically comprises a film growth mechanism 01 and a sample injection bearing mechanism. The film growing mechanism 01 is connected with the sample feeding structure 02 in the sample feeding bearing mechanism through a gate valve with the size of CF100, so that the vacuum environments inside the two cavities are separated.
The film growth mechanism 01 is a double-layer cavity, the thickness of an interlayer is 3mm, 22 flanges are communicated, and 5 CF150 flanges are respectively marked as a first CF150 flange 1, a second CF150 flange 14, a third CF150 flange 17, a fourth CF150 flange 19 and a fifth CF150 flange 20;3 CF100 flanges, labeled first CF100 flange 6, second CF100 flange 13, and third CF100 flange 18, respectively; 10 CF63 flanges, labeled first CF63 flange 2, second CF63 flange 3, third CF63 flange 4, fourth CF63 flange 5, fifth CF63 flange 25, sixth CF63 flange 26, seventh CF63 flange 27, eighth CF63 flange 28, ninth CF63 flange 29, and tenth CF63 flange 30, respectively; 3 CF35 flanges, labeled first CF35 flange 15, second CF35 flange 16, and third CF35 flange 24, respectively; 1 flange for converting the CF35 interface to the CF150 interface, labeled as reducing flange 31;
Further, the first CF150 flange 1 of the film growth mechanism 01 is hermetically connected with a sample-carrying heating structure 35 for carrying the sample 52 and controlling the position and temperature of the sample 52 during the preparation process.
The first CF63 flange 2 of the film growth mechanism 01 is used for introducing a cooling medium such as liquid nitrogen into the interlayer.
The second CF63 flange 3 of the film growth mechanism 01 is used to introduce additional electrodes.
The third CF100 flange 18 of the film growth mechanism 01 is hermetically connected with a secondary vacuum pump. The secondary vacuum pump here comprises a third mechanical pump 65 which takes a rough vacuum and a first molecular pump 37 which takes a higher vacuum.
The third CF63 flange 4, the fourth CF63 flange 5, the first CF100 flange 6, the second CF150 flange 14, the third CF150 flange 17, the fourth CF150 flange 19 and the fifth CF150 flange 20 of the film growing mechanism 01 are hermetically connected with glass observation windows.
The third CF35 flange 24 of the film growth mechanism 01 is hermetically connected with a vacuum measuring system. The vacuum measurement system here is a first full-scale vacuum gauge 40.
The first CF35 flange 15 and the second CF35 flange 16 of the film growing mechanism 01 are correspondingly and hermetically connected with a first micro-leakage valve 53 and a second micro-leakage valve 54.
Further, the first micro-drain valve 53 and the second micro-drain valve 54 may be connected to a source of high purity gas, such as high purity hydrogen. That is, the gas supply unit is formed by the cooperation between the first and second micro-leakage valves 53 and 54 and the high purity gas source, that is, a chemical reaction occurs on the surface of the sample 52 by generating a gaseous substance, thereby forming a solid deposition film.
The second CF100 flange 13 of the film growth mechanism 01 is connected with the sample feeding structure 02 through a gate valve.
The film growth mechanism 01 is welded with a support 41, and the film growth mechanism 01 can be supported on the support 41.
Further, 6 support members 41 are provided, each support member 41 having an M8 threaded hole, and are disposed at an angle of 60 ° to each other.
The fifth CF63 flange 25, the sixth CF63 flange 26, the seventh CF63 flange 27, the eighth CF63 flange 28, the ninth CF63 flange 29 and the tenth CF63 flange 30 of the thin film growth mechanism 01 are respectively and correspondingly connected with a first thermal evaporation source 43, a second thermal evaporation source 44, a third thermal evaporation source 45, a fourth thermal evaporation source 46, a fifth thermal evaporation source 47 and a sixth thermal evaporation source 48 in a sealing manner. The thermal evaporation sources may be each selected from a K-cell evaporation source or an electron beam evaporation source. By turning on the corresponding thermal evaporation source, a corresponding molecular beam current can be generated for molecular beam epitaxy of the sample 52. It should be noted that, the provision of a plurality of thermal evaporation sources is to correspondingly start the thermal evaporation sources with corresponding epitaxial growth materials to perform corresponding molecular beam epitaxial growth according to the requirement of molecular beam epitaxial growth without opening the whole equipment to replace materials. Further, the material types in each thermal evaporation source may be completely different, and the material types may be selected from Se, V, te, etc. which can be understood and used by any person skilled in the art, and will not be described herein.
The reducing flange 31 at the bottom of the film growth mechanism 01 is connected with a CF three-way cavity 03 in a sealing way. The reducing flange 31 can effectively reduce the size of the input interface of the CF three-way cavity 03 communicated with the film growth mechanism 01, thereby being beneficial to creating a triple differential vacuum environment and removing non-target ions simply and efficiently.
Further, the CF three-way cavity 03 is provided with 2 CF150 flanges, which are respectively labeled as a seventh CF150 flange 32 and an eighth CF150 flange 34;1 CF35 flange, labeled fourth CF35 flange 33.
The fourth CF35 flange 33 of the CF three-way cavity 03 is connected with a secondary vacuum pump in a sealing way and is used for pumping off waste gas discharged by the screening of the mass spectrum below, so as to create a differential vacuum environment. The secondary vacuum pump here comprises a second mechanical pump 64 for taking a rough vacuum and a second molecular pump 49 for taking a higher vacuum.
The eighth CF150 flange 34 of the CF three-way cavity 03 is connected with the Wien mass spectrum 58 (i.e. mass spectrometer) through a flange from CF150 caliber to CF35 caliber, and is used for ion screening, and is externally connected with a CF15 flange in a sealing connection manner with the rotary importer 66, so as to control the ion beam to enter the film growing mechanism 01.
Further, the Wien mass spectrum 58 is sealingly connected to the ion source 50 (which may be of the type commonly used in the art, and which will be understood and used herein by those skilled in the art, and will not be described in detail) at one end via a second connection flange 57, and to the ion beam focusing structure 60 at the other end via a third connection flange 59. The upper end of the Wien mass spectrum 58 is connected with a fourth molecular pump 62 in a sealing way through a fourth connecting flange 61.
Further, the fourth molecular pump 62 is coordinated with the first molecular pump 37 and the second molecular pump 49, so that the Wien mass spectrum 58, the CF three-way cavity 03 and the film growth mechanism 01 can be maintained in different vacuum environments respectively, and the vacuum degree is gradually increased, so that a differential vacuum environment is created, non-target ions are effectively pumped step by step, and the preparation of the isotope-level purity sample is realized. Based on this, the device can make triple difference vacuum environment through the cooperation of above-mentioned a plurality of pump package, pump off waste gas step by step, can effectively solve the pollution of non-target ion to the sample in the ion deposition process, and then realize the sample preparation of isotope level purity.
Further, the ion source 50 is sealingly connected to a third micro-leak valve 55 via a first connection flange 56.
Further, the third micro-leak valve 55 is hermetically connected to a source of high purity gas, such as high purity hydrogen.
The sample introduction structure 02 is provided with 9 flanges, wherein 6 CF100 flanges are respectively marked as a fourth CF100 flange 7, a fifth CF100 flange 9, a sixth CF100 flange 10, a seventh CF100 flange 11, an eighth CF100 flange 12 and a ninth CF100 flange 23; the 3 CF35 flanges are labeled as fifth CF35 flange 8, sixth CF35 flange 21, and seventh CF35 flange 22, respectively.
Further, the eighth CF100 flange 12 of the sample introduction structure 02 is connected with the film growth mechanism 01 in a sealing manner through a gate valve.
The sixth CF100 flange 10 of the sample introduction structure 02 is connected with a magnetic sample transmission rod 36 in a sealing manner.
Further, one end of the magnetic force sample transmission rod 36 is connected with a sample holder 51.
And a ninth CF100 flange 23 of the sample introduction structure 02 is connected with a secondary vacuum pump in a sealing way. The secondary vacuum pump here comprises a first mechanical pump 63 which takes a rough vacuum and a third molecular pump 42 which takes a higher vacuum.
The seventh CF35 flange 22 of the sample introduction structure 02 is connected with a vacuum measurement system in a sealing way.
Further, the vacuum measuring system is a second full-scale vacuum gauge 39.
The sixth CF35 flange 21 of the sample introduction structure 02 is connected with a cryogenic adsorption pump 38 in a sealing manner.
Further, the cryopump 38 may be referred to as a vacuum acquisition apparatus described in patent application publication number CN110230588 a.
And a shutter is connected with the fourth CF100 flange 7 of the sample introduction structure 02 in a sealing way.
And a glass observation window is hermetically connected with the fifth CF35 flange 8, the fifth CF100 flange 9 and the seventh CF100 flange 11 of the sample introduction structure 02.
The supporting frame 04 consists of 8 stainless steel struts, 1 layer of aluminum alloy panel and a plurality of stainless steel bars. Wherein 8 stainless steel struts are welded and connected by stainless steel bars, and 4 screw holes with M6 reserved at the tops of the adjacent stainless steel struts are used for fixing the film growth mechanism 01; the aluminum alloy panel is welded in an area surrounded by 8 stainless steel struts and is used for placing a mechanical pump; a stainless steel bar at the top of the support is welded with a stainless steel support of a specific shape for supporting the sample introduction structure 02.
Further, based on the above-mentioned multifunctional ion deposition film preparation device, the present invention specifically proposes a film deposition method, specifically comprising:
step one, a step of obtaining ultrahigh vacuum:
Adding substances required by experiments into the first evaporation source 43, the second evaporation source 44, the third evaporation source 45, the fourth evaporation source 46, the fifth evaporation source 47 and the sixth evaporation source 48, and then sealing and connecting the substances with a cavity;
Connecting the first, second, third, fourth, fifth, sixth thermal evaporation sources 43, 44, 45, 46, 47, 48, the first, second and sample-carrying heating structures 40, 39 with a control unit;
opening a secondary vacuum pump group (a first mechanical pump 63, a second mechanical pump 64, a third mechanical pump 65, a first molecular pump 37, a second molecular pump 49, a third molecular pump 42, a fourth molecular pump 62) connected with the film growing mechanism 01, the sample feeding mechanism 02 and the ion source providing mechanism;
introducing liquid nitrogen into the low-temperature adsorption pump 38 of the sample injection structure 02;
turning on the power supply of the second full-range vacuum gauge 39 and the first full-range vacuum gauge 40;
when the indication number of the first full-range vacuum gauge 40 reaches the magnitude of 1X 10 -7 mbar, covering the device with aluminum foil, winding a heating belt, and turning on a heating belt power supply to bake the device;
After baking for 48 hours, removing the aluminum foil and the heating belt covered on the device;
turning on power supplies of the first, second, third, fourth, fifth, sixth and sample-carrying heating structures 43, 44, 45, 46, 47, 48, 35 to degas the plurality of thermal evaporation sources and the sample-carrying heating structure 35;
After the indication of the first full-range vacuum gauge 40 reaches the order of 1X 10 -9 mbar, the power supplies of the first evaporation source 43, the second thermal evaporation source 44, the third thermal evaporation source 45, the fourth thermal evaporation source 46, the fifth thermal evaporation source 47, the sixth thermal evaporation source 48 and the sample bearing heating structure 35 are turned off, the degassing is stopped, and the device is kept stand for 1h to cool the temperature to the room temperature;
Liquid nitrogen is introduced into the interlayer of the film growth mechanism 01.
Step two, a sample is transmitted from the sample injection structure 02 to the film growth mechanism 01:
Closing a gate valve between the sample injection structure 02 and the film growth mechanism 01;
Closing the power supply of the second full-range vacuum gauge 39;
Stopping the supply of liquid helium to cryogenic adsorption pump 38;
Closing the power supply of the third molecular pump 42 of the secondary vacuum pump set and the valve between the third molecular pump 42 and the first mechanical pump 63;
closing the power supply of the first mechanical pump 63 of the secondary vacuum pump unit, and opening an air inlet valve connected with the high-purity inert gas steel cylinder on the third molecular pump 42 until the overpressure valve of the third molecular pump 42 is out after the third molecular pump 42 becomes low-speed and reaches a resonance state;
Opening a quick door of the sample injection structure 02, and loading a sample 52 into a sample support 51 of the magnetic sample transmission rod 36;
closing a quick opening door of the sample injection structure 02;
opening the power supply of the first mechanical pump 63 in the secondary vacuum pump group and opening a valve between the first mechanical pump 63 and the third molecular pump 42;
Turning on the power of the third molecular pump 42 in the secondary vacuum pump set;
introducing liquid nitrogen into the cryogenic adsorption pump 38;
Turning on the power supply of the second full-range vacuum gauge 39;
When the second full-range vacuum gauge 39 indicates that the vacuum degree reaches the magnitude of 1X 10 -8 mbar, a gate valve between the sample feeding structure 02 and the film growing mechanism 01 is opened;
Lowering the sample-carrying heating structure 35 in the film-growing mechanism 01 into position;
Feeding the sample 52 into the film growth mechanism 01 through the magnetic force sample transmission rod 36;
Confirming through the observation window that the sample 52 on the sample support 51 of the magnetic force sample transmission rod 36 is positioned above the supporting plate of the sample bearing heating structure 35, below the heating plate and at a designated position at the center of the notch of the supporting plate;
lifting the sample carrying heating structure 35 and removing the sample 52 from the magnetic sample transfer rod 36;
the magnetic force sample transmission rod 36 is retreated to an initial position in the sample injection structure 02;
Closing a gate valve between the sample feeding structure 02 and the film growing mechanism 01.
Step three, a step of growing a sample 52 in the thin film growing mechanism 01:
turning on the power supply to the first evaporation source 43 (here, the first evaporation source 43 is taken as an example) and the sample-carrying heating structure 35 to degas the first evaporation source 43 and the sample-carrying heating structure 35;
adjusting the position and angle of the sample carrying heating structure 35 to enable the sample 52 to be in the range of the beam current generated by the first evaporation source 43;
opening the Wien mass spectrum 58 and setting relevant parameters as required by the experiment;
When the indication number of the first full-range vacuum gauge 40 of the film growing mechanism 01 reaches the vacuum degree of the order of 1X 10 -9 mbar, opening a third micro-leakage valve 55 of the ion source 50 to allow the ion source 50 to enter air;
After waiting 3 hours, opening a shutter behind the ion beam focusing structure 60 by rotating the introducer 66, and opening a shutter of the first evaporation source 43;
after the film preparation is completed, the shutter is closed, the third micro drain valve 55 of the ion source 50 is closed, and the power supply of the first evaporation source 43 and the ion source 50 is turned off.
Step four, the step of taking out the sample 52 from the film growth mechanism 01:
Adjusting the sample carrying heating structure 35 carrying the sample 52 in the film growth mechanism 01 to a proper position through the observation window;
Opening a gate valve between the film growing mechanism 01 and the sample feeding structure 02;
feeding the magnetic force sample transmission rod 36 into the film growing mechanism 01, so that a sample support 51 of the magnetic force sample transmission rod 36 is positioned right below a sample 52;
Lowering the sample carrying heating structure 35 so that the sample 52 falls just above the sample holder 51;
withdrawing the magnetic force sample transmission rod 36 carrying the sample 52 into the sample introduction structure 02;
closing a gate valve between the sample injection structure 02 and the film growth mechanism 01;
Closing the power supply of the second full-range vacuum gauge 39;
Stopping the supply of liquid helium to cryogenic adsorption pump 38;
Closing the power supply of the third molecular pump 42 of the secondary vacuum pump group and the valve between the third molecular pump and the first mechanical pump 63;
closing the power supply of the first mechanical pump 63 of the secondary vacuum pump unit, and opening an air inlet valve connected with the high-purity inert gas steel cylinder on the third molecular pump 42 until the overpressure valve of the third molecular pump 42 is out after the third molecular pump 42 becomes low-speed and reaches a resonance state;
the quick door of the sample introduction structure 02 is opened, and the sample 52 is taken out.
While the invention has been described in detail in the foregoing general description and specific examples, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (10)
1. The multifunctional ion deposition film preparation device is characterized by comprising a film growth mechanism (01), a sample injection bearing mechanism capable of being connected with the film growth mechanism (01) in an open or closed mode, and an ion source providing mechanism, a molecular beam epitaxy mechanism and a chemical vapor deposition mechanism which are connected to the film growth mechanism (01) in a communicating mode; wherein,
The sample introduction carrier means being at least partially positionable in the film growth means (01) and for providing a sample (52) into the film growth means (01);
The ion source providing mechanism provides screened ions to be deposited into the film growing mechanism (01) for ion deposition of a sample (52);
The molecular beam epitaxy mechanism generates a molecular beam current for molecular beam epitaxy growth of the sample (52);
The chemical vapor deposition mechanism produces gaseous species for chemical vapor deposition of a sample (52).
2. The ion deposition thin film production apparatus as claimed in claim 1, wherein the thin film growth mechanism (01) is a double-layer chamber, and the chamber comprises a production chamber and an interlayer which are sequentially arranged from inside to outside; wherein,
The preparation cavity is used for depositing a film;
And the interlayer is communicated with a cooling medium supply structure.
3. An ion deposited film preparation apparatus as claimed in claim 1 or 2, wherein the sample loading mechanism comprises a sample loading structure (02) and a sample loading heating structure (35) respectively in communication with the film growth mechanism (01);
The sample feeding structure (02) comprises a feeding cavity which is connected with the film growing mechanism (01) in an openable or closable way through a gate valve, and a magnetic sample transmission rod (36) which is arranged in the feeding cavity and can extend into the film growing mechanism (01);
the sample bearing heating structure (35) comprises a sample heating table which can be extended and positioned in the film growing mechanism (01), wherein the sample heating table is used for bearing a sample (52) and controlling the placement position and the temperature of the sample (52);
The magnetic sample transfer bar (36) is capable of transferring a sample (52) to the sample heating stage.
4. An ion deposited film manufacturing apparatus according to claim 1 or 2, wherein the molecular beam epitaxy mechanism comprises at least one thermal evaporation source, each of the thermal evaporation sources being selected from a K-cell evaporation source or an electron beam evaporation source;
preferably, the element types of the molecular beam generated by each thermal evaporation source are not identical;
More preferably, the element of each of the molecular beams is selected from at least one of Se, V and Te.
5. An ion deposition thin film production apparatus according to claim 1 or 2, wherein the ion source providing mechanism comprises a CF three-way cavity (03) and a mass spectrometer which are sequentially communicated with the thin film growing mechanism (01), and the mass spectrometer is further communicably connected with an ion source (50) and an ion beam focusing structure (60), respectively;
the mass spectrometer is used for screening ions provided by the ion body source (50);
Preferably, the chemical vapor deposition mechanism comprises at least one gas supply unit connected to the film growth mechanism (01).
6. The ion deposition thin film formation apparatus according to claim 5, wherein the ion source supply mechanism further comprises a rotary introducer (66) connected to the thin film growth mechanism (01), and the rotary introducer (66) and the mass spectrometer are both connected to the thin film growth mechanism (01) via a reducing flange.
7. The ion deposition thin film preparation apparatus as claimed in claim 5, wherein the thin film growth mechanism (01), the sample loading mechanism and the ion source providing mechanism are further communicated with a vacuum providing system;
The ion source providing mechanism and the chemical vapor deposition mechanism at least further comprise a high purity gas source;
the vacuum providing system is used for adjusting and monitoring the vacuum degree of the film growing mechanism (01), the sample loading mechanism and the ion source providing mechanism;
The high purity gas source is used for providing high purity gas;
Preferably, the CF three-way cavity (03) and the mass spectrometer are respectively communicated with a vacuum providing system, and the film growing mechanism (01), the CF three-way cavity (03) and the vacuum providing system on the mass spectrometer are matched to manufacture a triple differential vacuum environment so as to remove non-target ions screened out by the mass spectrometer step by step.
8. The ion deposition thin film formation apparatus according to claim 7, wherein the vacuum supply system comprises at least one of a secondary vacuum pump and a low-temperature adsorption pump (38), and a vacuum degree measurement device;
the secondary vacuum pump includes a mechanical pump for obtaining a rough vacuum state and a molecular pump for obtaining a high vacuum state.
9. The ion deposition thin film production apparatus according to claim 1 or 2, further comprising a support frame (04), wherein at least one of the thin film growth mechanism (01), the sample introduction carrying mechanism, the ion source providing mechanism, the molecular beam epitaxy mechanism, and the chemical vapor deposition mechanism is mounted on the support frame (04).
10. A film deposition method, characterized in that the ion deposition film production apparatus according to any one of claims 1 to 9 is employed, the film deposition method comprising:
S100, vacuumizing the film growing mechanism, the sample injection bearing mechanism and the ion source providing mechanism to a preset value;
S200, moving a sample into the film growth mechanism through the sample injection bearing mechanism;
s300, opening at least one of the ion source providing mechanism, the molecular beam epitaxy mechanism and the chemical vapor deposition mechanism to deposit a thin film on a sample;
s400, taking out the sample after film deposition.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101128911A (en) * | 2005-02-28 | 2008-02-20 | 爱普斯碧德股份有限公司 | System and process for high-density, low-energy plasma enhanced vapor phase epitaxy |
| CN101348903A (en) * | 2008-08-29 | 2009-01-21 | 中国石油大学(北京) | Multifunctional Small Thin Film Deposition Equipment |
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| JP3769059B2 (en) * | 1996-02-02 | 2006-04-19 | 雅弘 西川 | Ultrasonic / plasma / particle beam combined process apparatus, thin film forming method and surface smoothing method |
| US20150179418A1 (en) * | 2012-08-08 | 2015-06-25 | Milman Thin Film Systems Pvt. Ltd. | Miniature physical vapour deposition station |
| US20160083838A1 (en) * | 2014-09-23 | 2016-03-24 | Directed Vapor Technologies International, Inc. | Systems, Devices, and/or Methods for Managing Coatings |
| CN112239849B (en) * | 2019-07-01 | 2022-12-09 | 无锡科硅电子技术有限公司 | Film growth system and method |
| KR102336228B1 (en) * | 2020-04-06 | 2021-12-09 | 티오에스주식회사 | Epi-growth apparatus of separate chamber type |
| CN112048704B (en) * | 2020-08-13 | 2021-05-25 | 北京航空航天大学合肥创新研究院 | Integrated processing equipment for ultrathin multilayer film and application method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101128911A (en) * | 2005-02-28 | 2008-02-20 | 爱普斯碧德股份有限公司 | System and process for high-density, low-energy plasma enhanced vapor phase epitaxy |
| CN101348903A (en) * | 2008-08-29 | 2009-01-21 | 中国石油大学(北京) | Multifunctional Small Thin Film Deposition Equipment |
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