CN114908336A - Preparation method of tubular PECVD enhanced vapor deposition microcrystalline silicon - Google Patents
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- CN114908336A CN114908336A CN202210094985.3A CN202210094985A CN114908336A CN 114908336 A CN114908336 A CN 114908336A CN 202210094985 A CN202210094985 A CN 202210094985A CN 114908336 A CN114908336 A CN 114908336A
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- 229910021424 microcrystalline silicon Inorganic materials 0.000 title claims abstract description 18
- 238000007740 vapor deposition Methods 0.000 title claims abstract description 16
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims description 8
- 239000007789 gas Substances 0.000 claims abstract description 36
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000010453 quartz Substances 0.000 claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003513 alkali Substances 0.000 claims abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 239000001307 helium Substances 0.000 claims description 9
- 229910052734 helium Inorganic materials 0.000 claims description 9
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000011856 silicon-based particle Substances 0.000 claims description 2
- 239000002367 phosphate rock Substances 0.000 abstract description 3
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 2
- 239000001301 oxygen Substances 0.000 abstract 2
- 229910052760 oxygen Inorganic materials 0.000 abstract 2
- 239000002699 waste material Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- -1 chlorine hydrogen silicon compound Chemical class 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 238000005238 degreasing Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910021422 solar-grade silicon Inorganic materials 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Classifications
-
- 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
- C23C16/50—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 using electric discharges
-
- 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
- C23C16/22—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 deposition of inorganic material, other than metallic material
- C23C16/24—Deposition of silicon only
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a process for preparing microcrystalline silicon by tubular PECVD enhanced vapor deposition, which comprises the steps of removing oxygen in silicon tetrafluoride, hydrogen and protective gas through an oxygen removal tube. Introducing the deoxidized mixed gas into a high-vacuum quartz tube, carrying out vapor deposition to obtain microcrystalline silicon at the plasma power of 50-400W and the heating furnace temperature of 100-600 ℃, and absorbing and washing the generated hydrogen fluoride and the residual silicon tetrafluoride gas by alkali liquor. The method utilizes the phosphorite associated resource silicon tetrafluoride as a raw material, greatly improves the effective utilization of the phosphorite associated resource and reduces the resource waste.
Description
Technical Field
The invention relates to a process for preparing microcrystalline silicon by tubular PECVD enhanced plasma vapor deposition, which belongs to the technical field of fluorine silicon chemical industry.
Background
Silicon is a basic material required by the electronic industry, the photovoltaic industry developed in recent years, the optical fiber industry and the solar energy industry. The use amount is large, and the use amount accounts for more than 95% of the semiconductor materials in the world, so that the material is the first major functional material and is already a strategic material and an industry. The simple substance silicon is prepared by heating mineral substances at high temperature by a metallurgy method, reducing the mineral substances by carbon materials at the temperature of more than 2000 ℃, and the purity of the prepared product is still between industrial silicon and solar grade silicon due to more impurities in the raw materials.
At present, 80% of high-purity simple substance silicon is produced by a Siemens method or an improved Siemens method, chlorine radicals are combined with silicon atoms, silicon tetrachloride in a flowing state or a chlorine hydrogen silicon compound with partial chlorine ions replaced by hydrogen ions is combined with hydrogen at normal temperature, and the chlorine ions are replaced by the hydrogen to further obtain the simple substance silicon.
In 1986, EverettM. Marlett et al, by Ethyl corporation, invented a method of producing silane by reacting silicon tetrafluoride with sodium aluminum hydride, and then dehydrogenating the silane at high temperature to obtain elemental silicon. The present inventors have prepared an n-type or p-type amorphous silicon thin film using silane and hydrogen in a method of double-sided deposition of an amorphous silicon layer of a solar cell in a tubular PECVD apparatus (cn109950132. a).
Disclosure of Invention
The technical problem to be solved by the invention is as follows: preparing microcrystalline silicon by utilizing phosphorite associated resource silicon tetrafluoride through tubular PECVD vapor deposition, and carrying out tail gas treatment on tail gas hydrogen fluoride.
The technical scheme of the invention is as follows: a preparation method of tubular PECVD enhanced vapor deposition microcrystalline silicon comprises the following steps:
(1) putting the carrier into a tube furnace, pushing the carrier to a constant-temperature area of a reaction chamber of the heating furnace, closing two ends of a quartz tube, and sealing;
(2) opening a vacuum pump to vacuumize the quartz tube, detecting the air tightness of the preparation system, heating the heating furnace to 100-600 ℃, and opening a radio frequency power supply to adjust the power to 50-400W;
(3) introducing deoxidized protective gas, hydrogen and silicon tetrafluoride gas, regulating the flow rate through a gas mixing system, and preparing microcrystalline silicon through vapor deposition.
The carrier is a silicon wafer, silicon particles, a glass sheet, a copper sheet or a steel sheet.
The protective gas is argon or helium.
In the step (2), the vacuum pump vacuumizes the quartz tube, and the vacuum degree is 1.0 to 10 -2 Pa below, degree of vacuum during deposition: 1-300Pa, and the vacuum pump is formed by combining a roots pump and a mechanical pump.
The silicon tetrafluoride, the hydrogen and the argon/helium are respectively controlled by a mass flow meter, the volume flow of the silicon tetrafluoride is 1-100SCCM, the volume flow of the hydrogen is 2-300SCCM, and the volume flow of the argon/helium is 20-600 SCCM.
The method also comprises the following step of washing the tail gas containing the hydrogen fluoride and the silicon tetrafluoride by alkali liquor.
The alkali liquor is sodium hydroxide or potassium hydroxide solution.
The invention has the beneficial effects that: the microcrystalline silicon is prepared by utilizing the phosphorus ore associated resource silicon tetrafluoride, the value of the fluorine silicon associated resource is effectively improved, and the decomposition temperature of the silicon tetrafluoride is reduced by a PECVD tube furnace.
Drawings
FIG. 1 is a scanning electron microscope image of microcrystalline silicon deposited on a silicon wafer substrate;
FIG. 2 is a scanning electron microscope image of microcrystalline silicon deposited on a steel sheet as a substrate;
FIG. 3 is a scanning electron microscope image of microcrystalline silicon deposited on a copper sheet as a substrate;
fig. 4 is a raman spectrum of microcrystalline silicon with a crystallization rate of 64.76%.
Detailed Description
Fixing the silicon, quartz glass, steel sheet and copper sheet substrate on an objective table, pushing the objective table to a constant temperature area of a reaction chamber of a constant temperature furnace, and closing a quartz pipe orifice.
Closing a gas inlet valve of the quartz pipeline, opening a tail gas outlet valve of the gas pipeline, starting a vacuum pump for vacuumizing, observing the vacuum degree index, maintaining the vacuum degree below 0.01Pa, closing the tail gas outlet valve, and stopping the pump. And (5) waiting for more than 10 minutes, observing the readings of the vacuum degree, and judging that the air tightness of the preparation system is good if the readings are maintained unchanged, otherwise, judging that the air leakage exists.
Introducing argon, adjusting the flow rate to be 30-300sccm, and flowing through the deoxygenation tube. And opening a vacuum pump for continuous vacuum pumping, wherein the pressure range in the quartz tube is 10-300 Pa. And repeatedly vacuumizing the quartz tube for 3-5 times, and discharging inert gas.
Setting a temperature control program of the constant-temperature heating furnace, wherein the temperature range is as follows: and when the gear is driven to run gear at the temperature of 600 ℃ below zero at 100 ℃, a power switch is started, and the temperature is waited to rise.
Setting the flow of hydrogen and silicon tetrafluoride gas through mass flow, opening a valve and continuously introducing Ar, Ar and H 2 The gas mixture of (2) was observed for the indication of the degree of vacuum and whether the flow rate tended to be stable.
Firstly, the power is adjusted to be below 20W, then the radio frequency switch is turned on, the power is gradually adjusted to be 30-450W, the gas is enabled to continuously react and deposit in the reaction tube, and then the color change process of the reaction is observed in the experimental process.
After the reaction time is over, closing a main valve of a silicon tetrafluoride gas cylinder, adjusting the gear of a constant temperature heating furnace to a STOP gear, adjusting the power to be below 50W, closing a radio frequency switch, opening an emptying valve and a purge valve, exhausting silicon tetrafluoride in a gas pipeline, enabling the silicon tetrafluoride to not enter a reaction system, after the pressure of a silicon tetrafluoride pressure reducing valve is reduced, closing a power switch of a hydrogen generator, opening a valve for adjusting a gas flow control cabinet to control hydrogen to be adjusted to a cleaning gear, exhausting the hydrogen, finally closing the emptying valve, opening two valves of a reaction tube, enabling the gas in the gas pipeline to be exhausted from the system, after 10 minutes of purging, closing the main valve of argon, waiting for the pressure indication number of the argon gas cylinder to be zero, simultaneously controlling the valves of the argon to be driven to the cleaning gear by a mass flow control meter and the mass flow control cabinet, waiting for the indication numbers of all pressure gauges to be reduced to be zero, and closing the air inlet valve, pumping the reaction system to a vacuum state, closing the vacuum pump, and closing all power supplies.
And after the temperature of the reaction system is reduced to normal temperature, introducing protective gas to restore the reaction system to normal pressure, preventing the plug from being flushed out due to overlarge system pressure, taking out the silicon wafer after the operation is finished, weighing the mass of the silicon wafer after the reaction by using an electronic balance, bagging the prepared sample by using the sample, recording relevant experimental conditions by using a label, and analyzing the appearance, the substance type and the content of the prepared silicon-based membrane by using characterization methods such as Ram and SEM.
Example 1
Soaking and cleaning a carrier silicon wafer by using washing liquor, degreasing by using acetone and ethanol, drying, putting into a quartz tube, pushing to a constant-temperature area of a reaction chamber of a heating furnace, and closing the tubular reactor. And starting a vacuum pump to vacuumize the quartz tube, and checking the air tightness of the system. Heating the heating furnace to 300 ℃, and turning on a radio frequency power supply to adjust the power to 100W. And introducing 100ml/min of deoxidized helium, 15ml/min of hydrogen and 10ml/min of silicon tetrafluoride gas step by step, preparing silicon by vapor deposition for 120min, and depositing at the pressure of 120 pa. Washing tail gas containing hydrogen fluoride and silicon tetrafluoride with alkali liquor. The deposited silicon was analyzed by a raman spectrometer, and the crystallization rate was 64.76%.
Example 2
Cleaning a carrier steel sheet, degreasing the carrier steel sheet by using acetone and ethanol, drying the carrier steel sheet in inert gas, putting the carrier steel sheet into a quartz tube, pushing the quartz tube to a constant-temperature area of a reaction chamber of a heating furnace, and closing the tubular reactor. And starting a vacuum pump to vacuumize the quartz tube, and checking the air tightness of the system. And heating the heating furnace to 200 ℃, and turning on a radio frequency power supply to adjust the power to 200W. And introducing the deoxidized helium gas at 150ml/min, hydrogen gas at 20ml/min, and silicon tetrafluoride gas at 10ml/min, preparing silicon by vapor deposition for 60min, wherein the deposition pressure is 160 pa. Washing tail gas containing hydrogen fluoride and silicon tetrafluoride with alkali liquor. The deposited silicon was analyzed by a raman spectrometer, and the crystallization rate was 34.63%.
Example 3
Cleaning a carrier copper sheet, degreasing by using acetone and ethanol, drying under inert gas, putting into a quartz tube, pushing to a constant temperature area of a reaction chamber of a heating furnace, and closing the tubular reactor. And starting a vacuum pump to vacuumize the quartz tube, and checking the air tightness of the system. Heating the heating furnace to 600 ℃, and turning on a radio frequency power supply to adjust the power to 150W. And introducing 100ml/min of deoxidized helium, 15ml/min of hydrogen and 5ml/min of silicon tetrafluoride gas step by step, preparing silicon by vapor deposition for 60min, wherein the deposition pressure is 80 pa. Washing tail gas containing hydrogen fluoride and silicon tetrafluoride with alkali liquor. The deposited silicon was analyzed by a raman spectrometer, and the crystallization rate was 32.34%.
Claims (7)
1. A preparation method of tubular PECVD enhanced vapor deposition microcrystalline silicon is characterized by comprising the following steps:
comprises the following steps:
(1) putting the carrier into a tube furnace, pushing the carrier to a constant-temperature area of a reaction chamber of the heating furnace, closing two ends of a quartz tube, and sealing;
(2) opening a vacuum pump to vacuumize the quartz tube, detecting the air tightness of the preparation system, heating the heating furnace to 100-;
(3) introducing deoxidized protective gas, hydrogen and silicon tetrafluoride gas, regulating the flow rate through a gas mixing system, and preparing microcrystalline silicon through vapor deposition.
2. The method of claim 1, wherein the method comprises the steps of: the carrier is a silicon wafer, silicon particles, a glass sheet, a copper sheet or a steel sheet.
3. The method of claim 1, wherein the method comprises the steps of: the protective gas is argon or helium.
4. A tubular according to claim 1The preparation method of PECVD enhanced vapor deposition microcrystalline silicon is characterized by comprising the following steps: in the step (2), the vacuum pump vacuumizes the quartz tube, and the vacuum degree is 1.0 x 10 -2 Pa below, degree of vacuum during deposition: 1-300Pa, and the vacuum pump is composed of a Roots pump and a mechanical pump.
5. The method according to claim 1, wherein the step of preparing microcrystalline silicon by tubular PECVD enhanced vapor deposition comprises the following steps: the silicon tetrafluoride, the hydrogen and the argon/helium are respectively controlled by a mass flow meter, the volume flow of the silicon tetrafluoride is 1-100SCCM, the volume flow of the hydrogen is 2-300SCCM, and the volume flow of the argon/helium is 20-600 SCCM.
6. The method of claim 1, wherein the method comprises the steps of: the method also comprises the following step of washing the tail gas containing the hydrogen fluoride and the silicon tetrafluoride by alkali liquor.
7. The method according to claim 6, wherein the step of preparing the tubular PECVD enhanced vapor deposition microcrystalline silicon comprises the following steps: the alkali liquor is sodium hydroxide or potassium hydroxide solution.
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