CN111118479A - Process method for graphite boat saturation - Google Patents
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- CN111118479A CN111118479A CN201911372652.7A CN201911372652A CN111118479A CN 111118479 A CN111118479 A CN 111118479A CN 201911372652 A CN201911372652 A CN 201911372652A CN 111118479 A CN111118479 A CN 111118479A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 43
- 239000010439 graphite Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000007599 discharging Methods 0.000 claims abstract description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 18
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000077 silane Inorganic materials 0.000 claims abstract description 12
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 11
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000000087 stabilizing effect Effects 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims description 2
- 238000009738 saturating Methods 0.000 claims 3
- 239000007789 gas Substances 0.000 abstract description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 5
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 5
- 230000008021 deposition Effects 0.000 abstract description 2
- 230000005684 electric field Effects 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- AWAUBADRMJIRAK-UHFFFAOYSA-N azane;methane Chemical compound C.N AWAUBADRMJIRAK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002294 plasma sputter deposition Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- -1 silicon nitride saturated graphite Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C23C16/50—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
- C23C16/515—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 using pulsed 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
- C23C16/0245—Pretreatment of the material to be coated by cleaning or etching by etching with a plasma
-
- 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
- C23C16/325—Silicon carbide
-
- 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/345—Silicon nitride
-
- 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
- C23C16/52—Controlling or regulating the coating process
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/673—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere using specially adapted carriers or holders; Fixing the workpieces on such carriers or holders
- H01L21/67303—Vertical boat type carrier whereby the substrates are horizontally supported, e.g. comprising rod-shaped elements
- H01L21/67306—Vertical boat type carrier whereby the substrates are horizontally supported, e.g. comprising rod-shaped elements characterized by a material, a roughness, a coating or the like
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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)
- Inorganic Chemistry (AREA)
- Plasma & Fusion (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a graphite boat saturation process method, which comprises the following steps: 1) feeding the graphite boat into a furnace tube; 2) vacuumizing, introducing 15slm nitrogen, and raising the temperature to 420 ℃; 3) vacuumizing, introducing nitrogen for 15slm for 300 seconds, vacuumizing again, and recovering the vacuum after repeating for three times; 4) introducing ammonia gas of 5slm, controlling the temperature at 450460 ℃, and performing pre-deposition for 300 seconds; 5) vacuumizing, introducing silane and methane, and continuously discharging for 5000-; 6) vacuumizing, introducing silane and ammonia gas, and continuously discharging for 200 seconds; 7) stopping introducing the gas, vacuumizing until the pressure reaches 30mTorr, introducing 15slm nitrogen, vacuumizing again, repeating the steps for two times, and recovering; 8) and (6) unloading the boat. By adopting the method, the graphite boat is plated with the superposed layers of silicon carbide and silicon nitride, the boat sheet of the graphite boat is more compact and flat and has excellent heat-conducting property and electric field uniformity, so that the film color of the battery sheet in the process is more uniform and consistent, and the rework rate and the yield of the battery sheet are obviously increased.
Description
Technical Field
The invention relates to the technical field of solar cells, in particular to a graphite boat saturation process method.
Background
At present, the requirement of the crystalline silicon solar cell on the film color is higher and higher, the graphite boat is not fully saturated or the performance of the saturated material is limited in the production process, so that the film coating color of the cell plate of the graphite boat is changed in the service life period, and the influence is usually compensated by adopting a correction process.
The existing graphite boat saturation method is to insert a graphite dummy wafer or a silicon wafer and deposit a layer of silicon nitride film on the inner wall of the graphite boat, so that all parts of the inner wall are in a silicon nitride state, and the silicon nitride deposition rates of all parts in the graphite boat tend to be consistent in the process.
The principle of the silicon nitride saturated graphite boat is as follows:
heating to raise the temperature of the sample to the preset temperature by using low temperature plasma as an energy source, introducing a proper amount of reaction gas (silane and ammonia), forming plasma by the gas under radio frequency excitation, and depositing a silicon nitride layer on the surface of the silicon wafer.
SiH4+NH3→SixNyHz+H2↑
At present, in a graphite boat saturation mode, the uniformity of the color of a coating film of a silicon wafer is relatively poor, so that part of the silicon wafer is reddish or whitish, and certain negative effects are caused by the color difference rework rate and the appearance yield of a battery piece.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: at present, in a graphite boat saturation mode, the uniformity of the color of a coating film of a silicon wafer is relatively poor, so that the problem that part of the silicon wafer is reddish or whitish is caused.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a graphite boat saturation process method is characterized in that: comprises the following steps;
step one, feeding an empty graphite boat into a quartz furnace tube by using a silicon nitride paddle;
vacuumizing, introducing nitrogen with the flow of 15 standard liters per minute, and heating all temperature areas to 420 ℃;
vacuumizing until the pressure reaches 30mTorr, introducing nitrogen with the flow of 15 standard liters per minute for 300 seconds, vacuumizing again, and repeating the step for three times;
introducing ammonia gas with the flow of 5 standard liters per minute to ensure that the pressure in the furnace tube is stabilized at 1700mTorr, the temperature is controlled at 450-460 ℃, the discharge power is 3600 watts, and pre-cleaning is carried out for 300 seconds;
step five, vacuumizing, when the pressure reaches 30mTorr, introducing silane with the flow rate of 600-700 standard milliliters per minute, introducing methane with the flow rate of 6.5 standard liters per minute, stabilizing the pressure at 1500mTorr, discharging power of 6500 watts, and continuously discharging for 5000-11000 seconds;
step six, vacuumizing, when the pressure reaches 30 millitorr, introducing silane with the flow rate of 850-950 standard milliliters per minute, introducing ammonia with the flow rate of 7.8 standard liters per minute, discharging with the power of 7500 watts, and continuously discharging for 200 seconds;
step seven, stopping ventilation, vacuumizing, introducing nitrogen with the flow of 15 standard liters per minute when the pressure reaches millitorr, vacuumizing again, and repeating the step twice;
and step eight, unloading the boat.
Preferably, in the fourth step, the pulse switching ratio of the discharging process is 6:12 to 6: 18.
Preferably, in the fifth step, the pulse switching ratio of the discharging process is 5:70 to 5: 80.
Preferably, in the fifth step, the pulse switching ratio of the discharging process is 5:45 to 5: 50.
The invention has the beneficial effects that: the invention solves the problems of non-ideal saturation effect and complex saturation process of the graphite boat and effectively improves the film color uniformity of the silicon wafer. After the graphite boat is treated by the saturation method, the graphite boat is plated with the superposed layers of silicon carbide and silicon nitride, so that the boat sheet of the graphite boat is more compact and smoother, has excellent heat-conducting property and electric field uniformity, the film color of the battery sheet in the process is more uniform and consistent, and the rework rate and the yield of the battery sheet are obviously increased.
The graphite boat processed by the method is an empty graphite boat (a new graphite boat or a cleaned graphite boat), a graphite dummy wafer or a silicon wafer does not need to be inserted and unloaded, and the flow steps are saved.
And in the second step, nitrogen is introduced to facilitate temperature transmission, and the temperature in the furnace tube is uniform.
And step three, drying the residual moisture of the graphite boat, and introducing nitrogen to carry the moisture.
And step four, cleaning impurities adsorbed on the surface of the graphite boat by using plasma sputtering.
And step five, plating a silicon carbide layer on the surface of the graphite boat, wherein the graphite boat has a compact lattice structure, is smoother, and has excellent heat conduction and electric conduction properties.
And sixthly, plating a silicon nitride film on the surface of the silicon carbide to prevent the silicon carbide film from contacting with air, so as to avoid adsorbing water vapor and impurities.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
A graphite boat saturation process method specifically comprises the following steps:
firstly, feeding a graphite boat into a quartz furnace tube by using a silicon nitride paddle;
the specific process is as follows:
A. preparing a new graphite boat or a cleaned graphite boat;
B. placing the graphite boat in a boat position;
C. inputting the boat number, selecting the furnace tube number and the saturation process, operating the process, and automatically feeding the graphite boat into the selected furnace tube by the program.
Secondly, vacuumizing, introducing 15slm nitrogen, and raising the temperature of all temperature areas to 420 ℃;
the specific process comprises the following steps:
A. the pressure of the furnace tube is set to be 0mTorr, the opening of the butterfly valve is 100, and the time is 30 s;
B. setting the pressure of the furnace tube to 10000 mTorr, opening the butterfly valve to 0, introducing N215 slm, and keeping the time to 60 s;
C. wait for all warm zone temperatures to rise to 420 ℃.
Thirdly, vacuumizing until the pressure reaches 30mTorr, introducing nitrogen for 15slm for 300 seconds, vacuumizing again, and recovering the vacuum after repeating for three times;
the specific process comprises the following steps:
A. the pressure of the furnace tube is set to be 0mTorr, the opening of the butterfly valve is 100, and the butterfly valve is closed (the opening is 0) when the pressure reaches 30 mTorr;
B. introducing nitrogen gas for 300 seconds to reach atmospheric pressure at 15 slm;
C. the pressure of the furnace tube is set to be 0mTorr, the opening of the butterfly valve is 100, and the butterfly valve is closed (the opening is 0) when the pressure reaches 30 mTorr;
D. the process step B, C was repeated three times.
Fourthly, introducing ammonia gas 5slm to stabilize the pressure in the furnace tube at 1700mTorr, controlling the temperature at 450460 ℃, discharging power 3600W, pre-cleaning for 300 seconds:
the specific process comprises the following steps:
A. introducing ammonia gas of 5slm, stabilizing the pressure in a furnace tube at 1700mTorr, and controlling the temperature at 450460 ℃;
B. discharge power setting 3600W, high frequency switch setting: on/off 6/12ms, process time 300 s.
Fifthly, vacuumizing, when the pressure reaches 30mTorr, introducing silane of 600sccm-700sccm, introducing methane of 6.5slm, stabilizing the pressure at 1500mTorr, discharging power of 6500W, continuously discharging 5000 + 10000 seconds:
A. the pressure of the furnace tube is set to be 0mTorr, the opening of the butterfly valve is 100, and the pressure is equal to 30 mTorr;
B. introducing 660sccm of silane, introducing 6.5slm of methane, and stabilizing the pressure at 1500 mTorr;
C. discharge power setting 6500W, high frequency switch setting: on/off 5/80ms, process time 10000 s.
The specific chemical reaction formula is as follows: SiH4+ CH4 → SixCy + H2 ↓ @
Sixthly, vacuumizing until the pressure reaches 30mTorr, introducing 850sccm-950sccm of silane, introducing 7.8slm of ammonia gas, discharging at the power of 7500W, and continuously discharging for 200 seconds;
A. the pressure of the furnace tube is set to be 0mTorr, the opening of the butterfly valve is 100, and the pressure is equal to 30 mTorr;
B. introducing silane of 900sccm, introducing methane ammonia gas of 7.8slm, and stabilizing the pressure at 1500 mTorr;
C. discharge power setting 7500W, high frequency switch setting: on/off 5/50ms, process time 200 s.
The specific chemical reaction formula is as follows: SiH4+ NH3 → SixNyHz + H2 ↓
Seventhly, stopping introducing the gas, vacuumizing until the pressure reaches 30mTorr, introducing 15slm of nitrogen, vacuumizing again, and recovering after repeating twice;
A. closing all special gas (ammonia gas, silane and methane) switches, setting the pressure of the furnace tube to be 0mTorr, setting the opening of the butterfly valve to be 100, and closing the butterfly valve (opening 0) when the pressure reaches 30 mTorr;
B. setting the pressure of the furnace tube to 10000 mTorr, opening the butterfly valve to 0, introducing N215 slm, and keeping the time to 60 s;
C. the pressure of the furnace tube is set to be 0mTorr, the opening of the butterfly valve is 100, and the butterfly valve is closed (the opening is 0) when the pressure reaches 30 mTorr;
D. the process step B, C was repeated twice.
Eighthly, unloading the boat;
A. after the process operation is finished, automatically conveying the graphite boat to a lower boat position by a program;
B. the graphite boat is placed in a nitrogen cabinet for standby.
It will be obvious to those skilled in the art that the present invention may be varied in many ways, and that such variations are not to be regarded as a departure from the scope of the invention. All such modifications as would be obvious to one skilled in the art are intended to be included within the scope of this claim.
Claims (4)
1. A graphite boat saturation process method is characterized in that: comprises the following steps;
step one, feeding an empty graphite boat into a quartz furnace tube by using a silicon nitride paddle;
vacuumizing, introducing nitrogen with the flow of 15 standard liters per minute, and heating all temperature areas to 420 ℃;
vacuumizing until the pressure reaches 30mTorr, introducing nitrogen with the flow of 15 standard liters per minute for 300 seconds, vacuumizing again, and repeating the step for three times;
introducing ammonia gas with the flow of 5 standard liters per minute to ensure that the pressure in the furnace tube is stabilized at 1700mTorr, the temperature is controlled at 450-460 ℃, the discharge power is 3600 watts, and pre-cleaning is carried out for 300 seconds;
step five, vacuumizing, when the pressure reaches 30mTorr, introducing silane with the flow rate of 600-700 standard milliliters per minute, introducing methane with the flow rate of 6.5 standard liters per minute, stabilizing the pressure at 1500mTorr, discharging power of 6500 watts, and continuously discharging for 5000-11000 seconds;
step six, vacuumizing, when the pressure reaches 30 millitorr, introducing silane with the flow rate of 850-950 standard milliliters per minute, introducing ammonia with the flow rate of 7.8 standard liters per minute, discharging with the power of 7500 watts, and continuously discharging for 200 seconds;
step seven, stopping ventilation, vacuumizing, introducing nitrogen with the flow of 15 standard liters per minute when the pressure reaches millitorr, vacuumizing again, and repeating the step twice;
and step eight, unloading the boat.
2. The process of saturating graphite boats as recited in claim 1, wherein: in the fourth step, the pulse switching ratio in the discharging process is 6:12 to 6: 18.
3. The process of saturating graphite boats as recited in claim 1, wherein: in the fifth step, the pulse switching ratio in the discharging process is 5:70 to 5: 80.
4. The process of saturating graphite boats as recited in claim 1, wherein: in the fifth step, the pulse switching ratio in the discharging process is 5: 45-5: 50.
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| CN201911372652.7A CN111118479A (en) | 2019-12-27 | 2019-12-27 | Process method for graphite boat saturation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113981417A (en) * | 2021-10-19 | 2022-01-28 | 常州亿晶光电科技有限公司 | Method for optimizing saturation effect of graphite boat |
| CN114361084A (en) * | 2021-12-22 | 2022-04-15 | 宁波尤利卡太阳能股份有限公司 | Saturated deposition process of graphite boat |
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| CN103560171A (en) * | 2013-10-29 | 2014-02-05 | 宁夏银星能源股份有限公司 | Method for saturating solar cell graphite boats |
| CN107564844A (en) * | 2017-07-28 | 2018-01-09 | 韩华新能源（启东）有限公司 | A kind of graphite boat saturation double membrane structure and coating process and graphite boat |
| CN107742603A (en) * | 2017-10-19 | 2018-02-27 | 西安黄河光伏科技股份有限公司 | A kind of crystal silicon solar battery graphite boat and its saturated process method |
| CN109244019A (en) * | 2018-08-01 | 2019-01-18 | 浙江爱旭太阳能科技有限公司 | A kind of graphite boat and its saturation process of crystal silicon solar PERC battery |
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- 2019-12-27 CN CN201911372652.7A patent/CN111118479A/en active Pending
Patent Citations (4)
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| CN103560171A (en) * | 2013-10-29 | 2014-02-05 | 宁夏银星能源股份有限公司 | Method for saturating solar cell graphite boats |
| CN107564844A (en) * | 2017-07-28 | 2018-01-09 | 韩华新能源（启东）有限公司 | A kind of graphite boat saturation double membrane structure and coating process and graphite boat |
| CN107742603A (en) * | 2017-10-19 | 2018-02-27 | 西安黄河光伏科技股份有限公司 | A kind of crystal silicon solar battery graphite boat and its saturated process method |
| CN109244019A (en) * | 2018-08-01 | 2019-01-18 | 浙江爱旭太阳能科技有限公司 | A kind of graphite boat and its saturation process of crystal silicon solar PERC battery |
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| CN113981417A (en) * | 2021-10-19 | 2022-01-28 | 常州亿晶光电科技有限公司 | Method for optimizing saturation effect of graphite boat |
| CN113981417B (en) * | 2021-10-19 | 2023-11-21 | 常州亿晶光电科技有限公司 | Method for optimizing saturation effect of graphite boat |
| CN114361084A (en) * | 2021-12-22 | 2022-04-15 | 宁波尤利卡太阳能股份有限公司 | Saturated deposition process of graphite boat |
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