CN115287632A - Pretreatment method of graphite boat and modified graphite boat - Google Patents
Pretreatment method of graphite boat and modified graphite boat Download PDFInfo
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- CN115287632A CN115287632A CN202210945895.0A CN202210945895A CN115287632A CN 115287632 A CN115287632 A CN 115287632A CN 202210945895 A CN202210945895 A CN 202210945895A CN 115287632 A CN115287632 A CN 115287632A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 87
- 239000010439 graphite Substances 0.000 title claims abstract description 87
- 238000002203 pretreatment Methods 0.000 title claims abstract description 40
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 108
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 108
- 238000000151 deposition Methods 0.000 claims abstract description 107
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 49
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 46
- 230000008021 deposition Effects 0.000 claims abstract description 44
- 230000008569 process Effects 0.000 claims abstract description 40
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000007599 discharging Methods 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 50
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 32
- 229910000077 silane Inorganic materials 0.000 claims description 32
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 26
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 12
- 235000013842 nitrous oxide Nutrition 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 17
- 238000007747 plating Methods 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000010408 film Substances 0.000 description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 238000002161 passivation Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 101001073212 Arabidopsis thaliana Peroxidase 33 Proteins 0.000 description 3
- 101001123325 Homo sapiens Peroxisome proliferator-activated receptor gamma coactivator 1-beta Proteins 0.000 description 3
- 102100028961 Peroxisome proliferator-activated receptor gamma coactivator 1-beta Human genes 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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
- C23C16/458—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 characterised by the method used for supporting substrates in the reaction chamber
- C23C16/4581—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 characterised by the method used for supporting substrates in the reaction chamber characterised by material of construction or surface finish of the means for supporting the substrate
-
- 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
- C23C16/22—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
- C23C16/40—Oxides
- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
-
- 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
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4404—Coatings or surface treatment on the inside of the reaction chamber or on parts thereof
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
- H01L31/1868—Passivation
-
- 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
Abstract
The invention relates to a pretreatment method of a graphite boat and a modified graphite boat, wherein the pretreatment method comprises the following steps: (1) Carrying out constant temperature treatment and vacuumizing heating treatment on the graphite boat; (2) Carrying out composite deposition coating treatment on the graphite boat treated in the step (1); (3) Vacuumizing the graphite boat processed in the step (2), introducing nitrogen, and discharging to finish pretreatment; and (3) the composite deposition coating treatment in the step (2) comprises the step of depositing a silicon oxide inner layer and a silicon nitride outer layer on the surface. Through the pretreatment before the existing saturation process, the inner silicon oxide layer with a compact structure and the outer silicon nitride layer with a stable film surface are plated on the surface of the graphite boat, so that on one hand, the impurities of the graphite boat are prevented from overflowing, meanwhile, the pollution of aluminum oxide during back film plating can be reduced, the uniformity of an aluminum oxide film is improved, and the occurrence of the condition that the edge is dark is reduced.
Description
Technical Field
The invention belongs to the field of solar energy single crystal PERC, and relates to a pretreatment method of a graphite boat and a modified graphite boat.
Background
At present, a PERC battery technical route basically goes through three stages, wherein the first stage is to directly upgrade on a conventional production line, and the efficiency can be improved by 1%; the second stage is to add a thermal oxidation process, optimize etching and diffusion matching, and improve the efficiency to 21.7%; and the third stage, namely, the SE technical efficiency of scale popularization is improved to 22% of mass production. Regardless of the process stage, the core process is the growth of the back passivation film layer.
The back passivation process can be classified into plasma enhanced chemical vapor deposition, thermal oxidation, atomic layer deposition and other methods, wherein the preparation of the two-layer film of aluminum oxide and silicon nitride can be completed by using the same equipment for the aluminum oxide prepared by the plasma enhanced chemical vapor deposition, namely the preparation of the aluminum oxide by the two-in-one equipment. The plasma enhanced chemical vapor deposition method is a chemical vapor deposition reaction for activating particles by utilizing the physical action of glow discharge, is a thin film deposition technology integrating plasma glow discharge and chemical vapor deposition, and has a very high reaction speed compared with a thermal oxidation method and an atomic layer deposition method.
However, this method is not dense but thick, and especially when a new graphite boat is used, the alumina film is susceptible, the edge is thin, the EL is dark, and the conversion efficiency of the cell is low.
CN 114107955A provides a graphite boat pretreatment process for improving the back passivation uniformity of a two-in-one apparatus, said pretreatment process comprising the following steps: soaking and washing a used graphite boat by adopting a first acid solution, then cleaning by adopting a second acid solution, and drying after cleaning; carrying out constant temperature treatment, first silicon nitride plating treatment and silicon oxide plating treatment on the dried graphite boat in sequence, and then discharging the graphite boat; and (4) sequentially carrying out second silicon nitride plating treatment and aluminum oxide plating treatment on the treated graphite boat to finish the pretreatment process. The pretreatment process optimizes the cleaning method for the used graphite boat, and simultaneously increases a silicon nitride layer and an aluminum oxide layer on the basis of the traditional process in the secondary treatment process, thereby improving the surface flatness of the graphite boat and being beneficial to improving the effect of back coating.
CN 109285801A relates to a method for solving graphite boat pollution of PERC battery with double-sided alumina structure, comprising the following steps: firstly, a silicon nitride film layer is deposited on the surface of the graphite boat, and then a silicon oxide film layer is deposited on the surface of the silicon nitride film layer. The invention utilizes the excellent passivation performance and blocking performance of metal impurities of silicon oxide as the contact isolation layer between the battery piece and the graphite boat, can effectively enhance the passivation and isolation effect of the graphite boat surface film layer on the graphite boat surface metal ions, and prevents the pollution of the graphite boat surface impurities on the silicon chip front side aluminum oxide during back side coating under high temperature condition.
In the technical scheme, although the film quality is improved, the back alumina pollution can not be improved, so that the uniformity of alumina is improved.
How to improve the back alumina pollution in the graphite boat saturation process so as to improve the quality of a coating film is a technical problem which needs to be solved urgently in the field of solar single crystal batteries.
Disclosure of Invention
In order to solve the technical problems, the invention provides a pretreatment method of a graphite boat and a modified graphite boat, wherein a silicon oxide layer is coated on the surface of the graphite boat by pretreatment before back surface coating, so that impurities in the graphite boat are prevented from overflowing, a silicon nitride layer is coated on the silicon oxide layer, and the surface alumina pollution is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a pretreatment method for a graphite boat, comprising the steps of:
(1) Carrying out constant temperature treatment and vacuumizing heating treatment on the graphite boat;
(2) Carrying out composite deposition coating treatment on the graphite boat treated in the step (1);
(3) Vacuumizing the graphite boat processed in the step (2), introducing nitrogen, and discharging to finish pretreatment;
and (2) the composite deposition coating treatment comprises the step of sequentially depositing a silicon oxide inner layer and a silicon nitride outer layer on the surface.
The invention provides a pretreatment method of a graphite boat, which is characterized in that a silicon oxide inner layer with a compact structure and a silicon nitride outer layer with a stable film surface are plated on the surface of the graphite boat before the existing graphite boat saturation process, so that on one hand, the impurity overflow of the graphite boat is prevented, meanwhile, the pollution of aluminum oxide during back film plating can be reduced, the uniformity of an aluminum oxide film is improved, and the occurrence of the condition that the edge is dark is reduced.
The production line of the solar single crystal battery is completed according to the steps of texturing, low-pressure diffusion, laser doping, oxidation, wet etching, alkali polishing, annealing, back coating, front coating, laser windowing, screen printing sintering, light injection and testing and packaging, wherein the pretreatment method is between annealing and back coating.
Preferably, the temperature of the constant temperature treatment in step (1) is 300 to 400 ℃, for example, 300 ℃, 320 ℃, 340 ℃, 360 ℃, 380 ℃, 390 ℃ or 400 ℃, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the constant temperature treatment time in the step (1) is 100-200 s, such as 100s, 110s, 120s, 140s, 160s, 180s, 190s or 200s, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the constant temperature treatment process in the step (1) further comprises introducing nitrogen.
Preferably, the nitrogen gas is introduced at a flow rate of 5000 to 30000sccm, such as 5000sccm, 5500sccm, 6000sccm, 10000sccm, 15000sccm, 25000sccm, or 30000sccm, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the gas pressure at the constant temperature treatment in the step (1) is controlled to be 1000 to 10000mtorr, for example, 1000mtorr, 1200mtorr, 1500mtorr, 2000mtorr, 5000mtorr, 9000mtorr or 10000mtorr, but is not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the temperature of the vacuuming and temperature raising treatment in the step (1) is 400 to 500 ℃, for example, 400 ℃, 420 ℃, 450 ℃, 460 ℃, 480 ℃, 490 ℃ or 500 ℃, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the time of the vacuuming and temperature raising treatment in the step (1) is 100 to 1000s, for example, 100s, 200s, 400s, 600s, 800s, 900s or 1000s, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the step (1) further comprises leak detection after the vacuum pumping and temperature raising treatment.
Preferably, the leak detection time is 5 to 30s, for example 5s, 6s, 10s, 15s, 20s, 25s or 30s, but is not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the time for depositing the silicon oxide inner layer is 100 to 1000s, and may be, for example, 100s, 200s, 400s, 600s, 800s, 900s, or 1000s, but is not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the temperature at which the inner layer of silicon oxide is deposited is in the range of 400 to 500 c, and may be, for example, 420 c, 450 c, 460 c, 480 c or 490 c, but is not limited to the recited values, and other values not recited in the numerical range are equally applicable.
Preferably, silane and laughing gas are introduced during the deposition of the silicon oxide inner layer.
Preferably, the silane is introduced at a flow rate of 500 to 2000sccm, such as 500sccm, 600sccm, 1000sccm, 1200sccm, 1500sccm, 1800sccm, or 2000sccm during the deposition of the silicon oxide inner layer, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the flow rate of the laughing gas introduced during the deposition of the inner silicon oxide layer is 1000 to 8000sccm, such as 1000sccm, 2000sccm, 4000sccm, 6000sccm, 7000sccm, 7500sccm, or 8000sccm, although not limited to the recited values, other unrecited values within the recited range are equally applicable.
Preferably, the gas pressure during deposition of the inner layer of silicon oxide is controlled to be between 1200 and 1900mtorr, such as 1200mtorr, 1300mtorr, 1400mtorr, 1500mtorr, 1600mtorr, 1700mtorr or 1900mtorr, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
Preferably, the rf power for depositing the silicon oxide inner layer is 5000-15000W, such as 5000W, 6000W, 7000W, 10000W, 12000W, 14000W or 15000W, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the duty cycle of depositing the silicon oxide inner layer is 20 (1000 to 1500), and may be, for example, 20.
The silicon oxide inner layer provided by the invention has a compact structure and is not easy to fall off, and can prevent impurities of the graphite boat from overflowing.
Preferably, the thickness of the inner layer of silicon oxide is 1 to 50nm, for example 1nm, 5nm, 10nm, 20nm, 30nm, 40nm or 50nm, but is not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the silicon nitride outer layer has a thickness of 10 to 100nm, which may be, for example, 10nm, 30nm, 50nm, 70nm, 90nm or 100nm, but is not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the silicon nitride outer layer comprises at least two silicon nitride deposition layers, which may be, for example, 2, 3, 5, 6 or 8 layers, but is not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the outer layer of silicon nitride comprises a first layer of silicon nitride and a second layer of silicon nitride.
The two silicon nitride layers have different proportion and refractive index to form a gradual change film structure of the silicon nitride outer layer. Two layers of silicon nitride gradient films, the inner layer is high-fold, the outer layer is low-fold, and the film layer plated on the graphite boat is advanced with the silicon wafer.
Preferably, the time for depositing the first layer of silicon nitride on the surface is 100 to 1000s, for example, 100s, 200s, 400s, 600s, 800s, 900s or 1000s, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the temperature at which the first layer of silicon nitride is deposited on the surface is 400 to 500 ℃, and may be, for example, 400 ℃, 420 ℃, 450 ℃, 460 ℃, 480 ℃, 490 ℃ or 500 ℃, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, silane and ammonia gas are introduced during the process of depositing the first layer of silicon nitride on the surface.
Preferably, the silane is introduced at a flow rate of 500sccm to 2000sccm, such as 500sccm, 600sccm, 1000sccm, 1200sccm, 1500sccm, 1800sccm, or 2000sccm, during the surface deposition of the first layer of silicon nitride, but is not limited to the recited values, and other values within the range of values are equally applicable.
Preferably, the ammonia gas is introduced at a flow rate of 1000 to 10000sccm, such as 1000sccm, 1200mtorr, 1500mtorr, 2000mtorr, 5000mtorr, 9000mtorr or 10000sccm during the surface deposition of the first layer of silicon nitride, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the gas pressure during the surface deposition of the first layer of silicon nitride is controlled to be between 1200 and 1900mtorr, such as 1200mtorr, 1300mtorr, 1400mtorr, 1500mtorr, 1600mtorr, 1700mtorr or 1900mtorr, but is not limited to the values recited, and other values not recited in the range of values are equally applicable.
Preferably, the RF power for surface deposition of the first layer of silicon nitride is 10000-20000W, such as 10000W, 12000W, 14000W, 16000W, 17000W, 18000W or 20000W, but not limited to the values listed, and other values not listed in the range are equally applicable.
Preferably, the duty cycle of the surface deposition of the first layer of silicon nitride is 20 (500-1000), and may be, for example, 20.
Preferably, the time for depositing the second layer of silicon nitride on the surface is 100 to 500s, for example, 100s, 150s, 200s, 300s, 400s, 450s or 500s, but is not limited to the values listed, and other values not listed in the range of values are also applicable.
Preferably, the second layer of silicon nitride is surface deposited at a temperature of 400 to 500 deg.C, such as 400 deg.C, 420 deg.C, 450 deg.C, 460 deg.C, 480 deg.C, 490 deg.C or 500 deg.C, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, silane and ammonia gas are introduced during the process of depositing the second layer of silicon nitride on the surface.
Preferably, the flow rate of silane introduced during the surface deposition of the second layer of silicon nitride is 100-2000 sccm, such as 100sccm, 150sccm, 200sccm, 500sccm, 600sccm, 1000sccm, 1200sccm, 1500sccm, 1800sccm, or 2000sccm, but is not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the flow rate of the ammonia gas introduced during the surface deposition of the second layer of silicon nitride is 1000sccm to 10000sccm, such as 1000sccm, 2000sccm, 4000sccm, 6000sccm, 8000sccm, 9000sccm or 10000sccm, but is not limited to the recited values, and other values within the range of values are also applicable.
Preferably, the gas pressure during surface deposition of the first layer of silicon nitride is controlled to be between 1200 and 1900mtorr, such as 1200mtorr, 1300mtorr, 1400mtorr, 1500mtorr, 1700mtorr, 1800mtorr or 1900mtorr, but is not limited to the values recited and other values not recited in the range are equally suitable.
Preferably, the RF power for surface deposition of the first layer of silicon nitride is 10000-20000W, such as 10000W, 12000W, 14000W, 16000W, 18000W, 19000W or 20000W, but not limited to the values listed, and other values not listed in the range are equally applicable.
Preferably, the duty cycle of the surface-deposited first layer of silicon nitride is 20 (500 to 1000), which can be, for example, 20.
Preferably, the time period for the vacuum pumping in step (3) is 20 to 60s, for example, 20s, 25s, 30s, 40s, 50s, 55s or 60s, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the temperature of the vacuum in step (3) is 200 to 500 ℃, for example, 200 ℃, 250 ℃, 300 ℃, 400 ℃, 450 ℃ or 500 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the nitrogen is introduced in step (3) for 10 to 50s, such as 10s, 15s, 20s, 30s, 40s, 45s or 50s, but not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the temperature of the nitrogen gas introduced in step (3) is 200 to 500 ℃, for example 200 ℃, 250 ℃, 300 ℃, 400 ℃, 450 ℃ or 500 ℃, but not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the flow rate of the introduced nitrogen in step (3) is 10000 to 30000sccm, such as 10000sccm, 12000sccm, 15000sccm, 20000sccm, 25000sccm, 28000sccm or 30000sccm, but not limited to the recited values, and other unrecited values within the range of values are also applicable.
Preferably, the gas pressure during the nitrogen gas introduction in the step (3) is controlled to be 5000 to 15000mtorr, for example, 5000mtorr, 6000mtorr, 8000mtorr, 10000mtorr, 12000mtorr, 14000mtorr or 15000mtorr, but is not limited to the enumerated values, and other non-enumerated values within the numerical range are also applicable.
As a preferable technical solution of the pretreatment method provided by the present invention, the pretreatment method comprises the steps of:
(1) Carrying out constant temperature treatment on the graphite boat for 100-200 s at the temperature of 300-400 ℃, introducing nitrogen with the flow of 5000-30000 sccm in the constant temperature treatment process, and controlling the gas pressure at 1000-10000 mtorr;
vacuumizing and heating for 100-1000 s, heating to 400-500 ℃, and detecting leakage for 5-30 s;
(2) Depositing a silicon oxide inner layer and at least two silicon nitride deposition layers on the surface of the graphite boat processed in the step (1), wherein the silicon nitride deposition layers comprise a first silicon nitride layer and a second silicon nitride layer;
(3) Vacuumizing the graphite boat processed in the step (2) for 20-60 s at the temperature of 200-500 ℃, introducing nitrogen with the flow of 10000-30000 sccm for 10-50 s, controlling the gas pressure at 5000-15000 mtorr, and discharging to finish pretreatment;
the surface deposition method of the silicon oxide inner layer comprises the following steps: introducing silane with the flow rate of 500-2000 sccm and ammonia gas with the flow rate of 1000-10000 sccm at the temperature of 400-500 ℃, controlling the gas pressure at 1200-1900 mtorr, and depositing for 100-1000 s under the conditions that the radio frequency power is 10000-20000W and the duty ratio is 20 (500-1000);
the surface deposition method of the first layer of silicon nitride comprises the following steps: introducing silane with the flow rate of 500-2000 sccm and ammonia gas with the flow rate of 1000-10000 sccm at the temperature of 400-500 ℃, controlling the gas pressure at 1200-1900 mtorr, and depositing for 100-1000 s under the conditions that the radio frequency power is 10000-20000W and the duty ratio is 20 (500-1000);
the surface deposition method of the second layer of silicon nitride comprises the following steps: silane with the flow rate of 100-2000 sccm and ammonia gas with the flow rate of 1000-10000 sccm are introduced at the temperature of 400-500 ℃, the gas pressure is controlled at 1200-1900 mtorr, and the deposition is carried out for 100-500 s under the conditions that the radio frequency power is 10000-20000W and the duty ratio is 20 (500-1000).
In a second aspect, the present invention provides a modified graphite boat obtained by the pretreatment method of the first aspect.
Compared with the prior art, the invention at least has the following beneficial effects:
the invention provides a pretreatment method of a graphite boat before the saturation process of the existing graphite boat. Through plating the silicon oxide inlayer that the structure is compact and the silicon nitride skin of membrane surface stability on graphite boat surface, on the one hand, prevented that the impurity of graphite boat is excessive, the pollution of aluminium oxide when can reducing the back coating film simultaneously has promoted the homogeneity of aluminium oxide membrane, has reduced the condition production that the edge is dark.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a pretreatment method of a graphite boat, which comprises the following steps:
(1) Carrying out constant temperature treatment on the graphite boat for 150s at 400 ℃, introducing nitrogen with the flow of 25000sccm in the constant temperature treatment process, and controlling the gas pressure to 10000mtorr;
vacuumizing and heating up for 800s, heating up to 450 ℃, detecting leakage for 15s, introducing no gas, and controlling the gas pressure to 10000mtorr;
vacuumizing for 30s at 450 ℃, and controlling the gas pressure to be 0mtorr without introducing any gas;
(2) Depositing a silicon oxide inner layer and two silicon nitride deposition layers on the surface of the graphite boat processed in the step (1); the two silicon nitride deposition layers comprise a first silicon nitride layer and a second silicon nitride layer which are distributed from inside to outside;
(3) Vacuumizing the graphite boat processed in the step (2) for 50s at the temperature of 350 ℃, introducing nitrogen with the flow of 20000sccm for 30s, controlling the gas pressure at 10000mtorr, and discharging to finish pretreatment;
the surface deposition method of the silicon oxide inner layer comprises the following steps: introducing silane with the flow rate of 700sccm and ammonia gas with the flow rate of 4200sccm at the temperature of 450 ℃, controlling the gas pressure at 1500mtorr, and depositing for 100s under the conditions that the radio frequency power is 12500W and the duty ratio is 20;
the surface deposition method of the first layer of silicon nitride comprises the following steps: introducing silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 6000sccm at the temperature of 450 ℃, controlling the gas pressure at 1700mtorr, and depositing for 300s under the conditions that the radio frequency power is 13500W and the duty ratio is 20;
the surface deposition method of the second layer of silicon nitride comprises the following steps: silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 8000sccm are introduced at the temperature of 450 ℃, the gas pressure is controlled at 1700mtorr, and the deposition is carried out for 300s under the conditions that the radio frequency power is 14000W and the duty ratio is 20.
Example 2
The embodiment provides a pretreatment method of a graphite boat, which comprises the following steps:
(1) Carrying out constant temperature treatment on the graphite boat for 200s at the temperature of 300 ℃, introducing nitrogen with the flow of 30000sccm in the constant temperature treatment process, and controlling the gas pressure at 10000mtorr;
vacuumizing and heating for 1000s, heating to 400 ℃, detecting leakage for 5s, and controlling the gas pressure to 10000mtorr without introducing any gas;
vacuumizing for 30s at 450 ℃, and controlling the gas pressure to be 0mtorr without introducing any gas;
(2) Depositing a silicon oxide inner layer and two silicon nitride deposition layers on the surface of the graphite boat processed in the step (1), wherein the silicon oxide inner layer and the two silicon nitride deposition layers are respectively a first layer of silicon nitride and a second layer of silicon nitride from inside to outside;
(3) Vacuumizing the graphite boat processed in the step (2) for 60s at the temperature of 200 ℃, introducing nitrogen with the flow of 10000sccm for 50s, controlling the gas pressure at 5000mtorr, and taking out the boat to finish pretreatment;
the surface deposition method of the silicon oxide inner layer comprises the following steps: introducing silane with the flow rate of 700sccm and ammonia gas with the flow rate of 5600sccm at the temperature of 480 ℃, controlling the gas pressure at 1500mtorr, and depositing for 500s under the conditions that the radio frequency power is 12500W and the duty ratio is 20;
the surface deposition method of the first layer of silicon nitride comprises the following steps: introducing silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 6000sccm at the temperature of 480 ℃, controlling the gas pressure at 1700mtorr, and depositing for 300s under the conditions that the radio frequency power is 13500W and the duty ratio is 20;
the surface deposition method of the second layer of silicon nitride comprises the following steps: silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 8000sccm are introduced at the temperature of 480 ℃, the gas pressure is controlled at 1700mtorr, and the deposition is carried out for 500s under the conditions that the radio frequency power is 14000W and the duty ratio is 20.
Example 3
The embodiment provides a pretreatment method of a graphite boat, which comprises the following steps:
(1) Carrying out constant temperature treatment on the graphite boat for 100s at 400 ℃, introducing nitrogen with the flow of 30000sccm in the constant temperature treatment process, and controlling the gas pressure at 1000mtorr;
vacuumizing and heating for 100s, heating to 500 ℃, detecting leakage for 30s, introducing no gas, and controlling the gas pressure to 10000mtorr;
then vacuumizing for 30s at 450 ℃, not introducing any gas, and controlling the gas pressure to be 0mtorr;
(2) Depositing a silicon oxide inner layer and two silicon nitride deposition layers on the surface of the graphite boat processed in the step (1), wherein the silicon oxide inner layer and the two silicon nitride deposition layers are respectively a first layer of silicon nitride and a second layer of silicon nitride from inside to outside;
(3) Vacuumizing the graphite boat processed in the step (2) for 20s at the temperature of 500 ℃, introducing nitrogen with the flow of 30000sccm for 10s, controlling the gas pressure at 15000mtorr, and discharging to finish the pretreatment;
the surface deposition method of the silicon oxide inner layer comprises the following steps: introducing silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 5600sccm at the temperature of 480 ℃, controlling the gas pressure at 1500mtorr, and depositing for 800s under the conditions that the radio frequency power is 12500W and the duty ratio is 20;
the surface deposition method of the first layer of silicon nitride comprises the following steps: introducing silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 6000sccm at the temperature of 480 ℃, controlling the gas pressure at 1700mtorr, and depositing for 500s under the conditions that the radio frequency power is 13500W and the duty ratio is 20;
the surface deposition method of the second layer of silicon nitride comprises the following steps: silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 8000sccm are introduced at the temperature of 480 ℃, the gas pressure is controlled at 1700mtorr, and the deposition is carried out for 500s under the conditions that the radio frequency power is 14000W and the duty ratio is 20.
Example 4
This example provides a pretreatment method for a graphite boat, which is different from example 1 in that three silicon nitride deposition layers are deposited on the surface in step (2), namely a first silicon nitride layer, a second silicon nitride layer and a third silicon nitride layer from inside to outside.
The surface deposition method of the first layer of silicon nitride comprises the following steps: introducing silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 6000sccm at the temperature of 450 ℃, controlling the gas pressure at 1700mtorr, and depositing for 300s under the conditions that the radio frequency power is 13500W and the duty ratio is 20;
the surface deposition method of the second layer of silicon nitride comprises the following steps: silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 8000sccm are introduced at the temperature of 450 ℃, the gas pressure is controlled at 1700mtorr, and the deposition is carried out for 300s under the conditions that the radio frequency power is 14000W and the duty ratio is 20.
The surface deposition method of the third layer of silicon nitride comprises the following steps: silane with the flow rate of 1000sccm and ammonia gas with the flow rate of 8000sccm are introduced at the temperature of 450 ℃, the gas pressure is controlled at 1700mtorr, and the deposition is carried out for 300s under the conditions that the radio frequency power is 14000W and the duty ratio is 20.
Example 5
This example provides a pretreatment method of a graphite boat, which is the same as example 1 except that the temperature of the inner layer of surface-deposited silica in step (2) is 300 ℃.
Example 6
This example provides a pretreatment method for a graphite boat, which is the same as that of example 1 except that the temperature of the inner layer of surface-deposited silica in step (2) is 600 ℃.
Example 7
This example provides a pretreatment method of a graphite boat, which is the same as example 1 except that the silicon oxide inner layer is surface-deposited in step (2) and silane is introduced at a flow rate of 300 sccm.
Example 8
This example provides a pretreatment method of a graphite boat, which is the same as example 1 except that the inner layer of silicon oxide is deposited on the surface in step (2) and silane is introduced at a flow rate of 2500 sccm.
Example 9
This example provides a pretreatment method for graphite boat, which is the same as example 1 except that the inner layer of silicon oxide is deposited on the surface in step (2) and laughing gas is introduced at a flow rate of 800 sccm.
Example 10
This example provides a pretreatment method for graphite boat, which is the same as example 1 except that the inner layer of silicon oxide is deposited on the surface in step (2) and the flow rate of laughing gas is 8500 sccm.
Example 11
This example provides a pretreatment method of graphite boat, which is the same as example 1 except that the rf power of the surface deposited silicon oxide inner layer in step (2) is 4000W.
Example 12
This example provides a pretreatment method for graphite boat, which is the same as example 1 except that the rf power of the surface deposited silicon oxide inner layer in step (2) is 16000W.
Example 13
This example provides a pretreatment method of graphite boat, which is the same as example 1 except that the silicon nitride outer layer is deposited on the surface in step (2), and only one silicon nitride deposition layer is deposited as the first silicon nitride layer.
Example 14
This example provides a pretreatment method for graphite boat, which is the same as example 1 except that in step (2), an outer layer of silicon nitride is deposited on the surface, and only one silicon nitride deposition layer is deposited as a second silicon nitride layer.
Comparative example 1
This comparative example provides a pretreatment method of a graphite boat, which is the same as example 1 except that the inner layer of silica was not deposited in step (2).
Comparative example 2
This comparative example provides a pretreatment method of a graphite boat, which is the same as example 1 except that the silicon nitride outer layer was not deposited in step (2).
Comparative example 3
This comparative example provides a graphite boat that was not pretreated prior to the backside coating process.
The graphite boat obtained above was subjected to a back surface coating process and then subjected to surface observation, and the edge darkening ratio was obtained, and the results are shown in table 1.
The graphite boat processed by the above process was used to prepare a battery plate, and the electrical performance test was performed, and the results are shown in table 2.
And (3) testing conditions: edge darkening ratio = number of edge darkening pieces per total pieces in the same batch.
TABLE 1
| Test number | Edge darkening ratio (%) |
| Example 1 | 0.7 |
| Example 2 | 0.78 |
| Example 3 | 1.1 |
| Example 4 | 1.3 |
| Example 5 | 4.2 |
| Example 6 | 4.31 |
| Example 7 | 3.9 |
| Example 8 | 3.79 |
| Example 9 | 4.3 |
| Example 10 | 3.2 |
| Example 11 | 4.25 |
| Example 12 | 4.9 |
| Example 13 | 5.1 |
| Example 14 | 5.2 |
| Comparative example 1 | 4 |
| Comparative example 2 | 4.2 |
| Comparative example 3 | 5 |
TABLE 2
Uoc is open circuit voltage, isc is short circuit current, rs is series resistance, rsh is parallel resistance, FF is fill factor, and Ncell is conversion efficiency of the cell.
From tables 1 and 2, the following conclusions can be drawn:
(1) As can be seen from examples 1-4 and comparative example 3, the present invention provides a method for pretreating graphite boats prior to the prior art graphite boat saturation process. Through plating the silicon oxide inner layer with compact structure and the silicon nitride outer layer with stable film surface on the surface of the graphite boat, on one hand, the impurity overflow of the graphite boat is prevented, meanwhile, the pollution of aluminum oxide during back film plating can be reduced, the uniformity of the aluminum oxide film is improved, the generation of the condition of dark edge is reduced, and thus the electrochemical performance of the solar cell is improved.
(2) It can be seen from the comparison between examples 5-12 and example 1 that when the process parameters for depositing the silicon oxide inner layer on the surface are not in the preferred range, the silicon oxide film layer structure is not dense, and the contamination of aluminum oxide during back surface coating can not be reduced, thereby affecting the electrochemical performance of the solar cell.
(3) As can be seen from comparison between examples 13 and 14 and example 1, when only one layer of silicon nitride is deposited on the surface, the structural stability of the silicon nitride layer cannot be ensured, and the occurrence of edge darkening cannot be reduced, which affects the improvement of the electrochemical performance of the solar cell.
(4) As can be seen from comparative examples 1 and 2, when the structure of the surface deposited film layer is different from that of the present application, the contamination of the aluminum oxide during the back surface coating cannot be reduced, the uniformity of the aluminum oxide film cannot be improved, and the occurrence of the edge darkening cannot be reduced.
In summary, the present invention provides a method for pre-treating a graphite boat prior to the saturation process of the graphite boat. Through plating the silicon oxide inner layer with compact structure and the silicon nitride outer layer with stable film surface on the surface of the graphite boat, on one hand, the impurity overflow of the graphite boat is prevented, meanwhile, the pollution of aluminum oxide during back film plating can be reduced, the uniformity of the aluminum oxide film is improved, the generation of the condition of dark edge is reduced, and thus the electrochemical performance of the solar cell is improved.
The present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed process flow, i.e. it is not meant to imply that the present invention must rely on the above detailed process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A pretreatment method of a graphite boat is characterized by comprising the following steps:
(1) Carrying out constant temperature treatment and vacuumizing heating treatment on the graphite boat;
(2) Carrying out composite deposition coating treatment on the graphite boat treated in the step (1);
(3) Vacuumizing the graphite boat processed in the step (2), introducing nitrogen, and discharging to finish pretreatment;
and (2) the composite deposition coating treatment comprises the step of sequentially depositing a silicon oxide inner layer and a silicon nitride outer layer on the surface.
2. The pretreatment method according to claim 1, wherein the constant temperature treatment in the step (1) is at a temperature of 300 to 400 ℃;
preferably, the constant temperature treatment time in the step (1) is 100-200 s;
preferably, the constant temperature treatment process in the step (1) further comprises introducing nitrogen;
preferably, the flow rate of the introduced nitrogen is 5000-30000 sccm;
preferably, the gas pressure at the constant temperature treatment in the step (1) is controlled to be 1000 to 10000mtorr.
3. The pretreatment method according to claim 1 or 2, wherein the temperature of the vacuuming and heating treatment in the step (1) is 400 to 500 ℃;
preferably, the time of the vacuumizing and heating treatment in the step (1) is 100 to 1000s;
preferably, the step (1) further comprises leak detection after the vacuum pumping and temperature raising treatment;
preferably, the time for leak detection is 5-30 s.
4. The pretreatment method according to any one of claims 1 to 3, wherein the time for depositing the silicon oxide inner layer is 100 to 1000s;
preferably, the temperature for depositing the silicon oxide inner layer is 400-500 ℃;
preferably, silane and laughing gas are introduced in the process of depositing the silicon oxide inner layer;
preferably, in the process of depositing the silicon oxide inner layer, the flow of silane is introduced into the silicon oxide inner layer and is 500-2000 sccm;
preferably, in the process of depositing the silicon oxide inner layer, the flow of the introduced laughing gas is 1000-8000 sccm;
preferably, the gas pressure during deposition of the silicon oxide inner layer is controlled to be 1200-1900 mtorr;
preferably, the radio frequency power for depositing the silicon oxide inner layer is 5000-15000W;
preferably, the duty cycle of the deposition of the silicon oxide inner layer is 20 (1000-1500).
5. The pretreatment method according to any one of claims 1 to 4, wherein the thickness of the silicon oxide inner layer is 1 to 50nm;
preferably, the thickness of the silicon nitride outer layer is 10-100 nm;
preferably, the outer layer of silicon nitride comprises at least two deposited layers of silicon nitride;
preferably, the outer layer of silicon nitride comprises a first layer of silicon nitride and a second layer of silicon nitride.
6. The pretreatment method according to claim 5, wherein the time for depositing the first layer of silicon nitride on the surface is 100 to 1000s;
preferably, the temperature for depositing the first layer of silicon nitride on the surface is 400-500 ℃;
preferably, silane and ammonia gas are introduced in the process of depositing the first layer of silicon nitride on the surface;
preferably, in the process of depositing the first layer of silicon nitride on the surface, the flow of introducing silane is 500-2000 sccm;
preferably, the flow of the introduced ammonia gas is 1000-10000 sccm in the process of depositing the first layer of silicon nitride on the surface;
preferably, the gas pressure is controlled to be 1200-1900 mtorr during the process of depositing the first layer of silicon nitride on the surface;
preferably, the radio frequency power of the first layer of silicon nitride deposited on the surface is 10000-20000W;
preferably, the duty ratio of the surface deposition of the first layer of silicon nitride is 20 (500-1000).
7. The pretreatment method according to claim 5 or 6, wherein the time for depositing the second layer of silicon nitride on the surface is 100 to 500s;
preferably, the temperature for depositing the second layer of silicon nitride on the surface is 400-500 ℃;
preferably, silane and ammonia gas are introduced in the process of depositing the second layer of silicon nitride on the surface;
preferably, in the process of depositing the second layer of silicon nitride on the surface, the flow of introducing silane is 100-2000 sccm;
preferably, the flow of the introduced ammonia gas is 1000-10000 sccm in the process of depositing the second layer of silicon nitride on the surface;
preferably, the gas pressure in the process of depositing the first layer of silicon nitride on the surface is controlled between 1200 and 1900mtorr;
preferably, the radio frequency power of the first layer of silicon nitride deposited on the surface is 10000-20000W;
preferably, the duty ratio of the surface deposition of the first layer of silicon nitride is 20 (500-1000).
8. The pretreatment method according to any one of claims 1 to 7, wherein the evacuation time in the step (3) is 20 to 60 seconds;
preferably, the temperature of the vacuum pumping in the step (3) is 200-500 ℃;
preferably, the time for introducing the nitrogen in the step (3) is 10 to 50s;
preferably, the temperature of the nitrogen introduced in the step (3) is 200-500 ℃;
preferably, the flow rate of the introduced nitrogen in the step (3) is 10000-30000 sccm;
preferably, the gas pressure during the nitrogen gas introduction in the step (3) is controlled to be 5000 to 15000mtorr.
9. The pretreatment method according to any one of claims 1 to 8, wherein the pretreatment method comprises the steps of:
(1) Carrying out constant temperature treatment on the graphite boat for 100-200 s at the temperature of 300-400 ℃, introducing nitrogen with the flow of 5000-30000 sccm in the constant temperature treatment process, and controlling the gas pressure at 1000-10000 mtorr;
vacuumizing and heating for 100-1000 s, heating to 400-500 ℃, and detecting leakage for 5-30 s;
(2) Depositing a silicon oxide inner layer and at least two silicon nitride deposition layers on the surface of the graphite boat processed in the step (1), wherein the silicon nitride deposition layers comprise a first silicon nitride layer and a second silicon nitride layer;
(3) Vacuumizing the graphite boat processed in the step (2) for 20-60 s at the temperature of 200-500 ℃, introducing nitrogen with the flow of 10000-30000 sccm for 10-50 s, controlling the gas pressure at 5000-15000 mtorr, and discharging to finish pretreatment;
the thickness of the silicon oxide inner layer is 1-50 nm, and the surface deposition method comprises the following steps: introducing silane with the flow rate of 500-2000 sccm and ammonia gas with the flow rate of 1000-10000 sccm at the temperature of 400-500 ℃, controlling the gas pressure at 1200-1900 mtorr, and depositing for 100-1000 s under the conditions that the radio frequency power is 10000-20000W and the duty ratio is 20 (500-1000);
the surface deposition method of the first layer of silicon nitride comprises the following steps: introducing silane with the flow rate of 500-2000 sccm and ammonia gas with the flow rate of 1000-10000 sccm at the temperature of 400-500 ℃, controlling the gas pressure at 1200-1900 mtorr, and depositing for 100-1000 s under the conditions that the radio frequency power is 10000-20000W and the duty ratio is 20 (500-1000);
the surface deposition method of the second layer of silicon nitride comprises the following steps: silane with the flow rate of 100-2000 sccm and ammonia gas with the flow rate of 1000-10000 sccm are introduced at the temperature of 400-500 ℃, the gas pressure is controlled at 1200-1900 mtorr, and the deposition is carried out for 100-500 s under the conditions that the radio frequency power is 10000-20000W and the duty ratio is 20 (500-1000).
10. A modified graphite boat obtained by the pretreatment method according to any one of claims 1 to 9.
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| US20120108079A1 (en) * | 2010-10-29 | 2012-05-03 | Applied Materials, Inc. | Atomic Layer Deposition Film With Tunable Refractive Index And Absorption Coefficient And Methods Of Making |
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