CN114107955A - Graphite boat pretreatment process for improving back passivation uniformity of two-in-one equipment - Google Patents
Graphite boat pretreatment process for improving back passivation uniformity of two-in-one equipment Download PDFInfo
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- CN114107955A CN114107955A CN202111366312.0A CN202111366312A CN114107955A CN 114107955 A CN114107955 A CN 114107955A CN 202111366312 A CN202111366312 A CN 202111366312A CN 114107955 A CN114107955 A CN 114107955A
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- Prior art keywords
- graphite boat
- silicon nitride
- pretreatment process
- plating treatment
- washing
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 125
- 239000010439 graphite Substances 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 73
- 238000002161 passivation Methods 0.000 title claims abstract description 17
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 60
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000007747 plating Methods 0.000 claims abstract description 59
- 238000005406 washing Methods 0.000 claims abstract description 33
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 16
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 16
- 238000002791 soaking Methods 0.000 claims abstract description 15
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 238000007599 discharging Methods 0.000 claims abstract description 3
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 34
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 24
- 229910000077 silane Inorganic materials 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 19
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 19
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 15
- 235000013842 nitrous oxide Nutrition 0.000 claims description 14
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 7
- 238000000576 coating method Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 6
- 239000010408 film Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 12
- 239000010703 silicon Substances 0.000 description 12
- 235000012431 wafers Nutrition 0.000 description 12
- 239000007888 film coating Substances 0.000 description 7
- 238000009501 film coating Methods 0.000 description 7
- 210000002381 plasma Anatomy 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005202 decontamination Methods 0.000 description 3
- 230000003588 decontaminative effect Effects 0.000 description 3
- 239000001272 nitrous oxide Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 101001073212 Arabidopsis thaliana Peroxidase 33 Proteins 0.000 description 1
- 101001123325 Homo sapiens Peroxisome proliferator-activated receptor gamma coactivator 1-beta Proteins 0.000 description 1
- 102100028961 Peroxisome proliferator-activated receptor gamma coactivator 1-beta Human genes 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- -1 aluminum ions Chemical class 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011268 retreatment Methods 0.000 description 1
- 239000000758 substrate Substances 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
- C23C16/458—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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
-
- 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
- C23C16/22—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
- C23C16/403—Oxides of aluminium, magnesium or beryllium
-
- 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
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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
- C23C16/505—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 radio frequency discharges
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- 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)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention provides a graphite boat pretreatment process for improving the back passivation uniformity of two-in-one equipment, which comprises the following steps: soaking and washing a used graphite boat by using a first acid solution, then washing by using a second acid solution, and drying after washing; 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.
Description
Technical Field
The invention belongs to the technical field of crystalline silicon solar cells, relates to a graphite boat pretreatment process for improving back passivation uniformity, and particularly relates to a graphite boat pretreatment process for improving back passivation uniformity of two-in-one equipment.
Background
PECVD is a process in which a gas containing atoms constituting a thin film is ionized by means of microwave or radio frequency to locally form plasma, which is chemically very reactive and is easily reacted to deposit a desired thin film on a substrate. The PECVD process needs to use a graphite boat, when the graphite boat is used, the thickness of a film deposited on the surface of a silicon wafer is easily uneven due to different surface states, and if the graphite boat is unstable, the back passivation effect and the front color are influenced, and the yield and the conversion efficiency of the battery plate are finally influenced.
The graphite boat used by the tubular PECVD is of a porous structure at present, and in order to deposit a uniform passivation film, a thicker passivation film layer needs to be deposited on the surface of a boat sheet in advance before use so as to eliminate the influence of the porous structure graphite boat sheet on the uniformity of a coated film. After the graphite boat is used for a certain number of times, the coated film layer on the surface of the graphite boat is too thick, so that the coated film is poor, and the graphite boat needs to be washed by acid again and then dried. Usually, the graphite boat is plated with the SiC film, so that the surface of the graphite boat is smooth, but the SiC film is not easy to corrode and is difficult to clean and popularize.
With the large-scale application of the PERC technology, particularly when the two-in-one equipment is used for coating, aluminum ions generated by the reaction of aluminum oxide coated on the graphite boat are difficult to be removed by hydrofluoric acid, and the graphite boat body is polluted to a certain extent. In addition, the graphite boat after being cleaned again has a rough surface and obviously better conductivity, and the graphite boat can absorb more plasmas in the film coating process, so that the thickness of the deposited film in the edge area of the silicon wafer is thinner. Therefore, the surface of the graphite boat is pretreated, so that the surface of the graphite boat is flattened, plasma absorption of boat sheets during film coating is reduced, and the method has great significance for improving the back film coating effect in the early stage.
Therefore, it is an urgent problem to provide a pretreatment process for improving the passivation film on the surface of the graphite boat, so as to flatten the surface of the graphite boat after re-cleaning and to prevent the graphite boat from absorbing TMA (trimethyl aluminum) plasma during use.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a graphite boat pretreatment process for improving the back passivation uniformity of two-in-one equipment, the pretreatment process optimizes a cleaning method for the used graphite boat, and meanwhile, in the process of retreatment, a silicon nitride layer and an aluminum oxide layer are added on the basis of the traditional process, so that the surface flatness of the graphite boat is improved, and the improvement of the back film coating effect is facilitated.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a graphite boat pretreatment process for improving the back passivation uniformity of a two-in-one apparatus, wherein the pretreatment process comprises the following steps:
providing a graphite boat to be cleaned after use;
(1) soaking and washing the graphite boat by adopting a first acid solution, then cleaning by adopting a second acid solution, and drying after cleaning;
(2) sequentially carrying out constant temperature treatment, first silicon nitride plating treatment and silicon oxide plating treatment on the graphite boat dried in the step (1), and then discharging the graphite boat;
(3) and (3) sequentially carrying out second silicon nitride plating treatment and aluminum oxide plating treatment on the graphite boat treated in the step (2) to finish the pretreatment process.
In the invention, the pretreatment process effectively improves the decontamination capability of the used graphite boat by adopting a soaking and washing and acid washing mode; then, on the basis of a conventional coating (namely a first silicon nitride layer and a silicon oxide layer), a silicon nitride layer is pre-coated to further increase the surface flatness, and then an aluminum oxide layer is deposited to ensure that ionized gas is not easily absorbed by the boat when the silicon wafer is coated with an aluminum oxide passivation film in the early stage, so as to achieve a better back passivation effect; the pretreatment process provided by the invention does not increase the difficulty of cleaning the graphite boat after the graphite boat is used for a certain number of times, is simple and convenient in practical process and easy to popularize, and is beneficial to improving the film coating uniformity of the battery piece and improving the yield and conversion efficiency.
In the invention, the graphite boat processed in the step (2) can be temporarily stored after being taken out of the boat, and then is processed in the step (3) when being used.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferred technical solution of the present invention, the first acid solution in step (1) comprises hydrochloric acid.
Preferably, the concentration of the first acid solution in step (1) is 0.5 to 2 wt%, such as 0.5 wt%, 0.7 wt%, 0.9 wt%, 1.1 wt%, 1.3 wt%, 1.5 wt%, 1.7 wt%, or 2 wt%, etc., but is not limited to the recited values, and other non-recited values within this range are equally applicable.
Preferably, the soaking and washing time in step (1) is 20-60min, such as 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min or 60min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the second acid solution of step (1) comprises hydrofluoric acid.
Preferably, the concentration of the second acid solution in step (1) is 10-20% wt, such as 10%, 12%, 14%, 16%, 18% wt or 20% wt, and the like, but is not limited to the recited values, and other values not recited within the range are equally applicable.
Preferably, the washing time in step (1) is 6-10h, such as 6h, 7h, 8h, 9h or 10h, but not limited to the recited values, and other values not recited in the range of values are also applicable.
As a preferable technical means of the present invention, water washing is performed between the washing and the drying in the step (1).
Preferably, the number of water washes is 5-8, such as 5, 6, 7, or 8, but not limited to the recited values, and other values not recited within this range are equally applicable.
Preferably, each washing time is 30-60min, such as 30min, 35min, 40min, 45min, 50min, 55min or 60min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, after said washing, the graphite boat surface has a pH of 5 to 7, such as 5, 6 or 7, but not limited to the recited values, and other values not recited within this range of values are equally applicable.
As a preferable technical scheme of the invention, the drying in the step (1) comprises natural draining and drying which are sequentially carried out.
Preferably, the temperature of the drying is 120-180 ℃, such as 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃ or 180 ℃, but not limited to the recited values, and other unrecited values within the range of values are also applicable.
Preferably, the drying time is 5-10h, such as 5h, 6h, 7h, 8h, 9h or 10h, but not limited to the recited values, and other values not recited in the range of values are also applicable.
As a preferred embodiment of the present invention, the temperature of the constant temperature treatment in step (2) includes 400-500 deg.C, such as 120 deg.C, 130 deg.C, 140 deg.C, 150 deg.C, 160 deg.C, 170 deg.C or 180 deg.C, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the constant temperature treatment in step (2) is carried out for 10-30min, such as 10min, 15min, 20min, 25min or 30min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferred embodiment of the present invention, the operation of the first silicon nitride plating treatment in step (2) includes: and introducing silane and ammonia gas after vacuumizing, and plating a first silicon nitride layer on the surface of the graphite boat by adopting PECVD.
Preferably, the silane and ammonia gas are present in a volumetric flow ratio of 1 (6-12), such as 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, or 1:12, but not limited to the recited values, and other values not recited within this range are equally applicable.
Preferably, the pressure of the first silicon nitride plating treatment in step (2) is 1600-.
Preferably, the first silicon nitride plating treatment of step (2) includes a one-time full deposition or a batch deposition.
Preferably, the thickness of the first silicon oxide layer is 500-800nm, such as 500nm, 600nm, 700nm or 800nm, but not limited to the values listed, and other values not listed in the range of values are also applicable.
As a preferred technical scheme of the invention, the operation steps of the silicon oxide plating treatment in the step (2) comprise: and introducing silane and laughing gas after vacuumizing, and plating a silicon oxide layer on the surface of the graphite boat by adopting PECVD.
Preferably, the volumetric flow ratio of silane to laughing gas is 1 (6-10), for example 1:6, 1:7, 1:8, 1:9 or 1:10, but not limited to the recited values, and other values not recited in this range of values are equally applicable.
Preferably, the pressure of the silicon oxide plating treatment in step (2) is 1300-.
Preferably, the time of the silicon oxide plating treatment in the step (2) is 2 to 5min, such as 2min, 3min, 4min or 5min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferred embodiment of the present invention, the second silicon nitride plating step in step (3) includes: and introducing silane and ammonia gas after vacuumizing, and plating a second silicon nitride layer on the surface of the graphite boat.
Preferably, the volume flow ratio of silane to ammonia gas in the second silicon nitride plating treatment in step (3) is 1 (5-12), such as 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, or 1:12, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the temperature of the second silicon nitride plating treatment in step (3) is 370-420 ℃, such as 370 ℃, 380 ℃, 390 ℃, 400 ℃, 410 ℃ or 420 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the pressure of the second silicon nitride plating treatment in step (3) is 1600-.
Preferably, the time for plating the second silicon nitride layer in step (3) is 700-1500s, such as 700s, 800s, 900s, 1000s, 1100s, 1200s, 1300s, 1400s, 1500s, etc., but is not limited to the recited values, and other unrecited values within the range are also applicable.
As a preferable technical scheme of the invention, the operation steps of the aluminum oxide plating treatment in the step (3) comprise: and (3) introducing laughing gas and a trimethyl aluminum carrying source after vacuumizing, and plating an aluminum oxide layer on the surface of the graphite boat.
Preferably, the ratio of the volumetric flow rates of the laughing gas and the trimethylaluminum bearing source is (6-12):1, e.g., 6:1, 7:1, 8:1, 9:1, 10:1, 11:1 or 12:1, etc., but is not limited to the recited values, and other values not recited in this range of values are equally applicable.
Preferably, the temperature after the vacuum pumping in the step (3) is controlled at 400 ℃, for example, 330 ℃, 340 ℃, 350 ℃, 360 ℃, 370 ℃, 380 ℃, 390 ℃ or 400 ℃ and the like; then the temperature is reduced for 10-20min, and then laughing gas and trimethylaluminum are introduced, for example for 10min, 12min, 14min, 16min, 18min or 20min, etc., the selection of the above values is not limited to the recited values, and other values not recited in the respective numerical ranges are also applicable.
Preferably, the pressure of the alumina treatment in step (3) is 1100-.
Preferably, the time for plating the aluminum oxide layer in the step (3) is 2-5min, such as 2min, 3min, 4min or 5min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferable technical scheme of the invention, the pretreatment process comprises the following steps:
providing a graphite boat to be cleaned after use;
(1) soaking and washing the graphite boat for 20-60min by adopting hydrochloric acid with the concentration of 0.5-2 wt%, then washing for 6-10h by adopting hydrofluoric acid with the concentration of 10-20 wt%, and then washing for 5-8 times, wherein each time is 30-60min, and the pH value of the surface of the cleaned graphite boat is 5-7;
naturally draining the cleaned graphite boat, and drying at the temperature of 120-;
(2) the graphite boat dried in the step (1) is sent into a PECVD furnace tube with the temperature of 400-; after vacuumizing, introducing a mixture with the volume flow ratio of 1: (6-12) silane and ammonia gas, setting the pressure to be 1600-;
after the first silicon nitride layer is plated, vacuumizing is carried out, and then introducing a mixture of a silicon nitride layer and a silicon nitride layer with the volume flow ratio of 1: (6-10) setting the pressure of the silane and the laughing gas to be 1300-;
after the graphite boat is plated, closing a gas source and vacuumizing, and taking out the graphite boat for later use after residual gas in the tube is purged by nitrogen;
(3) and (3) sending the plated graphite boat into a furnace tube with the temperature of 370-420 ℃, and introducing a material with the volume flow ratio of 1: (5-12) depositing the silane and the ammonia gas on the surface of the graphite boat for 700-1500 seconds to form a second silicon nitride layer, wherein the pressure is set to be 1600-1900 mTorr;
and after the second silicon nitride layer is plated, vacuumizing, controlling the temperature at 330-.
In the invention, after the pretreatment process is finished, the gas source is closed and vacuumized, then the residual gas in the tube is purged by nitrogen, the plated graphite boat is taken out, and a silicon wafer is inserted in one hour for a back film plating process.
Compared with the prior art, the invention has the following beneficial effects:
(1) the pretreatment process disclosed by the invention has the advantages that the decontamination capability of the used graphite boat is effectively improved by adopting a soaking and pickling mode, and meanwhile, in the secondary treatment process, the silicon nitride layer and the aluminum oxide layer are added on the basis of the traditional process, so that the surface of the graphite boat is smoother, TMA (trimethylaluminum) plasma is not easy to absorb in use, the back coating effect of the aluminum oxide and the silicon nitride at the early stage is favorably improved, the coating uniformity of a battery piece is improved, and the yield and the conversion efficiency are improved;
(2) the pretreatment process of the invention does not need to access special gas CH4The process is simple and convenient, and is beneficial to industrial application.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a graphite boat pretreatment process for improving the back passivation uniformity of a two-in-one device, which comprises the following steps:
providing a graphite boat used for 60 times;
(1) soaking and washing the graphite boat for 30min by adopting hydrochloric acid with the concentration of 0.6 wt%, then washing for 7.2h by adopting hydrofluoric acid with the concentration of 13 wt%, then carrying out water for 6 times, 60min each time, and taking out the graphite boat after the pH value of the surface of the graphite boat is 6;
naturally draining the cleaned graphite boat, and drying at 130 ℃ for 7 h;
(2) sending the graphite boat dried in the step (1) into a PECVD furnace tube with the temperature of 450 ℃, carrying out constant temperature treatment for 15min, and then carrying out vacuum pumping; introducing 1050sccm silane and 7600sccm ammonia gas after vacuumizing, setting the pressure to 1700mTorr, turning on a radio frequency power supply, plating a first silicon nitride layer on the surface of the graphite boat by using PECVD, and depositing for 4 times in the whole process to form the first silicon nitride layer with the thickness of 600 nm;
after the first silicon nitride layer is plated, vacuumizing, introducing silane and nitrous oxide with the volume flow ratio of 700sccm and 5500sccm, setting the pressure to be 1500mTorr, turning on a radio frequency power supply, and plating a silicon oxide layer for 3min by adopting PECVD;
after the graphite boat is plated, closing a gas source and vacuumizing, and taking out the graphite boat for later use after residual gas in the tube is purged by nitrogen;
(3) sending the plated graphite boat into a furnace tube with the temperature of 375-;
and after the second silicon nitride layer is plated, vacuumizing is carried out, the temperature is controlled at 360 ℃, then the temperature is reduced for 10min, then 5500sccm of laughing gas and a trimethyl aluminum gas inlet source with the opening degree of 55% are introduced, the pressure is set to be 1300mTorr, a radio frequency power supply is turned on, and an aluminum oxide layer is plated on the surface of the graphite boat for 3min, so that the pretreatment process is completed.
Example 2:
the embodiment provides a graphite boat pretreatment process for improving the back passivation uniformity of a two-in-one device, which comprises the following steps:
providing a graphite boat used for 60 times;
(1) soaking and washing the graphite boat for 20min by adopting hydrochloric acid with the concentration of 2 wt%, then washing for 6h by adopting hydrofluoric acid with the concentration of 20 wt%, then carrying out water for 8 times, 30min each time, and taking out the graphite boat after the pH value of the surface of the graphite boat is 7;
naturally draining the cleaned graphite boat, and drying at 180 ℃ for 5 h;
(2) sending the graphite boat dried in the step (1) into a PECVD furnace tube with the temperature of 400 ℃, carrying out constant temperature treatment for 30min, and then carrying out vacuum pumping; introducing 1267sccm of silane and 7600sccm of ammonia gas after vacuumizing, setting the pressure to 1600mTorr, turning on a radio frequency power supply, plating a first silicon nitride layer on the surface of the graphite boat by using PECVD (plasma enhanced chemical vapor deposition), and depositing for 5 times in the whole process to form the first silicon nitride layer with the thickness of 750 nm;
after the first silicon nitride layer is plated, vacuumizing, introducing silane with the volume flow ratio of 460sccm and nitrous oxide with the volume flow ratio of 5500sccm, setting the pressure to be 1300mTorr, turning on a radio frequency power supply, and plating the silicon oxide layer for 2min by adopting PECVD;
after the graphite boat is plated, closing a gas source and vacuumizing, and taking out the graphite boat for later use after residual gas in the tube is purged by nitrogen;
(3) sending the plated graphite boat into a furnace tube with the temperature of 375-;
and after the second silicon nitride layer is plated, vacuumizing is carried out, the temperature is controlled at 330 ℃, then the temperature is reduced for 15min, then 5500sccm of laughing gas and a trimethyl aluminum gas inlet source with the opening degree of 55% are introduced, the pressure is set to be 1100mTorr, a radio frequency power supply is turned on, and an aluminum oxide layer is plated on the surface of the graphite boat for 5min, so that the pretreatment process is completed.
Example 3:
the embodiment provides a graphite boat pretreatment process for improving the back passivation uniformity of a two-in-one device, which comprises the following steps:
providing a graphite boat used for 60 times;
(1) soaking and washing the graphite boat for 20min by adopting hydrochloric acid with the concentration of 1 wt%, then washing for 7.2h by adopting hydrofluoric acid with the concentration of 10 wt%, then carrying out water for 6 times, 60min each time, and taking out the graphite boat after the pH value of the surface of the graphite boat is 6;
naturally draining the cleaned graphite boat, and drying at 120 ℃ for 10 h;
(2) sending the graphite boat dried in the step (1) into a PECVD furnace tube with the temperature of 500 ℃, carrying out constant temperature treatment for 30min, and then carrying out vacuum pumping; introducing silane of 633sccm and ammonia gas of 7600sccm after vacuumizing, setting the pressure to be 1900mTorr, turning on a radio frequency power supply, plating a first silicon nitride layer on the surface of the graphite boat by using PECVD, and depositing for 4 times in the whole process to form the first silicon nitride layer with the thickness of 550 nm;
after the first silicon nitride layer is plated, vacuumizing, introducing silane and nitrous oxide with the volume flow ratio of 917sccm and 5500sccm, setting the pressure to be 1600mTorr, turning on a radio frequency power supply, and plating a silicon oxide layer for 5min by adopting PECVD;
after the graphite boat is plated, closing a gas source and vacuumizing, and taking out the graphite boat for later use after residual gas in the tube is purged by nitrogen;
(3) the plated graphite boat is sent into a furnace tube with the temperature of 375-;
and after the second silicon nitride layer is plated, vacuumizing is carried out, the temperature is controlled at 400 ℃, then the temperature is reduced for 20min, then 5500sccm of laughing gas and a 65% opening trimethylaluminum gas inlet source are introduced, the pressure is set to be 1400mTorr, a radio frequency power supply is turned on, and an aluminum oxide layer is plated on the surface of the graphite boat for 2min, so that the pretreatment process is completed.
Comparative example 1:
this comparative example provides a pretreatment process for a graphite boat, which is referred to the pretreatment process of example 1, except that: the second silicon nitride layer and aluminum oxide layer plating operation of step (3) is not performed.
Comparative example 2:
this comparative example provides a pretreatment process for a graphite boat, which is referred to the pretreatment process of example 1, except that: the operation of plating the second silicon nitride layer of step (3) is not performed.
Comparative example 3:
this comparative example provides a pretreatment process for a graphite boat, which is referred to the pretreatment process of example 1, except that: the operation of plating the alumina layer of the step (3) is not performed.
Comparative example 4:
this comparative example provides a pretreatment process for a graphite boat, which is referred to the pretreatment process of example 1, except that: in the step (1), hydrochloric acid is not adopted for soaking and washing.
The graphite boat after the pretreatment process of examples 1 to 3 and comparative examples 1 to 4 was taken out, and the silicon wafer was inserted for one hour to perform a back film plating operation (only the surface of the silicon wafer was plated with an aluminum oxide layer). After the back film plating operation was completed, the silicon wafers at the furnace mouth, the furnace and the furnace tail were sampled and the thickness and uniformity deviation of the alumina layer were measured, and the results are shown in table 1.
TABLE 1
Embodiments 1-3 adopt the pretreatment process of the present invention, which effectively reduces the film thickness range of the alumina layer during the film coating of the silicon wafer after the newly cleaned graphite boat is used on line, and improves the film coating uniformity.
Comparative example 1 the cleaned graphite boat was pretreated only conventionally, resulting in a uniformity deviation of the alumina layer of the silicon wafer of > 9%; comparative example 2 only one alumina layer is added on the basis of the conventional pretreatment mode, so that the boat surface is loose, and the uniformity deviation of the alumina layer of the silicon wafer is more than 12%; comparative example 3 only one silicon nitride layer is added on the basis of the conventional pretreatment mode, so that the aluminum oxide layer of the silicon wafer is thin and the uniformity deviation is more than 9 percent; comparative example 4 in the cleaning process, hydrochloric acid is not used for soaking and cleaning, but hydrofluoric acid is directly used for pickling, so that the cleaning is not thorough, and the uniformity of the aluminum oxide layer is poor when the back film plating is carried out on the silicon wafer in the later period.
It can be seen from the above examples and comparative examples that the pretreatment process of the present invention employs a soaking and pickling method to effectively improve the decontamination capability of the used graphite boat, and a silicon nitride layer and an aluminum oxide layer are added on the basis of the conventional process in the secondary treatment processThe graphite boat has smoother surface, and TMA (trimethyl aluminum) plasma is not easy to absorb when in use, thus being beneficial to improving the back coating effect of the earlier-stage aluminum oxide and silicon nitride, and further improving the coating uniformity of the cell, the yield and the conversion efficiency; the pretreatment process does not need to access special gas CH4The process is simple and convenient, and is beneficial to industrial application.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents thereof, additions of additional operations, selection of specific ways, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A graphite boat pretreatment process for improving the back passivation uniformity of two-in-one equipment is characterized by comprising the following steps:
providing a graphite boat to be cleaned after use;
(1) soaking and washing the graphite boat by adopting a first acid solution, then cleaning by adopting a second acid solution, and drying after cleaning;
(2) sequentially carrying out constant temperature treatment, first silicon nitride plating treatment and silicon oxide plating treatment on the graphite boat dried in the step (1), and then discharging the graphite boat;
(3) and (3) sequentially carrying out second silicon nitride plating treatment and aluminum oxide plating treatment on the graphite boat treated in the step (2) to finish the pretreatment process.
2. The pretreatment process of claim 1, wherein the first acid solution of step (1) comprises hydrochloric acid;
preferably, the concentration of the first acid solution in the step (1) is 0.5-2 wt%;
preferably, the soaking and washing time in the step (1) is 20-60 min;
preferably, the second acid solution of step (1) comprises hydrofluoric acid;
preferably, the concentration of the second acid solution in the step (1) is 10-20% wt;
preferably, the washing time in the step (1) is 6-10 h.
3. The pretreatment process according to claim 1 or 2, wherein a water washing is performed between the washing and the drying of step (1);
preferably, the number of times of water washing is 5 to 8;
preferably, the time of each water washing is 30-60 min;
preferably, after the water washing, the pH value of the surface of the graphite boat is 5-7.
4. The pretreatment process according to any one of claims 1 to 3, wherein the drying of step (1) comprises sequential natural draining drying;
preferably, the drying temperature is 120-180 ℃;
preferably, the drying time is 5-10 h.
5. The pretreatment process according to any one of claims 1 to 4, wherein the constant temperature treatment in step (2) comprises 400-500 ℃;
preferably, the constant temperature treatment time in the step (2) is 10-30 min.
6. The pretreatment process according to any one of claims 1 to 5, wherein the operation of the first silicon nitride plating treatment of step (2) comprises: vacuumizing, introducing silane and ammonia gas, and plating a first silicon nitride layer on the surface of the graphite boat by adopting PECVD;
preferably, the volume flow ratio of the silane to the ammonia gas is 1 (6-12);
preferably, the pressure of the first silicon nitride plating treatment in the step (2) is 1600-1900 mTorr;
preferably, the first silicon nitride plating treatment of step (2) comprises a one-time full deposition or a batch deposition;
preferably, the thickness of the first silicon nitride layer is 500-800 nm.
7. The pretreatment process according to any one of claims 1 to 6, wherein the step (2) of silicon oxide plating treatment comprises the steps of: introducing silane and laughing gas after vacuumizing, and plating a silicon oxide layer on the surface of the graphite boat by adopting PECVD;
preferably, the volume flow ratio of the silane to the laughing gas is 1 (6-10);
preferably, the pressure of the silicon oxide plating treatment in the step (2) is 1300-;
preferably, the time of the silicon oxide plating treatment in the step (2) is 2-5 min.
8. The pretreatment process according to any one of claims 1 to 7, wherein the operation of the second silicon nitride plating treatment of step (3) comprises: vacuumizing, introducing silane and ammonia gas, and plating a second silicon nitride layer on the surface of the graphite boat;
preferably, the volume flow ratio of silane to ammonia gas in the second silicon nitride plating treatment in the step (3) is 1 (5-12);
preferably, the temperature of the second silicon nitride plating treatment in the step (3) is 370-420 ℃;
preferably, the pressure of the second silicon nitride plating treatment in the step (3) is 1600-1900 mTorr;
preferably, the time for plating the second silicon nitride layer in the step (3) is 700-.
9. The pretreatment process according to any one of claims 1 to 8, wherein the step (3) of the alumina plating treatment comprises: vacuumizing, introducing laughing gas and a trimethyl aluminum carrying source, and plating an aluminum oxide layer on the surface of the graphite boat;
preferably, the ratio of the volume flow rates of the laughing gas and the trimethylaluminum carrying source is (6-12) to 1;
preferably, the temperature after the vacuum pumping in the step (3) is controlled to be at 330-;
preferably, the pressure of the alumina treatment in the step (3) is 1100-;
preferably, the time for plating the aluminum oxide layer in the step (3) is 2-5 min.
10. The pretreatment process according to any one of claims 1 to 9, wherein the pretreatment process comprises the steps of:
providing a graphite boat to be cleaned after use;
(1) soaking and washing the graphite boat for 20-60min by adopting hydrochloric acid with the concentration of 0.5-2 wt%, then washing for 6-10h by adopting hydrofluoric acid with the concentration of 10-20 wt%, and then washing for 5-8 times, wherein each time is 30-60min, and the pH value of the surface of the cleaned graphite boat is 5-7;
naturally draining the cleaned graphite boat, and drying at the temperature of 120-;
(2) the graphite boat dried in the step (1) is sent into a PECVD furnace tube with the temperature of 400-; after vacuumizing, introducing a mixture with the volume flow ratio of 1: (6-12) silane and ammonia gas, setting the pressure to be 1600-;
after the first silicon nitride layer is plated, vacuumizing is carried out, and then introducing a mixture of a silicon nitride layer and a silicon nitride layer with the volume flow ratio of 1: (6-10) setting the pressure of the silane and the laughing gas to be 1300-;
after the graphite boat is plated, closing a gas source and vacuumizing, and taking out the graphite boat for later use after residual gas in the tube is purged by nitrogen;
(3) and (3) sending the plated graphite boat into a furnace tube with the temperature of 370-420 ℃, and introducing a material with the volume flow ratio of 1: (5-12) depositing the silane and the ammonia gas on the surface of the graphite boat for 700-1500 seconds to form a second silicon nitride layer, wherein the pressure is set to be 1600-1900 mTorr;
and after the second silicon nitride layer is plated, vacuumizing, controlling the temperature at 330-.
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Denomination of invention: A graphite boat pre-treatment process for improving the uniformity of passivation on the back of a two in one device Granted publication date: 20221220 Pledgee: Dongyang Branch of China Construction Bank Co.,Ltd. Pledgor: HENGDIAN GROUP DMEGC MAGNETICS Co.,Ltd. Registration number: Y2024330000801 |
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