CN115233181A - Phosphorus-doped polycrystalline silicon film, preparation method and application thereof - Google Patents
Phosphorus-doped polycrystalline silicon film, preparation method and application thereof Download PDFInfo
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- CN115233181A CN115233181A CN202210886651.XA CN202210886651A CN115233181A CN 115233181 A CN115233181 A CN 115233181A CN 202210886651 A CN202210886651 A CN 202210886651A CN 115233181 A CN115233181 A CN 115233181A
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 60
- 239000010703 silicon Substances 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 50
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 238000000151 deposition Methods 0.000 claims abstract description 37
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 230000008021 deposition Effects 0.000 claims abstract description 34
- 238000004050 hot filament vapor deposition Methods 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000007789 gas Substances 0.000 claims abstract description 21
- 238000000137 annealing Methods 0.000 claims abstract description 18
- 229910021417 amorphous silicon Inorganic materials 0.000 claims abstract description 14
- 239000005922 Phosphane Substances 0.000 claims abstract description 11
- 229910000064 phosphane Inorganic materials 0.000 claims abstract description 11
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims abstract description 11
- 230000001681 protective effect Effects 0.000 claims abstract description 11
- 238000005086 pumping Methods 0.000 claims abstract description 3
- 239000012495 reaction gas Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 48
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- 229920005591 polysilicon Polymers 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 15
- 239000012159 carrier gas Substances 0.000 claims description 13
- 238000002161 passivation Methods 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims description 9
- 239000011574 phosphorus Substances 0.000 claims description 9
- 238000009489 vacuum treatment Methods 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims 2
- 238000007664 blowing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 8
- 230000004913 activation Effects 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 71
- 235000012431 wafers Nutrition 0.000 description 46
- 238000000354 decomposition reaction Methods 0.000 description 10
- 238000009792 diffusion process Methods 0.000 description 10
- 239000000758 substrate Substances 0.000 description 9
- 230000005855 radiation Effects 0.000 description 8
- 230000005641 tunneling Effects 0.000 description 7
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 6
- 229910052581 Si3N4 Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 125000004437 phosphorous atom Chemical group 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/24—Deposition of silicon only
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- 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
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- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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Abstract
The invention provides a phosphorus-doped polycrystalline silicon film, a preparation method and application thereof, wherein the preparation method comprises the following steps: taking tetraethoxysilane and phosphine as reaction gas sources, and depositing on the surface of a silicon wafer in a reaction cavity by adopting a hot filament chemical vapor deposition method to obtain a phosphorus-doped amorphous silicon film; and (3) pumping out gas in the reaction cavity, introducing protective gas, adjusting the distance of a hot wire in a hot wire chemical vapor deposition method to heat and anneal the phosphorus-doped amorphous silicon film, and preparing the phosphorus-doped polycrystalline silicon film after heating and annealing. The invention takes phosphane and tetraethoxysilane as raw materials, prepares a phosphorus-doped polycrystalline silicon film by using a hot wire chemical vapor deposition method, realizes catalytic deposition and annealing heating activation by adjusting the distance of a hot wire, greatly shortens the preparation time and avoids the pollution of atmosphere to a phosphorus-doped amorphous silicon film.
Description
Technical Field
The invention belongs to the technical field of solar cells, and relates to a phosphorus-doped polycrystalline silicon film, and a preparation method and application thereof.
Background
The TOPCon battery, namely a tunneling oxide layer passivation contact battery, is based on an N-type silicon wafer, the front side adopts an aluminum oxide coating and a silicon nitride coating to passivate a boron diffusion emitter, and the core technology of the battery is back passivation contact: a layer of ultrathin silicon oxide (SiO) is adopted on the back surface 2 ) The film and a layer of phosphorus doped polysilicon (Poly-Si) film are used as a passivation layer.
The mainstream route of the phosphorus-doped poly-Si thin film used in TOPCon technology at present is intrinsic + phosphorus diffusion, i.e. a polysilicon film prepared by LPCVD is combined with a phosphorus diffusion process. The LPCVD decomposes the introduced silane by utilizing the conditions of high temperature and low pressure to deposit a layer of microcrystalline and amorphous mixed silicon-based film; and then, the mixed silicon-based microcrystalline amorphous film enters a diffusion furnace for P doping, the passivation performance is activated under the high-temperature condition, and the crystallinity of the mixed silicon-based microcrystalline amorphous film is changed at high temperature and gradually changed into polycrystal.
However, the LPCVD and phosphorus diffusion methods have long preparation time, need two devices for completion, and are not beneficial to the improvement of productivity in the large-scale growth process; in addition, during the transferring process, the silicon wafer is easily polluted, and the efficiency and yield of the battery piece are affected.
CN111276568A discloses a passivated contact solar cell and a preparation method thereof, wherein the solar cell comprises an N-type crystal silicon substrate, and the front surface of the N-type crystal silicon substrate sequentially comprises an emitter layer, an aluminum oxide passivation layer, a silicon nitride antireflection layer and a metal slurry layer from bottom to top; the back surface of the N-type crystal silicon substrate sequentially comprises a tunneling oxide layer, a phosphorus-doped polycrystalline silicon layer, a silicon nitride antireflection layer and a metal slurry layer from bottom to top.
Therefore, how to provide a method for preparing a phosphorus-doped polysilicon film, which reduces film contamination and increases the preparation rate, is a technical problem that needs to be solved urgently at present.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a phosphorus-doped polycrystalline silicon film, a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a phosphorus-doped polycrystalline silicon film, the method comprising the steps of:
depositing a phosphorus-doped amorphous silicon film on the surface of a silicon wafer in a reaction cavity by adopting a hot filament chemical vapor deposition method by taking tetraethoxysilane and phosphine as reaction gas sources;
and (3) pumping out gas in the reaction cavity, introducing protective gas, adjusting the distance of a hot wire in a hot wire chemical vapor deposition method to heat and anneal the phosphorus-doped amorphous silicon film, and preparing the phosphorus-doped polycrystalline silicon film after heating and annealing.
The method is based on hot wire chemical vapor deposition equipment, the preparation of the phosphorus-doped amorphous silicon film is completed only by introducing protective gas into a reaction cavity and adjusting the distance of a hot wire, phosphine and tetraethoxysilane are used as raw materials in the hot wire chemical vapor deposition equipment, then heating annealing is carried out, the hot wire is close to the surface of the silicon wafer, the silicon wafer is rapidly heated by using the heat radiation of the hot wire, rapid annealing is realized, doped phosphorus atoms are activated, and the phosphorus-doped polycrystalline silicon film is prepared.
It should be noted that the invention does not make specific requirements and special limitations on the types of silicon wafers, and those skilled in the art can reasonably select the silicon wafer according to the actual deposition requirements, for example, the silicon wafer is an N-type silicon wafer which has been prepared by a tunneling oxide layer.
As a preferable technical scheme of the invention, the silicon wafer is subjected to preheating treatment in a vacuum state, and the silicon wafer is subjected to preheating treatment in a vacuum stateThe temperature of the preheating treatment is 100 to 200 ℃ and is, for example, 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ or 200 ℃. Optionally, the pressure in the vacuum state is less than or equal to 10 -4 Pa。
Preferably, the reaction chamber is subjected to vacuum treatment. Optionally, the pressure in the reaction chamber after vacuum treatment is less than or equal to 10 -4 Pa。
As a preferred embodiment of the present invention, the temperature of the hot wire in the hot wire chemical vapor deposition method is 1600 to 2000 ℃, for example, 1600 ℃, 1650 ℃, 1700 ℃, 1750 ℃, 1800 ℃, 1850 ℃, 1900 ℃, 1950 ℃ or 2000 ℃. Optionally, the hot wire is preheated in vacuum before the hot wire chemical vapor deposition reaction, and the preheating temperature is 1000-1200 ℃.
The invention ensures the decomposition efficiency of the raw materials and the decomposition products by controlling the temperature of the hot wire to be 1600-2000 ℃ in the chemical vapor deposition process of the hot wire, thereby avoiding the generation of by-products in the reaction process from influencing the film quality. If the temperature is lower than 1600 ℃, not only the decomposition efficiency of the raw material is affected, but also the decomposition product has adverse substances, affecting the film performance.
Preferably, the deposition pressure in the hot filament chemical vapor deposition method is 1 to 50Pa, such as 1Pa, 5Pa, 10Pa, 15Pa, 20Pa, 25Pa, 30Pa, 35Pa, 40Pa, 45Pa or 50Pa.
According to the invention, by controlling the deposition pressure to be 1-50 Pa, the film forming quality is prevented from being influenced by overlarge concentration of the phosphane under the condition of ensuring the deposition rate, if the deposition pressure is lower than 1Pa, the film deposition efficiency is influenced, and if the deposition pressure is higher than 50Pa, the concentration of the phosphane is increased, and a Si-H-P compound without electric activity is easily generated, so that the carrier concentration is reduced, and the film forming quality is influenced.
Preferably, the distance between the hot wire and the silicon wafer in the hot wire chemical vapor deposition method is 40-150 mm, such as 40mm, 50mm, 60mm, 70mm, 80mm, 90mm, 100mm, 110mm, 120mm, 130mm, 140mm or 150mm, and preferably 45mm.
As a preferred technical solution of the present invention, the volume flow ratio of the phosphane to the nitrogen gas is 1: (9 to 99), for example, 1.
As a preferable technical scheme of the invention, the tetraethoxysilane is blown by carrier gas through tetraethoxysilane liquid and carried into the reaction cavity.
Preferably, the concentration of tetraethoxysilane in the reaction chamber is 10-30%, such as 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28% or 30%.
Preferably, the temperature of the tetraethoxysilane liquid is 85 to 100 ℃, for example 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃, 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or 100 ℃.
The carrier gas is brought into the tetraethoxysilane, namely the carrier gas blows through tetraethoxysilane liquid, so that the tetraethoxysilane is brought into the reaction cavity according to the evaporation effect, the concentration of the tetraethoxysilane entering the reaction cavity is further ensured by controlling the temperature of the tetraethoxysilane liquid, when the temperature is lower than 85 ℃, the concentration of the gaseous tetraethoxysilane is low, the reaction amount is small, the deposition efficiency is influenced, and when the temperature is higher than 100 ℃, the concentration of the gaseous tetraethoxysilane is high, the decomposition is easy to be incomplete, so that impurity particles exist in a deposited film, and the film forming quality is influenced.
Preferably, the carrier gas comprises nitrogen.
As a preferred embodiment of the present invention, the shielding gas includes nitrogen.
Preferably, in the heating annealing process, the distance between the hot wire and the phosphorus-doped amorphous silicon film is 2-10 mm, such as 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm or 10mm, and preferably 5mm.
The invention respectively controls the hot wire distance in the hot wire chemical vapor deposition process and the heating annealing process, thereby ensuring the temperature in the hot wire chemical vapor deposition process and the annealing heating process and ensuring that the two processes are carried out in a proper temperature state.
Preferably, the pressure of the heating annealing is the same as the deposition pressure in the hot wire chemical vapor deposition method.
Preferably, the time for the heat annealing is 50 to 150s, for example 50s, 60s, 70s, 80s, 90s, 100s, 110s, 120s, 130s, 140s, or 150s.
Illustratively, there are provided specific steps of the above method for preparing a phosphorus-doped polysilicon film, the steps including:
the first step is as follows: placing the silicon chip in a preheating cavity of hot filament chemical vapor deposition equipment, and vacuumizing to 10 DEG -4 Pa, preheating the substrate at the preheating temperature of 100-200 ℃; simultaneously, the reaction cavity is also vacuumized to 10 DEG -4 Pa, preheating and heating the hot wire;
the second step is that: transferring the preheated silicon wafer into a reaction cavity, adjusting the distance between a hot wire and the silicon wafer to be 40-150 mm, and heating the hot wire to 1600-2000 ℃;
the third step: introducing phosphane and tetraethoxysilane, wherein tetraethoxysilane is carried into the reaction cavity by taking nitrogen as carrier gas, the liquid temperature of tetraethoxysilane is 85-100 ℃, the volume flow ratio of phosphane to nitrogen is 1 (9-99), and the phosphorated amorphous silicon film is obtained by deposition under the deposition pressure of 1-50 Pa;
the fourth step: after the deposition is finished, the gas in the reaction chamber is pumped out to 10 -4 Pa, introducing nitrogen as protective gas, wherein the pressure intensity is the same as the deposition pressure intensity after introducing the nitrogen; adjusting the distance between the hot wire and the silicon wafer to be 2-10 mm, rapidly heating the silicon wafer through the heat radiation of the temperature of the hot wire for 50-150 s, and preparing the phosphorus-doped polycrystalline silicon film with the thickness of 100-200 nm.
In a second aspect, the present invention provides a phosphorus-doped polysilicon film, which is prepared by the method for preparing a phosphorus-doped polysilicon film according to the first aspect.
In a preferred embodiment of the present invention, the thickness of the phosphorus-doped polysilicon film is 100 to 200nm, for example, 100nm, 110nm, 120nm, 130nm, 140nm, 150nm, 160nm, 170nm, 180nm, 190nm, or 200nm.
In a third aspect, the present invention provides a solar cell comprising a passivation layer employing the phosphorus-doped polysilicon film of the second aspect.
As a preferred embodiment of the present invention, the solar cell is a TOPCon cell.
Illustratively, a TOPCon cell structure is provided, which comprises an N-type silicon wafer, wherein the front surface of the N-type silicon wafer is coated with aluminum oxide and silicon nitride to passivate a boron diffusion emitter, and the back surface of the N-type silicon wafer is coated with an ultra-thin silicon oxide film and a phosphorus-doped polysilicon film as passivation layers, wherein the phosphorus-doped polysilicon film is a phosphorus-doped polysilicon film according to the present invention.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the following beneficial effects:
the method is based on hot wire chemical vapor deposition equipment, the preparation of the phosphorus-doped amorphous silicon film is completed only by introducing protective gas into a reaction cavity and adjusting the distance of a hot wire, phosphine and tetraethoxysilane are used as raw materials in the hot wire chemical vapor deposition equipment, then heating annealing is carried out, the hot wire is close to the surface of the silicon wafer, the silicon wafer is rapidly heated by using the heat radiation of the hot wire, rapid annealing is realized, doped phosphorus atoms are activated, and the phosphorus-doped polycrystalline silicon film is prepared.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific 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 limitation of the present invention.
Example 1
The embodiment provides a preparation method of a phosphorus-doped polycrystalline silicon film, which specifically comprises the following steps:
the first step is as follows: placing the N-type silicon wafer with the tunneling oxide layer in a preheating cavity of hot filament chemical vapor deposition equipment, and vacuumizing to 10 DEG -4 Pa, preheating the substrate at the temperature of 150 ℃; simultaneously, the reaction cavity is also vacuumized to 10 DEG -4 Pa, preheating the hot wire to 1000 ℃;
the second step is that: transferring the preheated silicon wafer into a reaction chamber, adjusting the distance between a hot wire and the silicon wafer to be 40mm, and heating the hot wire to 1800 ℃;
the third step: introducing phosphine and tetraethoxysilane, wherein the tetraethoxysilane is carried into the reaction cavity by taking nitrogen as a carrier gas, the temperature of tetraethoxysilane liquid is 85 ℃, the volume flow ratio of the phosphine to the nitrogen is 1;
the fourth step: after the deposition is finished, the gas in the reaction chamber is pumped out to 10 -4 Pa, introducing nitrogen as protective gas, wherein the pressure intensity after introducing nitrogen is the same as the deposition pressure intensity and is 50Pa; adjusting the distance between the hot wire and the silicon wafer to be 3mm, and quickly heating the silicon wafer through the heat radiation of the temperature of the hot wire for 50-120 s to prepare a phosphorus-doped polycrystalline silicon film with the thickness of 150 nm.
Example 2
The embodiment provides a preparation method of a phosphorus-doped polycrystalline silicon film, which specifically comprises the following steps:
the first step is as follows: placing the N-type silicon wafer with the tunneling oxide layer in a preheating cavity of hot filament chemical vapor deposition equipment, and vacuumizing to 10 DEG -4 Pa, preheating the substrate at the preheating temperature of 100 ℃; simultaneously, the reaction cavity is also vacuumized to 10 DEG -4 Preheating a hot wire to 1000 ℃ under Pa;
the second step is that: transferring the preheated silicon wafer into a reaction cavity, adjusting the distance between a hot wire and the silicon wafer to be 50mm, and heating the hot wire to 2000 ℃;
the third step: introducing phosphine and tetraethoxysilane, wherein tetraethoxysilane is carried into the reaction cavity by taking nitrogen as carrier gas, the liquid temperature of tetraethoxysilane is 85 ℃, the volume flow ratio of the phosphine to the nitrogen is 1;
the fourth step: after the deposition is finished, the gas in the reaction chamber is pumped out to 10 -4 Pa, introducing nitrogen as protective gas, wherein the pressure intensity after introducing nitrogen is the same as the deposition pressure intensity and is 20Pa; and adjusting the distance between the hot wire and the silicon wafer to be 5mm, rapidly heating the silicon wafer through the heat radiation of the temperature of the hot wire for 80s, and preparing the phosphorus-doped polycrystalline silicon film with the thickness of 120 nm.
Example 3
The embodiment provides a preparation method of a phosphorus-doped polycrystalline silicon film, which specifically comprises the following steps:
the first step is as follows: placing the N-type silicon wafer with the tunneling oxide layer in a preheating cavity of hot filament chemical vapor deposition equipment, and vacuumizing to 10 DEG -4 Pa, preheating the substrate at the preheating temperature of 200 ℃; meanwhile, the reaction cavity is also vacuumized to 10 DEG -4 Pa, preheating the hot wire to 1000 ℃;
the second step is that: transferring the preheated silicon wafer into a reaction cavity, adjusting the distance between a hot wire and the silicon wafer to be 150mm, and heating the hot wire to 1900 ℃;
the third step: introducing phosphane and tetraethoxysilane, wherein tetraethoxysilane is carried into the reaction cavity by taking nitrogen as carrier gas, the liquid temperature of tetraethoxysilane is 100 ℃, the volume flow ratio of phosphane to nitrogen is 1;
the fourth step: after the deposition is finished, the gas in the reaction chamber is pumped out to 10 -4 Pa, introducing nitrogen as protective gas, wherein the pressure intensity is the same as the deposition pressure intensity and is 5Pa after introducing the nitrogen; adjusting the distance between the hot wire and the silicon wafer to be 10mm, rapidly heating the silicon wafer through the heat radiation of the temperature of the hot wire for 50s, and preparing the phosphorus-doped polycrystalline silicon film with the thickness of 100 nm.
Example 4
The embodiment provides a preparation method of a phosphorus-doped polycrystalline silicon film, which specifically comprises the following steps:
the first step is as follows:placing the N-type silicon wafer with the tunneling oxide layer in a preheating cavity of hot filament chemical vapor deposition equipment, and vacuumizing to 10 DEG -4 Pa, preheating the substrate at the preheating temperature of 120 ℃; simultaneously, the reaction cavity is also vacuumized to 10 DEG -4 Preheating a hot wire to 1000 ℃ under Pa;
the second step is that: transferring the preheated silicon wafer into a reaction cavity, adjusting the distance between a hot wire and the silicon wafer to be 100mm, and heating the hot wire to 1600 ℃;
the third step: introducing phosphane and tetraethoxysilane, wherein tetraethoxysilane is carried into the reaction cavity by taking nitrogen as carrier gas, the liquid temperature of tetraethoxysilane is 90 ℃, the volume flow ratio of phosphane to nitrogen is 1 to 99, and the phosphorus-doped amorphous silicon film is obtained by deposition under the deposition pressure of 40Pa;
the fourth step: after the deposition is finished, the gas in the reaction chamber is pumped out to 10 -4 Introducing nitrogen as protective gas under the pressure of 40Pa, wherein the pressure is the same as the deposition pressure; and adjusting the distance between the hot wire and the silicon wafer to be 2mm, rapidly heating the silicon wafer through the heat radiation of the temperature of the hot wire for 80s, and preparing the phosphorus-doped polycrystalline silicon film with the thickness of 120 nm.
Example 5
This example provides a method for preparing a phosphorus-doped polycrystalline silicon film, which is different from example 1 in that the temperature of a hot filament in a hot filament chemical vapor deposition method is 1500 ℃, and the remaining parameters and steps are exactly the same as those of example 1.
Example 6
This example provides a method for preparing a phosphorus-doped polycrystalline silicon film, which is different from example 1 in that the temperature of a hot filament in a hot filament chemical vapor deposition method is 2200 ℃, and the remaining parameters and steps are identical to those of example 1.
Example 7
This example provides a method for preparing a phosphorus-doped polycrystalline silicon film, which is different from example 1 in that the deposition pressure in the hot filament chemical vapor deposition method is 0.05Pa, and the remaining parameters and steps are identical to those of example 1.
Example 8
This example provides a method for preparing a phosphorus-doped polycrystalline silicon film, which is different from example 1 in that the deposition pressure in the hot filament chemical vapor deposition method is 60Pa, and the remaining parameters and steps are exactly the same as those of example 1.
Example 9
This example provides a method for preparing a phosphorus-doped polycrystalline silicon film, which is different from example 1 in that the temperature of the tetraethoxysilane liquid is 70 deg.c, and the remaining parameters and steps are identical to those of example 1.
Example 10
This example provides a method for preparing a phosphorus-doped polysilicon film, which is different from example 1 in that the temperature of the tetraethoxysilane liquid is 110 deg.c, and the remaining parameters and steps are exactly the same as those of example 1.
Comparative example 1
The present comparative example provides a method for preparing a phosphorus-doped polysilicon film, which is a method of intrinsic + phosphorus diffusion in the prior art, and specifically comprises the following steps:
preparing a polycrystalline silicon film by LPCVD (low pressure chemical vapor deposition) and combining a phosphorus diffusion process, decomposing introduced silane by LPCVD under the conditions of high temperature and low pressure (the temperature is 610 ℃ and the pressure is 120 mTorr) to deposit a layer of microcrystalline amorphous mixed silicon-based film; and then, the silicon substrate enters a diffusion furnace for phosphorus doping, the passivation performance is activated under the high-temperature condition (the temperature is 920 ℃), and the crystallinity of the microcrystalline amorphous mixed silicon-based thin film is changed at high temperature and is gradually converted into a phosphorus-doped polycrystalline silicon film.
The invention also provides a solar cell which can be a TOPCon cell and specifically comprises an N-type silicon wafer, wherein the front surface of the N-type silicon wafer adopts an aluminum oxide and silicon nitride coating to passivate a boron diffusion emitter, and the back surface of the N-type silicon wafer adopts an ultrathin silicon oxide film and a phosphorus-doped polycrystalline silicon film as passivation layers, wherein the phosphorus-doped polycrystalline silicon film is the phosphorus-doped polycrystalline silicon film.
The phosphorus-doped polycrystalline silicon films prepared in the above examples and comparative examples were subjected to a minority carrier lifetime test, the test method including:
and (4) carrying out minority carrier lifetime test by adopting Semilab WT-2000 equipment. The test results are shown in table 1.
TABLE 1
| Minority carrier lifetime (ms) | |
| Example 1 | 2.32 |
| Example 2 | 2.26 |
| Example 3 | 2.15 |
| Example 4 | 2.21 |
| Example 5 | 1.78 |
| Example 6 | 1.84 |
| Example 7 | 1.67 |
| Example 8 | 1.73 |
| Example 9 | 1.23 |
| Example 10 | 1.43 |
| Comparative example 1 | 2.03 |
From the above table, it can be seen that:
(1) Compared with the examples 5-6, the invention can be seen that the decomposition efficiency and decomposition products of the raw materials are ensured by controlling the temperature of the hot wire in the hot wire chemical vapor deposition process to be 1600-2000 ℃, thereby avoiding the generation of byproducts in the reaction process from influencing the film quality. If the temperature is lower than 1600 ℃, not only the decomposition efficiency of the raw material is affected, but also the decomposition product has adverse substances, affecting the film performance.
(2) Compared with the embodiments 7-8, the embodiment 1 can see that the film forming quality is prevented from being influenced by overlarge concentration of the phosphine by controlling the deposition pressure to be 1-50 Pa under the condition of ensuring the deposition rate, if the deposition pressure is lower than 1Pa, the film deposition efficiency is influenced, and if the deposition pressure is higher than 50Pa, the concentration of the phosphine is increased, and Si-H-P compounds without electric activity are easily generated, so that the carrier concentration is reduced, and the film forming quality is influenced.
(3) Compared with the embodiments 9-10, the embodiment 1 shows that the carrier gas is carried into the tetraethoxysilane, namely the carrier gas blows through tetraethoxysilane liquid, so that the tetraethoxysilane is carried into the reaction cavity according to the evaporation effect, the concentration of the tetraethoxysilane entering the reaction cavity is further ensured by controlling the temperature of the tetraethoxysilane liquid, when the temperature is lower than 85 ℃, the concentration of the gaseous tetraethoxysilane is low, the reaction amount is small, the deposition efficiency is influenced, and when the temperature is higher than 100 ℃, the concentration of the gaseous tetraethoxysilane is high, the decomposition is easy to be incomplete, so that impurity particles exist in a deposited film, and the film forming quality is influenced.
(4) Compared with the comparative example 1, the method disclosed by the embodiment 1 has the advantages that based on hot wire chemical vapor deposition equipment, only through introducing protective gas into a reaction cavity and adjusting the distance of a hot wire, phosphorane and tetraethoxysilane are used as raw materials in the hot wire chemical vapor deposition equipment, the preparation of the phosphorus-doped amorphous silicon film is completed, further, heating annealing is carried out, the hot wire is enabled to be close to the surface of the silicon wafer, the silicon wafer is rapidly heated through the heat radiation of the hot wire, rapid annealing is realized, doped phosphorus atoms are activated, and the phosphorus-doped polycrystalline silicon film is prepared.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a phosphorus-doped polycrystalline silicon film is characterized by comprising the following steps:
depositing a phosphorus-doped amorphous silicon film on the surface of a silicon wafer in a reaction cavity by adopting a hot filament chemical vapor deposition method by taking tetraethoxysilane and phosphine as reaction gas sources;
and (3) pumping out gas in the reaction cavity, introducing protective gas, adjusting the distance of a hot wire in a hot wire chemical vapor deposition method to heat and anneal the phosphorus-doped amorphous silicon film, and preparing the phosphorus-doped polycrystalline silicon film after heating and annealing.
2. The method of preparing a phosphorus-doped polycrystalline silicon film according to claim 1, wherein the silicon wafer is subjected to a preheating treatment in a vacuum state, the temperature of the preheating treatment being 100 to 200 ℃;
preferably, the reaction chamber is subjected to vacuum treatment.
3. The method for preparing a phosphorus doped polysilicon film according to claim 1 or 2, wherein the temperature of the hot filament in the hot filament chemical vapor deposition method is 1600 to 2000 ℃;
preferably, the deposition pressure in the hot wire chemical vapor deposition method is 1-50 Pa;
preferably, the distance between the hot wire and the silicon wafer in the hot wire chemical vapor deposition method is 40-150 mm, and preferably 45mm.
4. The method for producing a phosphorus-doped polysilicon film according to any of claims 1 to 3, wherein the volume flow ratio of the phosphane to the nitrogen gas is 1: (9 to 99).
5. The method for preparing a phosphorus doped polysilicon film according to any of claims 1 to 4, wherein the tetraethoxysilane is carried into the reaction chamber by blowing tetraethoxysilane liquid with a carrier gas;
preferably, the concentration of the tetraethoxysilane in the reaction cavity is 10-30%;
preferably, the temperature of the tetraethoxysilane liquid is 85-100 ℃;
preferably, the carrier gas comprises nitrogen.
6. The method for preparing a phosphorus-doped polysilicon film according to any one of claims 1 to 5, wherein the shielding gas includes nitrogen;
preferably, in the heating annealing process, the distance between the hot wire and the phosphorus-doped amorphous silicon film is 2-10 mm, preferably 5mm;
preferably, the pressure of the heating annealing is the same as the deposition pressure in the hot wire chemical vapor deposition method;
preferably, the time for the heat annealing is 50 to 150 seconds.
7. A phosphorus-doped polycrystalline silicon film, characterized in that it is prepared by the method for preparing a phosphorus-doped polycrystalline silicon film according to any one of claims 1 to 6.
8. The phosphorous doped polysilicon film of claim 7, wherein the thickness of the phosphorous doped polysilicon film is 100-200 nm.
9. A solar cell comprising a passivation layer using the phosphorus-doped polycrystalline silicon film according to claim 7 or 8.
10. The solar cell of claim 9, wherein the solar cell is a TOPCon cell.
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