CN114765234A - Annealing enhanced back passivation method for P-type crystalline silicon double-sided battery - Google Patents
Annealing enhanced back passivation method for P-type crystalline silicon double-sided battery Download PDFInfo
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- 238000000137 annealing Methods 0.000 title claims abstract description 161
- 238000002161 passivation Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910021419 crystalline silicon Inorganic materials 0.000 title claims abstract description 14
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 79
- 230000008021 deposition Effects 0.000 claims abstract description 37
- 230000002708 enhancing effect Effects 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims description 57
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 33
- 230000007547 defect Effects 0.000 abstract description 5
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 46
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 27
- 229910052710 silicon Inorganic materials 0.000 description 27
- 239000010703 silicon Substances 0.000 description 27
- 235000013842 nitrous oxide Nutrition 0.000 description 23
- 239000007789 gas Substances 0.000 description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 11
- 238000009792 diffusion process Methods 0.000 description 10
- 239000000758 substrate Substances 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 101100409194 Rattus norvegicus Ppargc1b gene Proteins 0.000 description 7
- 230000006798 recombination Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000006388 chemical passivation reaction Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000005669 field effect Effects 0.000 description 4
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 101001073212 Arabidopsis thaliana Peroxidase 33 Proteins 0.000 description 2
- 101001123325 Homo sapiens Peroxisome proliferator-activated receptor gamma coactivator 1-beta Proteins 0.000 description 2
- 102100028961 Peroxisome proliferator-activated receptor gamma coactivator 1-beta Human genes 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010344 co-firing Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic System
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- 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
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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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- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/308—Oxynitrides
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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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/42—Silicides
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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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- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
- H01L31/1868—Passivation
Abstract
The invention relates to the field of back passivation of a P-type crystalline silicon double-sided solar cell. A method for annealing, enhancing and back passivating a P-type crystalline silicon double-sided battery comprises the following steps of first SiON film layer deposition and first annealing, second SiON film layer deposition and second annealing, third SiON film layer deposition and third annealing, fourth SiN film layer deposition, and fifth and fourth annealing. The SiON film layer is reasonably split and spliced with the annealing process, so that the internal defects of the SiON film layer when the SiON film layer is too thick can be reduced.
Description
Technical Field
The invention relates to the field of back passivation of a P-type crystalline silicon double-sided solar cell.
Background
The P-type crystalline silicon double-sided battery can greatly reduce the electrical recombination rate of the back surface by forming the passivation layer on the back surface of the solar battery, form a good internal optical back reflection mechanism, and improve the open-circuit voltage and the short-circuit current of the battery, thereby improving the conversion efficiency of the battery.
The double-sided PERC battery has the advantage of double-sided power generation due to the lower manufacturing cost, and finally becomes a mainstream product in the PERC battery.
The perc silicon solar cell production steps are as follows: 1. providing a p-type silicon substrate, and cleaning the p-type silicon substrate; 2. forming an n-type diffusion layer (n-type emitter) of reverse conduction type on a p-type silicon substrate by using a phosphorus oxychloride (pocl3) liquid source diffusion method; 3. after the diffusion layer is formed, etching is carried out by hydrofluoric acid, and pn junctions at the edges of the cross section of the silicon wafer generated by diffusion are removed; 4. depositing sinx on the n-type diffusion layer on the front surface to form a dielectric layer, and depositing alox/sinx on the back surface to form a passivation layer; 5. performing laser windowing on a passivation layer on the back of the perc silicon solar cell; 6. performing screen printing on the dielectric layer on the front side of the battery, drying front side silver paste to form a front side electrode, performing screen printing on the passivation layer perforated on the back side of the p-type substrate, and drying back side silver paste to form a back side electrode; 7. and co-firing to fully dry the electrode and form good electrical contact. The core of the perc solar cell is that a layer of aluminum oxide film is plated on the backlight surface of a silicon wafer to cover the silicon passivation, the surface passivation of the aluminum oxide is controlled by chemical passivation and field effect passivation, the chemical passivation effect of the aluminum oxide is hydrogen passivation, the aluminum oxide prepared under different conditions has different hydrogen contents, the hydrogen can be combined with internal defects of the silicon wafer and hanging bonds at crystal boundaries, a recombination center is reduced, and therefore an important factor of the passivation effect is achieved, and the hydrogen exists in-oh groups or-chx of the film. The alumina to silicon interface has a high fixed negative charge density, qf is about 1012-1013cm-2, and exhibits good field effect passivation by shielding the p-type silicon surface from minority carriers. The negative charge in the alumina film layer and the minority carrier (electron) in the p-type silicon substrate are mutually repelled, so that the combination of the negative charge and the recombination center on the surface of the silicon wafer is blocked, and the surface recombination rate is reduced. However, the back plating of the p-type cell, the atomic layer growth technology adopted by the aluminum oxide, has the disadvantages of slow speed, long time consumption, easy increase of reaction cost, low long-wave reflection and low short-circuit current in the current back passivation technology.
The perc solar cell has the advantages of simple process, low cost and high compatibility with the existing cell production line, is a newly developed high-efficiency solar cell, obtains wide attention of the industry, and is expected to become the mainstream direction of the future high-efficiency solar cell. Production of conventional silicon solar cells, perc silicon solar cells are produced as follows: 1. providing a p-type silicon substrate, and cleaning the p-type silicon substrate; 2. forming an n-type diffusion layer (n-type emitter) of reverse conduction type on a p-type silicon substrate by using a phosphorus oxychloride (pocl3) liquid source diffusion method; 3. after the diffusion layer is formed, etching is carried out by hydrofluoric acid, and pn junctions at the edges of the cross section of the silicon wafer generated by diffusion are removed; 4. depositing sinx on the n-type diffusion layer on the front surface to form a dielectric layer, and depositing alox/sinx on the back surface to form a passivation layer; 5. performing laser windowing on a passivation layer on the back of the perc silicon solar cell; 6. performing screen printing on the dielectric layer on the front side of the battery, drying front side silver paste to form a front side electrode, performing screen printing on the passivation layer perforated on the back side of the p-type substrate, and drying back side silver paste to form a back side electrode; 7. and co-firing to fully dry the electrode and form good electrical contact. The core of the perc solar cell is that a layer of aluminum oxide film is plated on the backlight surface of a silicon wafer to cover the silicon passivation, the surface passivation of the aluminum oxide is controlled by chemical passivation and field effect passivation, the chemical passivation effect of the aluminum oxide is hydrogen passivation, the aluminum oxide prepared under different conditions has different hydrogen contents, the hydrogen can be combined with internal defects of the silicon wafer and hanging bonds at crystal boundaries, a recombination center is reduced, and therefore an important factor of the passivation effect is achieved, and the hydrogen exists in-oh groups or-chx of the film. The alumina to silicon interface has a high fixed negative charge density, qf is about 1012-1013cm-2, and exhibits good field effect passivation by shielding the minority carriers on the p-type silicon surface. The negative charge in the alumina film layer and the minority carrier (electron) in the p-type silicon substrate are mutually repelled, so that the aluminum oxide film layer is prevented from being combined with the recombination center on the surface of the silicon wafer, and the surface recombination rate is reduced. However, the back plating of the p-type cell, the atomic layer growth technology adopted by the aluminum oxide, has the disadvantages of slow speed, long time consumption, easy increase of reaction cost, low long-wave reflection and low short-circuit current in the current back passivation technology.
Disclosure of Invention
The invention discloses a method for annealing and enhancing back passivation of a P-type crystalline silicon double-sided battery, and aims to improve the influence of positive charges which are not beneficial to passivation effect in the preparation of a back passivation process and further improve the passivation level of the back passivation process of the double-sided battery by optimizing the preparation process.
The technical scheme adopted by the invention is as follows: a method for annealing, enhancing and back passivating a P-type crystalline silicon double-sided battery comprises the following steps
Step one, first SiON film layer deposition and first annealing, wherein the thickness of a first SiON film layer formed after the first SiON film layer deposition is 10-12nm, and the annealing adopts vacuum annealing and NH3Annealing, wherein the first total annealing time is 250-400s, and the ratio of the first total annealing time to the thickness of the first SiON film layer in seconds is 30-35 according to a nanometer value;
step two, depositing a second SiON film layer and annealing for the second time, wherein the thickness of the second SiON film layer formed after the second SiON film layer is deposited is 8-10nm, and the annealing adopts vacuum annealing and NH3Annealing, wherein the second total annealing time is 150-300s, and the second total annealing time is 30-35 in terms of nanometer value ratio to the thickness of the second SiON film layer;
step three, depositing a second SiON film layer and annealing for the third time, wherein the thickness of a third SiON film layer formed after the third SiON film layer is deposited is 3-5nm, and the annealing adopts vacuum annealing and N2O+NH3Annealing, wherein the third total annealing time is 200-300s, and the ratio of the third total annealing time in seconds to the thickness of the third SiON film layer in nanometer value is 60-80; the total thickness of the three SiON film layers is 25-30 nm;
fourthly, a SiN film layer deposition structure is adopted, the SiN film layer is deposited in three layers, and SiH is deposited during deposition of the first SiN film layer4And NH3The ratio is 1/3.5-1/4.5, the deposition time is 350-400s, the ratio of the second layer deposition gas SiH4 to the NH3 is 1/6.5-1/7.5, the deposition time is 250-300s, and the third layer deposition gas SiH 3854The ratio of NH3 to NH3 is 1/9.5-1/10.5, the deposition time is 100-200s, and the total thickness of the three SiN layers is 60-70 nm.
Step five, annealing for the fourth time, wherein the SiN film layer is subjected to vacuum annealing at the annealing temperature of 440-460 ℃ for 100-200 s.
When depositing the SiON film layer in the first step, the pressure is 1500-2000mTorr, the power is 10000-12000W, the temperature is 450-500 ℃, the pulse on-off ratio is 1:16, the volume ratio of the introduced SiH4/NH3/N2O is 1/1/2.0-2.5/1/5.0, and the time is 30-35 s; no gas is introduced during vacuum annealing, the annealing temperature is 450-500 ℃, the power, the pressure and the duty ratio are all zero, the time length is 50-100s, NH3When annealing, NH3The flow rate is 5000-.
When the SiON film layer is deposited in the second step, the pressure is 1500-2000mTorr, the power is 10000-12000W, the temperature is 450-500 ℃, the pulse on-off ratio is 1:16, the volume ratio of the introduced SiH4/NH3/N2O is 1/1/2-2.5/1/5.0, the time is 25-30s, no gas is introduced during vacuum annealing, the annealing temperature is 450-500 ℃, the power, the pressure and the duty ratio are all zero, the time duration is 50-100s, and NH is added to the film layer3The duration of annealing is 100-3The flow rate is 5000-.
When the SiON film layer is deposited in the third step, the pressure is 1500-2000mTorr, the power is 10000-12000W, the temperature is 450-500 ℃, the pulse switching ratio is 1:16, the volume ratio of the introduced SiH4/NH3/N2O is 1/1/2-2.5/1/5.0, the time is 10-15s, no gas is introduced during vacuum annealing, the annealing temperature is 450-500 ℃, the power, the pressure and the duty ratio are all zero, and the duration is 50-100 s; n is a radical of2The duration of O annealing is 25-50s, N2The O flow is 3500 < SP > plus </SP > -4500 < SP > sccm </SP >, the pressure is 1500 < SP > plus </SP > -2000mTorr </SP >, and the temperature isThe temperature is 450-500 ℃, the power is 10000-12000W, and the pulse on-off ratio is 1: 13-1: 16; NH (NH)3The duration of annealing is 100-3The flow rate is 5000-.
In the fourth step, when the first SiN film layer is deposited, the pressure is 1500-: 15-1: 17.5; when the second SiN film layer is deposited and the third SiN film layer is deposited, the pressure is 1500-2000mTorr, the temperature is 450-500 ℃, the power is 10000-12000W, and the pulse on-off ratio is 1: 15-1: 17.5.
the invention has the beneficial effects that: due to the characteristics of the SiON layer, a formula structure with high silicon-nitrogen ratio and high laughing gas flow is needed for preparing the back film of the double-sided battery, and under the formula structure, the thickness of the SiON film layer exceeds a certain critical value of 10-15nm, and the passivation level is greatly reduced. According to the method, step-by-step deposition and step-by-step annealing are adopted in a PECVD mode, and the time proportion relation between the step-by-step deposition and the step-by-step annealing is reasonably controlled, so that the thickness window of the SiON film layer can be widened, and the passivation level of the SiON film layer is greatly improved.
The SiON film layer is reasonably split and spliced with the annealing process, so that the internal defects of the SiON film layer when the SiON film layer is too thick can be reduced. Firstly, the vacuum annealing in the first step and the second step can fully eliminate the stress defect of the SiON dielectric film in the preparation process, and the NH3 annealing can further passivate the Si/SiON interface state, but the annealing time needs to be accurately controlled; the annealing in the third step is added with N2O annealing, which can further diffuse the ionized oxygen in N2O to the Si/SiON interface through pores, thereby reducing the interface state to the maximum extent; in the fifth step, vacuum annealing is performed for a short time after SiN, which is beneficial to realizing passivation of Si/SiON interface or body through hydrogen in the SiN dielectric film, but the annealing temperature needs to be controlled at 460 ℃ of 440 ℃, the Si-H bond is broken when the temperature is lower than 440 ℃, and the H overflow condition is aggravated when the temperature is higher than 460 ℃.
Detailed Description
Examples
A method for annealing, enhancing and back passivating a P-type crystalline silicon double-sided battery comprises the following steps:
first SiON film deposition + annealing. Depositing SiON film under the pressure of 1700mTorr, at 490 deg.c, at 12000W, with the pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5 for 35 s; during annealing, firstly, performing vacuum annealing for 50s, wherein no gas is introduced during the vacuum annealing, the annealing temperature is 490 ℃, and the power, the pressure and the duty ratio are all zero; then, NH3 was used for annealing at a time of 300s, wherein NH3 flow was 7000sccm, pressure was 1700mTorr, temperature was 490 ℃, power was 10000W, and pulse on/off ratio was 1: 13.
And depositing and annealing the SiON film for the second time. Depositing SiON film layer under the pressure of 1700mTorr, temperature of 490 deg.c, power of 12000W, pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5 for 30 s; during annealing, firstly, performing vacuum annealing for 50s, wherein no gas is introduced during the vacuum annealing, the annealing temperature is 490 ℃, and the power, the pressure and the duty ratio are all zero; then, NH3 was used for annealing with a time control of 200s, wherein the NH3 flow rate was 7000sccm, the pressure was 1700mTorr, the temperature was 490 ℃, the power was 10000W, and the pulse on/off ratio was 1: 13.
Third SiON film deposition + annealing. Depositing SiON film layer under the pressure of 1700mTorr, temperature of 490 deg.c, power of 12000W, pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5 for 10 s; during annealing, firstly, vacuum annealing is carried out for 80s, no gas is introduced during the vacuum annealing, the annealing temperature is 490 ℃, and the power, the pressure and the duty ratio are all zero; then N2O is used for annealing, the time is controlled to be 30s, wherein the flow rate of N2O is 4000sccm, the pressure is 1700mTorr, the temperature is 490 ℃, the power is 10000W, and the pulse on-off ratio is 1: 13; and finally, NH3 annealing is carried out, the time is controlled to be 100s, the NH3 flow is 7000sccm, the pressure is 1700mTorr, the temperature is 490 ℃, the power is 10000W, and the pulse on-off ratio is 1: 13.
The SiN film layer is a three-layer film, the pressure of the first SiN film layer close to the SiON film layer is 1700mTorr during deposition, the temperature is 490 ℃, the power is 12000W, and the pulse on-off ratio is 1: 17.5, the SiN film layer is SiH4/NH3=1/4, and the process time is 400 s; the second SiN film was deposited at a pressure of 1700mTorr, a temperature of 490 ℃, a power of 12000W, a pulse on/off ratio of 1: 17.5, SiH4/NH3=1/7 of the SiN film layer, the process time is 270s, the pressure is 1700mTorr when the third SiN film layer is deposited, the temperature is 490 ℃, the power is 12000W, and the pulse on-off ratio is 1: 17.5, the process time is 150s, and the SiN film layer is SiH4/NH3= 1/10.
And performing post-annealing on the SiN. And (3) vacuum annealing is used, the time length is 100s, no gas is introduced during the vacuum annealing, the annealing temperature is 450 ℃, and the power, the pressure and the duty ratio are all zero.
Comparative example 1
SiON film deposition + annealing. Depositing SiON film layer under the pressure of 1700mTorr, temperature of 490 deg.c, power of 12000W, pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5 for 60 s; and NH3 annealing is carried out, wherein the annealing time is controlled to be 600s, the NH3 flow is 7000sccm, the pressure is 1700mTorr, the temperature is 490 ℃, the power is 10000W, and the pulse on-off ratio is 1: 13.
The SiN film layer is a three-layer film, the pressure of the first SiN film layer close to the SiON film layer is 1700mTorr during deposition, the temperature is 490 ℃, the power is 12000W, and the pulse on-off ratio is 1: 17.5, the SiN film layer is SiH4/NH3=1/4, and the process time is 400 s; the second SiN film was deposited at a pressure of 1700mTorr, a temperature of 490 ℃, a power of 12000W, a pulse on/off ratio of 1: 17.5, SiH4/NH3=1/7 of the SiN film layer, wherein the process time is 270s; the second SiN film was deposited at a pressure of 1700mTorr, a temperature of 490 ℃, a power of 12000W, a pulse on/off ratio of 1: 17.5, the process time is 150s, and the SiN film layer is SiH4/NH3= 1/10.
Comparative example 2:
SiON film deposition + annealing. Depositing SiON film layer under the pressure of 1700mTorr, temperature of 490 deg.C, power of 12000W, pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5, and time of 70s; and NH3 annealing is carried out, and the annealing time is controlled to be 600s, wherein the NH3 flow is 7000sccm, the pressure is 1700mTorr, the temperature is 490 ℃, the power is 10000W, and the pulse on-off ratio is 1: 13.
The SiN film layer is a three-layer film, the pressure of the first SiN film layer close to the SiON film layer is 1700mTorr during deposition, the temperature is 490 ℃, the power is 12000W, and the pulse on-off ratio is 1: 17.5, the process time is 400s, and the SiN film layer is SiH4/NH3= 1/4; the pressure during deposition of the second SiN film was 1700mTorr, the temperature was 490 ℃, the power was 12000W, the pulse on-off ratio was 1: 17.5, the process time is 270s, and the SiN film layer is SiH4/NH3= 1/7; the second SiN film was deposited at a pressure of 1700mTorr, a temperature of 490 ℃, a power of 12000W, a pulse on/off ratio of 1: 17.5, the SiN film layer SiH4/NH3=1/10, and the process time is 150 s.
Comparative example 3:
first SiON film deposition + annealing. Depositing SiON film under the pressure of 1700mTorr, at 490 deg.c, at 12000W, with the pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5 for 35 s; when annealing, firstly, vacuum annealing is carried out for 50s, no gas is introduced during the vacuum annealing,
the annealing temperature is 490 ℃, and the power, the pressure and the duty ratio are all zero; then, NH3 annealing was used, the time was controlled at 300s, where NH3 flow was 7000sccm, pressure was 1700mTorr, temperature was 490 ℃, power was 10000W, and pulse on/off ratio was 1: 13.
And depositing and annealing the SiON film for the second time. Depositing SiON film layer under the pressure of 1700mTorr, temperature of 490 deg.c, power of 12000W, pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5 for 30 s; during annealing, firstly, vacuum annealing is carried out for 50s, no gas is introduced during the vacuum annealing, the annealing temperature is 490 ℃, and the power, the pressure and the duty ratio are all zero; then, NH3 annealing was used, the time was controlled at 200s, where NH3 flow was 7000sccm, pressure was 1700mTorr, temperature was 490 ℃, power was 10000W, and pulse on/off ratio was 1: 13.
Third SiON film deposition + annealing. Depositing SiON film under the pressure of 1700mTorr, at 490 deg.c, at 12000W, with the pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5 for 10 s; during annealing, firstly, vacuum annealing is carried out for 80s, no gas is introduced during the vacuum annealing, the annealing temperature is 490 ℃, and the power, the pressure and the duty ratio are all zero; then N2O is used for annealing, the time is controlled to be 30s, wherein the flow rate of N2O is 4000sccm, the pressure is 1700mTorr, the temperature is 490 ℃, the power is 10000W, and the pulse on-off ratio is 1: 13; and finally, NH3 annealing is carried out, the time is controlled to be 100s, the NH3 flow is 7000sccm, the pressure is 1700mTorr, the temperature is 490 ℃, the power is 10000W, and the pulse on-off ratio is 1: 13.
The SiN film layer is a three-layer film, the pressure of the first SiN film layer close to the SiON film layer is 1700mTorr during deposition, the temperature is 490 ℃, the power is 12000W, and the pulse on-off ratio is 1: 17.5, the SiN film layer is SiH4/NH3=1/4.5, and the process time is 400 s; the second SiN film was deposited at a pressure of 1700mTorr, a temperature of 490 ℃, a power of 12000W, a pulse on/off ratio of 1: 17.5, SiH4/NH3=1/7 of the SiN film layer, the process time is 270s, the pressure is 1700mTorr when the second SiN film layer is deposited, the temperature is 490 ℃, the power is 12000W, and the pulse on-off ratio is 1: 17.5, the SiN film layer SiH4/NH3=1/10, and the process time is 150 s.
Comparative example 4
First SiON film deposition + annealing. Depositing SiON film layer under the pressure of 1700mTorr, temperature of 490 deg.C, power of 12000W, pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5, and time of 35 s; when annealing, firstly, vacuum annealing is carried out for 50s, no gas is introduced during the vacuum annealing,
the annealing temperature is 490 ℃, and the power, the pressure and the duty ratio are all zero; then, NH3 annealing was used, the time was controlled at 300s, where NH3 flow was 7000sccm, pressure was 1700mTorr, temperature was 490 ℃, power was 10000W, and pulse on/off ratio was 1: 13.
And depositing and annealing the SiON film for the second time. Depositing SiON film under the pressure of 1700mTorr, at 490 deg.c, at 12000W, with the pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5 for 30 s; during annealing, firstly, vacuum annealing is carried out for 50s, no gas is introduced during the vacuum annealing, the annealing temperature is 490 ℃, and the power, the pressure and the duty ratio are all zero; then, NH3 was used for annealing with a time control of 200s, wherein the NH3 flow rate was 7000sccm, the pressure was 1700mTorr, the temperature was 490 ℃, the power was 10000W, and the pulse on/off ratio was 1: 13.
Third SiON film deposition + annealing. Depositing SiON film layer under the pressure of 1700mTorr, temperature of 490 deg.c, power of 12000W, pulse on-off ratio of 1:16, introducing SiH4/NH3/N2O =2.5/1/2.5 for 10 s; during annealing, firstly, vacuum annealing is carried out for 80s, no gas is introduced during the vacuum annealing, the annealing temperature is 490 ℃, and the power, the pressure and the duty ratio are all zero; then N2O is used for annealing, the time is controlled to be 30s, wherein the flow rate of N2O is 4000sccm, the pressure is 1700mTorr, the temperature is 490 ℃, the power is 10000W, and the pulse on-off ratio is 1: 13; and finally, NH3 annealing is carried out, the time is controlled to be 100s, the NH3 flow is 7000sccm, the pressure is 1700mTorr, the temperature is 490 ℃, the power is 10000W, and the pulse on-off ratio is 1: 13.
The SiN film layer is a three-layer film, the pressure of the first SiN film layer close to the SiON film layer is 1700mTorr during deposition, the temperature is 490 ℃, the power is 12000W, and the pulse on-off ratio is 1: 17.5, the SiN film layer is SiH4/NH3=1/5.5, and the process time is 400 s; the second SiN film was deposited at a pressure of 1700mTorr, a temperature of 490 ℃, a power of 12000W, a pulse on/off ratio of 1: 17.5, SiH4/NH3=1/7 of the SiN film, the process time is 270s, the pressure is 1700mTorr when the second SiN film is deposited, the temperature is 490 ℃, the power is 12000W, and the pulse on-off ratio is 1: 17.5, the SiN film layer SiH4/NH3=1/10, and the process time is 150 s.
And performing post-annealing on the SiN. And (3) vacuum annealing is used, the time length is 100s, no gas is introduced during the vacuum annealing, the annealing temperature is 450 ℃, and the power, the pressure and the duty ratio are all zero.
Table 1 shows the differences between the preparation methods of the examples and the comparative examples 1 to 4, and table 2 shows the comparison between the mass production efficiency of the corresponding examples and the comparative examples 1 to 4, and the specific data are as follows:
TABLE 1 difference in preparation methods between examples and comparative examples 1 to 4
TABLE 2 conversion efficiency differences between examples and comparative examples 1-4
As seen from the data in the tables 1 and 2, the SiON dielectric film is deposited by adopting the three-step deposition and the three-step annealing in the patent of the invention, the problem that the conversion efficiency of single-step deposition is deteriorated along with the SiON film thickness is greatly solved, and meanwhile, the adjustment of the chemical composition ratio of SiN close to the SiON film layer and the post-annealing are superposed, so that the conversion efficiency is further improved.
Claims (5)
1. A method for annealing, enhancing and back passivating a P-type crystalline silicon double-sided battery is characterized by comprising the following steps: the method comprises the following steps
Step one, first SiON film layer deposition and first annealing are carried out, wherein the thickness of a first SiON film layer formed after the first SiON film layer deposition isAt 10-12nm, vacuum annealing and NH are adopted for annealing3Annealing, wherein the first total annealing time is 250-400s, and the ratio of the first total annealing time to the thickness of the first SiON film layer in seconds is 30-35 according to a nanometer value;
step two, depositing a second SiON film layer and annealing for the second time, wherein the thickness of the second SiON film layer formed after the second SiON film layer is deposited is 8-10nm, and the annealing adopts vacuum annealing and NH3Annealing, wherein the second total annealing time is 150-300s, and the second total annealing time is 30-35 in terms of nanometer value ratio to the thickness of the second SiON film layer;
step three, depositing the SiON film layer for the second time and annealing for the third time, wherein the thickness of the SiON film layer formed after depositing the SiON film layer for the third time is 3-5nm, and the annealing adopts vacuum annealing and N2O+NH3Annealing, wherein the third total annealing time is 200-300s, and the ratio of the third total annealing time to the third SiON film layer thickness in seconds is 60-80 according to the nanometer value; the total thickness of the three SiON film layers is 25-30 nm;
fourthly, a SiN film layer is deposited, the SiN film layer adopts three-layer deposition, and SiH is deposited during the deposition of the first SiN film layer4And NH3The ratio is 1/3.5-1/4.5, the deposition time is 350-4The ratio of the thickness of the SiN film to NH3 is 1/9.5-1/10.5, the deposition time is 100-200s, and the total thickness of the three SiN film layers is 60-70 nm;
step five, annealing for the fourth time, wherein the SiN film layer is subjected to vacuum annealing at the annealing temperature of 440-460 ℃ for 100-200 s.
2. The annealing-enhanced back passivation method for the P-type crystalline silicon double-sided battery as claimed in claim 1, wherein: when the SiON film layer is deposited in the first step, the pressure is 1500-2000mTorr, the power is 10000-12000W, the temperature is 450-500 ℃, the pulse on-off ratio is 1:16, the volume ratio of SiH4/NH3/N2O is 1/1/2.0-2.5/1/5.0, and the time is 30-35 s; no gas is introduced during vacuum annealing, the annealing temperature is 450-500 ℃, the power, the pressure and the duty ratio are all zero, the time length is 50-100s, NH3When annealing, NH3The flow rate is 5000-The force is 1500-2000mTorr, the temperature is 450-500 ℃, the power is 10000-12000W, the pulse on-off ratio is 1: 13-1: 16, and the time duration is 200-300 s.
3. The annealing-enhanced back passivation method for the P-type crystalline silicon double-sided battery as claimed in claim 1, wherein: when the SiON film layer is deposited in the second step, the pressure is 1500-2000mTorr, the power is 10000-12000W, the temperature is 450-500 ℃, the pulse on-off ratio is 1:16, the volume ratio of the introduced SiH4/NH3/N2O is 1/1/2-2.5/1/5.0, the time is 25-30s, no gas is introduced during vacuum annealing, the annealing temperature is 450-500 ℃, the power, the pressure and the duty ratio are all zero, the time duration is 50-100s, and NH is added to the film layer3The duration of annealing is 100-200s, NH3The flow rate is 5000-.
4. The annealing-enhanced back passivation method for the P-type crystalline silicon double-sided battery as claimed in claim 1, wherein: when the SiON film layer is deposited in the third step, the pressure is 1500-2000mTorr, the power is 10000-12000W, the temperature is 450-500 ℃, the pulse switching ratio is 1:16, the volume ratio of the introduced SiH4/NH3/N2O is 1/1/2-2.5/1/5.0, the time is 10-15s, no gas is introduced during vacuum annealing, the annealing temperature is 450-500 ℃, the power, the pressure and the duty ratio are all zero, and the duration is 50-100 s; n is a radical of2The duration of O annealing is 25-50s, N2The O flow is 3500-4500sccm, the pressure is 1500-2000mTorr, the temperature is 450-500 ℃, the power is 10000-12000W, and the pulse on-off ratio is 1: 13-1: 16; NH3The duration of annealing is 100-3The flow rate is 5000-.
5. The annealing-enhanced back passivation method for the P-type crystalline silicon double-sided battery as claimed in claim 1, wherein: in the fourth step, when the first SiN film layer is deposited, the pressure is 1500-2000mTorr, the temperature is 450-500 ℃, the power is 10000-12000W, and the pulse on-off ratio is 1: 15-1: 17.5; when the second SiN film layer is deposited and the third SiN film layer is deposited, the pressure is 1500-2000mTorr, the temperature is 450-500 ℃, the power is 10000-12000W, and the pulse on-off ratio is 1: 15-1: 17.5.
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