CN113066903B - Silicon wafer texturing process - Google Patents
Silicon wafer texturing process Download PDFInfo
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- CN113066903B CN113066903B CN202110325033.3A CN202110325033A CN113066903B CN 113066903 B CN113066903 B CN 113066903B CN 202110325033 A CN202110325033 A CN 202110325033A CN 113066903 B CN113066903 B CN 113066903B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 124
- 239000010703 silicon Substances 0.000 title claims abstract description 124
- 238000000034 method Methods 0.000 title claims abstract description 16
- 230000003647 oxidation Effects 0.000 claims description 50
- 238000007254 oxidation reaction Methods 0.000 claims description 50
- 238000005554 pickling Methods 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000002253 acid Substances 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 7
- 150000007529 inorganic bases Chemical class 0.000 claims description 7
- 210000002268 wool Anatomy 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 241000519995 Stachys sylvatica Species 0.000 abstract description 8
- 235000012431 wafers Nutrition 0.000 description 93
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010405 reoxidation reaction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0236—Special surface textures
- H01L31/02363—Special surface textures of the semiconductor body itself, e.g. textured active layers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a silicon wafer texturing process, which is characterized in that before texturing, a silicon wafer is subjected to high-temperature treatment, so that organic dirt on the surface of the silicon wafer is decomposed, the organic dirt on the surface of the silicon wafer can be completely removed, and the problems of white spots, bright spots and the like caused by the fact that the organic dirt remains on the surface of the silicon wafer during texturing can be avoided.
Description
Technical Field
The invention relates to a silicon wafer texturing process.
Background
The photovoltaic power generation is the most important component in the utilization of solar energy, is an environment-friendly renewable energy source which is inexhaustible, and accords with the pursuit of high efficiency and low cost in the photovoltaic industry. For a monocrystalline silicon cell, the surface reflectivity is one of the important factors influencing the efficiency conversion of the solar cell, and the texturing process plays an important role in reducing the surface reflectivity.
The texturing aims to generate texture on the surface of a primary silicon wafer to achieve the light trapping effect, so that the sunlight absorption rate is improved, and the photoelectric conversion rate of the cell is further improved. At present, the texturing process on the market is still the traditional wet process, and after the texturing process is finished, the problems of white spots, bright spots and the like can appear on the silicon wafer at a high probability, so that the through rate of the silicon wafer in a production line is seriously influenced, and the production line efficiency is reduced.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a silicon wafer texturing process, wherein before texturing, the silicon wafer is subjected to high-temperature treatment, so that organic dirt on the surface of the silicon wafer is decomposed, and the organic dirt on the surface of the silicon wafer is removed.
Specifically, the silicon wafer texturing process comprises the following specific steps:
1) Carrying out high-temperature oxidation treatment on the silicon wafer to decompose organic dirt on the surface of the silicon wafer so as to remove the organic dirt on the surface of the silicon wafer and form a first oxidation layer on the surface of the silicon wafer;
2) Pickling the silicon wafer treated in the step 1) by using a first acid solution to remove a first oxide layer on the surface of the silicon wafer;
3) Rinsing the silicon wafer treated in the step 2) to remove the first acid liquid remaining on the surface of the silicon wafer;
4) Oxidizing the silicon wafer treated in the step 3) by using an oxidation treatment liquid to form a second oxidation layer on the surface of the silicon wafer so that the surface of the silicon wafer is in a hydrophilic state, wherein the thickness of the second oxidation layer is not more than 0.6nm;
5) Rinsing the silicon wafer treated in the step 4) to remove residual oxidation treatment liquid on the surface of the silicon wafer;
6) And 5) adopting a texturing solution to perform texturing on the silicon wafer treated in the step 5), and forming a textured structure on the surface of the silicon wafer.
Researches show that the problems of white spots, bright spots and the like can occur in the texturing of the silicon wafer, and mainly because organic dirt remains on the surface of the silicon wafer. Before texturing, the silicon wafer is subjected to high-temperature treatment, so that organic dirt on the surface of the silicon wafer is decomposed, the organic dirt on the surface of the silicon wafer can be completely removed, and the problems of white spots, bright spots and the like caused by the fact that the organic dirt remains on the surface of the silicon wafer during texturing can be avoided.
The silicon wafer with organic dirt left on the surface can be subjected to high-temperature treatment (namely high-temperature oxidation treatment) in an oxidation furnace/sintering furnace, but the inventor of the invention discovers that the high-temperature oxidation treatment is carried out at a high temperature (300-800 ℃) for a long time (180-250 s) in order to completely remove the organic dirt on the surface of the silicon wafer, and a thicker SiO layer is formed on the surface of the silicon wafer after the high-temperature oxidation treatment is finished 2 The layer (namely the first oxidation layer) has the thickness not less than 2nm (the thickness of the first oxidation layer is 2-8 nm), and the thicker first oxidation layer can influence the wool making and is not beneficial to the wool making.
In order to prevent the influence of the thicker first oxide layer on texturing, the invention uses a first acid solution (hydrofluoric acid solution) to carry out acid cleaning on the silicon wafer after high-temperature oxidation treatment, so as to completely remove the first oxide layer on the surface of the silicon wafer.
However, the inventor of the present invention finds that the surface of the silicon wafer after the first oxide layer is removed is in a hydrophobic state, and the hydrophobic state of the surface of the silicon wafer also affects texturing and is not beneficial to texturing.
In order to prevent the silicon wafer surface from being in a hydrophobic state to influence texturing, the oxidation treatment liquid is adopted to carry out reoxidation on the silicon wafer with the first oxide layer removed so as to form SiO again on the silicon wafer surface 2 Layer (i.e. second oxidation layer), and the invention controls the technological parameters of reoxidation (by adopting 2-6% H) 2 O 2 Oxidizing the silicon wafer for 2-3 min at 60-70 ℃ by using an oxidation treatment liquid prepared from 1-3% of inorganic base and the balance of deionized water to control the thickness of the second oxidation layer, so that the thickness of the second oxidation layer is not more than 0.6nm (the thickness of the second oxidation layer is controlled to be 0.2-0.6 nm), the ultrathin second oxidation layer does not influence the texturing, the surface of the silicon wafer is changed into a hydrophilic state, the surface energy of the silicon wafer is reduced, and the texturing is facilitated.
The root of the texturing is that Si reacts with the texturing liquid. If SiO on the surface of the silicon chip 2 The thickness is not less than 2nm, the surface treatment of the silicon wafer is insufficient during the texture surface making, and the reaction is causedIncomplete, too high a reflectivity of the silicon wafer surface. When SiO is present 2 When the thickness is not more than 0.6nm, the wool can be made completely by matching with the existing wool making process, and the wool making is not influenced.
In conclusion, the invention not only can solve the problems of white spots, bright spots and the like caused by the residual organic dirt on the surface of the silicon chip, but also can reduce the reject ratio of texturing and has popularization value.
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The invention provides a silicon wafer texturing process, which comprises the following specific steps:
1) Carrying out high-temperature oxidation treatment on the silicon wafer at the temperature of 300-800 ℃ for 180-250 s to decompose the organic dirt on the surface of the silicon wafer so as to remove the organic dirt on the surface of the silicon wafer, and forming a first oxidation layer on the surface of the silicon wafer, wherein the first oxidation layer is SiO 2 ；
2) Pickling the silicon wafer treated in the step 1) for 2-6 min at normal temperature by using a first acid solution to remove a first oxide layer on the surface of the silicon wafer; the first acid solution comprises the following components in percentage by mass: 5% -10% of HF and the balance of deionized water;
3) Rinsing the silicon wafer treated in the step 2) at normal temperature for 3-9 min to remove the first acid liquid remaining on the surface of the silicon wafer;
4) Oxidizing the silicon wafer treated in the step 3) for 2-3 min at 60-70 ℃ by adopting an oxidizing treatment liquid to form a second oxide layer on the surface of the silicon wafer, wherein the second oxide layer is SiO 2 So that the surface of the silicon chip is in a hydrophilic state, and the thickness of the second oxide layer is controlled to be 0.2-0.6 nm; the oxidation treatment liquid comprises the following components in percentage by mass: h 2 O 2 2-6 percent of inorganic base, 1-3 percent of inorganic base and the balance of deionized water; the inorganic base can be KOH or NaOH;
5) Rinsing the silicon wafer treated in the step 4) at normal temperature for 3-5 min to remove residual oxidation treatment liquid on the surface of the silicon wafer;
6) Texturing the silicon wafer treated in the step 5) for 6-8 min at 75-85 ℃ by using a texturing solution, and forming a textured structure on the surface of the silicon wafer; the wool making liquid comprises the following components in percentage by mass: 0.5-1% of texturing additive, 1-3% of inorganic alkali and the balance of deionized water; the inorganic base can be KOH or NaOH;
7) Rinsing the silicon wafer treated in the step 6) at normal temperature for 3-5 min to remove the residual texturing solution on the surface of the silicon wafer;
8) Pickling the silicon wafer treated in the step 7) for 2-6 min at normal temperature by using a second acid solution to remove an oxide layer and metal ions on the surface of the silicon wafer; the second acid liquid comprises the following components in percentage by mass: 5-10% of HF, 5-10% of HCL and the balance of deionized water;
9) Rinsing the silicon wafer treated in the step 8) at normal temperature for 3-9 min to remove the second acid solution remaining on the surface of the silicon wafer;
10 ) drying the silicon slice treated in the step 9) for 10-30 min at 80-90 ℃.
The specific embodiment of the invention is as follows:
example 1
1) Putting 1200 silicon chips into a chain type oxidation furnace for high-temperature oxidation treatment at 700 ℃ for 180s;
2) Feeding the 1200 silicon wafers treated in the step 1) into a pickling area of a first chain type pickling machine for pickling for 5min at normal temperature, wherein acid liquor used for pickling is prepared from 5wt% of HF and 95wt% of deionized water;
3) Feeding the 1200 silicon wafers treated in the step 2) into a rinsing area of a first chain type pickling machine for rinsing for 6min at normal temperature;
4) Allowing 1200 silicon wafers treated in the step 3) to pass through a first wafer inserting machine, and then entering an oxidation tank for oxidation treatment, wherein the time is 2min and 10s, the temperature is 60 ℃, and the oxidation treatment liquid in the oxidation tank is prepared from 5wt% of H 2 O 2 2wt% of NaOH and 93wt% of deionized water;
5) Putting the 1200 silicon chips treated in the step 4) into a first clean water tank for rinsing at normal temperature for 3min;
6) Allowing 1200 silicon wafers treated in the step 5) to enter a texturing groove to be textured for 6min and 30s at 78 ℃, wherein a texturing solution in the texturing groove is prepared from 1wt% of a texturing additive, 2wt% of NaOH and 97wt% of deionized water;
7) Putting the 1200 silicon chips treated in the step 6) into a second clean water tank for rinsing at normal temperature for 3min;
8) Placing the 1200 silicon wafers treated by the step 7) by a second wafer inserting machine, and then entering a pickling area of a second chain type pickling machine for pickling at normal temperature for 5min, wherein acid liquid used for pickling is prepared from 5wt% of HF, 5wt% of HCL and 90wt% of deionized water;
9) The 1200 silicon chips treated in the step 8) enter a rinsing area of a second chain type acid washing machine to be rinsed for 6min at normal temperature;
10 1200 silicon wafers processed by the step 9) enter a chain type drying furnace and are dried for 15min at 88 ℃.
In example 1, 1200 sheets of the pile-making sheets were produced, and all had no white spots or bright spots on the surface, and the defective rate was 0.005%.
Example 2
1) 1200 silicon chips enter a chain type oxidation furnace to be subjected to high-temperature oxidation treatment, wherein the temperature is 500 ℃, and the time is 200s;
2) Feeding the 1200 silicon wafers treated in the step 1) into a pickling area of a first chain type pickling machine for pickling at normal temperature for 3min, wherein acid liquor used for pickling is prepared from 7wt% of HF and 93wt% of deionized water;
3) Feeding the 1200 silicon wafers treated in the step 2) into a rinsing area of a first chain type pickling machine for rinsing for 5min at normal temperature;
4) Allowing 1200 silicon wafers treated in the step 3) to pass through a first wafer inserting machine, and then entering an oxidation tank for oxidation treatment, wherein the time is 2min and 10s, the temperature is 60 ℃, and the oxidation treatment liquid in the oxidation tank is prepared from 5wt% of H 2 O 2 2wt% of NaOH and 93wt% of deionized water;
5) Putting the 1200 silicon chips treated in the step 4) into a first clean water tank, and rinsing at normal temperature for 3min;
6) Allowing 1200 silicon wafers treated in the step 5) to enter a texturing groove for texturing for 6min and 30s at 78 ℃, wherein a texturing solution in the texturing groove is prepared from 1wt% of a texturing additive, 2wt% of NaOH and 97wt% of deionized water;
7) Putting the 1200 silicon chips treated in the step 6) into a second clean water tank for rinsing at normal temperature for 3min;
8) Placing the 1200 silicon wafers treated by the step 7) by a second wafer inserting machine, and then entering a pickling area of a second chain type pickling machine for pickling at normal temperature for 5min, wherein acid liquid used for pickling is prepared from 5wt% of HF, 5wt% of HCL and 90wt% of deionized water;
9) Feeding the 1200 silicon wafers treated in the step 8) into a rinsing area of a second chain type pickling machine for rinsing for 6min at normal temperature;
10 1200 silicon wafers processed by the step 9) enter a chain type drying furnace and are dried for 15min at 88 ℃.
Example 2 1200 pile-making sheets were produced, all having no white spots or bright spots on the surface and a defective rate of 0.01%.
Example 3
1) Putting 1200 silicon chips into a chain type oxidation furnace for high-temperature oxidation treatment at 300 ℃ for 240s;
2) Feeding the 1200 silicon wafers treated in the step 1) into a pickling area of a first chain type pickling machine for pickling for 2min at a normal temperature for 30s, wherein acid liquor used for pickling is prepared from 9wt% of HF and 91wt% of deionized water;
3) Feeding the 1200 silicon wafers treated in the step 2) into a rinsing area of a first chain type pickling machine for rinsing for 3min at normal temperature;
4) Allowing 1200 silicon wafers treated in the step 3) to pass through a first wafer inserting machine, and then entering an oxidation tank for oxidation treatment at 60 ℃ for 2min, wherein the oxidation treatment liquid in the oxidation tank is prepared from 6wt% of H 2 O 2 3wt% of NaOH and 91wt% of deionized water;
5) Putting the 1200 silicon chips treated in the step 4) into a first clean water tank for rinsing at normal temperature for 3min;
6) Allowing 1200 silicon wafers treated in the step 5) to enter a texturing groove for texturing for 6min and 40s at 78 ℃, wherein a texturing solution in the texturing groove is prepared from 0.8wt% of a texturing additive, 2wt% of NaOH and 97.2wt% of deionized water;
7) Putting the 1200 silicon chips treated in the step 6) into a second clean water tank for rinsing at normal temperature for 3min;
8) Placing the 1200 silicon wafers treated by the step 7) by a second wafer inserting machine, and then entering a pickling area of a second chain type pickling machine for pickling at normal temperature for 5min, wherein acid liquid used for pickling is prepared from 5wt% of HF, 5wt% of HCL and 90wt% of deionized water;
9) Feeding the 1200 silicon wafers treated in the step 8) into a rinsing area of a second chain type pickling machine for rinsing for 6min at normal temperature;
10 1200 silicon wafers processed by the step 9) enter a chain type drying furnace and are dried for 15min at 88 ℃.
Example 3 1200 pile-making sheets were produced, all having no white spots or bright spots on the surface and a defective rate of 0.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. The silicon wafer texturing process is characterized by comprising the following specific steps:
1) Carrying out high-temperature oxidation treatment on the silicon wafer to decompose organic dirt on the surface of the silicon wafer so as to remove the organic dirt on the surface of the silicon wafer and form a first oxidation layer on the surface of the silicon wafer; the temperature of the high-temperature oxidation treatment is 300-800 ℃, and the time is 180-250 s; the first oxide layer is SiO 2 (ii) a The thickness of the first oxide layer is not less than 2nm;
2) Pickling the silicon wafer treated in the step 1) by using a first acid solution to remove a first oxide layer on the surface of the silicon wafer; the first acid solution comprises the following components in percentage by mass: 5% -10% of HF and the balance of deionized water; the pickling temperature is normal temperature, and the pickling time is 2-6 min;
3) Rinsing the silicon wafer treated in the step 2) to remove the first acid liquid remaining on the surface of the silicon wafer; rinsing at normal temperature for 3-9 min;
4) Oxidizing the silicon wafer treated in the step 3) by using an oxidizing treatment liquid to form a second oxide layer on the surface of the silicon wafer so as to enable the silicon wafer to be oxidizedThe surface of the silicon chip is in a hydrophilic state; the oxidation treatment liquid comprises the following components in percentage by mass: h 2 O 2 2-6 percent of inorganic base, 1-3 percent of inorganic base and the balance of deionized water; the temperature of the oxidation treatment is 60-70 ℃, and the time is 2-3 min; the second oxide layer is SiO 2 (ii) a The thickness of the second oxide layer is not more than 0.6nm;
5) Rinsing the silicon wafer treated in the step 4) to remove residual oxidation treatment liquid on the surface of the silicon wafer; rinsing at normal temperature for 3-5 min;
6) And 5) adopting a texturing solution to perform texturing on the silicon wafer treated in the step 5), and forming a textured structure on the surface of the silicon wafer.
2. The silicon wafer texturing process according to claim 1, further comprising the following specific steps:
7) Rinsing the silicon wafer treated in the step 6) to remove the residual texturing solution on the surface of the silicon wafer;
8) Pickling the silicon wafer treated in the step 7) by using a second acid solution to remove an oxide layer and metal ions on the surface of the silicon wafer;
9) Rinsing the silicon wafer treated in the step 8) to remove the second acid liquor remained on the surface of the silicon wafer;
10 Carrying out drying treatment on the silicon wafer treated in the step 9).
3. The silicon wafer texturing process according to claim 1 or 2, characterized in that: in the step 6), the texture surface making liquid comprises the following components in percentage by mass: 0.5-1% of texturing additive, 1-3% of inorganic alkali and the balance of deionized water; the temperature of the wool making is 75-85 ℃, and the time is 6-8 min.
4. The silicon wafer texturing process of claim 2, wherein:
in the step 7), the rinsing temperature is normal temperature, and the time is 3-5 min;
in the step 8), the second acid solution comprises the following components in percentage by mass: 5-10% of HF, 5-10% of HCL and the balance of deionized water; the pickling temperature is normal temperature, and the pickling time is 2-6 min;
in the step 9), the rinsing temperature is normal temperature, and the rinsing time is 3-9 min;
in the step 10), the drying temperature is 80-90 ℃ and the drying time is 10-30 min.
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