CN110707163A - Method for texturing on surface of single crystal silicon by using tetramethylguanidine organic alkali - Google Patents
Method for texturing on surface of single crystal silicon by using tetramethylguanidine organic alkali Download PDFInfo
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- CN110707163A CN110707163A CN201910893517.0A CN201910893517A CN110707163A CN 110707163 A CN110707163 A CN 110707163A CN 201910893517 A CN201910893517 A CN 201910893517A CN 110707163 A CN110707163 A CN 110707163A
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- 238000000034 method Methods 0.000 title claims abstract description 20
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000003513 alkali Substances 0.000 title claims abstract description 17
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 44
- 239000010703 silicon Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000243 solution Substances 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 238000005530 etching Methods 0.000 claims description 6
- 229910021645 metal ion Inorganic materials 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000001579 optical reflectometry Methods 0.000 abstract description 3
- 235000012431 wafers Nutrition 0.000 description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 238000003486 chemical etching Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001020 plasma etching Methods 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 235000008216 herbs Nutrition 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910020448 SiO2(OH)2-2+2H2 Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- 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 Table
-
- 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
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
The invention discloses a method for preparing texture on a monocrystalline silicon wafer by using tetramethylguanidine organic alkali, which comprises the steps of firstly cleaning the silicon wafer, then preparing a mixed solution of tetramethylguanidine and isopropanol by using a deionized water solvent, wherein the volume ratio of tetramethylguanidine is 10 percent, the volume ratio of isopropanol is 7 percent, and preheating the mixed solution for later use in a water bath kettle at the temperature of 80 ℃; and (3) putting the silicon wafer into the texturing solution, heating the silicon wafer in water bath at 80 ℃ for 35min, washing the silicon wafer with deionized water for two to three times, and then carrying out ultrasonic treatment on the silicon wafer with the deionized water for 5min to remove the solution residues. The optical reflectivity of the tetramethyl guanidine organic alkali monocrystalline silicon after texturing is greatly reduced, the pollution of metal ions in the texturing solution to a silicon wafer is eliminated, and the subsequent treatment cost of the texturing waste liquid is reduced.
Description
Technical Field
The invention belongs to the technical field of photovoltaics, and particularly relates to a method for texture surface making of a monocrystalline silicon wafer by using tetramethylguanidine organic alkali.
Background
The texture characteristic of the monocrystalline silicon solar cell is one of important factors influencing the conversion efficiency of the monocrystalline silicon solar cell. The existing texturing methods include: chemical etching, reactive ion etching, photolithography, mechanical grooving, and the like. Among the above methods, mechanical grooving is to simultaneously form V-grooves on the surface of polysilicon by using a plurality of blades to reduce optical reflection. Although the method has the advantages of simple process and high grooving speed, the mechanical grooving is deep, requires a thicker silicon wafer and is not suitable for manufacturing a thin-substrate solar cell. Meanwhile, in the etching process, the surface of the silicon wafer can be damaged, and impurities can be introduced. The reactive ion etching method is also called plasma etching, and is a dry etching process which adopts low-pressure gas to generate plasma and utilizes a physical mechanism to assist chemical etching or generates reactive ions to participate in chemical etching. The reflectivity of the formed texture is particularly low, the reflectivity in the spectral range of 450 to 1000nm can be less than 2%, but the silicon surface is seriously damaged, the open-circuit voltage and the filling factor of the battery can be reduced, and in addition, the defects of low yield and high manufacturing cost are realized. The chemical etching method generally uses a mixed solution of alkali (NaOH or KOH) alcohol (isopropanol or ethanol) as an etching system. Wherein, the alkali is a corrosive agent used for corroding the silicon chip, and the alcohol is a defoaming agent used for removing hydrogen bubbles generated by the reaction.
The formation of "pyramids" is due to the anisotropic reaction of the base with silicon. In a certain concentration of alkali solution, OH-The reaction speed of the ions and the (100) surface of the silicon is several times or even dozens of times faster than that of the (111) surface, the corrosion reaction starts from the (100) surface, and finally, staggered (111) crystal surfaces are exposed, so that a plurality of tetrahedral pyramids, commonly called pyramid structures, are formed on the surface of the silicon wafer.
At present, the most persuasive model for texturing monocrystalline silicon is an electrochemical model. The main principle of the model is that the anisotropic etching of silicon by alkali is mainly caused by the difference of dangling bond density and back bond structure and energy level of the silicon surface. During the whole etching process, the first 4 OH groups-Ions react with silicon on one surface while OH-The ions combine with unpaired electrons on the surface of the silicon wafer to form Si-O bonds. Since the energy level of electrons on the dangling bond is relatively high, the reaction proceeds further as the reaction proceeds by thermally exciting the electrons into the conduction band. And the electrons entering the conduction band neutralize H in solution2O reacts to form new OH-And H2. The entire reaction can be simply written as:
Si+2OH-+2H2O→SiO2(OH)2 2-+2H2↑
the pyramid structure is mainly increased by two refractions of light rays in the pyramid structureThe times of light absorption are increased, so that the light absorption rate of the silicon chip is increased, and the reflectivity of the surface of the silicon chip is reduced. Has extremely wide application in the field of solar cells. Most of the existing texturing methods use inorganic alkali to provide OH-Ionic. The commonly used inorganic alkali mainly comprises KOH, NaOH and the like, so that a large amount of metal ions exist in the texturing solution, the existence of the metal ions has certain influence on the minority carrier lifetime of the silicon wafer, and the influence of the metal ions is particularly important in the manufacturing process of a high-efficiency solar cell. Therefore, in recent years, organic alkali texturing solutions have come into widespread use. Another major reason organic bases begin to dominate the market for texturing solutions is the treatment of waste streams. Along with the increasing importance of our country on environmental protection in recent years, the treatment of waste liquid in the process of making herbs into wool also becomes another important principle for people to select the making herbs into wool.
Disclosure of Invention
The invention aims to provide a method for texturing a monocrystalline silicon wafer by using tetramethylguanidine organic alkali.
The technical scheme of the invention is as follows:
a method for texture etching of a monocrystalline silicon wafer by using tetramethylguanidine organic alkali comprises the following steps:
1) cleaning a silicon wafer;
2) preparing a mixed solution of tetramethylguanidine and isopropanol by using a deionized water solvent, wherein the volume ratio of the tetramethylguanidine is 10 percent, the volume ratio of the isopropanol is 7 percent, and preheating the mixed solution for later use in a water bath kettle at the temperature of 80 ℃;
3) putting the silicon wafer obtained in the step 1) into the texturing solution obtained in the step 2), heating the silicon wafer in water bath at 80 ℃ for 35min, washing the silicon wafer with deionized water for two to three times, and then carrying out ultrasonic treatment on the silicon wafer with deionized water for 5min to remove solution residues.
According to the invention, organic alkali-tetramethylguanidine is used for replacing the traditional sodium hydroxide or potassium hydroxide to be used as a corrosion solution for monocrystalline silicon texturing, the pyramid distribution on the surface of the textured monocrystalline silicon is dense and uniform in size, and the average optical reflectivity of the silicon wafer is 3.14% within the wavelength range of 400-1000 nm. Compared with the traditional inorganic alkali monocrystalline silicon texturing, the optical reflectivity of the tetramethylguanidine organic alkali monocrystalline silicon provided by the invention after texturing is greatly reduced, the pollution of metal ions in the texturing solution to silicon wafers is eliminated, and the subsequent treatment cost of the texturing waste liquid is also reduced.
Drawings
The following detailed description is made with reference to the accompanying drawings and embodiments of the present invention
FIG. 1 is a metallographic microscope photograph of a sample of this example;
FIG. 2 is a reflectance chart of the sample of this example.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
1.1 Main raw materials
P-type monocrystalline silicon piece: 2 inches in diameter.
Chemical reagents: acetone, absolute ethyl alcohol, sodium hydroxide, isopropanol, hydrofluoric acid, tetramethylguanidine, ammonia water, hydrochloric acid and hydrogen peroxide.
1.2 Main test Instrument
Metallographic microscope, ultraviolet visible spectrophotometer.
1.3 preparation Process
(1) Silicon wafer cleaning
a. Putting a silicon wafer into a clean polytetrafluoroethylene beaker, adding a proper amount of acetone, performing ultrasonic treatment for 10min, washing with deionized water for two to three times, and adding deionized water, performing ultrasonic treatment for 5min to remove solution residues;
b. adding a proper amount of absolute ethyl alcohol into a beaker, carrying out ultrasonic treatment for 10min, washing with deionized water for two to three times, and carrying out ultrasonic treatment with deionized water for 5min to remove solution residues;
c. putting the silicon wafer into 25% NaOH solution, heating the silicon wafer in water bath at 80 ℃ for 20min to remove mechanical damage on the surface of the silicon wafer, then washing the silicon wafer with deionized water for two to three times, and then carrying out ultrasonic treatment on the silicon wafer with deionized water for 5min to remove solution residues;
d. adding into a beaker at a ratio of 1:1:5Addition of NH4OH、H2O2、H2Heating O in water bath at 80 deg.C for 15min, washing with deionized water for two to three times, and ultrasonic treating with deionized water for 5min to remove solution residue;
e. adding the mixture into a beaker according to the proportion of 1:1:5 adding HCl and H2O2、H2Heating O in water bath at 80 deg.C for 15min, washing with deionized water for two to three times, and ultrasonic treating with deionized water for 5min to remove solution residue;
f. soaking for 3min with 1% hydrofluoric acid, washing with deionized water for two to three times, and ultrasonically treating with deionized water for 5min to remove the solution residue;
g. with N2And drying for later use.
(2) Texturing process
a. Preparing a mixed solution of 10 percent (vl) of tetramethylguanidine and 7 percent (vl) of isopropanol, and preheating for 10min in a water bath kettle at the temperature of 80 ℃.
b. And (3) putting the cleaned silicon wafer into a preheated texturing solution, heating the silicon wafer in water bath at 80 ℃ for 35min, washing the silicon wafer with deionized water for two to three times, and performing ultrasonic treatment on the silicon wafer with the deionized water for 5min to remove solution residues.
(3) Sample characterization
a. Preliminarily observing the surface appearance of the sample by using a metallographic microscope;
b. the reflectance of the sample was measured using an ultraviolet-visible-near infrared spectrophotometer.
1.4 results and analysis
The metallographic microscope image in fig. 1 can preliminarily observe that the pyramid-shaped texture surface is successfully prepared on the surface of the silicon wafer, and the pyramids are densely distributed and uniform in size. However, due to the problems of depth of field and resolution of the metallographic microscope, the specific morphological characteristics of the pyramid cannot be accurately and finely observed.
From the reflectance graph of fig. 2, it can be seen that the overall reflectance of the sample is less than 7% in the wavelength range of 200nm to 1000nm, indicating that the sample has a good antireflection effect.
Claims (1)
1. A method for texture etching of a monocrystalline silicon wafer by using tetramethylguanidine organic alkali is characterized by comprising the following steps: the method comprises the following steps:
1) cleaning a silicon wafer;
2) preparing a mixed solution of tetramethylguanidine and isopropanol by using a deionized water solvent, wherein the volume ratio of the tetramethylguanidine is 10 percent, the volume ratio of the isopropanol is 7 percent, and preheating the mixed solution for later use in a water bath kettle at the temperature of 80 ℃;
3) putting the silicon wafer obtained in the step 1) into the texturing solution obtained in the step 2), heating the silicon wafer in water bath at 80 ℃ for 35min, washing the silicon wafer with deionized water for two to three times, and then carrying out ultrasonic treatment on the silicon wafer with deionized water for 5min to remove solution residues.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910893517.0A CN110707163A (en) | 2019-09-20 | 2019-09-20 | Method for texturing on surface of single crystal silicon by using tetramethylguanidine organic alkali |
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| CN201910893517.0A CN110707163A (en) | 2019-09-20 | 2019-09-20 | Method for texturing on surface of single crystal silicon by using tetramethylguanidine organic alkali |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110180132A1 (en) * | 2010-01-28 | 2011-07-28 | Curtis Dove | Texturing and damage etch of silicon single crystal (100) substrates |
| CN102169818A (en) * | 2009-12-17 | 2011-08-31 | 罗门哈斯电子材料有限公司 | Improved method of texturing semiconductor substrates |
| CN102400225A (en) * | 2010-09-16 | 2012-04-04 | 上海神舟新能源发展有限公司 | Texture etching solution of monocrystaline silicon solar cell, preparation method, and application thereof |
| CN103314448A (en) * | 2010-09-03 | 2013-09-18 | 肖特太阳能股份公司 | Method for the wet-chemical etching of a highly doped semiconductor layer |
| CN106521635A (en) * | 2016-11-17 | 2017-03-22 | 上海交通大学 | All-solution preparation method of nanoscale pyramid suede on silicon surface |
-
2019
- 2019-09-20 CN CN201910893517.0A patent/CN110707163A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102169818A (en) * | 2009-12-17 | 2011-08-31 | 罗门哈斯电子材料有限公司 | Improved method of texturing semiconductor substrates |
| US20110180132A1 (en) * | 2010-01-28 | 2011-07-28 | Curtis Dove | Texturing and damage etch of silicon single crystal (100) substrates |
| CN103314448A (en) * | 2010-09-03 | 2013-09-18 | 肖特太阳能股份公司 | Method for the wet-chemical etching of a highly doped semiconductor layer |
| CN102400225A (en) * | 2010-09-16 | 2012-04-04 | 上海神舟新能源发展有限公司 | Texture etching solution of monocrystaline silicon solar cell, preparation method, and application thereof |
| CN106521635A (en) * | 2016-11-17 | 2017-03-22 | 上海交通大学 | All-solution preparation method of nanoscale pyramid suede on silicon surface |
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