WO2012169722A1 - Composition de type solution de gravage texturante et procédé de gravage texturant pour plaquette de silicium cristallin - Google Patents

Composition de type solution de gravage texturante et procédé de gravage texturant pour plaquette de silicium cristallin Download PDF

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WO2012169722A1
WO2012169722A1 PCT/KR2012/001750 KR2012001750W WO2012169722A1 WO 2012169722 A1 WO2012169722 A1 WO 2012169722A1 KR 2012001750 W KR2012001750 W KR 2012001750W WO 2012169722 A1 WO2012169722 A1 WO 2012169722A1
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cellulose
silicon wafer
crystalline silicon
texture
texture etching
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PCT/KR2012/001750
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English (en)
Korean (ko)
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홍형표
이재연
박면규
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동우화인켐 주식회사
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Priority to CN201280024303.6A priority Critical patent/CN103562344B/zh
Publication of WO2012169722A1 publication Critical patent/WO2012169722A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/02—Etching, surface-brightening or pickling compositions containing an alkali metal hydroxide
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Definitions

  • the present invention relates to a texture etching liquid composition and a texture etching method of a crystalline silicon wafer capable of uniformly forming a crystalline silicon wafer surface in a fine pyramid structure to increase light efficiency.
  • Solar cells which are rapidly spreading in recent years, are electronic devices that directly convert solar energy, which is clean energy, into electricity as a next-generation energy source, and diffuse phosphorus on its surface based on P-type silicon semiconductors containing boron in silicon. It consists of the PN junction semiconductor substrate in which the N type silicon semiconductor layer was formed.
  • the surface of the solar cell silicon wafer constituting the PN junction semiconductor substrate is formed into a fine pyramid structure and the antireflection film is treated.
  • the surface of the silicon wafer textured with the fine pyramid structure increases the intensity of the light absorbed by lowering the reflectance of incident light having a wide wavelength band, thereby improving the performance of the solar cell.
  • U.S. Patent No. 4,137,123 discloses 0.5-10 weight in an anisotropic etching solution containing 0-75% by volume of ethylene glycol, 0.05-50% by weight of potassium hydroxide and the remaining amount of water.
  • a silicon texture etching solution in which% silicon is dissolved is disclosed.
  • this etchant can cause pyramid formation defects to increase the light reflectance and cause a decrease in efficiency.
  • European Patent No. 0477424 discloses a texture etching method of supplying oxygen to a texture etching solution in which silicon is dissolved in ethylene glycol, potassium hydroxide and residual water, that is, performing an air rating process.
  • this etching method has a disadvantage in that it causes poor pyramid formation, which leads to an increase in light reflectivity and a decrease in efficiency, and requires the installation of a separate air rating equipment.
  • Korean Patent No. 0180621 discloses a texture etching solution mixed at a ratio of 0.5-5% potassium hydroxide solution, 3-20% by volume of isopropyl alcohol, and 75-96.5% by volume of deionized water
  • US Patent No. 6,451,218 No. discloses a texture etching solution comprising an alkali compound, isopropyl alcohol, a water soluble alkaline ethylene glycol and water.
  • these etching solutions contain isopropyl alcohol having a low boiling point and need to be added during the texturing process, it is not economical in terms of productivity and cost, and the addition of isopropyl alcohol causes a temperature gradient of the etching solution, resulting in the surface of the silicon wafer.
  • the texture quality variation of each position may increase, resulting in poor uniformity.
  • An object of the present invention is to provide a texture etching liquid composition of a crystalline silicon wafer that can improve the light efficiency by improving the uniformity of the texture by position in forming a texture of the fine pyramid structure on the surface of the crystalline silicon wafer.
  • an object of the present invention is to provide a texture etching liquid composition of a crystalline silicon wafer that does not require the addition of an additional etching liquid component and the application of an air rating process during the etching process.
  • Another object of the present invention is to provide a texture etching method using the texture etching liquid composition of the crystalline silicon wafer.
  • alkali compound 1. 0.1-20% by weight of alkali compound; Polysaccharides 10 -9 to 10% by weight; Silica compounds 10 -9 to 10% by weight; And a residual amount of water.
  • composition according to the above 1, wherein the alkali compound is at least one selected from the group consisting of potassium hydroxide, sodium hydroxide, ammonium hydroxide, tetrahydroxymethylammonium and tetrahydroxyethylammonium.
  • polysaccharide is at least one selected from the group consisting of glucan-based compounds, fructan-based compounds, mannan-based compounds, galactan-based compounds and metal salts of the texture etching liquid composition of the crystalline silicon wafer.
  • the polysaccharide is cellulose, dimethylaminoethyl cellulose, diethylaminoethyl cellulose, ethyl hydroxyethyl cellulose, methyl hydroxyethyl cellulose, 4-aminobenzyl cellulose, triethylaminoethyl cellulose, cyanoethyl cellulose , Ethyl cellulose, methyl cellulose, carboxymethyl cellulose, carboxyethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, alginic acid, amylose, amylopectin, pectin, starch, dextrin, ⁇ -cyclodextrin, ⁇ -cyclodextrin, ⁇ - 1 type selected from the group consisting of cyclodextrin, hydroxypropyl- ⁇ -cyclodextrin, methyl- ⁇ -cyclodextrin, dextran, dextransulfate sodium, sapon
  • the polysaccharide has an average molecular weight of 5,000 to 1,000,000 texture etching liquid composition of a crystalline silicon wafer.
  • the silica compound is fine powder silica; Colloidal silica solution stabilized with Na 2 O; Colloidal silica solution stabilized with K 2 O; Colloidal silica solution stabilized with acid solution; Colloidal silica solution stabilized with NH 3 ; Colloidal silica solution stabilized with at least one organic solvent selected from the group consisting of ethyl alcohol, propyl alcohol, ethylene glycol, methyl ethyl ketone and methyl isobutyl ketone; Liquid sodium silicate; Liquid potassium silicate; And a liquid etching silicate composition of at least one crystalline silicon wafer selected from the group consisting of liquid lithium silicate.
  • the texture etching method of the crystalline silicon wafer comprising the step of depositing, spraying or depositing and spraying the crystalline silicon wafer with the texture etching liquid composition of any one of the above 1 to 7.
  • the deposition, spraying or deposition and spraying is a texture etching method of a crystalline silicon wafer is carried out for 30 seconds to 60 minutes at a temperature of 50 to 100 °C.
  • the texture of the fine pyramid structure is uniformly formed on the surface of the crystalline silicon wafer to maximize the absorption of solar light and lower the light reflectance to increase the light efficiency.
  • the present invention does not need to add a separate etching liquid component during the texturing process and does not need to introduce an air rating equipment, thereby improving the quality and productivity, and also has an advantage in terms of process cost.
  • Example 1 is a 3D optical micrograph showing the surface of a single crystal silicon wafer texture-etched with the texture etching liquid composition of the crystalline silicon wafer of Example 10 of the present invention
  • FIG. 2 is a SEM photograph showing the surface of a single crystal silicon wafer textured etched with the texture etching solution composition of the crystalline silicon wafer of Example 10 of the present invention.
  • the present invention relates to a texture etching liquid composition of a crystalline silicon wafer and a method of etching the texture of a crystalline silicon wafer using the same.
  • the texture etching solution composition of the crystalline silicon wafer of the present invention is an alkali compound; Polysaccharides; Silica compounds; And a residual amount of water.
  • the alkali compound 0.1 to 20% by weight; Polysaccharides 10 -9 to 10% by weight; Silica compounds 10 -9 to 10% by weight; And residual amount of water.
  • An alkali compound is a component which etches the surface of a crystalline silicon wafer,
  • the kind is not specifically limited.
  • potassium hydroxide, sodium hydroxide, ammonium hydroxide, tetrahydroxymethylammonium, tetrahydroxyethylammonium, etc. are mentioned, Among these, potassium hydroxide and sodium hydroxide are preferable. These can be used individually or in mixture of 2 or more types.
  • the alkali compound is preferably included in an amount of 0.1 to 20% by weight, and more preferably 1 to 5% by weight, based on 100% by weight of the total amount of the texture etching solution composition of the crystalline silicon wafer.
  • the silicon wafer surface can be etched.
  • the present invention is characterized by including the polysaccharide in an optimum content.
  • Polysaccharides are saccharides in which two or more monosaccharides are glycosidic bonds to form large molecules, and are formed by etching while forming a uniform fine pyramid and improving appearance by preventing overetching and accelerated etching by alkaline compounds. It is a component that prevents the bubble stick phenomenon by quickly dropping the hydrogen bubbles from the silicon wafer surface.
  • polysaccharides examples include glucan compounds, fructan compounds, mannan compounds, galactan compounds, or metal salts thereof, among which glucan compounds and metal salts thereof (e.g., Alkali metal salts) are preferred. These can be used individually or in mixture of 2 or more types.
  • glucan compound examples include cellulose, dimethylaminoethyl cellulose, diethylaminoethyl cellulose, ethyl hydroxyethyl cellulose, methyl hydroxyethyl cellulose, 4-aminobenzyl cellulose, triethylaminoethyl cellulose, cyanoethyl cellulose, ethyl cellulose, Methyl cellulose, carboxymethyl cellulose, carboxyethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, alginic acid, amylose, amylopectin, pectin, starch, dextrin, ⁇ -cyclodextrin, ⁇ -cyclodextrin, ⁇ -cyclodextrin, hydrate Oxypropyl- ⁇ -cyclodextrin, methyl- ⁇ -cyclodextrin, dextran, dextransulfate sodium, saponin, glycogen, zymoic acid
  • the polysaccharide may have an average molecular weight of 5,000 to 1,000,000, preferably 50,000 to 200,000.
  • the polysaccharide may be included in an amount of 10 -9 to 10% by weight, preferably 10 -6 to 1% by weight, based on 100% by weight of the texture etching solution composition of the crystalline silicon wafer. If the content falls within the above range, it is possible to effectively prevent over-etching and etching acceleration. If the content is more than 10% by weight, it is difficult to form the desired fine pyramid by drastically lowering the etching rate by the alkali compound.
  • the present invention is characterized by including the silica compound in an optimal content together with the polysaccharide.
  • the silica compound is a component that is physically adsorbed on the surface of the crystalline silicon wafer to serve as a kind of mask, so that the surface of the crystalline silicon wafer is more easily formed in a fine pyramid shape.
  • silica compound examples include powder, colloidal solution, or liquid metal silicate compounds. Specifically, fine powder silica; Colloidal silica solution stabilized with Na 2 O; Colloidal silica solution stabilized with K 2 O; Colloidal silica solution stabilized with acid solution; Colloidal silica solution stabilized with NH 3 ; Colloidal silica solution stabilized with at least one organic solvent selected from the group consisting of ethyl alcohol, propyl alcohol, ethylene glycol, methyl ethyl ketone and methyl isobutyl ketone; Liquid sodium silicate; Liquid potassium silicate; Liquid lithium silicate etc. can be mentioned, These can be used individually or in mixture of 2 or more types.
  • the silica compound may be included in an amount of 10 -9 to 10% by weight, preferably 10 -6 to 1% by weight, based on 100% by weight of the total amount of the texture etching solution composition of the crystalline silicon wafer. If the content falls within the above range, it is possible to easily form a fine pyramid on the surface of the crystalline silicon wafer.
  • the texture etching solution composition of the crystalline silicon wafer of the present invention may further include a fluorine-based surfactant.
  • the fluorine-based surfactant lowers the surface tension of the etching solution composition to further promote the wettability improvement of the surface of the crystalline silicon wafer, thereby preventing overetching by the alkali compound.
  • fluorine-type surfactant such as a perfluoroalkyl carboxylate, a perfluoroalkyl sulfonate, a perfluoroalkyl sulfate, a perfluoroalkyl phosphate; Cationic surfactants such as perfluoroalkyl amine salts and perfluoroalkyl quaternary ammonium salts; Amphoteric ionic surfactants such as perfluoroalkyl carboxybetaine and perfluoroalkyl sulfobetaine; And nonionic surfactants such as fluorinated alkyl polyoxyethylene and perfluoroalkyl polyoxyethylene. These compounds may be those having 1 to 30 carbon atoms in each alkyl group. These can be used individually or in mixture of 2 or more types.
  • the fluorine-based surfactant may be included in an amount of 10 -9 to 10% by weight, preferably 10 -6 to 1% by weight, based on 100% by weight of the texture etching solution composition of the crystalline silicon wafer. When the content falls within the above range, the wettability of the silicon wafer surface can be effectively improved.
  • Water may be included in the remaining amount in the total 100% by weight of the texture etching solution composition of the crystalline silicon wafer.
  • the kind of water is not specifically limited, It is preferable that it is deionized distilled water, More preferably, it is preferable that the specific resistance value is 18 kW / cm or more as deionized distilled water for a semiconductor process.
  • the texture etching solution composition of the crystalline silicon wafer of the present invention comprising the above components, in particular, by forming an optimal content of the silica compound with polysaccharides to uniformly form the surface of the crystalline silicon wafer with the texture of the fine pyramid structure
  • an optimal content of the silica compound with polysaccharides to uniformly form the surface of the crystalline silicon wafer with the texture of the fine pyramid structure
  • the texture etching liquid composition of the crystalline silicon wafer of the present invention can be applied to all conventional etching processes, such as dip, spray and single wafer etching processes.
  • the present invention provides a texture etching method of a crystalline silicon wafer using the texture etching liquid composition of the crystalline silicon wafer.
  • the texture etching method of the crystalline silicon wafer includes depositing, spraying or depositing and spraying the crystalline silicon wafer using the texture etching liquid composition of the crystalline silicon wafer of the present invention.
  • the number of depositions and sprays is not particularly limited, and the order of both deposition and spraying is not limited.
  • Deposition, spraying or depositing and spraying may be performed for 30 seconds to 60 minutes at a temperature of 50 to 100 ° C.
  • the texture etching method of the crystalline silicon wafer of the present invention does not need to introduce a separate air-rating apparatus for supplying oxygen, so it is economical in terms of initial production and processing costs, and is uniform even in a simple process. It allows the formation of a structure.
  • KOH potassium hydroxide
  • DMAEC dimethylaminoethylcellulose
  • SSS liquid sodium silicate
  • Example 2 The same procedure as in Example 1, except that the same ingredients and contents as in Table 1 were used. Here, the content represents weight percent.
  • a 1.5% by weight potassium hydroxide (KOH), 5% by weight isopropyl alcohol (IPA) and the remaining amount of deionized distilled water was mixed to prepare a texture etching solution composition of the crystalline silicon wafer.
  • the single crystal silicon wafer substrate was immersed in the texture etching liquid composition of the prepared silicon wafer for 20 minutes at a temperature of 80 ° C.
  • Texture variation that is, uniformity, formed on the surface of the etched single crystal silicon wafer substrate was visually observed using a digital camera, a 3D optical microscope, and a scanning electron microscope (SEM), and evaluated based on the following criteria. .
  • the size of the fine pyramid formed on the surface of the textured etched single crystal silicon wafer substrate was measured using a scanning electron microscope (SEM). At this time, the size of the fine pyramid formed in the unit area was measured and expressed as their average value.
  • the average reflectance when the surface of the texture-etched single crystal silicon wafer substrate was irradiated with light having a wavelength band of 400-800 nm using a UV spectrophotometer was measured.
  • the alkali compound according to the present invention Polysaccharides; Silica compounds; And when the texture was etched using the texture etching solution composition of Examples 1 to 14 containing the optimum amount of water was excellent in the uniformity of the fine pyramid formed on the surface of the single crystal silicon wafer and the light reflectance was able to increase the light efficiency .
  • FIG. 1 is a 3D optical micrograph showing the surface of the crystalline silicon wafer texture etched with the texture etching solution composition of Example 10,
  • Figure 2 is a SEM photograph showing the surface of the texture etched crystalline silicon wafer. Through this, it can be seen that the fine pyramid is formed over the entire surface of the wafer so that the quality variation is small and the texture uniformity is improved.
  • Comparative Example 1 which does not include polysaccharides, the etching proceeds rapidly, so that the pyramid is not only large, but the pyramids are hardly formed. .
  • Comparative Example 3 containing an excess of the silica compound did not completely dissolve the silica compound, so that it was difficult to obtain a sufficient effect.
  • Comparative Example 4 containing an excess of the polysaccharide, the etching rate was too slow to increase the reflectance.
  • the texture etching solution composition of Comparative Example 5 due to the low temperature of the isopropyl alcohol (IPA) due to the temperature gradient generated by the continuous input of the texture during the texture failure and cost more,
  • the texture etchant composition showed significantly inferior characteristics in comparison with Examples in terms of texture uniformity and light reflectance.
  • the texture etching solution compositions of Comparative Examples 7 and 8 exhibited a change with time in the etching solution composition itself when heated to the texture process temperature.

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Abstract

Cette invention concerne une composition de type solution de gravage texturante et un procédé de gravage texturant pour plaquette de silicium cristallin, et plus spécifiquement, une composition de type solution de gravage texturante et un procédé de gravage texturant pour plaquette de silicium cristallin ayant la teneur optimale suivante : un composé alcalin ; un polysaccharide ; un composé de silice ; le reste étant de l'eau, pour améliorer ainsi l'uniformité d'une texture constituée d'une fine structure pyramidale à la surface de la plaquette en silicium cristallin de façon à maximiser l'absorption de la lumière solaire, et à réduire le taux de réflexion de la lumière pour augmenter le rendement lumineux.
PCT/KR2012/001750 2011-06-10 2012-03-09 Composition de type solution de gravage texturante et procédé de gravage texturant pour plaquette de silicium cristallin WO2012169722A1 (fr)

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KR1020110056075A KR20120136882A (ko) 2011-06-10 2011-06-10 결정성 실리콘 웨이퍼의 텍스쳐 에칭액 조성물 및 텍스쳐 에칭방법

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CN104562011A (zh) * 2013-10-09 2015-04-29 上海太阳能工程技术研究中心有限公司 多晶硅片的制绒辅助剂及制绒工艺
CN114086259A (zh) * 2021-11-29 2022-02-25 浙江奥首材料科技有限公司 一种无醇型两亲性制绒添加剂及其制备方法

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KR101994084B1 (ko) * 2012-12-24 2019-06-28 동우 화인켐 주식회사 결정성 실리콘 웨이퍼의 텍스쳐 에칭액 조성물 및 텍스쳐 에칭방법
WO2015020243A1 (fr) * 2013-08-06 2015-02-12 동우화인켐 주식회사 Composition de solution de gravure de texture pour plaquettes de silicium cristallin et procédé de gravure de texture
CN105206687A (zh) * 2015-08-21 2015-12-30 合肥中南光电有限公司 一种高效快速单晶硅片制绒液及其制备方法

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CN114086259A (zh) * 2021-11-29 2022-02-25 浙江奥首材料科技有限公司 一种无醇型两亲性制绒添加剂及其制备方法
CN114086259B (zh) * 2021-11-29 2023-01-13 浙江奥首材料科技有限公司 一种无醇型两亲性制绒添加剂及其制备方法

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