WO2013118739A1 - テクスチャー形成用エッチング液 - Google Patents
テクスチャー形成用エッチング液 Download PDFInfo
- Publication number
- WO2013118739A1 WO2013118739A1 PCT/JP2013/052663 JP2013052663W WO2013118739A1 WO 2013118739 A1 WO2013118739 A1 WO 2013118739A1 JP 2013052663 W JP2013052663 W JP 2013052663W WO 2013118739 A1 WO2013118739 A1 WO 2013118739A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- etching solution
- mass
- texture
- phosphonic acid
- present
- Prior art date
Links
- 238000005530 etching Methods 0.000 title claims abstract description 50
- 239000007788 liquid Substances 0.000 title abstract 3
- 150000003007 phosphonic acid derivatives Chemical class 0.000 claims abstract description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 21
- 239000010703 silicon Substances 0.000 claims abstract description 21
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 35
- 239000003513 alkali Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 3
- IIRVGTWONXBBAW-UHFFFAOYSA-M disodium;dioxido(oxo)phosphanium Chemical compound [Na+].[Na+].[O-][P+]([O-])=O IIRVGTWONXBBAW-UHFFFAOYSA-M 0.000 claims description 2
- 235000012431 wafers Nutrition 0.000 abstract description 29
- 239000000654 additive Substances 0.000 abstract description 10
- 230000000996 additive effect Effects 0.000 abstract description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 21
- 238000000034 method Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- -1 alkali metal salts Chemical class 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- SZHQPBJEOCHCKM-UHFFFAOYSA-N 2-phosphonobutane-1,2,4-tricarboxylic acid Chemical compound OC(=O)CCC(P(O)(O)=O)(C(O)=O)CC(O)=O SZHQPBJEOCHCKM-UHFFFAOYSA-N 0.000 description 2
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 229940042400 direct acting antivirals phosphonic acid derivative Drugs 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- DUYCTCQXNHFCSJ-UHFFFAOYSA-N dtpmp Chemical compound OP(=O)(O)CN(CP(O)(O)=O)CCN(CP(O)(=O)O)CCN(CP(O)(O)=O)CP(O)(O)=O DUYCTCQXNHFCSJ-UHFFFAOYSA-N 0.000 description 1
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000001179 sorption measurement 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
- H01L31/02—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
- C09K13/02—Etching, surface-brightening or pickling compositions containing an alkali metal hydroxide
-
- 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
-
- 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 an etching solution for forming an uneven structure called texture on the surface of a silicon substrate.
- a crystalline silicon substrate used in a solar cell is subjected to a surface structure treatment called texture in order to reduce light reflectance on the substrate surface and efficiently absorb light.
- an etching solution for forming a texture for example, as described in Patent Document 1, a solution obtained by adding isopropyl alcohol (IPA) to an aqueous solution of sodium hydroxide or potassium hydroxide is known.
- IPA isopropyl alcohol
- the texture is formed by immersing the silicon wafer for 10 to 30 minutes under a heating condition of 60 to 95 ° C.
- the IPA is widely recognized as an additive for forming a pyramidal texture on a silicon wafer, and although it can be finished into a wafer of good quality, the boiling point of IPA is 82.4 ° C. Since the temperature is about the same as the etching temperature, there is a problem that the composition of the etching solution is likely to change due to volatilization of IPA during the processing. In addition, care is required in handling because of its low flash point.
- the slicing method of silicon wafers is shifting from the conventional free abrasive method to the fixed abrasive method. In these methods, the surface state of the wafer after slicing is different from each other. There is also a problem that the etching solution that can be used may not be used as it is for the fixed abrasive wafer.
- the present invention has been made in view of the above problems, and can form a good texture uniformly and stably on the wafer surface.
- the additive component It is an object of the present invention to provide an etching solution for forming a texture of a silicon wafer, which does not volatilize and can be applied to both a free abrasive wafer and a fixed abrasive wafer.
- the etching solution of the present invention is an etching solution for forming irregularities on the surface of a silicon substrate, and includes (A) an alkali component and (B) a phosphonic acid derivative or a salt thereof in order to solve the above problems. It shall consist of an aqueous solution.
- sodium hydroxide or potassium hydroxide can be used as the most preferable alkali component.
- the concentration of the alkali component is preferably 0.3% by mass to 25% by mass.
- concentration of the phosphonic acid derivative or a salt thereof is preferably 0.1% by mass to 25% by mass.
- the alkali component used in the present invention is not particularly limited, and those conventionally used as etching solutions for silicon wafers can be used as appropriate. Examples thereof include alkali metal or alkaline earth metal hydroxides such as sodium hydroxide and potassium hydroxide, or salts thereof, and sodium hydroxide is preferred in terms of easy availability. These alkali components may be used in combination of two or more as required.
- the phosphonic acid derivative used as an additive in the present invention is not particularly limited as long as it is generally used as a sequestering agent.
- 1-hydroxyethylene-1,1-diphosphonic acid represented by the following formula (1) nitrilotris (methylenephosphonic acid) represented by the following formula (2),
- alkali metal salts examples include alkali metal salts, alkaline earth metal salts, amine salts, and ammonium salts. Since they are generally easily available, alkali metal salts such as sodium salts and potassium salts are preferred. Used. Two or more of these phosphonic acid derivatives can be used as needed.
- 1-hydroxyethylene-1,1-diphosphonic acid is obtained because of the high uniformity of the obtained texture structure and the high purity product with few impurities to be avoided in this application.
- Nitrilotris (methylenephosphonic acid) or phosphonobutanetricarboxylic acid is particularly preferred.
- the etching solution of the present invention is an aqueous solution in which the alkali component and the phosphonic acid derivative are dissolved in water.
- the water used is preferably water from which impurities have been removed, such as ion exchange water or distilled water.
- the concentration of the alkali component is preferably in the range of 0.3% by mass to 25% by mass, more preferably 1% by mass to 15% by mass. If the concentration of the alkali component is less than 0.3% by mass, the etching power is insufficient, and it takes time to form the texture. If the concentration exceeds 25% by mass, the required amount of the etching inhibitor used as an additive increases, resulting in cost. Disadvantageous.
- the content of the phosphonic acid derivative in this etching solution is preferably 0.1% by mass to 25% by mass, and more preferably 0.5% by mass to 15% by mass. If the content of the phosphonic acid derivative is less than 0.1% by mass, the effect of suppressing alkali etching may not be sufficiently obtained. If the content exceeds 25% by mass, the etching of alkali is excessively suppressed, and it takes time to form the texture. May take too much.
- the ratio of the content of the phosphonic acid derivative to the content of the alkali component is preferable to control the ratio of the content of the phosphonic acid derivative to the content of the alkali component, and the blending ratio of the alkali component (A) and the phosphonic acid derivative (B) is
- additives such as isopropyl alcohol and fatty acid, which are usually used in the etching solution for texture formation of silicon wafers, are added as necessary, as long as they do not contradict the purpose of the present invention. be able to.
- the phosphonic acid derivative is regularly arranged on the surface of the silicon wafer of either the free abrasive type or the fixed abrasive type due to the excellent adsorption power of the phosphonic acid derivative. Since etching by alkali can be moderately suppressed, the present invention is applicable to both free abrasive wafers and fixed abrasive wafers.
- the etching method using the etching solution of the present invention is not particularly limited. As in the conventional method, the etching solution is heated to about 60 ° C. to 95 ° C., and the target silicon wafer is immersed for 10 to 30 minutes. Can be used.
- a uniform pyramidal texture structure can be formed on the surface of the silicon substrate. Further, since the additive component does not volatilize in the range of 60 ° C. to 95 ° C., which is the use temperature, a stable texture can be formed and safety is high. Furthermore, the etching solution of the present invention can be applied to either a free abrasive wafer or a fixed abrasive wafer. Therefore, by using the etching solution of the present invention, a high-quality silicon wafer that can enhance the performance of the solar cell can be supplied more stably.
- Examples and Comparative Examples Sodium hydroxide and a phosphonic acid derivative or a salt thereof were mixed at a ratio shown in Table 1, and ion exchange water was added to prepare an aqueous solution, which was used as an etching solution of the present invention.
- This etching solution was heated to 80 ° C., and a single crystal silicon wafer of either the free abrasive type or the fixed abrasive type shown in Table 1 was immersed for 20 minutes, then washed with water and dried.
- the texture structure of the obtained silicon wafer was evaluated according to the following two items.
- the etching solution of the present invention can be used for etching silicon substrates of solar cells.
- This application is based on a Japanese patent application filed on Feb. 8, 2012 (Japanese Patent Application No. 2012-025387), the contents of which are incorporated herein by reference.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Weting (AREA)
- Photovoltaic Devices (AREA)
- ing And Chemical Polishing (AREA)
Abstract
Description
水酸化ナトリウムとホスホン酸誘導体またはその塩を表1に示す割合で混合し、イオン交換水を加えて水溶液を調製し、これを本発明のエッチング液とした。このエッチング液を80℃に加温して、これに表1に示した遊離砥粒方式又は固定砥粒方式のいずれかの単結晶シリコンウェハを20分間浸漬した後、水洗して乾燥させた。得られたシリコンウェハのテクスチャー構造の評価を、次の2項目により実施した。
走査電子顕微鏡(日本電子製 JSM-6380LV)を用いてテクスチャー構造を観察した。倍率1000倍で観察した際に、基板表面上に、ピラミッドがない平坦な領域が全面積に対して5%以下となるようにピラミッド構造を形成しているものを「○」とし、全面積に対して5%を超えて平坦な領域が生じているものを「×」とした。
シリコン基板の反射率を紫外・可視分光光度計(日立ハイテクノロジーズ社製、U-3900H)で測定した。波長600nmの光の反射率が13%以下の場合は良好と判断して「○」とし、13%より大きい場合は不良と判断して「×」とした。
本出願は、2012年2月8日出願の日本特許出願(特願2012-025387)に基づくものであり、その内容はここに参照として取り込まれる。
Claims (6)
- シリコン基板表面に凹凸を形成させるエッチング液であって、
(A)アルカリ成分、及び(B)ホスホン酸誘導体またはその塩を含む水溶液からなることを特徴とする、エッチング液。 - 前記アルカリ成分が、水酸化ナトリウムまたは水酸化カリウムであることを特徴とする、請求項1に記載のエッチング液。
- 前記アルカリ成分の濃度が、0.3質量%~25質量%であることを特徴とする、請求項1に記載のエッチング液。
- 前記アルカリ成分の濃度が、0.3質量%~25質量%であることを特徴とする、請求項2に記載のエッチング液。
- 前記ホスホン酸誘導体またはその塩の濃度が、0.1質量%~25質量%であることを特徴とする、請求項1~4のいずれか1項に記載のエッチング液。
- 前記アルカリ成分(A)とホスホン酸誘導体またはその塩(B)との配合割合が、質量比でA/B=0.1~10であることを特徴とする、請求項1~5のいずれか1項に記載のエッチング液。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201380008345.5A CN104094411A (zh) | 2012-02-08 | 2013-02-06 | 用于形成纹理的蚀刻液 |
KR1020147022327A KR101608610B1 (ko) | 2012-02-08 | 2013-02-06 | 텍스처 형성용 에칭액 |
US14/376,692 US20150014580A1 (en) | 2012-02-08 | 2013-02-06 | Etching liquid for forming texture |
PH12014501790A PH12014501790A1 (en) | 2012-02-08 | 2014-08-07 | Etching liquid for forming texture |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2012025387A JP5575822B2 (ja) | 2012-02-08 | 2012-02-08 | テクスチャー形成用エッチング液 |
JP2012-025387 | 2012-02-08 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2013118739A1 true WO2013118739A1 (ja) | 2013-08-15 |
Family
ID=48947500
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2013/052663 WO2013118739A1 (ja) | 2012-02-08 | 2013-02-06 | テクスチャー形成用エッチング液 |
Country Status (8)
Country | Link |
---|---|
US (1) | US20150014580A1 (ja) |
JP (1) | JP5575822B2 (ja) |
KR (1) | KR101608610B1 (ja) |
CN (1) | CN104094411A (ja) |
MY (1) | MY171110A (ja) |
PH (1) | PH12014501790A1 (ja) |
TW (1) | TW201343877A (ja) |
WO (1) | WO2013118739A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015191946A (ja) * | 2014-03-27 | 2015-11-02 | 第一工業製薬株式会社 | テクスチャー形成用エッチング液およびそれを用いたテクスチャー形成方法 |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105220235B (zh) * | 2015-10-12 | 2017-12-08 | 常州捷佳创精密机械有限公司 | 一种单多晶制绒方法 |
CN111663186A (zh) * | 2020-06-30 | 2020-09-15 | 常州时创能源股份有限公司 | 金刚线切割单晶硅片制绒用添加剂及其应用 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0641773A (ja) * | 1992-05-18 | 1994-02-15 | Toshiba Corp | 半導体ウェーハ処理液 |
JP2012004528A (ja) * | 2010-05-18 | 2012-01-05 | Shinryo Corp | エッチング液およびシリコン基板の表面加工方法 |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3207636B2 (ja) * | 1993-10-18 | 2001-09-10 | 三菱重工業株式会社 | スマット除去液 |
TW200842970A (en) * | 2007-04-26 | 2008-11-01 | Mallinckrodt Baker Inc | Polysilicon planarization solution for planarizing low temperature poly-silicon thin filim panels |
TWI467055B (zh) * | 2007-12-21 | 2015-01-01 | Wako Pure Chem Ind Ltd | 蝕刻劑及蝕刻方法 |
JP5302551B2 (ja) * | 2008-02-28 | 2013-10-02 | 林純薬工業株式会社 | シリコン異方性エッチング液組成物 |
SG192033A1 (en) * | 2011-01-21 | 2013-08-30 | Cabot Microelectronics Corp | Silicon polishing compositions with improved psd performance |
-
2012
- 2012-02-08 JP JP2012025387A patent/JP5575822B2/ja active Active
-
2013
- 2013-02-06 US US14/376,692 patent/US20150014580A1/en not_active Abandoned
- 2013-02-06 KR KR1020147022327A patent/KR101608610B1/ko active IP Right Grant
- 2013-02-06 WO PCT/JP2013/052663 patent/WO2013118739A1/ja active Application Filing
- 2013-02-06 MY MYPI2014702156A patent/MY171110A/en unknown
- 2013-02-06 CN CN201380008345.5A patent/CN104094411A/zh active Pending
- 2013-02-08 TW TW102105285A patent/TW201343877A/zh unknown
-
2014
- 2014-08-07 PH PH12014501790A patent/PH12014501790A1/en unknown
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0641773A (ja) * | 1992-05-18 | 1994-02-15 | Toshiba Corp | 半導体ウェーハ処理液 |
JP2012004528A (ja) * | 2010-05-18 | 2012-01-05 | Shinryo Corp | エッチング液およびシリコン基板の表面加工方法 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015191946A (ja) * | 2014-03-27 | 2015-11-02 | 第一工業製薬株式会社 | テクスチャー形成用エッチング液およびそれを用いたテクスチャー形成方法 |
Also Published As
Publication number | Publication date |
---|---|
CN104094411A (zh) | 2014-10-08 |
KR20140116193A (ko) | 2014-10-01 |
JP5575822B2 (ja) | 2014-08-20 |
JP2013162093A (ja) | 2013-08-19 |
PH12014501790B1 (en) | 2014-11-17 |
PH12014501790A1 (en) | 2014-11-17 |
KR101608610B1 (ko) | 2016-04-01 |
MY171110A (en) | 2019-09-26 |
US20150014580A1 (en) | 2015-01-15 |
TW201343877A (zh) | 2013-11-01 |
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