JP6411499B2 - 銅リッチな銅インジウム(ガリウム)ジセレニド/ジスルフィドの調製 - Google Patents
銅リッチな銅インジウム(ガリウム)ジセレニド/ジスルフィドの調製 Download PDFInfo
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- JP6411499B2 JP6411499B2 JP2016531670A JP2016531670A JP6411499B2 JP 6411499 B2 JP6411499 B2 JP 6411499B2 JP 2016531670 A JP2016531670 A JP 2016531670A JP 2016531670 A JP2016531670 A JP 2016531670A JP 6411499 B2 JP6411499 B2 JP 6411499B2
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- 239000010949 copper Substances 0.000 title claims description 75
- 229910052802 copper Inorganic materials 0.000 title description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title description 17
- 229910052733 gallium Inorganic materials 0.000 title description 5
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 title description 3
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 title description 3
- 238000002360 preparation method Methods 0.000 title description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title description 2
- XIMIGUBYDJDCKI-UHFFFAOYSA-N diselenium Chemical compound [Se]=[Se] XIMIGUBYDJDCKI-UHFFFAOYSA-N 0.000 title 1
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- 150000003839 salts Chemical class 0.000 claims description 52
- 239000002243 precursor Substances 0.000 claims description 48
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- 150000001787 chalcogens Chemical class 0.000 claims description 45
- 239000011669 selenium Substances 0.000 claims description 37
- 229910052711 selenium Chemical group 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 19
- 229910052717 sulfur Inorganic materials 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical group [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- KZCOBXFFBQJQHH-UHFFFAOYSA-N octane-1-thiol Chemical group CCCCCCCCS KZCOBXFFBQJQHH-UHFFFAOYSA-N 0.000 claims description 13
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadec-1-ene Chemical compound CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 12
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 10
- 150000002258 gallium Chemical class 0.000 claims description 10
- 150000002471 indium Chemical class 0.000 claims description 10
- 150000001879 copper Chemical class 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- MHDVGSVTJDSBDK-UHFFFAOYSA-N dibenzyl ether Chemical compound C=1C=CC=CC=1COCC1=CC=CC=C1 MHDVGSVTJDSBDK-UHFFFAOYSA-N 0.000 claims description 8
- 239000011593 sulfur Substances 0.000 claims description 8
- 239000006227 byproduct Substances 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- QWDGPLAREJUSJA-UHFFFAOYSA-N octane-1-selenol Chemical compound CCCCCCCC[SeH] QWDGPLAREJUSJA-UHFFFAOYSA-N 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 125000003118 aryl group Chemical group 0.000 claims description 5
- ZTPZXOVJDMQVIK-UHFFFAOYSA-N dodecane-1-selenol Chemical compound CCCCCCCCCCCC[SeH] ZTPZXOVJDMQVIK-UHFFFAOYSA-N 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- ZAKSIRCIOXDVPT-UHFFFAOYSA-N trioctyl(selanylidene)-$l^{5}-phosphane Chemical compound CCCCCCCCP(=[Se])(CCCCCCCC)CCCCCCCC ZAKSIRCIOXDVPT-UHFFFAOYSA-N 0.000 claims description 4
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 3
- YJTKZCDBKVTVBY-UHFFFAOYSA-N 1,3-Diphenylbenzene Chemical group C1=CC=CC=C1C1=CC=CC(C=2C=CC=CC=2)=C1 YJTKZCDBKVTVBY-UHFFFAOYSA-N 0.000 claims description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- PIOZWDBMINZWGJ-UHFFFAOYSA-N trioctyl(sulfanylidene)-$l^{5}-phosphane Chemical compound CCCCCCCCP(=S)(CCCCCCCC)CCCCCCCC PIOZWDBMINZWGJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000013529 heat transfer fluid Substances 0.000 claims description 2
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- 239000003446 ligand Substances 0.000 description 11
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- IRPLSAGFWHCJIQ-UHFFFAOYSA-N selanylidenecopper Chemical compound [Se]=[Cu] IRPLSAGFWHCJIQ-UHFFFAOYSA-N 0.000 description 11
- 239000000758 substrate Substances 0.000 description 11
- 238000000137 annealing Methods 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000000151 deposition Methods 0.000 description 9
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- -1 copper chalcogenide compound Chemical class 0.000 description 7
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 6
- 150000004770 chalcogenides Chemical class 0.000 description 6
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 6
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- 239000006096 absorbing agent Substances 0.000 description 5
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- 239000011733 molybdenum Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 150000003958 selenols Chemical class 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000005486 sulfidation Methods 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- JAONJTDQXUSBGG-UHFFFAOYSA-N dialuminum;dizinc;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Zn+2].[Zn+2] JAONJTDQXUSBGG-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 4
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 4
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 235000012431 wafers Nutrition 0.000 description 4
- YHQGMYUVUMAZJR-UHFFFAOYSA-N α-terpinene Chemical compound CC(C)C1=CC=C(C)CC1 YHQGMYUVUMAZJR-UHFFFAOYSA-N 0.000 description 4
- 239000012530 fluid Substances 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical group [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- KWKAKUADMBZCLK-UHFFFAOYSA-N methyl heptene Natural products CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- WSTYNZDAOAEEKG-UHFFFAOYSA-N Mayol Natural products CC1=C(O)C(=O)C=C2C(CCC3(C4CC(C(CC4(CCC33C)C)=O)C)C)(C)C3=CC=C21 WSTYNZDAOAEEKG-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
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- 125000005595 acetylacetonate group Chemical group 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
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- 150000001649 bromium compounds Chemical class 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 2
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- 239000003795 chemical substances by application Substances 0.000 description 2
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- ZZEMEJKDTZOXOI-UHFFFAOYSA-N digallium;selenium(2-) Chemical compound [Ga+3].[Ga+3].[Se-2].[Se-2].[Se-2] ZZEMEJKDTZOXOI-UHFFFAOYSA-N 0.000 description 2
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
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- BYHQTRFJOGIQAO-GOSISDBHSA-N 3-(4-bromophenyl)-8-[(2R)-2-hydroxypropyl]-1-[(3-methoxyphenyl)methyl]-1,3,8-triazaspiro[4.5]decan-2-one Chemical compound C[C@H](CN1CCC2(CC1)CN(C(=O)N2CC3=CC(=CC=C3)OC)C4=CC=C(C=C4)Br)O BYHQTRFJOGIQAO-GOSISDBHSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 229910005543 GaSe Inorganic materials 0.000 description 1
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 1
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- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
- C01G15/006—Compounds containing, besides gallium, indium, or thallium, two or more other elements, with the exception of oxygen or hydrogen
-
- 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
- H01L31/0248—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 characterised by their semiconductor bodies
- H01L31/0256—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 characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0322—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIBIIICVI chalcopyrite compounds, e.g. Cu In Se2, Cu Ga Se2, Cu In Ga Se2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
-
- 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
- H01L31/0203—Containers; Encapsulations, e.g. encapsulation of photodiodes
-
- 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
- H01L31/02366—Special surface textures of the substrate or of a layer on the substrate, e.g. textured ITO/glass substrate or superstrate, textured polymer layer on glass substrate
-
- 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
- H01L31/0248—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 characterised by their semiconductor bodies
- H01L31/036—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 characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes
- H01L31/0392—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 characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate
- H01L31/03923—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 characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate including AIBIIICVI compound materials, e.g. CIS, CIGS
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- H—ELECTRICITY
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Description
本願は、2013年11月13日に出願された米国仮出願第61/904,780号の利益を主張する。
銅インジウムジセレニド(CulnSe2)は、その独特な構造的及び電気的特性から、薄膜PV用途の最も有望な候補の一つである。1.0eVのバンドギャップは、太陽スペクトルに良く合っている。CulnSe2太陽電池は、CulnS2のセレン化によって作られる。なぜならば、セレン化プロセス中、SeがSと置き換わって、この置換が、体積膨張を生じるからである。体積膨張は、空隙を減少させ、高質で高密度のCulnSe2吸収層を再現性良く与える(Q. Guo, G.M. Ford, H.W. Hillhouse and R. Agrawal, Nano Lett., 2009, 9, 3060)。SeがSと完全に置換すると仮定すると、その結果の格子体積膨張は約14.6%であり、この値は、黄銅鉱(正方晶系)CulnS2(a=5.52Å,c=11.12Å)及びCulnSe2(a=5.78Å,c=11.62Å)の格子定数に基づいて計算されている。このことは、CulnS2ナノ結晶膜は、セレンリッチな雰囲気中にて膜をアニールすることで、セレンを主とする材料に容易に変換できることを意味している。それ故に、CulnS2は、CulnSe2又はCuln(S,Se)2吸収層を作製する代替的な前駆体として有望である。
a)溶媒中のCu塩、In塩及び/又はGa塩を第1温度で加熱する(102)。
b)有機カルコゲン前駆体を添加する(104)。
c)反応溶液を第2温度に加熱して、第1時間間隔撹拌する(106)。
d)随意選択的に、反応溶液を第3温度に冷却して、第2時間間隔撹拌する(108)。
e)反応溶液を室温に冷却する(110)。
f)ナノ粒子を単離する(112)。
a)Cu塩、In塩及び/又はGa塩を溶媒中で混合する(202)。
b)有機カルコゲン前駆体を添加する(204)。
c)反応溶液を第1温度に加熱して、第1時間間隔撹拌し、揮発性副産物を蒸留除去する(206)。
d)反応溶液を第2温度に加熱して、第2時間間隔に亘って第2のカルコゲン前駆体を加える(208)。
e)第3時間間隔、第2温度にて反応溶液を撹拌する(210)。
f)反応溶液を第3温度に冷却し、第4時間間隔撹拌する(212)。
g)反応溶液を室温に冷却する(214)。
h)ナノ粒子を単離する(216)。
a)溶媒にナノ粒子を溶解/分散させて、インクAを作る(302)。
b)インクAを基板に堆積させて膜を作る(304)。
c)不活性雰囲気中でアニールする(306)。
d)アニールされた膜が所望の厚さに至るまで、工程b)及び工程c)を繰り返す(309)。
e)必要に応じて、アニール、焼結、セレン化、KCNエッチングのような更なる膜処理工程を実行する(308)。
f)n型半導体層を堆積させて、ジャンクションを形成する(310)。
g)真性の(intrinsic)ZnOを堆積させて、拡張欠乏層を形成する(312)。
h)窓層を堆積する(314)。
i)金属グリッドを堆積する(316)。
j)デバイスを封じ込める(318)。
ln(OAc)3(32.057g、120.0mmol)と、Cu(OAc)(19.157g、156.3mmol)と、240mLのベンジルエーテルとを、リービヒ冷却器及びコレクタが付いた1−Lの丸底フラスコにて混合した。混合物を90分間、100℃で脱ガスし、その後N2を充填した。脱ガスした1−オクタンチオール(192mL、1.10mol)を加えて、混合物を200℃に加熱し、2時間撹拌し、その後、160℃まで冷まして、約18時間撹拌した。混合物を室温に冷却した。
ln(OAc)3(3.995g、13.7mmol)と、Cu(OAc)(2.422g、19.8mmol)と、100mLのベンジルエーテルとを、リービヒ冷却器及びコレクタが付いた100mLの丸底フラスコにて混合し、N2でパージした。脱ガスした30mLのベンジルエーテルを加えて、その後、混合物を100℃に加熱した。脱ガスした1−オクタンチオール(24mL、138mmol)を加えて、混合物を200℃に加熱し、6時間撹拌し、室温まで冷ました。
リービヒ冷却器及びコレクタが付いた丸底フラスコにて、15mLの1−オクタデセンを、約110℃で45分間脱ガスし、N2下で室温まで冷却した。Cu(OAc)(0.79g、6.4mmol)と、ln(OAc)3(1.54g、5.3mmol)とを加えて、更に10分間、140℃で脱ガスした。混合物を室温まで冷却した。1−オクタンセレノール(12mL、68mmol)を加えて、溶液を加熱した。酢酸が120℃で蒸留し始めて、シリンジを用いてコレクタから除去した。溶液を135乃至145℃で30分間加熱して、酢酸の残留物を蒸留させて、その後、トリオクチルホスフィンセレニド(1.71M、8mL、14mmol)を、10分間にわたって加えた。溶液を、140℃で1時間撹拌した。溶液を90℃に冷却し、その後、4時間半アニールして、室温まで冷却した。
1−オクタンチオールでキャッピングされた銅リッチなCuInS2ナノ粒子(Cu:In=1:0.76)をトルエンに溶解させて、200mg/mLの溶液Bを作った。
1−オクタンチオールでキャッピングされた銅リッチなCuInS2ナノ粒子(Cu:In=1:0.85)をトルエンに溶解して、インクCを作った。
Claims (16)
- CuInwGaxSeySz(CIGS)ナノ粒子を調製する方法において、
銅塩、インジウム塩及びガリウム塩からなる群から選択された塩を溶媒中にて第1温度で混合して、反応溶液を作る工程と、
反応溶液に有機カルコゲン前駆体を加える工程と、
第1時間間隔撹拌する間に、反応溶液を第2温度に加熱する工程と、
反応溶液を第3温度に加熱して、第2時間間隔にわたって第2カルコゲン前駆体を加える工程と、
第3温度にて、反応溶液を第3時間間隔撹拌する工程と、
反応溶液を第4温度に冷却して、第4時間間隔撹拌する工程と、
反応溶液を室温に冷却する工程と、
反応溶液からナノ粒子を単離する工程と、
を含んでおり、
0≦w、x<1、w+x<1、y,z≧0、y+z≒2である、方法。 - In塩及びGa塩を合わせた全体に対するCu塩のモル比は、1:0.65乃至1:0.85である、請求項1に記載の方法。
- 銅塩、インジウム塩及びガリウム塩からなる群は、酢酸塩、アセチルアセトネート、塩化物、臭化物、及びヨウ化物を含む群から選択された塩を含む、請求項1に記載の方法。
- 溶媒は、非配位性溶媒である、請求項1に記載の方法。
- 非配位性溶媒は、1−オクタデセン、ベンジルエーテル、ジフェニルエーテル、及び、水素化テルフェニルを含む熱伝導流体からなる群から選択される、請求項4に記載の方法。
- 有機カルコゲン前駆体は、式R−X−Hであって、Rはアルキル基又はアリール基であり、Xは硫黄又はセレンである、請求項1に記載の方法。
- 有機カルコゲン前駆体の沸点は、250℃未満である、請求項1に記載の方法。
- 有機カルコゲン前駆体は、1−オクタンチオール、1−オクタンセレノール、及び1−ドデカンセレノールからなる群から選択される、請求項6に記載の方法。
- 第1時間間隔は、実質的に揮発性副産物を蒸留除去するのに十分なものである、請求項1に記載の方法。
- 第3温度は、120℃乃至160℃である、請求項1に記載の方法。
- 第2カルコゲン前駆体は、配位性溶媒に溶解した元素カルコゲンを含んでいる、請求項1に記載の方法。
- 配位性溶媒は、トリオクチルホスフィンスルフィド及びトリオクチルホスフィンセレニドからなる群から選択される、請求項11に記載の方法。
- 第3時間間隔は、30分乃至2時間である、請求項1に記載の方法。
- 第4温度は、80℃乃至120℃である、請求項1に記載の方法。
- 第4時間間隔は、3分乃至6時間である、請求項1に記載の方法。
- ナノ粒子を単離する工程は、少なくとも1つのその他の溶媒を加えることで、溶液からナノ粒子を沈殿させる工程を含む、請求項1に記載の方法。
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EP2240286A4 (en) | 2007-12-20 | 2014-05-21 | Cima Nano Tech Israel Ltd | TRANSPARENT LINE COATING WITH FILLER MATERIAL |
CN101299446A (zh) * | 2008-05-30 | 2008-11-05 | 南开大学 | 硒化物前驱薄膜与快速硒硫化热处理制备薄膜电池方法 |
US7922804B2 (en) * | 2009-03-25 | 2011-04-12 | Jenn Feng Industrial Co., Ltd. | Method for preparing sol-gel solution for CIGS solar cell |
US8308973B2 (en) * | 2009-07-27 | 2012-11-13 | Rohm And Haas Electronic Materials Llc | Dichalcogenide selenium ink and methods of making and using same |
US20130087745A1 (en) * | 2009-08-04 | 2013-04-11 | Precursor Energetics, Inc. | Soluble precursors and solution-based processes for photovoltaics |
WO2011045989A1 (ja) * | 2009-10-12 | 2011-04-21 | 学校法人龍谷大学 | 化合物半導体薄膜の製造方法、太陽電池および化合物半導体薄膜製造装置 |
JP2011129564A (ja) * | 2009-12-15 | 2011-06-30 | Fujifilm Corp | 光電変換半導体膜を形成する塗布膜及びその製造方法、光電変換半導体膜、光電変換素子、及び太陽電池 |
US8889469B2 (en) * | 2009-12-28 | 2014-11-18 | Aeris Capital Sustainable Ip Ltd. | Multi-nary group IB and VIA based semiconductor |
US20110294254A1 (en) | 2009-12-28 | 2011-12-01 | Jackrel David B | Low cost solar cells formed using a chalcogenization rate modifier |
JP2011165790A (ja) * | 2010-02-08 | 2011-08-25 | Fujifilm Corp | 太陽電池およびその製造方法 |
TWI396782B (zh) * | 2010-09-15 | 2013-05-21 | Nat Univ Tsing Hua | 一種製造顆粒狀多元奈米組合物之方法 |
EP2617064A4 (en) * | 2010-09-15 | 2014-07-09 | Precursor Energetics Inc | METHOD AND DEVICES FOR DEPOSITION FOR PHOTOVOLTAIC ELEMENTS |
JP2014502052A (ja) * | 2010-12-03 | 2014-01-23 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | 硫化/セレン化銅インジウムガリウムコーティングおよび膜を製造するためのインクおよび方法 |
CN102694057B (zh) * | 2011-03-22 | 2015-02-18 | 昆山恒辉新能源有限公司 | 非真空预定量涂布法制备cigs太阳能电池光吸收层的方法 |
JP2013070032A (ja) * | 2011-09-05 | 2013-04-18 | Fujifilm Corp | バッファ層の製造方法および光電変換素子の製造方法 |
WO2014135979A1 (en) | 2013-03-04 | 2014-09-12 | Nanoco Technologies, Ltd. | Copper-indium-gallium-chalcogenide nanoparticle precursors for thin-film solar cells |
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CN108840312A (zh) | 2018-11-20 |
TWI595680B (zh) | 2017-08-11 |
JP2017501952A (ja) | 2017-01-19 |
CN105899462B (zh) | 2018-06-22 |
WO2015071671A1 (en) | 2015-05-21 |
US20180248057A1 (en) | 2018-08-30 |
KR101815277B1 (ko) | 2018-01-05 |
CN105899462A (zh) | 2016-08-24 |
US20150136213A1 (en) | 2015-05-21 |
TW201733153A (zh) | 2017-09-16 |
TW201526277A (zh) | 2015-07-01 |
US9960298B2 (en) | 2018-05-01 |
HK1222836A1 (zh) | 2017-07-14 |
JP2019024106A (ja) | 2019-02-14 |
KR20160086915A (ko) | 2016-07-20 |
EP3068729A1 (en) | 2016-09-21 |
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