JP5309521B2 - 電極形成用組成物及びその製造方法並びに該組成物を用いた電極の形成方法 - Google Patents
電極形成用組成物及びその製造方法並びに該組成物を用いた電極の形成方法 Download PDFInfo
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- JP5309521B2 JP5309521B2 JP2007258311A JP2007258311A JP5309521B2 JP 5309521 B2 JP5309521 B2 JP 5309521B2 JP 2007258311 A JP2007258311 A JP 2007258311A JP 2007258311 A JP2007258311 A JP 2007258311A JP 5309521 B2 JP5309521 B2 JP 5309521B2
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- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 239000011702 manganese sulphate Chemical group 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- BHVPEUGTPDJECS-UHFFFAOYSA-L manganese(2+);diformate Chemical compound [Mn+2].[O-]C=O.[O-]C=O BHVPEUGTPDJECS-UHFFFAOYSA-L 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical group [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- TXCOQXKFOPSCPZ-UHFFFAOYSA-J molybdenum(4+);tetraacetate Chemical compound [Mo+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O TXCOQXKFOPSCPZ-UHFFFAOYSA-J 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N n-hexyl alcohol Natural products CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- FLESAADTDNKLFJ-UHFFFAOYSA-N nickel;pentane-2,4-dione Chemical compound [Ni].CC(=O)CC(C)=O FLESAADTDNKLFJ-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- WMHSAFDEIXKKMV-UHFFFAOYSA-N oxoantimony;oxotin Chemical compound [Sn]=O.[Sb]=O WMHSAFDEIXKKMV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- WATYAKBWIQTPDE-UHFFFAOYSA-N pentane-2,4-dione;zinc Chemical compound [Zn].CC(=O)CC(C)=O WATYAKBWIQTPDE-UHFFFAOYSA-N 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229940071575 silver citrate Drugs 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 125000003396 thiol group Chemical class [H]S* 0.000 description 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 description 1
- QUTYHQJYVDNJJA-UHFFFAOYSA-K trisilver;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Ag+].[Ag+].[Ag+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QUTYHQJYVDNJJA-UHFFFAOYSA-K 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- OYQCBJZGELKKPM-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O-2].[Zn+2].[O-2].[In+3] OYQCBJZGELKKPM-UHFFFAOYSA-N 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 description 1
Images
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- H01L31/04—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 adapted as photovoltaic [PV] conversion devices
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- H01L31/04—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 adapted as photovoltaic [PV] conversion devices
- H01L31/054—Optical elements directly associated or integrated with the PV cell, e.g. light-reflecting means or light-concentrating means
- H01L31/056—Optical elements directly associated or integrated with the PV cell, e.g. light-reflecting means or light-concentrating means the light-reflecting means being of the back surface reflector [BSR] type
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- 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
- Y02E10/548—Amorphous silicon PV cells
Description
目的に応じた表面形状を作成することが可能となる。添加物の添加割合は組成物に対して0.1〜20質量%の範囲内が好ましい。このうち、1〜5質量%の範囲内が特に好ましい。添加物の添加割合が下限値未満では粒成長の抑制効果が得られず、添加物の含有割合が上限値を越えると比抵抗の著しい上昇という不具合を生じる。なお、本発明でいう金属酸化物には、金属元素の酸化物だけでなく、半金属元素の酸化物をも含む。また、本発明でいう金属水酸化物には、金属元素の水酸化物だけでなく、半金属元素の水酸化物をも含む。同様に、本発明でいう有機金属化合物には、金属元素だけでなく半金属元素を構成要素として含む。
先ず硝酸銀を脱イオン水等の水に溶解して金属塩水溶液を調製する。一方、クエン酸ナトリウムを脱イオン水等の水に溶解させて得られた濃度10〜40%のクエン酸ナトリウム水溶液に、窒素ガス等の不活性ガスの気流中で粒状又は粉状の硫酸第一鉄を直接加えて溶解させ、クエン酸イオンと第一鉄イオンを3:2のモル比で含有する還元剤水溶液を調製する。次に上記不活性ガス気流中で上記還元剤水溶液を撹拌しながら、この還元剤水溶液に上記金属塩水溶液を滴下して混合する。ここで、金属塩水溶液の添加量は還元剤水溶液の量の1/10以下になるように、各溶液の濃度を調整することで、室温の金属塩水溶液を滴下しても反応温度が30〜60℃に保持されるようにすることが好ましい。また上記両水溶液の混合比は、金属塩水溶液中の金属イオンの総原子価数に対する、還元剤水溶液中のクエン酸イオンと第一鉄イオンのモル比がいずれも3倍モルとなるようにする。金属塩水溶液の滴下が終了した後、混合液の撹拌を更に10〜300分間続けて金属コロイドからなる分散液を調製する。この分散液を室温で放置し、沈降した金属ナノ粒子の凝集物をデカンテーションや遠心分離法等により分離した後、この分離物に脱イオン水等の水を加えて分散体とし、限外ろ過により脱塩処理し、更に引き続いてアルコール類で置換洗浄して、金属(銀)の含有量を2.5〜50質量%にする。その後、遠心分離機を用いこの遠心分離機の遠心力を調整して粗粒子を分離することにより、銀ナノ粒子が一次粒径10〜50nmの範囲内の銀ナノ粒子を数平均で70%以上含有するように調製する、即ち数平均で全ての銀ナノ粒子100%に対する一次粒径10〜50nmの範囲内の銀ナノ粒子の占める割合が70%以上になるように調整する。これにより銀ナノ粒子を化学修飾する保護剤の有機分子主鎖の炭素骨格の炭素数が3である分散体が得られる。
還元剤水溶液を調製するときに用いたクエン酸ナトリウムをりんご酸ナトリウムに替えること以外は上記(a)と同様にして分散体を調製する。これにより銀ナノ粒子を化学修飾する有機分子主鎖の炭素骨格の炭素数が2である分散体が得られる。
還元剤水溶液を調製するときに用いたクエン酸ナトリウムをグリコール酸ナトリウムに替えること以外は上記(a)と同様にして分散体を調製する。これにより銀ナノ粒子を化学修飾する有機分子主鎖の炭素骨格の炭素数が1である分散体が得られる。
銀ナノ粒子以外の金属ナノ粒子を構成する金属としては、金、白金、パラジウム、ルテニウム、ニッケル、銅、錫、インジウム、亜鉛、鉄、クロム及びマンガンが挙げられる。金属塩水溶液を調製するときに用いた硝酸銀を、塩化金酸、塩化白金酸、硝酸パラジウム、三塩化ルテニウム、塩化ニッケル、硝酸第一銅、二塩化錫、硝酸インジウム、塩化亜鉛、硫酸鉄、硫酸クロム又は硫酸マンガンに替えること以外は上記(a)と同様にして分散体を調製する。これにより銀ナノ粒子以外の金属ナノ粒子を化学修飾する保護剤の有機分子主鎖の炭素骨格の炭素数が3である分散体が得られる。
本発明の電極形成用組成物を用いて形成したサブストレート型太陽電池について説明する。
先ず、次の表1に示す金属ナノ粒子を形成する種類の金属塩を脱イオン水に溶解して金属塩水溶液を調製した。また、クエン酸ナトリウムを脱イオン水に溶解して濃度が26質量%のクエン酸ナトリウム水溶液を調製した。このクエン酸ナトリウム水溶液に、35℃に保持された窒素ガス気流中で粒状の硫酸第1鉄を直接加えて溶解させ、クエン酸イオンと第1鉄イオンを3:2のモル比で含有する還元剤水溶液を調製した。
実施例1〜12及び比較例1で得られた塗布試験用組成物を次の表1に示す基材上に102〜2×103nmの膜厚となるように様々な成膜方法で塗布した後に、次の表1に示す熱処理条件で焼成することにより、基材上に導電性塗膜を形成した。
先ず、次の表3〜表5に示す金属ナノ粒子を形成する種類の金属塩を脱イオン水に溶解して金属塩水溶液を調製した。また、クエン酸ナトリウムを脱イオン水に溶解して濃度が26質量%のクエン酸ナトリウム水溶液を調製した。このクエン酸ナトリウム水溶液に、35℃に保持された窒素ガス気流中で粒状の硫酸第1鉄を直接加えて溶解させ、クエン酸イオンと第1鉄イオンを3:2のモル比で含有する還元剤水溶液を調製した。
実施例13〜49及び比較例2〜5で得られた塗布試験用組成物を次の表3〜表5に示す基材上に102〜2×103nmの膜厚となるように様々な成膜方法で塗布した後に、次の表3〜表5に示す熱処理条件で焼成することにより、基材上に導電性塗膜を形成した。
11 基材
12 透明電極
12a テクスチャ構造
13 光電変換層
13a アモルファスSi
13b 微結晶Si
14 透明導電膜
15 裏面電極
20 サブストレート型太陽電池
21 基材
22 裏面電極
22a テクスチャ構造
23 光電変換層
23a アモルファスSi
23b 微結晶Si
24 透明電極
25 封止材
30 電子ペーパー
31 基材
32 透明導電膜
33 動作層
34 電極層
Claims (4)
- 金属ナノ粒子が分散媒に分散し、更にこの分散媒に有機高分子の添加物を添加混合することにより調製された電極形成用組成物であって、
前記金属ナノ粒子が銀ナノ粒子を含み、前記銀ナノ粒子が前記分散媒を除く前記組成物中に72〜99質量%含まれ、かつ
前記添加物がポリビニルピロリドン、ポリビニルピロリドンの共重合体、ポリビニルアルコール及びセルロースエーテルからなる群より選ばれた1種又は2種以上の有機高分子であり、
前記添加物である有機高分子の含有率が金属ナノ粒子の0.1〜20質量%である
ことを特徴とする電極形成用組成物。 - 請求項1記載の電極形成用組成物の製造方法であって、
硝酸銀を水に溶解して金属塩水溶液を調製する工程と、
濃度10〜40%のクエン酸ナトリウム、りんご酸ナトリウム又はグリコール酸ナトリウムの水溶液に不活性ガスの気流中で粒状又は粉状の硫酸第一鉄を加えて溶解させて還元剤水溶液を調製する工程と、
前記不活性ガス気流中で前記還元剤水溶液を撹拌しながら、前記還元剤水溶液の量の1/10以下の割合で反応温度が30〜60℃に保持されるように室温の前記金属塩水溶液を前記還元剤水溶液に滴下して混合する工程と、
前記混合液の撹拌を更に10〜300分間続けて銀コロイドからなる分散液を調製する工程と、
前記分散液にポリビニルピロリドン、ポリビニルピロリドンの共重合体、ポリビニルアルコール及びセルロースエーテルからなる群より選ばれた1種又は2種以上の有機高分子を添加する工程と
含むことを特徴とする電極形成用組成物の製造方法。 - 前記有機高分子の添加は、前記有機高分子の含有率が金属ナノ粒子の0.1〜20質量%の範囲内になるように調整して行う請求項2記載の電極形成用組成物の製造方法。
- 請求項1記載の電極形成用組成物或いは請求項2又は3に記載の方法により製造された電極形成用組成物を基材上に湿式塗工法で塗工して成膜する工程と、前記上面に成膜された基材を130〜400℃で焼成する工程とを含む電極の形成方法。
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KR20090063265A (ko) | 2009-06-17 |
US20100096002A1 (en) | 2010-04-22 |
JP2015117434A (ja) | 2015-06-25 |
DE112007002342T5 (de) | 2009-11-05 |
JP5673698B2 (ja) | 2015-02-18 |
TW200829610A (en) | 2008-07-16 |
KR101419079B1 (ko) | 2014-07-14 |
US8822814B2 (en) | 2014-09-02 |
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CN101523511A (zh) | 2009-09-02 |
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