JP2016051757A - 増感色素染色法 - Google Patents
増感色素染色法 Download PDFInfo
- Publication number
- JP2016051757A JP2016051757A JP2014175200A JP2014175200A JP2016051757A JP 2016051757 A JP2016051757 A JP 2016051757A JP 2014175200 A JP2014175200 A JP 2014175200A JP 2014175200 A JP2014175200 A JP 2014175200A JP 2016051757 A JP2016051757 A JP 2016051757A
- Authority
- JP
- Japan
- Prior art keywords
- sensitizing dye
- amine
- semiconductor layer
- dye
- staining method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 230000001235 sensitizing effect Effects 0.000 title claims abstract description 68
- 238000007447 staining method Methods 0.000 title claims abstract description 22
- 239000004065 semiconductor Substances 0.000 claims abstract description 57
- 150000001412 amines Chemical class 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 10
- 150000003141 primary amines Chemical group 0.000 claims abstract description 7
- 150000003335 secondary amines Chemical class 0.000 claims abstract description 7
- 150000003512 tertiary amines Chemical class 0.000 claims abstract description 7
- 239000002798 polar solvent Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 18
- 238000004043 dyeing Methods 0.000 claims description 12
- 125000004432 carbon atom Chemical group C* 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 6
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 4
- 239000000975 dye Substances 0.000 description 90
- 239000010410 layer Substances 0.000 description 49
- 239000000243 solution Substances 0.000 description 26
- 239000010408 film Substances 0.000 description 18
- 150000002430 hydrocarbons Chemical group 0.000 description 14
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 11
- 229910044991 metal oxide Inorganic materials 0.000 description 10
- 150000004706 metal oxides Chemical class 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 7
- -1 nitrogen-containing heterocyclic compounds Chemical class 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 229920002799 BoPET Polymers 0.000 description 4
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 4
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 description 4
- 230000001976 improved effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 229920000768 polyamine Polymers 0.000 description 4
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 4
- 239000002344 surface layer Substances 0.000 description 4
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 3
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- RXYPXQSKLGGKOL-UHFFFAOYSA-N 1,4-dimethylpiperazine Chemical compound CN1CCN(C)CC1 RXYPXQSKLGGKOL-UHFFFAOYSA-N 0.000 description 2
- PAMIQIKDUOTOBW-UHFFFAOYSA-N 1-methylpiperidine Chemical compound CN1CCCCC1 PAMIQIKDUOTOBW-UHFFFAOYSA-N 0.000 description 2
- MXZROAOUCUVNHX-UHFFFAOYSA-N 2-Aminopropanol Chemical compound CCC(N)O MXZROAOUCUVNHX-UHFFFAOYSA-N 0.000 description 2
- FUIQBJHUESBZNU-UHFFFAOYSA-N 2-[(dimethylazaniumyl)methyl]phenolate Chemical compound CN(C)CC1=CC=CC=C1O FUIQBJHUESBZNU-UHFFFAOYSA-N 0.000 description 2
- JOMNTHCQHJPVAZ-UHFFFAOYSA-N 2-methylpiperazine Chemical compound CC1CNCCN1 JOMNTHCQHJPVAZ-UHFFFAOYSA-N 0.000 description 2
- UVLSCMIEPPWCHZ-UHFFFAOYSA-N 3-piperazin-1-ylpropan-1-amine Chemical compound NCCCN1CCNCC1 UVLSCMIEPPWCHZ-UHFFFAOYSA-N 0.000 description 2
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical class C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 description 2
- FKNQCJSGGFJEIZ-UHFFFAOYSA-N 4-methylpyridine Chemical compound CC1=CC=NC=C1 FKNQCJSGGFJEIZ-UHFFFAOYSA-N 0.000 description 2
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 description 2
- OJGMBLNIHDZDGS-UHFFFAOYSA-N N-Ethylaniline Chemical compound CCNC1=CC=CC=C1 OJGMBLNIHDZDGS-UHFFFAOYSA-N 0.000 description 2
- AFBPFSWMIHJQDM-UHFFFAOYSA-N N-methylaniline Chemical compound CNC1=CC=CC=C1 AFBPFSWMIHJQDM-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 description 2
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 2
- GGSUCNLOZRCGPQ-UHFFFAOYSA-N diethylaniline Chemical compound CCN(CC)C1=CC=CC=C1 GGSUCNLOZRCGPQ-UHFFFAOYSA-N 0.000 description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- RNVCVTLRINQCPJ-UHFFFAOYSA-N o-toluidine Chemical compound CC1=CC=CC=C1N RNVCVTLRINQCPJ-UHFFFAOYSA-N 0.000 description 2
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000010186 staining Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- SWZDQOUHBYYPJD-UHFFFAOYSA-N tridodecylamine Chemical compound CCCCCCCCCCCCN(CCCCCCCCCCCC)CCCCCCCCCCCC SWZDQOUHBYYPJD-UHFFFAOYSA-N 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
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- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
- FQUYSHZXSKYCSY-UHFFFAOYSA-N 1,4-diazepane Chemical compound C1CNCCNC1 FQUYSHZXSKYCSY-UHFFFAOYSA-N 0.000 description 1
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- PWGJDPKCLMLPJW-UHFFFAOYSA-N 1,8-diaminooctane Chemical compound NCCCCCCCCN PWGJDPKCLMLPJW-UHFFFAOYSA-N 0.000 description 1
- ZRMOLCPODIMNPJ-UHFFFAOYSA-N 1-[4-(2-hydroxypropyl)piperazin-1-yl]propan-2-ol Chemical compound CC(O)CN1CCN(CC(C)O)CC1 ZRMOLCPODIMNPJ-UHFFFAOYSA-N 0.000 description 1
- NPEIGRBGMUJNFE-UHFFFAOYSA-N 1-aminohexan-1-ol Chemical compound CCCCCC(N)O NPEIGRBGMUJNFE-UHFFFAOYSA-N 0.000 description 1
- WGAOZGUUHIBABN-UHFFFAOYSA-N 1-aminopentan-1-ol Chemical compound CCCCC(N)O WGAOZGUUHIBABN-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
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Abstract
【解決手段】[1]アミンと、少なくとも1つのカルボキシル基を有する増感色素と、溶媒とを含む色素溶液を、半導体層に接触させる工程を有する、増感色素染色法。[2]前記アミンが下記式(1)で表されるモノアミンである前記増感色素染色法。[3]前記アミンが1級アミン、2級アミン、又は3級アミンである前記増感色素染色法。[4]前記色素溶液における前記アミン濃度が0.004〜4Mである前記増感色素染色法。[5]前記溶媒が、極性溶媒である前記増感色素染色法。[6]前記半導体層が表面に形成された基材を前記色素溶液に浸漬する前記増感色素染色法。[7]前記基材がロールから巻き出された長尺の樹脂フィルムである前記増感色素染色法。
[化1]
【選択図】なし
Description
しかしながら、半導体層を色素溶液に浸漬して色素を吸着させる工程(吸着工程)に要する時間として、一般的に数時間〜数十時間を要することが、製造効率を高めるうえで障害になっている。
[2]前記アミンが下記式(1)で表されるモノアミンであることを特徴とする前記[1]に記載の増感色素染色法。
[3]前記アミンが1級アミン、2級アミン、又は3級アミンであることを特徴とする前記[1]に記載の増感色素染色法。
[4]前記色素溶液における前記アミン濃度が0.004〜4Mであることを特徴とする前記[1]〜[3]の何れか一項に記載の増感色素染色法。
[5]前記溶媒が、極性溶媒であることを特徴とする前記[1]〜[4]の何れか一項に記載の増感色素染色法。
[6]前記半導体層が表面に形成された基材を前記色素溶液に浸漬することを特徴とする前記[1]〜[5]の何れか一項に記載の増感色素染色法。
[7]前記基材がロールから巻き出された長尺の樹脂フィルムであることを特徴とする前記[1]〜[6]の何れか一項に記載の増感色素染色法。
《増感色素染色法》
本実施形態の増感色素染色法は、アミンと、少なくとも1つのカルボキシル基を有する増感色素と、溶媒とを含む色素溶液を、半導体層に接触させる工程を有する。
前記環を形成する方法として、例えばR2及びR3の2つが前記炭化水素基である場合、各炭化水素基から1つずつ水素原子を除いた基(2価の炭化水素基)の炭素原子同士が結合する方法が挙げられる。
前記1級アミンとして、例えば、エチルアミン、n−プロピルアミン、sec−プロピルアミン、n−ブチルアミン、sec−ブチルアミン、i−ブチルアミン、tert−ブチルアミン、ペンチルアミン、ヘキシルアミン、ヘプチルアミン、オクチルアミン、デシルアミン、ラウリルアミン、ミスチリルアミン、1,2−ジメチルヘキシルアミン、3−ペンチルアミン、2−エチルヘキシルアミン、アリルアミン、アミノエタノール、1−アミノプロパノール、2−アミノプロパノール、アミノブタノール、アミノペンタノール、アミノヘキサノール、3−エトキシプロピルアミン、3−プロポキシプロピルアミン、3−イソプロポキシプロピルアミン、3−ブトキシプロピルアミン、3−イソブトキシプロピルアミン、3−(2−エチルヘキシロキシ)プロピルアミン、アミノシクロペンタン、アミノシクロヘキサン、アミノノルボルネン、アミノメチルシクロヘキサン、アミノベンゼン、ベンジルアミン、フェネチルアミン、α−フェニルエチルアミン、ナフチルアミン、フルフリルアミン等の1級モノアミンが挙げられる。
前記2級アミンとして、例えば、ジエチルアミン、ジプロピルアミン、ジ−n−ブチルアミン、ジ−sec−ブチルアミン、ジイソブチルアミン、ジ−n−ペンチルアミン、ジ−3−ペンチルアミン、ジヘキシルアミン、ジオクチルアミン、ジ(2−エチルヘキシル)アミン、メチルヘキシルアミン、ジアリルアミン、ピロリジン、ピペリジン、2,4−、2,6−、3,5−ルペチジン、ジフェニルアミン、N−メチルアニリン、N−エチルアニリン、ジベンジルアミン、メチルベンジルアミン、ジナフチルアミン、ピロール、インドリン、インドール、モルホリン等の2級モノアミンが挙げられる。
前記3級アミンとして、例えば、トリメチルアミン、トリエチルアミン、トリ−n−プロピルアミン、トリ−iso−プロピルアミン、トリ−1,2−ジメチルプロピルアミン、トリ−3−メトキシプロピルアミン、トリ−n−ブチルアミン、トリ−iso−ブチルアミン、トリ−sec−ブチルアミン、トリ−ペンチルアミン、トリ−3−ペンチルアミン、トリ−n−ヘキシルアミン、トリ−n−オクチルアミン、トリ−2−エチルヘキシルアミン、トリ−ドデシルアミン、トリ−ラウリルアミン、ジシクロヘキシルエチルアミン、シクロヘキシルジエチルアミン、トリ−シクロヘキシルアミン、N,N−ジメチルヘキシルアミン、N−メチルジヘキシルアミン、N,N−ジメチルシクロヘキシルアミン、N−メチルジシクロヘキシルアミン、N、N−ジエチルエタノールアミン、N、N−ジメチルエタノールアミン、N−エチルジエタノールアミン、トリエタノールアミン、トリベンジルアミン、N,N−ジメチルベンジルアミン、ジエチルベンジルアミン、トリフェニルアミン、N,N−ジメチルアミノ−p−クレゾール、N,N−ジメチルアミノメチルフェノール、2−(N,N−ジメチルアミノメチル)フェノール、N,N−ジメチルアニリン、N,N−ジエチルアニリン、ピリジン、キノリン、N−メチルモルホリン、N−メチルピペリジン、2−(2−ジメチルアミノエトキシ)−4−メチル−1,3,2−ジオキサボルナン、2−、3−、4−ピコリン等の3級モノアミンが挙げられる。
上範囲の下限値以上であることにより、アミンを添加することによる半導体層中の増感色素の拡散性をより向上させることができる。上記範囲の上限値以下であることにより、アミンが色素吸着を阻害することを防止できる。
本実施形態の色素溶液を構成する溶媒は、増感色素及びアミンを溶解し、増感色素の半導体層に対する結合を完全に阻害する溶媒でなければ特に制限されず、極性溶媒であっても良いし、非極性溶媒であっても良いが、増感色素の半導体層に対する化学的結合を促進する観点から、極性溶媒であることが好ましい。
前記極性溶媒としては、例えば、ニトリル系溶媒、アルコール系溶媒、アミド系溶媒、スルホキシド系溶媒、ラクトン系溶媒等が挙げられる。
前記溶媒は1種単独で使用しても良いし、2種以上を併用した混合溶媒として使用しても良い。
本実施形態における増感色素の種類は特に制限されず、半導体層と化学的に結合し得るカルボキシル基(−COOH又は水素原子が解離した−COO−)を少なくとも1つ有する増感色素であることが好ましい。このような増感色素として、従来の増感色素が適用できる。
本実施形態における色素溶液中の増感色素の濃度は特に制限されず、従来と同様の濃度で構わない。
本実施形態における半導体層を構成する半導体材料は特に制限されないが、色素吸着が良好であり、色素を担持した光電極として良好に機能する観点から、例えば酸化物半導体が好ましい半導体材料として挙げられる。酸化物半導体層を構成する金属酸化物の種類は特に制限されず、従来の色素増感太陽電池分野で使用される金属酸化物が適用可能である。例えば、表面に水酸基(−OH)を有する酸化チタン、酸化亜鉛、チタン酸ストロンチウム、酸化第二錫などの金属酸化物粒子によって構成された酸化物半導体層が好適である。半導体層は多孔質であってもよいし、緻密膜であってもよいが、色素結合量を増加させる観点から、通常は多孔質であることが好ましい。
上記範囲の下限値以上であるとフィルム強度が優れ、上記範囲の上限値以下であると軽量性が優れる。なお、本発明においてフィルムとシートは同義であり、区別しない。
まず、FTO膜が表面に成膜されたガラス基板の上に、150℃の焼成によって9〜10μmの厚みを有する多孔質の酸化チタン薄膜が形成された光電極を準備した。光電極の作用面積は0.16cm2であった。粒径15〜20nmの酸化チタン粒子を使用した。
また、増感色素N719([RuL2(NCS)2]:2TBA L、すなわち2,2’-bipyridyl-4,4’-dicarboxylic acid TBA)を0.3mMの濃度でアセトニトリルとtert-ブタノールの体積比1:1の混合溶媒に溶解した溶液に、ピロールを0.1vol%(約14.4mM)の濃度で添加した色素溶液を準備した。
増感色素N719の0.3mM(アセトニトリルとtert-ブタノールの体積比1:1)溶液に、添加剤としてピロールを10vol%の濃度で添加した色素溶液を使用した以外は、実施例1と同様に酸化チタン膜の色素染色を行った。その結果、実施例1と同様に、4時間弱(3〜4時間)の浸漬で、酸化チタン膜の厚み方向の全体に亘って充分な量の色素が吸着及び結合したことが確認された。
増感色素N719の0.3mM(アセトニトリルとtert-ブタノールの体積比1:1)溶液に、アミンの添加剤を加えずに、そのまま色素溶液として使用した以外は、実施例1と同様に酸化チタン膜の色素染色を行った。その結果、実施例1,2と同等の充分な量の色素を吸着及び結合するためには、6〜7時間の浸漬処理を要した。
増感色素N719の0.3mM(アセトニトリルとtert-ブタノールの体積比1:1)溶液に、トリフェニルホスフィンを0.1wt%(約4mM)の濃度で添加した色素溶液を使用した以外は、実施例1と同様にチタニア膜の色素染色を行った。その結果、実施例1,2と同等の充分な量の色素を吸着及び結合するためには、7時間を超える浸漬処理を要した。
Claims (7)
- アミンと、少なくとも1つのカルボキシル基を有する増感色素と、溶媒とを含む色素溶液を、半導体層に接触させる工程を有する、増感色素染色法。
- 前記アミンが1級アミン、2級アミン、又は3級アミンであることを特徴とする請求項1に記載の増感色素染色法。
- 前記色素溶液における前記アミン濃度が0.004〜4Mであることを特徴とする請求項1〜3の何れか一項に記載の増感色素染色法。
- 前記溶媒が、極性溶媒であることを特徴とする請求項1〜4の何れか一項に記載の増感色素染色法。
- 前記半導体層が表面に形成された基材を前記色素溶液に浸漬することを特徴とする請求項1〜5の何れか一項に記載の増感色素染色法。
- 前記基材がロールから巻き出された長尺の樹脂フィルムであることを特徴とする請求項1〜6の何れか一項に記載の増感色素染色法。
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2001257013A (ja) * | 2000-03-13 | 2001-09-21 | Fuji Photo Film Co Ltd | 光電極の作成方法、光電極、光電変換素子および光電池 |
JP2010205582A (ja) * | 2009-03-04 | 2010-09-16 | Hitachi Zosen Corp | 光電変換素子用電極の製造方法 |
JP2013065434A (ja) * | 2011-09-16 | 2013-04-11 | Pgs Home Co Ltd | 色素増感型太陽電池用増感色素溶液及びそれを用いる負極の製造方法 |
WO2015178257A1 (ja) * | 2014-05-20 | 2015-11-26 | 株式会社Adeka | 担持方法、担持体及び光電変換素子 |
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Publication number | Priority date | Publication date | Assignee | Title |
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JP2001257013A (ja) * | 2000-03-13 | 2001-09-21 | Fuji Photo Film Co Ltd | 光電極の作成方法、光電極、光電変換素子および光電池 |
JP2010205582A (ja) * | 2009-03-04 | 2010-09-16 | Hitachi Zosen Corp | 光電変換素子用電極の製造方法 |
JP2013065434A (ja) * | 2011-09-16 | 2013-04-11 | Pgs Home Co Ltd | 色素増感型太陽電池用増感色素溶液及びそれを用いる負極の製造方法 |
WO2015178257A1 (ja) * | 2014-05-20 | 2015-11-26 | 株式会社Adeka | 担持方法、担持体及び光電変換素子 |
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