JP2016516256A - 燃料電池の電極のための酸化チタン・ナノ構造体 - Google Patents
燃料電池の電極のための酸化チタン・ナノ構造体 Download PDFInfo
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- JP2016516256A JP2016516256A JP2015558358A JP2015558358A JP2016516256A JP 2016516256 A JP2016516256 A JP 2016516256A JP 2015558358 A JP2015558358 A JP 2015558358A JP 2015558358 A JP2015558358 A JP 2015558358A JP 2016516256 A JP2016516256 A JP 2016516256A
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- nanostructure
- titanium oxide
- nanotubes
- structure according
- substrate
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 60
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000000446 fuel Substances 0.000 title claims description 20
- 239000002071 nanotube Substances 0.000 claims abstract description 73
- 239000012528 membrane Substances 0.000 claims abstract description 60
- 239000000758 substrate Substances 0.000 claims abstract description 33
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 31
- 239000002322 conducting polymer Substances 0.000 claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000003825 pressing Methods 0.000 claims abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 57
- 238000000034 method Methods 0.000 claims description 44
- 229910000510 noble metal Inorganic materials 0.000 claims description 31
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000010936 titanium Substances 0.000 claims description 22
- 229920006254 polymer film Polymers 0.000 claims description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 150000002500 ions Chemical class 0.000 claims description 15
- 229910052697 platinum Inorganic materials 0.000 claims description 14
- 229920000642 polymer Polymers 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- 239000000956 alloy Substances 0.000 claims description 11
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- 125000000542 sulfonic acid group Chemical group 0.000 claims description 7
- 125000000129 anionic group Chemical group 0.000 claims description 6
- RRZIJNVZMJUGTK-UHFFFAOYSA-N 1,1,2-trifluoro-2-(1,2,2-trifluoroethenoxy)ethene Chemical group FC(F)=C(F)OC(F)=C(F)F RRZIJNVZMJUGTK-UHFFFAOYSA-N 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 description 34
- 239000000463 material Substances 0.000 description 25
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- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229920003935 Flemion® Polymers 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910017855 NH 4 F Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000011865 Pt-based catalyst Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
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- 238000005234 chemical deposition Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
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- 230000009477 glass transition Effects 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
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- 239000001257 hydrogen Substances 0.000 description 2
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- 238000012545 processing Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 2
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
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- VEJOYRPGKZZTJW-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;platinum Chemical compound [Pt].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O VEJOYRPGKZZTJW-FDGPNNRMSA-N 0.000 description 1
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 1
- 125000005595 acetylacetonate group Chemical group 0.000 description 1
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- ATHGHQPFGPMSJY-UHFFFAOYSA-Q spermidine(3+) Chemical compound [NH3+]CCCC[NH2+]CCC[NH3+] ATHGHQPFGPMSJY-UHFFFAOYSA-Q 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8673—Electrically conductive fillers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C66/00—General aspects of processes or apparatus for joining preformed parts
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Abstract
Description
(1)支持された触媒(Pt/C)と、イオノマー(イオン伝導性ポリマー)と、適切な溶媒を混合することによってインクを調製する;
(2)膨張せず、ガラス転移温度がポリマー電解質膜よりも高い中間疎水性基材(例えばPTFEをベースとした膜)の上にそのインクを載せる;
(3)100℃未満の温度で乾燥させて溶媒を除去すると、触媒層がPTFE基材上に形成される;
(4)「転写」法:触媒層で被覆されたPTFE基材をポリマー電解質膜(例えばNafion(登録商標))にホット・プレスし;そのPTFE基材を剥がすと、触媒層がポリマー膜の上に移されて膜電極接合体(MEA)が形成される。
(a)インクに基づく製造法であるため、(最大数の「三相境界」部位を形成することによって)ミクロン/ナノレベルで構造を制御してPtの利用効率を最大にすることができない。この製造法を実施している間に、炭素粒子は凝集する可能性があり、イオノマーは細かく分散しない可能性があるため、イオノマーがPt粒子を完全に覆ってしまい、触媒反応のためにPt粒子に近づけなくなる可能性がある;
(b)炭素は一般に安定ではない。燃料電池を作動させている間に炭素が腐食し、Pt凝集体の表面積が減少する。安定性を大きくするには、炭素をグラファイト化することが可能だが、その場合には表面積が失われて性能が低下する;
(c)イオノマー自体がPtの溶解を促進する可能性があるため、性能が低下する。
(a)(二)酸化チタン・ナノ構造体を第1の基材上に設けること;
(b)第1の基材上に固定されたナノ構造体の基部から見てそのナノ構造体の他端にあるそのナノ構造体の頂部をイオン伝導性ポリマー膜に接触させること;
(c)ホット・プレスを利用してナノ構造体の頂部をポリマー膜の表面に圧入させること;
(d)ナノ構造体を第1の基材から剥がすこと
を含んでいる。
(a)粉砕;
(b)研磨;
(c)硝酸とフッ酸に基づく化学的エッチング溶液1(CES−1)。典型的な一実施態様では、CES−1は、5MのHNO3と40g/リットルのHFを含んでいて、そこに3分間完全に浸す。
(d)硫酸と過酸化水素に基づく化学的エッチング溶液2(CES−2)。典型的な一実施態様では、CES−2は、H2O+H2SO4(95%)+H2O2(30%)を1:2:2の体積比で含んでおり、そこに約15分間完全に浸す。
・陰極アーク堆積:ここでは、標的(供給)材料の位置で放電させる高電力電気アークにより、この材料の外面上で一部の材料を除去することで、高度にイオン化された蒸気を生み出し、あとでそれを被覆する基材の表面に堆積させる。
・電子ビーム物理気相蒸着。ここでは、堆積させる材料を高真空中の電子衝撃によって加熱して大きな蒸気圧にし、被覆する(より冷たい)表面へと拡散によって移動させ、凝縮により堆積させる。
・蒸着。ここでは、堆積させる材料を低真空中で電気抵抗加熱により加熱して大きな蒸気圧にする。
・パルス式レーザー堆積。ここでは、高電力レーザーが標的(供給材料)から材料を削って蒸気を生成させる。
・スパッタ堆積。ここでは、グロー・プラズマ放電(通常は磁石によって標的の周囲に局在する)が材料に衝突してその一部を蒸気として外部に飛散させ、その後それを被覆する表面に堆積させる。
本発明の実施形態としては下記の実施形態を挙げることができる:
〈実施形態1〉
プロトン伝導性ポリマーを含む膜層と接触している(二)酸化チタン・ナノ構造体含有層を備えている構造体。
〈実施形態2〉
前記(二)酸化チタン・ナノ構造体が、(二)酸化チタン・ナノチューブ(TNT)、(二)酸化チタン・ナノロッド、及び/又は(二)酸化チタン・ナノファイバーである、実施形態1に記載の構造体。
〈実施形態3〉
前記(二)酸化チタン・ナノ構造体含有層が、(二)酸化チタン・ナノチューブ(TNT)のアレイを含んでいて、前記膜層の平面に対するそのナノチューブの長手方向の平均仰角が少なくとも30°、好ましくは少なくとも70°であり、最も好ましくは、そのナノチューブが前記膜上で鉛直方向又は実質的に鉛直方向に揃っている(仰角が約90°)、実施形態1又は2に記載の構造体。
〈実施形態4〉
隣り合ったナノチューブの外面間で測定される平均距離が、50nm〜400nm、好ましくは60〜200nm、より好ましくは80〜150nmである、実施形態3に記載の構造体。
〈実施形態5〉
ナノチューブの平均内径が80nm〜400nmであり、ナノチューブの平均外径が100nm〜500nmである、実施形態3又は4に記載の構造体。
〈実施形態6〉
ナノチューブの平均長が2.0μm未満、好ましくは0.5μm〜1.5μmである、実施形態3〜5のいずれか一項に記載の構造体。
〈実施形態7〉
前記プロトン伝導性ポリマー膜が、一部又は全体がフッ素化された主鎖と、アニオン基を含んでいて一部又は全体がフッ素化された側鎖とを有する少なくとも1種類のポリマーを含む、実施形態1〜6のいずれか一項に記載の構造体。
〈実施形態8〉
前記プロトン伝導性ポリマー膜が、テトラフルオロエチレンに由来する単位と、末端にスルホン酸基を持つペルフルオロビニルエーテル基を含む、実施形態7に記載の構造体。
〈実施形態9〉
前記ポリマー膜が、10ミクロン(μm)〜200ミクロン(μm)、好ましくは少なくとも20μmかつ最大で50μmの厚みを持つ、実施形態1〜8のいずれか一項に記載の構造体。
〈実施形態10〉
前記(二)酸化チタン・ナノ構造体が、貴金属又は貴金属合金で覆われている、実施形態1〜9のいずれか一項に記載の構造体。
〈実施形態11〉
前記貴金属が白金である、実施形態10に記載の構造体。
〈実施形態12〉
(a)(二)酸化チタン・ナノ構造体を第1の基材上に設けること;
(b)第1の基材の表面に固定された前記ナノ構造体の基部から見てそのナノ構造体の他端にあるそのナノ構造体の頂部を、イオン伝導性ポリマー膜に接触させること;
(c)ホット・プレスを利用して、前記ナノ構造体の頂部をポリマー膜の表面に圧入させること;
(d)前記ナノ構造体を前記第1の基材から剥がすこと
を含む、実施形態1〜11のいずれか一項に記載の構造体を製造する方法。
〈実施形態13〉
前記ナノ構造体が(二)酸化チタン・ナノチューブ(TNT)であり、好ましくはそのTNTが前記第1の基材上で実質的に鉛直方向に揃っている、実施形態12に記載の方法。
〈実施形態14〉
前記第1の基材が、金属チタン/チタン・ホイルの基材である、実施形態12又は13に記載の方法。
〈実施形態15〉
工程(c)において、圧力が10バール〜200バールの範囲内であり、温度が50℃〜130℃の範囲内である、実施形態12〜14のいずれか一項に記載の方法。
〈実施形態16〉
前記(二)酸化チタン・ナノ構造体を前記イオン伝導性ポリマー膜と接触させる前、又は前記(二)酸化チタン・ナノ構造体を前記イオン伝導性ポリマー膜に移した後に、その(二)酸化チタン・ナノ構造体を貴金属又は貴金属合金で被覆する、実施形態12〜15のいずれか一項に記載の方法。
〈実施形態17〉
前記貴金属が白金である、実施形態16に記載の方法。
〈実施形態18〉
実施形態12〜17のいずれか一項に記載の方法によって得られる構造体。
〈実施形態19〉
実施形態1〜11のいずれか一項又は実施形態18に記載の構造体の燃料電池における利用。
Claims (19)
- プロトン伝導性ポリマーを含む膜層と接触している(二)酸化チタン・ナノ構造体含有層を備えている構造体。
- 前記(二)酸化チタン・ナノ構造体が、(二)酸化チタン・ナノチューブ(TNT)、(二)酸化チタン・ナノロッド、及び/又は(二)酸化チタン・ナノファイバーである、請求項1に記載の構造体。
- 前記(二)酸化チタン・ナノ構造体含有層が、(二)酸化チタン・ナノチューブ(TNT)のアレイを含んでいて、前記膜層の平面に対するそのナノチューブの長手方向の平均仰角が少なくとも30°、好ましくは少なくとも70°であり、最も好ましくは、そのナノチューブが前記膜上で鉛直方向又は実質的に鉛直方向に揃っている(仰角が約90°)、請求項1又は2に記載の構造体。
- 隣り合ったナノチューブの外面間で測定される平均距離が、50nm〜400nm、好ましくは60〜200nm、より好ましくは80〜150nmである、請求項3に記載の構造体。
- ナノチューブの平均内径が80nm〜400nmであり、ナノチューブの平均外径が100nm〜500nmである、請求項3又は4に記載の構造体。
- ナノチューブの平均長が2.0μm未満、好ましくは0.5μm〜1.5μmである、請求項3〜5のいずれか一項に記載の構造体。
- 前記プロトン伝導性ポリマー膜が、一部又は全体がフッ素化された主鎖と、アニオン基を含んでいて一部又は全体がフッ素化された側鎖とを有する少なくとも1種類のポリマーを含む、請求項1〜6のいずれか一項に記載の構造体。
- 前記プロトン伝導性ポリマー膜が、テトラフルオロエチレンに由来する単位と、末端にスルホン酸基を持つペルフルオロビニルエーテル基を含む、請求項7に記載の構造体。
- 前記ポリマー膜が、10ミクロン(μm)〜200ミクロン(μm)、好ましくは少なくとも20μmかつ最大で50μmの厚みを持つ、請求項1〜8のいずれか一項に記載の構造体。
- 前記(二)酸化チタン・ナノ構造体が、貴金属又は貴金属合金で覆われている、請求項1〜9のいずれか一項に記載の構造体。
- 前記貴金属が白金である、請求項10に記載の構造体。
- (a)(二)酸化チタン・ナノ構造体を第1の基材上に設けること;
(b)第1の基材の表面に固定された前記ナノ構造体の基部から見てそのナノ構造体の他端にあるそのナノ構造体の頂部を、イオン伝導性ポリマー膜に接触させること;
(c)ホット・プレスを利用して、前記ナノ構造体の頂部をポリマー膜の表面に圧入させること;
(d)前記ナノ構造体を前記第1の基材から剥がすこと
を含む、請求項1〜11のいずれか一項に記載の構造体を製造する方法。 - 前記ナノ構造体が(二)酸化チタン・ナノチューブ(TNT)であり、好ましくはそのTNTが前記第1の基材上で実質的に鉛直方向に揃っている、請求項12に記載の方法。
- 前記第1の基材が、金属チタン/チタン・ホイルの基材である、請求項12又は13に記載の方法。
- 工程(c)において、圧力が10バール〜200バールの範囲内であり、温度が50℃〜130℃の範囲内である、請求項12〜14のいずれか一項に記載の方法。
- 前記(二)酸化チタン・ナノ構造体を前記イオン伝導性ポリマー膜と接触させる前、又は前記(二)酸化チタン・ナノ構造体を前記イオン伝導性ポリマー膜に移した後に、その(二)酸化チタン・ナノ構造体を貴金属又は貴金属合金で被覆する、請求項12〜15のいずれか一項に記載の方法。
- 前記貴金属が白金である、請求項16に記載の方法。
- 請求項12〜17のいずれか一項に記載の方法によって得られる構造体。
- 請求項1〜11のいずれか一項又は請求項18に記載の構造体の燃料電池における利用。
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JP2018080069A (ja) * | 2016-11-14 | 2018-05-24 | ナミックス株式会社 | 金属被覆粒子及び樹脂組成物 |
CN109306551A (zh) * | 2018-07-18 | 2019-02-05 | 湘潭大学 | 一种硼掺杂二氧化钛纳米纤维及其制备方法和作为锂离子电池负极材料的应用 |
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CN105122523B (zh) | 2018-05-15 |
EP2962347B8 (en) | 2019-07-24 |
EP2962347B1 (en) | 2019-01-09 |
EP2962347A1 (en) | 2016-01-06 |
US20150364769A1 (en) | 2015-12-17 |
JP6162825B2 (ja) | 2017-07-12 |
US10090531B2 (en) | 2018-10-02 |
CN105122523A (zh) | 2015-12-02 |
WO2014131432A1 (en) | 2014-09-04 |
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