JP2020023417A - カーボン基材上に金属酸化物が固定化された複合体の製造方法 - Google Patents
カーボン基材上に金属酸化物が固定化された複合体の製造方法 Download PDFInfo
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- JP2020023417A JP2020023417A JP2018149279A JP2018149279A JP2020023417A JP 2020023417 A JP2020023417 A JP 2020023417A JP 2018149279 A JP2018149279 A JP 2018149279A JP 2018149279 A JP2018149279 A JP 2018149279A JP 2020023417 A JP2020023417 A JP 2020023417A
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- 150000007522 mineralic acids Chemical class 0.000 description 1
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- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 description 1
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- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
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- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
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- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910003447 praseodymium oxide Inorganic materials 0.000 description 1
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- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Inert Electrodes (AREA)
- Fuel Cell (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
Description
そこで本発明は、カーボン基材の焼損と有機化合物成分の残留を抑制しつつ、カーボン基材上に金属酸化物を良好に固定化して、カーボン基材上に金属酸化物が固定化された複合体を製造するための方法を提供することを目的とする。
以下、本発明を示す。
前記金属酸化物を構成する金属成分および有機キレート剤を含む金属キレート溶液をカーボン基材に塗布する工程、および、
前記金属キレート溶液を塗布した前記カーボン基材の金属キレート溶液塗布面を、熱流体に接触させて熱処理する工程を含むことを特徴とする方法。
工程1: 金属キレート溶液の調製工程
本工程では、目的の金属酸化物を構成する金属成分および有機キレート剤を含む金属キレート溶液を調製する。
本工程では、目的の金属酸化物を構成する金属成分および有機キレート剤を含む金属キレート溶液をカーボン基材に塗布する。
本工程では、金属キレート溶液を塗布したカーボン基材の金属キレート溶液塗布面を熱流体に接触させて熱処理して、金属キレート溶液に含まれる有機成分を分解除去しつつ、金属成分を酸化することにより、カーボン基材上に金属酸化物を固定化する。
1Lのビーカーにエチレンジアミン四酢酸98.4gと水を加えて総量を800gとした後、アンモニア水23.0gを加え、撹拌しながら酸化ランタン54.9gを加えた。次いで、混合物の温度を100℃に昇温して2時間撹拌することにより、酸化ランタンを完全に溶解させた。この溶液に水を加えてLa濃度を4.51質量%に調整し、無色透明のランタン−エチレンジアミン四酢酸(La−EDTA)錯体水溶液を得た。
別途、1Lのビーカーにエチレンジアミン四酢酸283.8gと水を加えて総量を800gとした後、アンモニア水66.1gを加え、撹拌しながら炭酸ストロンチウム143.6gをゆっくり加えた。次いで、混合物の温度を100℃に昇温して2時間撹拌することにより、炭酸ストロンチウムを完全に溶解させた。この溶液に水を加えてSr濃度を7.20質量%に調整し、無色透明のストロンチウム−エチレンジアミン四酢酸(Sr−EDTA)錯体水溶液を得た。
1Lのビーカーに、上記で得たLa−EDTA錯体水溶液194.2g(La含量:4.51質量%)、上記で得たSr−EDTA錯体水溶液230.0g(Sr含量:7.20質量%)、およびエチレンジアミン四酢酸鉄アンモニウム2水塩(EDTA・Fe・NH4・2H2O)72.2g(Fe含量:14.63質量%)を精秤して加えた後、水を加えて総量を600gとした。次いで30分間撹拌してEDTA・Fe・NH4・2H2Oを完全に溶解し、金属組成比がLa:Sr:Fe=1:3:3(モル比)である赤褐色透明の(La,Sr,Fe)−EDTA錯体水溶液を得た。
上記で得た(La,Sr,Fe)−EDTA錯体水溶液を、市販の霧吹きを用いてカーボンペーパー(「TGP−H−090」東レ社製,厚さ:280μm)の表面に対して10cm離れた位置より5回スプレー後、50℃で乾燥した。その後、下記に示す条件で酸水素炎を発生させ、カーボンペーパー上に酸水素炎を2往復させた。
溶射機: 粉末フレーム溶射ガン「6P−II」Sulzer Metco社製
水素流量: 32.5L/min
酸素流量: 43.0L/min
溶射機ノズル−基板間距離: 200mm
酸水素炎の移動速度: 50mm/s
上記実施例1において、(La,Sr,Fe)−EDTA錯体水溶液100gに、ノニオン系界面活性剤(「NUOSPERSE FN265」Elementis社製)0.1gを添加し、撹拌して完全溶解した水溶液を用いた以外は同様の方法により、カーボンペーパー上に金属酸化物を固定化した。
上記実施例1において、(La,Sr,Fe)−EDTA錯体水溶液をスプレーしたカーボンペーパーをマッフル炉(「KM−280」アドバンテック社製)中に挿入し、850℃で3時間焼成した。その結果、カーボンペーパーはひどく焼損し、基材としての役割を果たすことができないほど著しく強度が低下してしまったため、以降のXRD測定とSEM観察が不可能であった。
上記実施例1,2で得られたカーボン基材の表面をX線回折法で分析した。それぞれの結果を図1,2に示す。
図1,2に示される結果の通り、いずれもカーボン基材表面に、ランタン系ペロブスカイト酸化物であるLaSr3Fe3O9.9が存在していることが確認された。
上記実施例1,2で得られたカーボン基材の表面を、走査型電子顕微鏡(SEM)で観察した。結果を図3に示す。
図3に示される結果の通り、比較例1ではカーボンペーパーが焼損してしまったのに対して、実施例1,2では、カーボンペーパー上にLaSr3Fe3O9.9とみられる粒子が担持されており、特に実施例2のカーボンペーパー上にはより微細な粒子が担持されていた。また、実施例1,2共に、基材であるカーボンペーパーに焼損は見られなかった。
Claims (7)
- カーボン基材上に金属酸化物が固定化された複合体を製造するための方法であって、
前記金属酸化物を構成する金属成分および有機キレート剤を含む金属キレート溶液をカーボン基材に塗布する工程、および、
前記金属キレート溶液を塗布した前記カーボン基材の金属キレート溶液塗布面を、熱流体に接触させて熱処理する工程を含むことを特徴とする方法。 - 前記金属キレート溶液に、更に界面活性剤を配合する請求項1に記載の方法。
- 前記界面活性剤が非イオン界面活性剤である請求項2に記載の方法。
- 前記有機キレート剤がアミノカルボン酸系キレート剤である請求項1〜3のいずれかに記載の方法。
- 前記アミノカルボン酸系キレート剤が、エチレンジアミン四酢酸、ジエチレントリアミン五酢酸、トリエチレンテトラミン六酢酸、およびニトリロ三酢酸から必須的になる群より選択される少なくとも1種である請求項4に記載の方法。
- 前記カーボン基材が、カーボン板、カーボン膜、カーボンファイバー、カーボンペーパー、カーボンクロス、カーボン不織布、またはカーボン粉末である請求項1〜5のいずれかに記載の方法。
- 前記カーボン基材の素材が、黒鉛、活性炭、カーボンブラック、ダイヤモンドライクカーボン、グラッシーカーボン、カーボンナノチューブ、フラーレンのうち少なくとも1つである請求項1〜6のいずれかに記載の方法。
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