JP5410775B2 - イオン伝導膜の製造方法 - Google Patents
イオン伝導膜の製造方法 Download PDFInfo
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- JP5410775B2 JP5410775B2 JP2009032643A JP2009032643A JP5410775B2 JP 5410775 B2 JP5410775 B2 JP 5410775B2 JP 2009032643 A JP2009032643 A JP 2009032643A JP 2009032643 A JP2009032643 A JP 2009032643A JP 5410775 B2 JP5410775 B2 JP 5410775B2
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- organic
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- inorganic composite
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- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- IKNCGYCHMGNBCP-UHFFFAOYSA-N propan-1-olate Chemical compound CCC[O-] IKNCGYCHMGNBCP-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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
- 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
Landscapes
- Fuel Cell (AREA)
- Measuring Oxygen Concentration In Cells (AREA)
- Conductive Materials (AREA)
Description
Mr=(Mg/Ms)×100
Wr={Ws/(Ws+Wp)}×100
(1)金属化合物の重縮合による、「曳糸性を有する無機系ゾル溶液」の調製
テトラエトキシシラン(TEOS)、水、塩酸及びエタノールを、(TEOS:水:塩酸:エタノール=1:2:0.1:20)のモル比で混和した。より具体的には、TEOS1モル量に対して、10モル量のエタノールを混和し、攪拌させながら、その溶液中に、水2モル量、塩酸0.1モル量を含む10モル量のエタノール溶液をゆっくりと滴下しながら混和することで、出発原料とした。この出発原料は冷却水を循環させながら、設定温度60℃、攪拌条件300rpmで粘性が生じるまで攪拌し、無機系ゾル溶液を得た。
市販のナフィオン5質量%アルコール水混合溶媒溶液(Aldrich社製)と上記「曳糸性を有する無機系ゾル溶液」とを、無機系ゾル質量の混和割合が5質量%(ナフィオン:曳糸性を有する無機系ゾル=95質量%:5質量%)となるように調製し、攪拌条件300rpmで攪拌しながら混和し、混和溶液を得た。
前記混和溶液をキャスティングにより製膜し、これを60℃のオーブンに導き、5時間加熱処理を行った。その後、120℃のオーブンに導き、10分間加熱処理を行った。
出発原料に、TEOS、メルカプトプロピルトリエトキシシラン、PTES、水、塩酸及びエタノールを、(TEOS:メルカプトプロピルトリエトキシシラン:PTES:水:塩酸:エタノール=0.6:0.3:0.1:1.65:0.1:20)のモル比で混和したものを用いたこと、ならびに60℃のオーブンでの加熱時間を15時間としたこと以外は、実施例1と同様の処理を行い、厚さが20μmの薄膜状有機無機複合材料を得た。
溶媒が完全に除去された後の薄膜状有機無機複合材料の厚さが50μmとなるように、キャスティング工程を調整した以外は、実施例2と同様の処理を行い、酸化処理した薄膜状有機無機複合材料を得た。
ポリエーテルスルホン(住友化学製、スミカエクセル5200P)20gを140℃オーブンで乾燥させた後、95%硫酸200gに溶解させた。この溶液を300rpmで撹拌しながら、窒素気流下で、クロロスルホン酸93gを滴下した。反応温度30℃で5時間反応させた後、反応液を純水1Lに滴下し、析出物をろ過した。純水で洗浄後、乾燥を行い、スルホン化ポリエーテルスルホンを得た。
「曳糸性を有する無機系ゾル溶液」を用いず、市販のナフィオン5質量%アルコール水混合溶媒(Aldrich社製)のみを用いたこと以外は、実施例1と同様の処理を行い、溶媒を完全に除去した後の厚さが20μmの、薄膜状イオン伝導性樹脂膜を得た。
「曳糸性を有する無機系ゾル溶液」を用いず、市販のナフィオン5質量%アルコール水混合溶媒(Aldrich社製)のみを用いたこと以外は、実施例3と同様の処理を行い、溶媒を完全に除去した後の厚さが50μmの、薄膜状イオン伝導性樹脂膜を得た。
「曳糸性を有する無機系ゾル溶液」を用いず、市販のナフィオン5質量%アルコール水混合溶媒(Aldrich社製)のみを用いたこと以外は、実施例4と同様の処理を行い、溶媒を完全に除去した後の厚さが20μmの、薄膜状イオン伝導性樹脂膜を得た。
縦16cm、横11cm、深さ1.5cmの角型容器に、縦15cm、横10cmに裁断したポリアクリロニトリルからなるナノファイバー不織布(平均繊維径300nm、厚さ24μm、空隙率85%、強度2.3N/10mm)を入れ、その上側から市販のナフィオン5質量%アルコール水混合溶媒(Aldrich社製)を、20g加えた。前記不織布の空隙に溶媒が十分に浸透するように、減圧下で30分間浸漬した後、50℃のオーブン中で5時間静置した。その後、120℃のオーブンに導き、10分間加熱処理を行った。
出発原料にTEOS、水、アンモニア及びエタノールを、(TEOS:水:アンモニア:エタノール=1:2:0.0025:5)のモル比で混和したものを用いたこと以外は、実施例1と同様の処理を行い、溶媒を完全に除去した後の厚さが20μmの、薄膜状イオン伝導性樹脂膜を得た。
出発原料に、粒子径が12nmのコロイダルシリカを12質量%の濃度となるように調製した5質量%エタノール溶液を用いたこと以外は、実施例1と同様の処理を行い、溶媒を完全に除去した後の厚さが20μmの、薄膜状イオン伝導性樹脂膜を得た。
測定法:JIS B7502(1994)に規定されている外側マイクロメーター(0〜25mm)を用いて、JIS C2111 5.1(1)の測定法により、無作為に選んだ薄膜の10点の厚さを測定し、その算術平均値を膜厚とした。
たて50mm、よこ10mmに切断した長方形状の薄膜試料を採取し、この試料を、インストロン型引張試験機(装置名:テンシロンUCT500)を用いて、引張強さを測定した。つまり、前記引張試験機の20mm離れて位置するチャック間に長方形状の薄膜試料を固定し、20mm/分の定速で引張り、試料が破断に至るまでの最大張力(引張強さ)を測定した。
薄膜を蒸留水中に保管した状態から取り出し、直ぐに10%過酸化水素水、pH2.0の硫酸で洗浄した後、湿潤状態でイオン伝導度を測定した。より具体的には、太さ0.2mmの白金ワイヤーを5mm間隔で5本平行に張り、幅5mmに裁断した薄膜を、ワイヤーの張った方向と薄膜の長さ方向とが、直交するようにワイヤー上に載せ、抵抗を測定した。そして、薄膜の厚さ(t、単位:cm)、幅(w=0.5cm)、測定距離を横軸とし、抵抗を縦軸としてプロットしたグラフの傾き(s)から、以下の式に基づいてイオン伝導度(Ic、単位:S/cm)を算出した。
Ic=1/(s×w×t)=2/(s×t)
ガス拡散電極用基材:市販のカーボンペーパー(東レ(株)製、TGP−H−060)をガス拡散電極用基材とした。
Claims (4)
- (1)金属化合物を溶媒に溶解して溶液とし、重縮合することで、曳糸性を有する無機系ゾル溶液を形成する工程、(2)前記無機系ゾル溶液と、イオン伝導性樹脂を溶媒に溶解した溶液とを混和し、混和溶液を形成する工程、(3)前記混和溶液を成型してから溶媒を除く工程、を含むことを特徴とする有機無機複合膜の製造方法。
- 前記金属化合物が酸化によってスルフォン酸基に変換できる反応基を1つ以上有しており、かつ(3)溶媒を除く工程の後に、酸化処理を行い、前記反応基をスルフォン酸基に変換する工程を更に含む、請求項1に記載の有機無機複合膜の製造方法。
- 請求項1または2に記載の製造方法によって製造された有機無機複合膜。
- 燃料電池用のイオン伝導膜として使用する、請求項3に記載の有機無機複合膜。
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