JP4824561B2 - 微孔性pvdfフィルムおよび製造方法 - Google Patents
微孔性pvdfフィルムおよび製造方法 Download PDFInfo
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- JP4824561B2 JP4824561B2 JP2006526064A JP2006526064A JP4824561B2 JP 4824561 B2 JP4824561 B2 JP 4824561B2 JP 2006526064 A JP2006526064 A JP 2006526064A JP 2006526064 A JP2006526064 A JP 2006526064A JP 4824561 B2 JP4824561 B2 JP 4824561B2
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- JP
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- Prior art keywords
- membrane
- polyvinylidene fluoride
- pvdf
- microporous
- copolymer
- 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.)
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Images
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Description
(1)全溶液含有量に対して、ポリマー成分を約10〜90質量部ならびに、希釈剤成分を約90〜10質量部で含む溶液を溶融ブレンドして形成し、前記希釈剤成分が、前記ポリマー成分の融解温度、または前記全溶液の液体−液体相分離温度より高い温度において前記ポリマー成分と混和性である、工程と、
(2)前記溶液を造形する工程と、
(3)(i)ポリマー成分を結晶化してポリマードメインの網目を形成するか、または(ii)液体−液体相分離してポリマーの少ない相の網目を形成するかのいずれかによって、造形された溶液を相分離して相分離された材料、すなわち、ポリマー領域を形成する工程と、
(4)前記材料領域に隣接した空気の領域を生じて多孔性物品を形成する工程。
PVDFポリマー
ハイラー(HYLAR)MP−20 1,1−ジフルオロエタンベースのポリマー、166〜170℃の溶融温度、1.57のメルトフローインデックス(ニュージャージー州、ソロフェアのソルベイ・ソレキス(Solvay Solexis,Thorofare、NJ))
ハイラーMP−32 1,1−ジフルオロエタンベースのポリマー、166〜170℃の溶融温度、0.13のメルトフローインデックス(ニュージャージー州、ソロフェアのソルベイ・ソレキス)
カイナー(Kynar)1000HD 1,1−ジフルオロエテンベースのポリマー、166〜170℃の溶融温度、1.86のメルトフローインデックス(ペンシルベニア州、フィラデルフィアのアトフィナ・ケミカルズ(Atofina Chemicals Philadelphia,PA))
ソルフ(SOLEF)1010 PVDFポリマー、170〜175℃の溶融温度、5.33のメルトフローインデックス(ニュージャージー州、ソロフェアのソルベイ・ソレキス)
ソルフ1012 PVDFポリマー、170〜175℃の溶融温度、1.3のメルトフローインデックス(ニュージャージー州、ソロフェアのソルベイ・ソレキス)
ソルフ1015 PVDFポリマー、170〜175℃の溶融温度、0.14のメルトフローインデックス(ニュージャージー州、ソロフェアのソルベイ・ソレキス)
トリアセチン(TRIACETIN) グリセリルトリアセテート(ニューヨーク州、ロチェスターのイーストマン・コダックカンパニー(Eastman Kodak Co.,Rochester,NY))
CI69800、ピグメントブルー60、インダンスロン、クロモフタルブルー(CHROMOPHTAL Blue)A3R(ニューヨーク州、ホーソーンのチバ・スペシャルティ・ケミカルズ(Ciba Specialty Chemicals、Hawthorne、NY))
CI71130、ピグメントレッド179、ペリレン、ぺリンド・マルーン(PERRINDO Maroon)R−6438(ペンシルベニア州、ピッツバーグのベイヤー・コーポレーション−コーティング・アンド・カラランツ)
METABLEN A−3000 ポリメチルメタクリレートでコーティングされたナノメートルサイズのPTFE粒子(ニューヨーク州、ニューヨークの三菱レイヨンコーポレーション)
ダイネオン(DYNEON)TF−5235 225nmのPTFE粒子の水性分散体(ミネソタ州、オークデールのダイネオン・コーポレーション(Dyneon Corp.,Oakdale,MN))
ナフィオン(NAFION)1000 そのスルホニル基をスルホン酸基に変換することによる、ペルフルオロスルホニルエトキシビニルエーテルによるポリテトラフルオロエチレンの加水分解コポリマーの溶液。溶液の組成:21.53%の固形分、21.33%の水、22.20%のエタノール、33.71%のプロパノールおよび1.23%他の組成物(デラウェア州、ウィルミントンのデュポン・ケミカルズ・カンパニー(DuPont Chemicals Company,Wilmington,DE))
引張強さ
インストロンモデル(INS(登録商標)TRON Model)1122引張試験機を用いて25cm/分のクロスヘッド速度および5cmのゲージ長で破断点引張強さをASTM D882によって測定した。試験片の幅は2.5cmであった。試料の破断点引張強さは、破断点における負荷(力)を試験片の元の断面積で割ることによって計算され、kg−力/cm2単位で記録される。破断点伸びのパーセントは、破断点伸びを元のゲージ長で割り、100で乗じることによって計算された。
ガーレイは、ASTM D726−58、方法Aに規定されているように、標準条件下でガスの所定の容積が膜の標準面積を通過するために必要な時間として表される、膜のガス流に対する耐性の尺度である。ガーレイは、空気、または別の特定の容積の50立方センチメートル(cc)が、水の124mmの圧力において膜の6.35cm2(1平方インチ)を通過するための秒単位の時間である。フィルム試料をシリンダーリングの間にクランプし、その最上部がピストンと空気の特定の容積とを含有し、解放時に、ピストンがその自重下で上シリンダー中の空気に圧力を加え、空気の特定の容積が膜を通過するためにかかった時間を測定した。約10秒/50ccより小さいガーレイ値を有する膜が複合イオン伝導性膜を製造するために好ましい。
泡立ち点の細孔寸法は、ASTM−F−316−80によるミクロン単位で測定された最大有効細孔寸法を表す泡立ち点の値である。
Hポンプ試験は、電流を印加し、膜電極接合体のアノード側で水素燃料をプロトンに分解させた。プロトンが膜を通過し、カソード側で再結合して水素−H2を製造した。水素を分離および再結合するこの水素間の反応は、診断のために用いられる。Hポンプは、水素イオンが膜を通ってz軸に(膜に垂直に)移動する時にそれらの抵抗を測定する。Hポンプ値を用いて膜抵抗を計算することが可能である。
H2クロスオーバーは、膜を通しての水素の拡散を測定する。H2クロスオーバーのより大きな値は概して、H2のより大きな拡散を示す。複合PVDF ICMは典型的に、通常の緻密なイオノマー膜に比べて水素の拡散が小さくなっている。H2クロスオーバーはまた、MEAに組み立てる前に膜にピンホールがあるかどうか調べるために用いられる。
0.8Vにおいての性能および0.6Vにおいての性能の値を用いて、70℃においてのMEAの電圧対電流プロットまたは分極曲線を得ることによってMEAの性能を評価する。これらの電池は、100%RH(相対湿度)の水素および100%RHの空気で実験された。触媒配合量は、アノードおよびカソードの両側で0.4mg/cm2であった。得られた分極曲線は、電池を流れる電流を電池の両端の電位差に関連づけた。
破壊強度試験は、膜の破壊ピーク負荷を測定する。特に、破壊強度試験を用いて、キャストナフィオン膜または複合PVDF/ナフィオン膜の破壊ピーク負荷を測定した。用いられた計測器は、10Nロードセルを有するインストロン(INS(登録商標)TRON)シリーズ5500Rであった。破壊先端は、0.0030インチ(0.0076cm)の先端直径を有する0.090インチ(0.23cm)のマンドレル上に取付けられた0.040インチ(0.10cm)の大きさのナジェット(NAJET)マンドレルマウントシリーズ#400−材料HSSC(品目0201)シャンクである。破壊強度は、公知の厚さのフィルムを破壊するために必要な平方センチメートル当たりの力を測定する。試料寸法は、1.5インチ(3.8cm)×1.5インチ(3.8cm)の正方形であった。クロスヘッド速度は2mm/分であった。
微孔性PVDFフィルムを以下に記載された方法を用いて図1に示された機器と同様な機器を用いて作製した。これらのフィルムの性質を以下の表1に示す。表1は、非核形成対照用PVDFフィルムに比べて核剤としてのCI69800ピグメントブルー60、CI71130ピグメントレッド179およびPTFEの有効性を示す。使用された核剤および量は、フィルム間で変えられ、溶融ブレンドの全重量によるパーセントとして表1に記載される。各フィルムの厚さを測定し、表1に示す。縦方向(MD)および横断方向(TD)の両方においてのフィルムの破断引張強さを測定した。核形成フィルムは、どんな測定可能な程度にも延伸することができない非核形成対照標準に比べてすぐれた破断強度および伸びを示した。
実施例10〜17および19の微孔性PVDFフィルムを実施例1〜7の場合と同様に作製した(すなわち試料を切り、15cm×28cmの大きさのフレーム内に置き、次いで20分間、脱イオン水の小皿内に置いた)。PVDF樹脂のタイプ、ポリマー対希釈剤の比、クロムロール温度(すなわち冷却速度)、ならびに延伸比および温度を変えて、以下の表2に示されるような広範囲の性質を生じさせる。P.B.60を溶融ブレンドの全重量による様々なパーセンテージで成核剤として用いた。実施例8〜12および14の予備洗浄トリアセチン含有量は50重量%であり、実施例13の予備洗浄トリアセチン含有量は55重量%であり、実施例15〜19の予備洗浄トリアセチン含有量は58重量%であった。クロムロールは、52℃から82℃まで変化された。クロムロールの後に、実施例8、9、および18の急冷された押出物を、周囲温度(22℃)に維持された水洗槽中に供給してグリセリルトリアセテート希釈剤を除去した。
PEMとして使用するための微孔性PVDFフィルムを実施例10〜17および19の場合と同様に作製したが、ただし、フィルムは、毎時9〜11.4キログラムの押出速度および216℃、271℃、221℃、188℃、188℃、188℃、および188℃のバレル温度プロフィールを用いて40mm同時回転二軸スクリュー押出機で製造された。150RPMのスクリュー速度を用いた。溶融ブレンドは、PVDFおよびグリセリルトリアセテート希釈剤を約45:55〜約40:60の範囲の比で含んだ。CI69800ピグメントブルー60を、溶融ブレンドの全重量によって約0.4パーセントの濃度において溶融ブレンドに添加した。溶融ブレンドを、冷却されたパターン化クロムロール上に、2度クロムめっきしたコートハンガースロットフィルムダイを通してポンプ輸送した。クロムロールは一連の交差ローレット線(25線/cm)で彫刻され、約140ミクロンの高さを有するロール面にわたって一連の隆起角錐構造をもたらした。クロムロール温度は、約35℃〜約74℃の範囲であった。フィルムは、希釈剤を除去するために洗浄されなかった。次に、フィルムを、実施例8〜9および18の場合と同様に延伸した。
微孔性PVDFフィルムを実施例8〜9の場合と同様にして作製し、それによって、クロムロールのすぐ後に水洗槽を用いてトリアセチン希釈剤を膜から洗い流した。微孔性PVDF膜は希釈剤の除去後に疎水性になり、膜細孔にイオン伝導溶液を充填してPEMとして使用するための膜を作製することを難しくした。膜の疎水性を減少させるために、約65:35〜75:25の範囲のn−プロパノールとグリセロールとの溶液を用いて、以下の手順を用いて膜を予備湿潤した。2つのガラスプレートを、イソプロパノールと水との50:50溶液で清浄にした。一片の微孔性フィルムを、清浄にされたプレートの1つにテープで付けた。次いで、プレートを両端を突き合わせて置き、次に、アプリケーターゲージを用いて、「ブランク」ガラスプレートをn−プロパノール/グリセロール溶液でコーティングし、フィルムを注意深く溶液中に置いた。ゴムローラーを用いて、大きいストロークを用いて過剰溶液をフィルムから押出した。第2のプレートを、清浄にされた/拭い取られたアプリケーターゲージを用いてナフィオン1000イオノマー溶液ですみやかにコーティングした。次いで、予備湿潤されたフィルムをイオノマー溶液中に置き、フィルムに気泡を閉じ込めるかまたは皺を形成するのを避けることを確実にした。次に、イオノマー溶液を10〜30秒間、膜を通して拡散させた。次いで、膜の上部を、アプリケーターゲージを用いて所望の厚さのイオノマー溶液でコーティングした。次いで、膜を10分間、90℃において乾燥させ、さらに10分間、160℃においてアニールした。引き続いて、得られたイオン伝導性膜(ICM)を、上述の試験方法によって試験のために膜電極接合体に組み立てた。ICMの多孔度および電気的性質を以下の表5および6に示す。
Claims (12)
- a)ポリフッ化ビニリデンまたはそのコポリマーと、
b)核剤を用いない結晶化に比べて多くの結晶化部位において前記ポリフッ化ビニリデンまたはそのコポリマーの結晶化を開始するために十分な量のナノメートル寸法の核剤と、
c)前記ポリフッ化ビニリデンまたはそのコポリマーが混和性である希釈剤であって、前記ポリフッ化ビニリデンまたはそのコポリマーが、前記ポリフッ化ビニリデンまたはそのコポリマーの融解温度以上の温度において溶解し、前記ポリフッ化ビニリデンまたはそのコポリマーの結晶化温度または相分離温度以下の温度に冷却した時に相分離する希釈剤と、を含み、
前記希釈剤がグリセリルトリアセテートであり、
微孔性であり、少なくとも1.1の延伸比において少なくとも1つの方向に延伸され、
前記核剤の十分な量が、ポリフッ化ビニリデンまたはそのコポリマーの0.2〜2.5質量パーセントである造形物品。 - 前記十分な量の核剤が、前記ポリフッ化ビニリデンまたはそのコポリマーと前記希釈剤との0.1質量パーセント〜1.0質量パーセントである、請求項1に記載の造形物品。
- 微小孔を有し、前記微小孔が、付加的な物質で部分的または完全に充填される、請求項1に記載の造形物品。
- イオン伝導性膜であって、
a)ポリフッ化ビニリデンまたはそのコポリマーと、
核剤を用いない結晶化に比べて多くの結晶化部位において前記ポリフッ化ビニリデンまたはそのコポリマーの結晶化を開始するために十分な量の核剤と、を含み、少なくとも1.1の延伸比において少なくとも1つの方向に延伸されて微小孔の網目を提供し、微小孔寸法が0.4ミクロンより大きく、1.5ミルより小さい厚さおよび10秒/50ccより小さいガーレイを有する、相互に連結した微小孔の形態の造形物品と、
b)前記造形物品の微小孔の少なくとも95体積%を充填して前記膜をイオン伝導性膜として機能させるために十分な量のイオノマー電解質と、
を含むイオン伝導性膜。 - 前記十分な量の核剤が、ポリフッ化ビニリデンまたはそのコポリマーの0.2質量パーセント〜2.5質量パーセントである、請求項4に記載のイオン伝導性膜。
- 前記ポリフッ化ビニリデンまたはそのコポリマーが半結晶質であり、0.13g/10分〜6.0g/10分のメルトフローインデックスを有する、請求項4に記載のイオン伝導性膜。
- 十分な量のイオノマー電解質が、前記膜の細孔容積の95〜100%を充填するために十分なイオノマー電解質の容積である、請求項4に記載のイオン伝導性膜。
- 前記イオノマー電解質がスルホン化フルオロポリマーイオノマーを含む、請求項4に記載のイオン伝導性膜。
- 前記核剤がナノメートル寸法の大きさである、請求項4に記載のイオン伝導性膜。
- 請求項4記載のイオン伝導性膜を含む膜電極接合体。
- 請求項10記載の膜電極接合体を含む電気化学デバイス。
- 請求項10記載の膜電極接合体を含む燃料電池。
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US7338692B2 (en) | 2008-03-04 |
JP2007505185A (ja) | 2007-03-08 |
CN1867622A (zh) | 2006-11-22 |
US8663868B2 (en) | 2014-03-04 |
KR20060122829A (ko) | 2006-11-30 |
US20050058821A1 (en) | 2005-03-17 |
ATE462748T1 (de) | 2010-04-15 |
US20080113242A1 (en) | 2008-05-15 |
CN1867622B (zh) | 2011-06-22 |
MXPA06002795A (es) | 2006-06-14 |
BRPI0414260A (pt) | 2006-11-07 |
EP1678245A1 (en) | 2006-07-12 |
DE602004026337D1 (de) | 2010-05-12 |
US20140134518A1 (en) | 2014-05-15 |
WO2005035641A1 (en) | 2005-04-21 |
US8962214B2 (en) | 2015-02-24 |
EP1678245B1 (en) | 2010-03-31 |
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