JP2007302890A - アセタール化されたポリビニルアルコールを用いてのセラミック生フィルムの製造法 - Google Patents
アセタール化されたポリビニルアルコールを用いてのセラミック生フィルムの製造法 Download PDFInfo
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Abstract
【解決手段】セラミック生フィルムまたはセラミック成形体を製造するためのアセタール化されたポリビニルアルコールの使用の場合に、このアセタール化されたポリビニルアルコールが、8〜50質量%のポリビニルアセテート含量および100〜1200の重合度を有する。
【選択図】なし
Description
電子産業のためのセラミック材料は、しばしば所謂生フィルム、即ちセラミック材料を含有するフィルム状薄手の成形体を焼結することによって製造される。前記の生フィルムを製造するために、最初に金属酸化物と有機溶剤とからなる懸濁液が可塑剤および分散助剤の補助下に製造される。引続き、この懸濁液は、適当な方法(例えば、ドクターブレード法)で望ましい厚さで担体フィルム上に塗布され、溶剤が除去される。こうして得られた生フィルムは、亀裂なしでなければならず、平滑な表面を有していなければならず、なお或る程度の弾性を有していなければならない。
セラミック生フィルムを製造するための結合剤または分散剤としては、しばしば魚油、ポリアクリレートまたは一定のポリビニルアセタール、例えばポリビニルブチラールが使用される。こうして、ドイツ連邦共和国特許出願公開第4003198号明細書A1には、セラミック生フィルムのための注型材料の製造が記載されており、この場合結合剤としては、0〜2質量%の残留ポリビニルアセテート含量を有するポリビニルブチラールが使用される。同様に、ドイツ連邦共和国特許出願公開第3724108号明細書A1には、ポリビニルブチラールの使用が開示されており、この場合残留ポリビニルアセテート含量は、0.5〜3.0質量%である。
従って、本発明の課題は、高い分散作用を有し、同時に懸濁液の低い粘度の際に高い固体含量を保証する、セラミック生フィルムのための懸濁液を製造するための結合剤または分散剤を提供することであった。
従って、本発明の対象は、セラミック生フィルムまたはセラミック成形体を製造するためのアセタール化されたポリビニルアルコールの使用であり、この場合このアセタール化されたポリビニルアルコールは、8〜50質量%のポリビニルアセテート含量および100〜1200の重合度
を有する。
を有するアセタール化されたポリビニルアルコールが使用される。
有機溶剤中での無機材料(顔料)の懸濁、
分散剤の添加、
場合による:溶剤と分散剤とからなる混合物中での無機材料の懸濁、
懸濁液の均一化、
可塑剤の添加、
結合剤の添加、場合によっては分散剤と同一、
懸濁液の均一化。
測定法
a)ポリビニルアセテート含量の測定
ポリビニルアセテート含量は、物質1gの鹸化に必要とされる量の苛性カリ液の使用量からもたらされる、アセチル基の質量%での含量である。
試験すべき物質約2gを500mlの丸底フラスコ中に1mgで正確に計量供給し、エタノール90mlおよびベンジルアルコール10mlと一緒にして還流下に溶解する。冷却後に、この溶液をフェノールフタレインに対して0.01nのNaOHで中性に調節する。引続き、0.1nのKOH25.0mlを添加し、還流下に1.5時間加熱する。このフラスコを閉鎖して冷却し、アルカリ液の過剰量を指示薬としてのフェノールフタレインに対して0.1nの塩酸で不変に脱色するまで滴定する。同様に、空試験の試料を処理する。PV−アセテート含量は、次のように算出される:PV−アセテート含量[%]=(b−a)*86/E、但し、この場合、aは、mlでの試料に対する0.1nのKOHの使用量であり、bは、mlでの空試験のための0.1nのKOHの使用量であり、Eは、gでの試験すべき物質の乾式での計量供給量である。
ポリビニルアルコール基含量(ポリビニルアルコール含量)は、無水酢酸での事後のアセチル化によって検出することができるヒドロキシル基の含量である。
Mowital約1gを300mlの研磨されたアーレンマイヤーフラスコ(ground Erlenmeyer flask)中に1mgで正確に計量供給し、無水酢酸−ピリジン混合物10.0ml(23:77 V/V)を添加し、15〜20時間50℃に加熱する。冷却後、1,2−ジクロロエタン17mlを添加し、短時間回転振動させる。引続き、攪拌しながら水8mlを添加し、フラスコを栓で閉鎖し、10分間攪拌する。フラスコの頸および栓を脱塩水50mlで洗浄し、n−ブタノール5mlで被覆し、無水酢酸をフェノールフタレインに対して1nの苛性ソーダ液で滴定する。同様に、空試験の試料を処理する。ポリビニルアルコール含量は、次のように算出される:
ポリビニルアルコール含量[%]=(b−a)*440/E、但し、この場合、aは、mlでの試料に対する1nのNaOHの使用量であり、bは、mlでの空試験のための1nのNaOHの使用量であり、Eは、gでの試験すべき物質の乾式での計量供給量である。
使用されるポリビニルアセタールの粘度をDIN53015によりエタノール中の10%の溶液で20℃でヘプラー粘度計中で測定する。
1)約600の重合度を有するMowital B45H、
2)約800の重合度を有するMowital B60H、
3)約400の重合度を有するMowital B20H。
使用された結合剤:
約800の重合度、20.2質量%のポリビニルアルコール含量、16.1%のポリビニルアセテート含量および122.5mPasのDIN 53015による20℃でのエタノール中の10%の溶液のヘプラー粘度計中で測定された粘度を有するドイツ連邦共和国特許出願公開第19816722号明細書A1に記載のポリビニルブチラール。
使用された結合剤:
約1100の重合度、20.7質量%のポリビニルアルコール含量、16.2%のポリビニルアセテート含量および275mPasのDIN 53015による20℃でのエタノール中の10%の溶液のヘプラー粘度計中で測定された粘度を有するドイツ連邦共和国特許出願公開第19816722号明細書A1に記載のポリビニルブチラール。
使用された結合剤:
約350の重合度、19.6質量%のポリビニルアルコール含量、19.4%のポリビニルアセテート含量および20.8mPasのDIN 53015による20℃でのエタノール中の10%の溶液のヘプラー粘度計中で測定された粘度を有するドイツ連邦共和国特許出願公開第19816722号明細書A1に記載のポリビニルブチラール。
a)結合剤用液のレオロジー挙動
測定法:レオロジー特性の測定のために、それぞれのPVBから溶剤混合物エタノール/トルエン中の10質量%の溶液を製造し、タンブラーミキサー中で24時間均一化した。
測定法:PVB結合剤の分散作用を評価するために、種々のAl2O3懸濁液(エタノール40質量%/トルエン/Al2O360質量%)を準備した。この懸濁液に段階的にそのつどPVB結合剤または分散剤を添加し、数時間均一化した。フィルムの製造の場合、最初に分散剤(この場合PVB)を溶剤中に溶解し、次に粉末を添加した。それぞれの懸濁液を回転粘度計により特性決定した。この場合、懸濁液の粘度を100l/秒の剪断速度で比較値として採用した。
こうして得られた懸濁液(注型用スリップ)を脱ガスし、固定された二重チャンバー注型器具を備えた4mの長さのフィルム注型装置上にドクターブレード法により注型した。注型支持体としてシリコーン処理されたPETフィルム(厚さ100μm)を使用した。このフィルムを注型後に48時間空気で乾燥し(温度=22℃;空気湿分=65%)、引続き引き剥がした。
Claims (8)
- アセタール化されたポリビニルアルコールの使用において、アセタール化されたポリビニルアルコールが10〜35質量%のポリビニルアルコール含量を有することを特徴とする、アセタール化されたポリビニルアルコールの使用。
- アセタール化されたポリビニルアルコールが100〜1000の重合度を有する、請求項1または2記載のアセタール化されたポリビニルアルコールの使用。
- アセタール化されたポリビニルアルコールが2〜500mPasのDIN 53015により測定された粘度を有する、請求項1または2記載のアセタール化されたポリビニルアルコールの使用。
- ポリビニルアルコールのアセタール化のために、ホルムアルデヒド、アセトアルデヒド、プロパナール、ブタナール、イソブタナール、ペンタナール、ヘキサナール、ヘプタナール、オクタナール、ノナナール、イソノナナールまたはデカナールの群からの1つ以上のアルデヒドが使用される、請求項1から4までのいずれか1項に記載のアセタール化されたポリビニルアルコールの使用。
- アセタール化されたポリビニルアルコールとしてポリビニルブチラールが使用される、請求項1から5までのいずれか1項に記載のアセタール化されたポリビニルアルコールの使用。
- 懸濁液がアセタール化されたポリビニルアルコール0.1〜10質量%を含有する、請求項7記載のセラミック生フィルムまたはセラミック成形体を製造するための方法。
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EP06113753.5 | 2006-05-10 | ||
EP06113753A EP1854771A1 (de) | 2006-05-10 | 2006-05-10 | Verfahren zur Herstellung von keramischen Grünfolien mit acetalisierten Polyvinylalkoholen |
EP07106006A EP1854772B1 (de) | 2006-05-10 | 2007-04-12 | Verfahren zur Herstellung von keramischen Grünfolien mit acetalisierten Polyvinylalkoholen |
EP07106006.5 | 2007-04-12 |
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CN102361835B (zh) | 2009-03-31 | 2016-03-23 | 积水化学工业株式会社 | 浆料组合物的制造方法 |
US20130148263A1 (en) * | 2010-08-19 | 2013-06-13 | Kuraray Co., Ltd | Polyvinyl acetal resin, slurry composition prepared therefrom, ceramic green sheet, and multilayer ceramic capacitor |
CN103124766B (zh) | 2010-09-29 | 2015-09-16 | 积水化学工业株式会社 | 浆料组合物的制造方法 |
TWI557096B (zh) * | 2011-09-28 | 2016-11-11 | 可樂麗股份有限公司 | 漿料組成物、陶瓷坯片及積層陶瓷電容器 |
JP2019178389A (ja) * | 2018-03-30 | 2019-10-17 | 株式会社フジミインコーポレーテッド | 溶射用スラリー |
EP4183761A1 (en) * | 2021-11-18 | 2023-05-24 | Kuraray Europe GmbH | Use of compacted polyvinyl acetals as binder in ceramic green sheets |
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US7745534B2 (en) | 2010-06-29 |
EP1854772A1 (de) | 2007-11-14 |
US20070262496A1 (en) | 2007-11-15 |
EP1854772B1 (de) | 2013-03-27 |
TWI424977B (zh) | 2014-02-01 |
KR101385943B1 (ko) | 2014-04-16 |
TW200812933A (en) | 2008-03-16 |
JP5511127B2 (ja) | 2014-06-04 |
KR20070109908A (ko) | 2007-11-15 |
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