JPWO2012153806A1 - セラミックス繊維の製造方法及びセラミックス繊維製造用のセラミックス原料組成液 - Google Patents
セラミックス繊維の製造方法及びセラミックス繊維製造用のセラミックス原料組成液 Download PDFInfo
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Abstract
Description
該セラミックス原料組成液をエレクトロスピニング法で紡糸して、紡糸繊維を得る紡糸工程と、
該紡糸繊維を焼成することにより、セラミックス化させて、セラミックス繊維を得る焼成工程と、
を有することを特徴とするセラミック繊維の製造方法を提供するものである。
該セラミックス原料組成液をエレクトロスピニング法で紡糸して、紡糸繊維を得る紡糸工程と、
該紡糸繊維を焼成することにより、セラミックス化させて、セラミックス繊維を得る焼成工程と、
を有することを特徴とするセラミック繊維の製造方法である。
・水の接触角(測定値、ミリポア社製−Simpli labによる超純水):78.9±1.3°(±は標準偏差、測定数12)
・水の表面張力(化学便覧):72〜73mN/m
・酢酸の接触角(測定値、和光純薬工業社製、試薬特級):19.3±1.9°(±は標準偏差、測定数12)
・酢酸の表面張力(化学便覧):27.6mN/m
・ギ酸の接触角(測定値、和光純薬工業社製、試薬特級):36.5±2.1°(±は標準偏差、測定数4)
・ギ酸の表面張力(化学便覧):39.9mN/m
・N’−ジメチルホルムアミドの接触角(測定値、和光純薬工業社製、試薬特級):32.3±3.2°(±は標準偏差、測定数10)
・N’−ジメチルホルムアミドの表面張力(化学便覧):32.3mN/m
生理食塩水溶解率(%)={ろ液量(L)×(a1+a2+a3+a4)×100}/{溶解前の生体溶解性セラミックス繊維の量(mg)×(b1+b2+b3+b4)/100}
なお、生体溶解性セラミックス繊維ごとに、その生体溶解性セラミックス繊維に含有されている金属元素に着目して、生体溶解性セラミックス繊維中の各金属元素が、生理食塩水に溶出される割合を元素毎に求め、合計して、生理食塩水溶解率(%)を求める。
(セラミックス原料組成液の粘度)
粘弾性測定装置(AntonPaar社製 Physica MCR301)を用い、セラミックス原料組成液の液温を25℃に維持し、せん断速度10s−1の時のせん断粘度を測定し、その値を、セラミックス原料組成液の粘度とした。
(セラミックス原料組成液の接触角)
セラミックス原料組成液を25℃に維持し、25℃、相対湿度50%RHの雰囲気において、SUS430板上に1.6〜1.7μL滴下し、直読法によって接触角を評価した。なお、用いたSUS板に対する水(ミリポア社製−Simpli
labによる超純水)の接触角は78.9°であった。
<接触角測定用SUS430板>
・主要成分がFe:80〜84質量%、Cr:16〜18質量%の組成を有するステンレス鋼
・BA処理(Blight Anneal)したもの、久宝金属社製、H334
・表面粗さ:Ra=0.3〜0.6μm、レーザ顕微鏡(キーエンス社製、VK−9710)を用いて、倍率200倍の3次元のレーザ顕微鏡像を撮影し、装置付属の解析ソフトにより算出した算術平均表面粗さRa
(繊維の平均繊維径)
走査型電子顕微鏡(日本電子製JSM−7600F)で、倍率30000倍のSEM写真を撮影し、その倍率30000倍の視野から無作為に20箇所選定して繊維の幅を計測し、測定した繊維径を平均して、平均繊維径を求めた。
(ビーズ)
走査型電子顕微鏡(日本電子製 JSM−7600F)で、倍率2000倍のSEM写真を撮影し、その倍率2000倍の視野において、直径が平均繊維径に比較して3倍以上であり且つ1μm以上の球形のものをビーズとし、そのようなビーズの数を確認した。倍率2000倍の視野内に、確認されたビーズの数が1個以下の場合を「ビーズなし」と、2個以上の場合を「ビーズあり」と評価した。
(フシ状の塊)
走査型電子顕微鏡(日本電子製 JSM−7600F)で、倍率10000倍のSEM写真を撮影し、その倍率10000倍の視野において、径がその近傍の繊維径に比較して1.5倍を超えている箇所をフシ状の塊とし、そのようなフシ状の塊の数を確認した。倍率10000倍の視野内に、確認されたフシ状の塊の数が10個以下の場合を「フシなし」と、11個以上の場合を「フシあり」と評価した。
<セラミックス原料組成液の調製>
表1〜5に示す配合割合で、水に、各配合物を混合し、撹拌して、セラミックス原料組成液を調製した。
・Al原料:塩基性カルボン酸アルミニウム(Al(OH)X(RCOO)3−Xで表され、RCOOはギ酸、酢酸及び乳酸のうちから選ばれるカルボン酸であり、X=1.0〜2.5である。)、不揮発分含有量24.7質量%、酸化物換算の含有量10.5質量%、
・Ca原料:酢酸カルシウム、不揮発分含有量20.7質量%、酸化物換算含有量7.3質量%
・Si原料:コロイダルシリカ、不揮発分含有量20.9質量%、酸化物換算含有量19.6質量%
・繊維形成助剤:ポリアクリル酸エステル、不揮発分含有量15.0質量%
・界面活性剤:第1級アルコールエトキシレート、不揮発分含有量10.0質量%
次いで、得られたセラミックス原料組成液を、エレクトロスピニング法で紡糸して、紡糸繊維を得た。紡糸条件は、表1〜5に示す通りである。
次いで、得られた紡糸繊維を、表1〜5に示す焼成温度及び焼成時間にて、焼成した。
Claims (14)
- セラミックス繊維を構成する金属酸化物源となる金属元素と、繊維形成助剤と、界面活性剤と、を含有し、溶媒が水であり、該金属酸化物源の金属元素の含有量が金属酸化物換算で3.0〜9.0質量%であり、該金属元素を有する化合物、該繊維形成助剤及び該界面活性剤の不揮発分の合計含有量が10.0〜21.0質量%であり、該界面活性剤の含有量が0.05〜5.0質量%であるセラミックス原料組成液を調製するセラミックス原料組成液調製工程と、
該セラミックス原料組成液をエレクトロスピニング法で紡糸して、紡糸繊維を得る紡糸工程と、
該紡糸繊維を焼成することにより、セラミックス化させて、セラミックス繊維を得る焼成工程と、
を有することを特徴とするセラミック繊維の製造方法。 - 前記セラミックス原料組成液のSUS430板に対する接触角が、30〜54°であることを特徴とする請求項1記載のセラミックス繊維の製造方法。
- 前記セラミックス原料組成物のpHが2.0〜4.5であることを特徴とする請求項1又は2いずれか1項記載のセラミックス繊維の製造方法。
- 前記セラミックス原料組成液の粘度が0.1〜1.0Pa・sであることを特徴とする請求項1〜3いずれか1項記載のセラミック繊維の製造方法。
- 前記セラミックス原料組成液調製工程において、前記セラミックス原料組成液に、硝酸、蟻酸又は酢酸を添加することにより、pHを2.0〜4.5に調節することを特徴とする請求項1〜4いずれか1項記載のセラミックス繊維の製造方法。
- 前記繊維形成助剤が水溶性高分子であることを特徴とする請求項1〜5いずれか1項記載のセラミックス繊維の製造方法。
- 前記紡糸工程において、前記セラミックス原料組成液を紡糸するときの雰囲気の湿度が10〜50%RHであることを特徴とする請求項1〜6いずれか1項記載のセラミックス繊維の製造方法。
- 前記セラミックス原料組成液が、アルミニウム化合物と、カルシウム化合物と、珪素化合物と、を混合して得られたものであることを特徴とする請求項1〜7いずれか1項記載のセラミックス繊維の製造方法。
- 前記アルミニウム化合物が塩基性酸アルミニウムであり、前記カルシウム化合物が水溶性のカルシウム化合物であり、前記珪素化合物がコロイダルシリカであることを特徴とする請求項1〜8いずれか1項記載のセラミックス繊維の製造方法。
- セラミックス繊維を構成する金属酸化物源となる金属元素と、繊維形成助剤と、界面活性剤と、を含有し、溶媒が水であり、該金属酸化物源の金属元素の含有量が金属酸化物換算で3.0〜9.0質量%であり、該金属元素を有する化合物、該繊維形成助剤及び該界面活性剤の不揮発分の合計含有量が10.0〜21.0質量%であり、該界面活性剤の含有量が0.05〜5.0質量%であることを特徴とする請求項1記載のセラミックス繊維製造用のセラミックス原料組成液。
- 前記セラミックス原料組成液のSUS430に対する接触角が、30〜54°であることを特徴とする請求項10記載のセラミックス繊維製造用のセラミックス原料組成液。
- pHが2.0〜4.5であることを特徴とする請求項10又は11いずれか1項記載のセラミックス原料組成液。
- 粘度が0.1〜1.0Pa・sであることを特徴とする請求項10〜12いずれか1項記載のセラミックス原料組成液。
- 前記繊維形成助剤が水溶性高分子であることを特徴とする請求項10〜13いずれか1項記載のセラミックス原料組成液。
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