TW200831727A - Polycrystalline corundum fibers and production thereof - Google Patents

Polycrystalline corundum fibers and production thereof Download PDF

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TW200831727A
TW200831727A TW096128857A TW96128857A TW200831727A TW 200831727 A TW200831727 A TW 200831727A TW 096128857 A TW096128857 A TW 096128857A TW 96128857 A TW96128857 A TW 96128857A TW 200831727 A TW200831727 A TW 200831727A
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corundum
fibers
micrometers
periodic table
oxide
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Norbert Roesch
Bernd Clauss
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Clariant Int Ltd
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Description

200831727 九、發明說明 【發明所屬之技術領域】 本發明係有關一種新穎多晶剛玉纖維及其製法，該製 法利用經基氯化銘（aluminum chlorohydrate)作爲起始化合 物。 【先前技術】 陶瓷纖維的製造及運用在各種不同領域上已行之有年 。它們由於耐化學性、熱穩定性與卓越的機械性質而受到 注意。儘管短纖維在作爲代替石綿的高溫絕緣材料方面非 常重要，但現有的絲狀纖維係用來構成利基產品，其因爲 高成本而只能在特殊應用上限量使用。 以氧化鋁和氧化鋁/二氧化矽（富鋁紅柱石）爲主的陶瓷 纖維係應用在爐體建造、航太及汽車領域上，作爲絕緣材 這些氧化鋁纖維與富鋁紅柱石纖維係使用適當的金屬 氧化物前驅物作爲起始原料所製造者。通常使用二氧化矽 使結晶相穩定並抑制晶體生長（EP 0 3 1 8 203及EP 0 206 63 4)。能影響纖維中的晶體結構與晶體生長的其他混合物 如MgO與氧化鐵在EP 0 294 2 08中有相關敍述。 用來製造氧化鋁與富鋁紅柱石纖維的前驅物包括鋁鹽 ，例如羥基氯化鋁（EP 0 318 203)或甲酸鋁-乙酸鋁混合鹽 (EP 0 294 208)。相比之下，118 3 808 0 1 5係由氧化鋁粒子 (13至80%分率）與例如羥基氯化鋁之適當黏合劑的混合物 -4- 200831727 開始進行。us 3 808 015所使用的氧化銘粒子須具有 99.5%小於5 0111，98%小於3 0111及5〇%大於〇.2 0111的粒度 分布。 紡絲液流變學及可紡性通常藉由摻入水溶性聚合物， 舉例來說，例如聚環氧乙烷或聚乙烯醇來加以改善。 【發明內容】 φ 本發明因此提供一種基本上由剛玉及週期表第I或第 II主族元素的氧化物所組成的多晶剛玉纖維，其中該等剛 玉纖維之微晶具有下列粒度分布：〇至微米（34%)、 0.15至0·29微米（5 5%)及0.29至0.43微米（1 1%)。較佳的粒 . 度分布爲0至0·06微米（34%) ; 0.06至0.122微米（55%)及 0.122至0.3微米（11%)。由於具有這樣的粒度分布，因此 本發明之剛玉纖維明顯異於ΕΡ 294 208所述之剛玉纖維， 根據該專利所報告的數據，其剛玉纖維具有完全不同的粒 # 度分布以及顯著較大的粒徑。 本發明之剛玉纖維較佳而言包含0.01重量％至20重量 %之第I或第II主族的氧化物。這類氧化物特別是CaO和 MgO。 本發明另外還提供上述剛玉纖維之製法。該製法包含 使羥基氯化鋁水溶液與週期表第I和第II主族元素的氧 化物生成劑以及能促進α-氧化鋁生成的晶核混合，將此混 合物與水溶性聚合物混合，紡成纖維並且在高於nocrc的 溫度下煅燒這些纖維。 -5- 200831727 【實施方式】 所使用的羥基氯化鋁具有化學式Al2(0H)xcly’其中 X爲2.5至5.5，y爲3·5至0.5，X和y的和恆爲6。較佳而言 是由市售的50%水溶液開始進行。使這類溶液和晶核混合 以促進α型A1203生成。更具體而言，這類晶核能在後續 熱處理中降低該α型Al2〇3的生成溫度。可用晶核較佳而 φ 言包括極細粉狀的剛玉、水鋁石或赤鐵礦。特佳爲使用具 有平均粒徑小於0.1 μιη之極細粉狀的α-Αΐ203晶核。以生 成的氧化鋁爲基準，使用0.1重量％至1〇重量％的晶核通常 是足夠的。 . 此起始溶液進一步包含氧化物生成劑以生成週期表第 I和第II主族元素之氧化物MeO。可用的氧化物生成劑包 括特別是氯化物，尤其是元素Ca和Mg的氯化物，但除 此之外還包括其他可溶性或可分散鹽類，例如氧化物、氧 φ 氯化物（oxychlorides)、碳酸鹽或硫酸鹽。決定氧化物生 成劑的量，使最終纖維含有0.01重量％至20重量％的氧化 物MeO。第I和第II主族的氧化物可爲與氧化鋁呈分離 相的形式存在或與後者結合形成純粹的混合氧化物，例如 尖晶石等。本文中的術語「混合氧化物」應理解爲包括上 述兩種類型。 在羥基氯化鋁、第I和第II主族元素之氧化物生成 劑與晶核的含水混合物中，另外添加水溶性聚合物以針對 紡絲液可紡性調整流變學。可用聚合物包括聚乙烯醇、聚 -6 - 200831727 環氧乙烷、聚乙烯吡咯酮和其他水溶性有機聚合物’聚合 物含量可在10至4 0重量％的範圍內（以該混合物的氧化物含 量爲基準）。爲了增加固體含量，可方便地移除可紡紗之 紡絲液中的水分。此程序可以在大氣壓力或減壓下藉由加 熱完成。 本發明可紡紗之紡絲液係透過模頭吹襲紡絲或擠壓紡 絲，集合所得到的生纖維（green fibers)成爲短纖維。也可 φ 使用本發明可紡紗之紡絲液來製造長纖維’在這種情況下 ，係將纖絲取出並纏繞在筒管上。以此方式所得到的生纖 維在後續煅燒步驟中，係轉變成所要的剛玉纖維。由本發 " 明可紡紗之紡絲液開始進行，在高於11001：的溫度下生成 . α-氧化鋁。以此方式所得到的纖維是由達到至少80%的氧 化鋁所組成且是由達到至少70%的α-Α1203(剛玉）所組成。 剛玉微晶之平均直徑小於3 00 nm，而所有微晶的平均直徑 小於0.5 μπι。由於微晶的微小尺寸和均勻分布，因此本發 • 明之纖維在保留可撓性之餘，還能表現出高拉伸模數與極 佳的機械強度。 本發明之長纖維對於製造陶瓷纖維織物及作爲製造陶 瓷基質與金屬基質複合材料的起始原料特別有用。 實施例1 使5 0%羥基氯化鋁水溶液與足量的氯化鎂混合，以形 成氧化鋁和氧化鎂爲9 9 · 5 : 0 · 5重量％的煅燒後比率。此外 ’將極細剛玉懸浮液形式的2 %晶核（以氧化物含量爲基準） 200831727 加入該溶液中。該溶液藉由攪拌均勻化之後，添加聚乙烯 吡咯酮水溶液。在減壓下藉由蒸發除去水分而濃縮後，使 可紡紗的紡絲液透過多孔模頭進行乾式紡紗。將所得到的 生纖維逐漸加熱至11 oot。所形成的剛玉纖維顯示出剛玉 微晶在10至150 nm的範圍內（掃描電子顯微照片）。 X射線結構分析顯示主要爲α-氧化鋁的存在。
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Claims (1)

  1. 200831727 十、申請專利範圍 1 · 一種多晶剛玉纖維，其基本上由剛玉及週期表第I 或第Π主族元素的氧化物所組成，其中該等剛玉纖維之 微晶具有下列粒度分布：0至0.15微米（34%)、0.15至0.29 微米（55%)及 0.29至 0.43微米（11%)。 2 ·如申請專利範圍第1項之多晶剛玉纖維，其中該等 剛玉纖維之微晶具有下列粒度分布：〇至0.06微米（34%); • 0.06 至 0.122 微米（55%)及 0.122 至 0.3 微米（11%)。 3 .如申請專利範圍第1項之多晶剛玉纖維，其包含 0.01重量％至20重量％之週期表第I或第II主族的氧化物 〇 4. 一種製造申請專利範圍第1項之多晶剛玉纖維之方 法，其包含使經基氯化銘（aluminum chlorohydrate)水溶液 與晶核及週期表第I和第Π主族元素的氧化物生成劑混 合，添加水溶性聚合物，使其紡成纖維，及在高於11〇〇 °C φ 的溫度下煅燒該等纖維。 5. 如申請專利範圍第4項之方法，其中該氧化物生成 劑包含週期表第I或第π主族元素的氯化物。 6. 如申請專利範圍第4項之方法，其中該晶核包含極 細粉狀的剛玉、水鋁石或赤鐵礦。 7. 如申請專利範圍第4項之方法，其中以最終的剛玉 纖維爲基準，添加0.1重量％至10重量％之晶核。 200831727 明 說 單 無簡 :號 為符 圖件 表元 代之 定圖 :指表 圖案代 表本本 無 代} 定一二 指c C 八、本案若有化學式時，請揭示最能顯示發明特徵的化學 式：無
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KR20090082201A (ko) 2009-07-29
US20100009187A1 (en) 2010-01-14
DE102006045816A1 (de) 2008-04-03
CA2664745A1 (en) 2008-04-03
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CN101516803B (zh) 2012-09-26
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