CN101516803A - 多晶刚玉纤维及其制备方法 - Google Patents

多晶刚玉纤维及其制备方法 Download PDF

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CN101516803A
CN101516803A CNA2007800360683A CN200780036068A CN101516803A CN 101516803 A CN101516803 A CN 101516803A CN A2007800360683 A CNA2007800360683 A CN A2007800360683A CN 200780036068 A CN200780036068 A CN 200780036068A CN 101516803 A CN101516803 A CN 101516803A
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N·罗什
B·克劳斯
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Clariant Finance BVI Ltd
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Abstract

本发明要求保护基本上由刚玉和周期表第I或II主族元素的氧化物构成的多晶刚玉纤维，其中所述刚玉纤维的微晶具有以下粒子尺寸分布：0至0.15微米(34％)，0.15至0.29微米(55％)和0.29至0.43微米(11％)。以如下方式制备所述刚玉纤维：用晶核和周期表第I和II主族元素的氧化物形成剂掺混羟基氯化铝，添加水溶性聚合物，由其纺成纤维，并在高于1100℃的温度下煅烧所述纤维。

Description

多晶刚玉纤维及其制备方法
技术领域
本发明涉及新型多晶刚玉纤维和制备它们的方法，其中羟基氯化铝(Aluminiumchlorohydrat)用作起始化合物。
背景技术
陶瓷纤维多年以来已经被生产并用于不同领域。它们的特征在于高的耐化学品性、高的热稳定性和突出的机械性能。虽然短纤维已经作为石棉的替代品在高温绝缘材料中获得巨大的重要性，但可获得的长丝纤维为利基产品(Nischenprodukt)，其由于高价格仅在有限的范围内用于特种应用。
作为绝缘材料，基于氧化铝和氧化铝/二氧化硅(莫来石)的陶瓷纤维在窑炉构造、在航空和航天和在汽车领域得到应用。
在制备这些氧化铝纤维和莫来石纤维时，相应的金属氧化物的前体用作起始材料。为了稳定晶相并抑制晶体生长，经常使用二氧化硅(EP 0 318 203和EP 0 206 634)。用于影响纤维中晶体结构和晶体生长的其它添加剂，例如MgO和氧化铁，描述于EP 0 294 208中。
作为用于制备氧化铝纤维和莫来石纤维的前体，使用铝盐例如羟基氯化铝(EP 0 318 203)或甲酸-乙酸铝混合盐(EP 0 294 208)。相反，在US 3 808 015中从由氧化铝颗粒(13-80％比例)和合适的粘结剂，例如羟基氯化铝组成的混合物出发。根据US 3 808 015所使用的氧化铝颗粒应具有99.5％的小于5μm，98％的小于3μm和50％大于0.2μm的刚玉尺寸分布。
为了改进所述物料的流变性和可纺性，经常添加水溶性聚合物，例如聚氧化乙烯或聚乙烯醇。
发明内容
本发明提供基本上由刚玉和周期表第I或II主族元素的氧化物构成的多晶刚玉纤维，其中这些刚玉纤维的微晶具有以下粒子尺寸分布：0至0.15微米(34％)，0.15至0.29微米(55％)和0.29至0.43微米(11％)。优选的是0至0.06微米(34％)；0.06至0.122微米(55％)和0.122至0.3微米(11％)的粒子尺寸分布。采用所述粒子尺寸分布，根据本发明的刚玉纤维明显地区别于根据EP 294 208的刚玉纤维，其根据在该文献中的数据具有完全不同的粒子尺寸分布且具有明显更大的粒子尺寸。
本发明的刚玉纤维优选包含0.01至20重量％的第I或II主族的氧化物。这类氧化物尤其是CaO和MgO。
本发明进一步提供制备前述的刚玉纤维的方法。这种方法包括，将羟基氯化铝的水溶液与元素周期表第I和II主族元素的氧化物形成剂和促进α-氧化铝形成的晶核混合，将该混合物用水溶性聚合物掺混，纺成纤维，并在高于1100℃的温度下煅烧这些纤维。
对于所使用的羟基氯化铝适合的是通式Al2(OH)xCly，其中x为2.5至5.5的数，且y为3.5至0.5的数，且x和y的总和总是为6。在此，优选从50％的水溶液出发，如其可商购的那样。用促进Al2O3的α-变形形成的晶核掺混这样的溶液。尤其是这样的晶核引起在后续热处理中α-变形形成温度的降低。作为晶核优选考虑极细分的刚玉、水铝石或赤铁矿。特别优选使用平均粒子尺寸小于0.1μm的极细分的α-Al2O3晶核。一般基于形成的氧化铝，0.1至10重量％的晶核是足够的。
此外，该起始溶液还包含氧化物形成剂，以便产生周期表第I和II主族元素的氧化物MeO。为此尤其考虑氯化物，特别是元素Ca和Mg的氯化物，但是此外还有其它的可溶性或可分散性盐如氧化物、氯氧化物、碳酸盐或硫酸盐。氧化物形成剂的量这样测定，使得成品纤维包含0.01至20重量％的氧化物MeO。第I和II主族的氧化物可作为在氧化铝旁边的单独的相存在或与所述氧化铝一起形成真混合氧化物，例如尖晶石等。术语“混合氧化物”在本发明的范围内应这样理解，即其一并包括这两种类型。
还向由羟基氯化铝、第I和II主族元素的氧化物形成剂和晶核形成的含水混合物中添加水溶性聚合物，借助其调节流变性以实现物料的可纺性。作为聚合物考虑聚乙烯醇、聚氧化乙烯、聚乙烯吡咯烷酮及其它的水溶性有机聚合物，其中聚合物的含量可为10-40重量％(基于该混合物的氧化物含量计)。为了提高固体含量，还可能有利的是，从纺丝物料中除去水。这可通过在常压或在减压下加热来进行。
将本发明的纺丝物料经过喷嘴吹出或压出，其中收集以短纤维形式的所形成的生纤维(Grünfaser)。还可能的是，用本发明的纺丝物料生产长纤维，其中在这种情况下，将丝线拾取并卷绕到线轴上。将如此获得的生纤维在随后的煅烧步骤中转化成所期望的刚玉纤维。从本发明的纺丝物料出发，α-氧化铝的形成在超过1100℃的温度下进行。如此获得的纤维由至少80％的氧化铝和至少70％的α-Al2O3(刚玉)构成。刚玉微晶的平均直径低于300nm并且所有微晶的平均直径低于0.5μm。由于微晶的小尺寸和它们的均匀分布导致本发明的纤维在保持柔韧性的同时，显示高拉伸模量和非常好的机械强度。
本发明的长纤维尤其适合于生产陶瓷纤维织物和作为起始材料用于生产陶瓷基体复合材料和金属基体复合材料。
具体实施方式
实施例1
将羟基氯化铝的50％水溶液用这样多的氯化镁掺混，以致于在煅烧后氧化铝与氧化镁的比例为99.5∶0.5重量％。此外，向该溶液中添加2％以极细刚玉的悬浮液形式的晶核(基于氧化物含量)。在通过搅拌均化该溶液之后，添加聚乙烯吡咯烷酮的水溶液。在通过在减压下蒸去水而浓缩之后，将该纺丝物料通过多孔喷嘴以干纺法纺丝。将所获得的生纤维缓慢地加热直至1100℃。形成的刚玉纤维显示在10-150nm范围中(扫描电子显微镜(REM)照片)的刚玉微晶。
X-射线结构分析显示主要存在α-氧化铝。

Claims (7)

1.基本上由刚玉和周期表第I或II主族元素的氧化物构成的多晶刚玉纤维，其中所述刚玉纤维的微晶具有以下粒子尺寸分布：0至0.15微米(34％)，0.15至0.29微米(55％)和0.29至0.43微米(11％)。
2.根据权利要求1的多晶刚玉纤维，其中所述刚玉纤维的微晶具有以下粒子尺寸分布：0至0.06微米(34％)；0.06至0.122微米(55％)和0.122至0.3微米(11％)。
3.根据权利要求1的多晶刚玉纤维，其特征在于，所述刚玉纤维含有0.01至20重量％的周期表第I或II主族的氧化物。
4.制备权利要求1的多晶刚玉纤维的方法，其特征在于，将羟基氯化铝的水溶液用晶核和周期表第I和II主族元素的氧化物形成剂掺混，添加水溶性聚合物，由其纺成纤维并在高于1100℃的温度下煅烧所述纤维。
5.根据权利要求3的方法，其特征在于，作为氧化物形成剂添加周期表第I或II主族元素的氯化物。
6.根据权利要求3的方法，其特征在于，作为晶核添加极细分的刚玉、水铝石或赤铁矿。
7.根据权利要求3的方法，其特征在于，基于成品刚玉纤维，添加0.1至10重量％的晶核。
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