CN1030566A - 非氧化物烧结的陶瓷纤维 - Google Patents

非氧化物烧结的陶瓷纤维 Download PDF

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CN1030566A
CN1030566A CN88104423A CN88104423A CN1030566A CN 1030566 A CN1030566 A CN 1030566A CN 88104423 A CN88104423 A CN 88104423A CN 88104423 A CN88104423 A CN 88104423A CN 1030566 A CN1030566 A CN 1030566A
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fiber
ceramic
monofilament
sintering
diameter
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弗朗西斯·J·弗雷谢特
沃尔夫纲·D·G·博卡
卡尔·休斯·麦克默特里
马丁·理查德·卡斯普里赛克
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Stemcor Corp
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Stemcor Corp
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Abstract

一种直径选择在1至200微米之间的高温多晶 陶瓷纤维，它在温度1700℃以上在一种惰性气氛中 是稳定的，在温度1500℃以上甚至在空气中通常也 是稳定的。该纤维包括最大粒径小于纤维直径，并且 平均粒径小于纤维直径0.2倍的一种烧结陶瓷粉 末。至少90％的陶瓷材料是选自硼化物，碳化物，氮 化物和硅化物。纤维的圆度大于1.15，并具有平滑 的表面。

Description

本发明涉及用于绝缘和增强目的的陶瓷纤维，更具体讲是涉及适用于这些用途的非氧化物纤维。
陶瓷纤维在现有技术中用于包括绝缘和一定范围的增强等多种用途中已有相当长久的时期。可考虑作为陶瓷纤维的例子是天然产出的石棉纤维，但由于有损健康现已不宜使用。另外，很长时间以来，氧化铝，氧化硅，铝硅酸盐纤维已被用于多种用途，包括用于增强、绝缘和作为填料。然而，这种含氧的纤维并不具备用于某些高性能用途所需要的特性。具体地说，这类氧化物型纤维常常达不到与用其增强的基质材料热膨胀系数尽可能相近的要求，和通常不具备在很高温度操作所希望有的耐热性能。另外，氧化物纤维的抗腐蚀性在某些环境中，例如在熔融金属中常常达不到要求。再者，在增强应用中，很多氧化物并不具有按增加劲度所希望高的弹性模量。可在美国专利（U.S.pat    4071594;4250    131;3808015和3992498中找到这种氧化物型纤维的例子。
在现有技术中的这类氧化物纤维一般通过对前体物质的熔融纺丝，或吹制或拉伸来制备，该前体物质中有时包括氧化物粉末，然后一般转化成氧化铝物质。这类方法，对于极高温度的非氧化物陶瓷来讲，一般并不适用。这类极高温度非氧化物陶瓷在可操作的温度并不熔融，而事实上在熔融前它们会分解或升华。曾经尝试通过某些前体的方法来制备非氧化物陶瓷纤维，例如在美国专利U.S.pat    3529044;4117057和4158687中所描述。然而，这类纤维并不如所希望的那样好，因为这类前体倾向在纤维中留下大量的物质，例如氧、常常会损害纤维的特性，通常会降低强度，耐温性能和抗化学侵蚀性能。
不过亦曾尝试将非氧化物陶瓷材料用于高温绝缘或高性能增强方面。这种增强材料的一个例子是碳化硅单晶纤维，有些人认为应列入纤维的总类别中。这种单晶纤维事实上被认为是一种单一的伸长晶体，而这种晶体即使用分批式方法也十分难制备，并且十分昂贵。另外，这类能够制备的单晶纤维的直径和长度都受很大限制。另外一些制备非氧化物陶瓷纤维的尝试通常并不很成功，因为一般有物料掺进纤维中，使纤维并不具有高性能特征。
因此需要一种最好能够连续制备成各种规格，包括横截面形状和长度具各种规格的高纯度高性能非氧化物陶瓷纤维。希望有这样一种纤维，该纤维在1700℃和更高的温度在一种惰性气体气氛中具有化学和物理稳定性，并且甚至在1500℃和更高的温度在空气中也是稳定的。
另外，现有技术制备的陶瓷纤维一般都难以处理，特别是希望利用这类纤维来生产纺织物时，尤其如此。因此希望有一种方法和一种产品，能够使准备研制的织造物含有非氧化物陶瓷纤维。
一种特别使人注意的现有技术专利是美国专利（U.S.pat    4559191），该专利描述了通过静水压将一种陶瓷粉末压制成一种纤维，以之作为一种中空聚合物纤维的核心。这种方法的缺点是明显的，即很难将粉末压进中心，且并水压加工设备及费用昂贵。另外，预期此纤维不能具备高的横截面纵横比以使得沿长轴方向达到改进的抗弯强度。再者，美国专利4559191号的纤维预期不具备平滑的表面，这种平滑表面对于减少缺陷是需要的。事实上，因为一般都知道各向等压烧结的制件比拉制或挤出烧结的制件具有较粗糙的表面。因此这里所说的“平滑”是指比用同一材料制成同一形状的各向等压制件的表面更为平滑。当这类平滑的制作足够大时，表面的特征一般是不会散射光线，因此能明亮的反射光线，即表面呈现光泽并且一般会反射影像。另一方面，一种烧结的各向等压制品的“粗糙”表面由于光散射的结果而倾向于是无光泽。然而，“平滑”并不意味着排除那些不是圆形或椭圆形的横截面。沿着纵向轴具有比较均匀横截面的表面能够从其表面反射光，例如星形横截面。
因此根据本发明，提供一种高温的，最好是多晶的，具有可选择直径在1至200微米之间的陶瓷纤维。这种纤维在温度约1700℃以上在一种惰性气体气氛中是稳定的，在温度1500℃以上甚至在空气中通常是稳定的。此纤维包括一种烧结的陶瓷粉末，该粉末的最大粒径小于纤维的直径，平均粒径小于纤维直径的0.2倍。此陶瓷粉末在温度约1700℃以上在一种惰性气体气氛中亦是稳定的。陶瓷中至少90%是选自硼化物，氮化物，碳化物和硅化物。这种纤维的特征是与通常由各向等压加工所得的粗糙表面相比具有平滑的表面。这种纤维最好具有高的横截面纵横比并且具有不圆度以在增强中提高劲度。此纤维亦因表面为锯齿形而具有能更好地粘结的优点。
这种纤维及其制备是特别意想不到的，因为在本发明以前未能预料到一种制品能具有如此的特性，以及这样小的横截面能从一种非常氧化物陶瓷粉末烧结而成。
本发明进一步包括一种可烧结的可纺织单丝，即可机械织造、可纺纱和可针织的单丝，包括含有高温可烧结陶瓷粉末颗粒的一种屈挠性聚合物基质。颗粒的平均粒径小于可烧结单丝的直径的0.15倍，最好是亚微米细粒。这种陶瓷粉末颗粒选自适于制陶瓷的硼化物，氮化物，碳化物，碳化物和硅化物。单丝的直径为2至300微米。本发明亦包括如前所描述通过可烧结的可纺织单丝的烧结来制备高温陶瓷纤维的方法，并且包括含有这种单丝的复合物。
图1-6为根据本发明制备的纤维的显微照片。
前面已讨论过，现已意外地发现可从未经涂覆的非氧化物陶瓷粉末烧结成直径为1至200微米之间的非氧化物陶瓷纤维。这纤维通常包括另一种元素的硼化物，碳化物，氮化物或硅化物，即当这种化合物是硅化合物时这种另一种元素不是硅，当化合物是硼化物时这种另一种元素不是硼，这些另一种元素选自铝、硼、铬、铪、钼、铌、硅、钽、钛、钨、钒和锆。
合适的陶瓷粉末，例如可以选自B4C、HfC、NbC、SiC、TaC、VC、WC、ZrC、CrB2、HfB2、NbB2、TaB2、TiB2，VB、WB、ZrB2、AlN、HfN、NbN、Si3N4、TaN、TiN、VN、ZrN、Mo5Si3、MoSi2和ZrSi以及它们的混合物等陶瓷物料粉末。
根据本发明特别希望使用的陶瓷是二硼化钛（TiB2），碳化硅（SiC）和碳化硼（B4C）。已经发现根据本发明的要求这些物质加进小量的烧结助剂是可以烧结的，并且所有这些物质在超过2200℃温度是稳定的。因此根据本发明的纤维可以主要由非氧化物陶瓷材料所组成，即几乎总是含有大于90%和最好大于95%的非氧化物。因此本发明氧化物的特性并不因氧化物相的操作而受到重大的影响，而现有技术中通过其它方法，例如使用前体制备的非氧化物陶瓷纤维就不能免受影响。
烧结的方法除存在屈挠性聚合物基质以外，与美国专利U.S.pat4123286中所示描述的方法类似。聚合物基质可以包括任何合适的聚合物，包括酚醛，聚烯烃，包括聚氯乙烯在内的聚囟代烯或不含在高温会使陶瓷材料分解的原子的其它聚合物。树脂本身必须能在烧结温度或低于烧结温度分解形成挥发性产物或在一些情况下生成有助烧结过程的少量残余碳。特别理想的聚烯烃是聚乙烯和聚丙烯。包括在形成该可纺织纤维组合物中的烧结助剂是那些为本专业人士所熟悉的烧结助剂。这类烧结助剂中不包括碳（因为碳通常至少可以部分地通过在体系中的聚合物和其它有机化合物来提供，有时至少亦可由亚微米的碳粉来提供，而是那些为本专业人士所熟悉的专用于涂层的烧结助剂。当陶瓷粉末是碳化硅的时候，一种特别理想的烧结助剂是碳化硼，其用量通常为碳化硅用量的0.2-1%（重量）。
颗粒的平均粒径小于可烧结的可纺织单丝直径的0.15倍，并且最好是亚微米。当可烧结单丝进行实际烧结时，丝的直径通常变得更小些，即体积缩小40至60%，在这种情况下粉末起始的平均粒径通常小于成品烧结丝直径的0.2倍。
可烧结的单丝和生成它的组合物最好含约75至约95%（重量）的陶瓷粉末和约5至约25%（重量）包括该聚合物的有机复合物。形成可烧结丝的组合物的有机部分不仅包括聚合物而且包括所需要的任何其它有机物质，这些物质包括如油酸、凡士林等润滑剂，如邻苯二甲酸二辛酯等表面活性剂、油类、如玉米油、作为一种聚合物溶剂的二甲基甲酰胺，和作为一种分散助剂的酞酸四乙基己酯。如上所述的关于该单丝的组合物并不包括用于体系中以制成烧结单丝的稀释剂。这类稀释可以包括若干有机化合物，如乙醇、丙酮、油类和挥发性烃类如甲苯和己烷。
可烧结单丝可经熔融纺丝或悬浮液纺丝法制备，接着在下面将要描述。
在熔融纺丝中，将碳化硅，烧结助剂和包括聚合物、增塑剂和分散剂等有机化合物熔融和混合。将混合的组份制成所需的颗粒，并将颗粒经挤出进行熔融丝纺。收集所得的可烧结的长单丝。
在悬浮液纺丝的情况中，将碳化硅粉末和烧结助剂研磨或用足够的稀释剂使其和有机成份混合以形成一种悬浮液。将所得的悬浮液纺丝并干燥。然后将所得的纤维烧结。可烧结的单丝亦可通过吹制或离心纺丝制成随机粗细的产物。在此情况中，可用与悬浮液纺丝相似的方法将各种成份混合在一起，不同的只是将所得的混合物利用一种装置将其吹制成单丝或用一种离心纺丝机纺丝。
本发明的可烧结单丝一般是可纺织的，并且可以制成织造的或者毡织产品或可用来制成较粗的纱线。该种单丝可以在其加工前烧结，也可以在制成其它产品之后烧结。陶瓷粉末的烧结温度根据体系的情况一般在1700和3000℃之间，并且当陶瓷物质是碳化硅时，烧结温度更具体规定要在2000和约2300℃之间。烧结时间通常在0.2至90分钟，最好为0.5至20分钟。烧结得到的产品可以任选用石墨或其它润滑剂涂布以便于处理。在适当控制条件情况下，所得的烧结单丝的拉伸强度超过100，000（psi）（689MPa），最好的超过175，000psi（1，200MPa）。最好纤维的弹性模量超过2.5×107psi（172GPa）和最好超过5.0×107psi（345GPa）。例如作比较，碳化硅的弹性模量为约5.5×107psi（318GPa），二硼化钛约7.6×107psi（524GPa），和碳化硼约6.5×107psi（448GPa）。成品纤维的直径最好在10和150微米之间。本发明的纤维可用于增强其它结构材料，例如金属，陶瓷、玻璃、玻璃陶瓷和聚合物。纤维一般包括一种选自铝、硼、铬、铪、钼、铌、硅、钽、钛、钨、钒和锆元素的硼化物，氮化物，碳化物或硅化物。
这类纤维常常具有很高的截面积平均纵横比，例如，最少为1.3∶1（最大的横截面积除以通过最大横截面的中心的最小横截面积）。纤维通常具有圆度大于1.15，并且最好大于1.5。这类纤维在纵截面方向上具有较大的抗弯强度。
这里所说的“圆度”是指将实测得的该纤维的截面周边长度化为一个理想的圆，将此圆的面积除以对该纤维实测得的截面积。此值越大表示越偏离理想圆。圆度可以很易地通过公式P2/4πA来计算，其中P是量得的周边长度，A是量得的横截面积。纤维表面通常是锯齿形的，这样可以使得能更好地表面粘合在一种基体内。圆度数值较大表示更偏离圆的形状。
本发明的单丝特别理想，因为可以选择一种特别的非氧化物陶瓷而获得，所需的热膨胀系数以便和被增强的材料相匹配。另外，为数众多的这类非氧化物陶瓷材料在和熔融金属相接触时具有良好的抗腐蚀性，这是氧化物型陶瓷材料所没有的。当选择适当的陶瓷材料时，这类纤维具有优良的耐热性能可以超过1700℃，在惰性气体气氛中甚至可以高达4000℃。另外，当适当地选择陶瓷材料的话，即使在空气中，纤维在温度1500℃以上甚至高达1700℃亦可以是稳定的。例如根据本发明制备的碳化硅纤维，在空气中高达1600℃是稳定的，并在惰性气氛中高达2300℃是稳定的。根据本发明制造的碳化硼单丝在惰性气体气氛中在高达2250℃同样是稳定的。根据本发明制备的二硼化钛纤维在温度高达2500℃是稳定的。根据本发明一种烧结的碳化锆单丝在一种烧结的碳化锆单丝在一种惰性气氛中温度高于3400℃是稳定的。“惰性气氛”这里是指一种和陶瓷不会反应的气氛。这种气氛是指包括一种惰性气体的气氛或真空。这里所谓稳定是指化学上和物理上的稳定，即物质基本上不会分解、熔化、软化或升华。
下面实例用于说明，但并不限制本发明。除非另有说明，所有百分数均为重量百分数。
实例1-熔融纺丝
配方
具有比表面积约10m2/g，平均粒径小于1.0微米，并含0.5%B4C的α-SiC
粉末    86.15g
酚醛树脂    （分子量～800），    5.82g
聚乙烯    （分子量200，000-250，000）    7.01g
聚乙烯    （分子量1，500，000-2，000，000）    6.01g
油酸    9.58g
将上述物质在一个混合皿预热至150℃的Brabender    Plastograph混合器中搅拌。将约一半的粉末和所有的有机物加进混合器中，叶片转速为20rpm直至混合物呈流动状。将剩余的粉末分成小份加入。当加料完毕后，混合速度增加至60rpm并且保持约30分钟。将组合物移出，制成颗粒，并装进配有一个0.50mm直径×2.54mm长模孔的纤维化装置中并加热至165℃。用活塞砝码的方式施加压力迫使物料通过模孔。
通过将其绕卷在一个旋转的转筒上使0.50mm的挤出物拉细至约0.20至0.10mm。将所得的长单丝从卷筒取出，涂敷上石墨粉末并挂在炉中在氮气气氛中在2300℃煅烧。测得这类丝的抗拉强度高达104，000psi（717MPa）。
将所得纤维用扫描电子显微镜以200X拍摄照片。在图1和图2展示出代表性的照片。用计算机影像分析器进行分析表明其中平均圆度为1.17。在200X放大下面可以看到一些微细的粗糙表面，而这些在没有放大的情况下是看不到的。没有放大的平滑外表从沿着纵轴的均匀强光表示得很明显，即使高倍放大也能显现出来。
实例Ⅱ-熔融纺丝
配方
实例Ⅰ的SiC粉末    72.99g
凡士林    11.55g
聚乙烯（分子量200，00-250，000）    5.50g
邻苯二甲酸二辛酯    4.00g
聚乙烯分子量（MW1，500，000-2，000，000）    5.00g
酚醛树脂（分子量～800）    3.25g
钛酸四乙基己酯    0.50g
用一个1 1/2 加仑水蒸汽加热的Sigma叶片混合器制备约9kg的上述组合物。在混合完成后将组合物制成颗粒，用一个实验室熔融纺丝装置制成纤维。在此情况下，将颗粒在一个小的挤出机中再融化，并送至一个齿轮泵中，该泵将物料计量送至一个含有20个直径为0.3mm的模孔喷丝板中。用导丝辊进一步将丝拉细成0.20至0.10mm。
将收集到的SiC单丝用石墨粉末涂布并悬挂在一个充有氩气的炉中在2150℃煅烧。测得这种单丝的拉伸强度达90，000psi（620MPa）。
实例    Ⅲ-悬浮液纺丝-干法
配方
同实例Ⅰ的SiC粉末    80.0g
聚乙烯醇缩丁醛（分子量225，000）    9.0g
邻苯二甲酸二辛酯    8.0g
玉米油    2.0g
聚乙二醇（分子量400）    3.0g
二甲基甲酰胺    8.0g
可溶酚醛树脂（分子量～300）    2.0g
在室温下用Brabender    Plastagrph混合器进行混合。加进小量三氯乙烯和乙醇以调节组合物的稠度至油灰状的程度。混合物用装备有一个直径为0.18mm模孔的熔体流动指数仪器挤出。用砝码加在活塞中用以挤出。将挤出物收集在吸水纸中使其干燥。干燥后测得单丝的直径为0.1mm。将单丝固定在SiC生板坯上并在氩气中在2150℃煅烧。这种单丝的拉伸强度高达192，000psi（1，324MPa）。
实例Ⅳ-悬浮液纺丝-干法
配方
同实例Ⅰ的SiC粉末    50.0g
聚环氧乙烷（分子量4，000，000）    10.0g
丙酮    17.0g
乙醇    17.0g
酚醛树脂（分子量～800）    2.3g
在Brabender    Plastograph混合器中在室温进行混合，用足量的蒸馏水使其达到油灰状稠度。将混合物在小的挤出装置中制成纤维，并收集在旋转的卷线筒上。在2150℃烧结15分钟。
将所得纤维用扫描电子显微镜以200X进行拍照。在图3和图4中示出代表性的照片。用电子计算机影像分析器进行测定得到平均圆度为2.08。将沿着纵轴的照片和纤维横截面照片进行比较，清楚地表明尽管横截面十分不规则，但是在纵轴方向上具有特征的一致平滑性。
实例Ⅴ-吹制单丝
配方
同实例1的SiC粉末    100.0g
可溶性酚醛树脂（分子量～300）    5.0g
玉米油    10滴
二甲基甲酰胺    20滴
乙醇/丙酮    50/50（体积）    以制成稀浆液
将上述成分在一个烧杯中混合用来分散并用酚醛树脂涂布SiC颗粒。将溶剂蒸发除掉。将所得的混合物在球磨缸中磨细16小时。将下面成分加进球磨缸中：
甲苯    70.0g
聚乙二醇（分子量400）    10.0g
邻苯二甲酸二辛酯    4.0g
玉米油    1.0g
二甲基甲酰胺    25.0g
球磨继续一小时。然后加进10.0g聚乙烯醇缩丁醛（分子量225，000）和10.0g乙醇并且再继续球磨3小时。将所得的流动料通过80筛目的筛过滤并在真空中脱气直至停止快速冒泡为止。这样的流动料就可用于制备纤维。将流动料充进一个注射器中并且射入一个空气喷射流中。空气的射角可从0°至90°并且使小滴仍能够被分成十分细的纤维。其大小各异，但测到有一些细小至2微米。
实例Ⅵ-制备AlN纤维
基本上按实例1的方法，只是配方改为：
具有比表面积约7m2/g、平均粒径约1.5微米和含1%Y2O3的Al
粉末    83.0g
凡士林    14.0G
聚乙烯（分子量200，000-250，000）    5.5g
聚乙烯（分子量1，500，000-2，000，000）2.0g
玉米油    1.5g
用Brabender    Plastograph混合器在160℃将上述成份混合20分钟。将加工所得的纤维置于一个石墨板上，在氮气中在1850℃烧结1小时以制得高温烧结的氮化铝纤维。
实例Ⅶ B4C纤维的制备
按实例1的方法，只是配方改为：
具有比表面积约8m2/g和平均粒径约
1.5微米的B4C颗粒 50.0g
聚环氧乙烷（分子量4，000，000）    10.0g
丙酮    16.0g
甲醇    16.0g
酚醛树脂（分子量～800）    5.0g
水    1.0g
纤维化装置包括具有20个直径为0.2mm的孔的喷丝板。以约70psi（0.5MPa）压力使混合的配料通过喷丝板。以每分钟30英尺（9.14米）的速度收集纺出的单丝。
将所得的挤出纤维在氩气中在一个B4C履层的石墨钳锅中悬挂煅烧。温度升至2150℃并保持6分钟以形成高温碳化硼纤维。
图5示出基本根据本发明制备的特征纤维的横截面的一幅200X照片。
实例Ⅷ-TiB2纤维制备
按照实例Ⅴ的方法，只是配方改为：
具有比表面积约8m2/g和平均粒径
约为1.5微米的TiB2粉末 50.0g
聚环氧乙烷（分子量600，000）    10.9g
丙酮    15.0g
乙醇    15.0g
酚醛树脂（分子量～800）    2.5g
水    5.3g
所得挤出丝的随机样品测得的直径在18.4和28.3微米之间。将丝悬挂在氩气中的涂B4C的坩埚中在约2150℃煅烧约15分钟以形成高温二硼化钛纤维。
经烧结的二硼化钛产品保持纤维状，并且是银灰色的。
图6示出基本根据本发明制备的此样品的特征纤维的一张500X横截面照片。
实例Ⅸ-由β-SiC制备的纤维
按照实例Ⅵ的方法，只是配方改为：
具有比表面积在15.1和18.7m2/g之间
和粒径在0.25和0.29微米，经HF和HNO3处理并洗涤的
β-SiC粉末    75.27g
纸密度聚乙烯（分子量200，000-250，000）    5.22g
聚乙烯（分子量1，500，000-2，000，000）    4.75g
钛酸四乙基己酯    0.48g
凡士林    10.92g
邻苯二甲酸二辛酯    3.80g
酚醛树脂（分子量～800）    3.09g
在纤维化过程中，纤维被拉细成直径约0.1mm（100微米）。将纤维在一个经由含9份SiC和1份B4C的料浆涂覆的石墨坩埚中的悬挂煅烧。烧结是在氩气气氛中进行。烧结温度升至1900℃并维持5分钟。所得产品是一种烧结的碳化硅单丝。
实例Ⅹ-铝-SiC单丝复合物
将由实例Ⅱ制备所得的未加工SiC单丝约60.0克切成6mm长。将切好的单丝随机装进一个75×150mm的压模中并用足够的压力压实成一片约6mm厚的块。将块在氩气中在2150℃烧结60分钟。将所得的丝压块计算得到的孔隙体积约为70%。将加压掺入熔融的铝烧结的丝压块制得经SiC丝增强的铝块。
实例Ⅺ-Al2O3+5% SiC多晶纤维复合物
将4.0g    SiC多晶纤维（直径约100微米）放在研钵中研碎，并轻轻地切成约1.5至3.0mm长的纤维。
将95.0gAl2O3粉末+0.45g（0.5%）Mg置于一个烧杯中。将4g切过的纤维加至此时粉末中并辗压混合1/2小时，使纤维分配于Al2O3中。
然后将经混合的粉末和纤维倒进一个直径为63.5mm经BN涂覆和用石墨纸衬里的石墨模中。将粉末摊平并插进一个顶模冲和冷加至约1500psi（10MPa）。
然后将模子放进一个热压炉中以1200℃/小时升温速率、在该制件上面最大压力约为1800psi（12MPa）热压升温至1500℃并在此温度保持1/2小时。
测得密度为3.89g/cc，为理论密度的98.5%，在基体中可看到微细裂缝。
实例Ⅻ-SiC+20%    SiC多晶纤维（非加压烧结的）复合物
同实例Ⅰ的α-SiC粉末    56.0g
可溶性酚醛树脂（分子量300）    1.3g
油酸    1.3g
聚乙二醇（分子量20，000）    1.3g
将上述化学品置于一个500ml球磨缸中用醇（掺有5%甲醇的乙醇）混合并一起研磨2小时。
将12.0g直径约100微米的SiC烧结多晶纤维置于研钵中并杵碎和轻轻切成约1.5和3.0mm长度。
将研磨后的混合物倒进一玻璃盘中任其沉降。倾析除去清澈的醇液并将留下浆液置于一块热盘中进一步蒸发溶剂并且使其稠厚。将12.0g经压碎的SiC纤维在搅拌下加进浆液中。然后任此混合物干燥。
将干燥的粉末置于一个63.5mm见方的钢模中并进行冷压。将该冷压过的板采用17，00psi（117MPa）各向等压压榨并在氩气中在2150℃烧结。
测得密度为2.73g/cc，此值等于理论密度的85.3%。基体显示出有些裂缝并且一些纤维并没有紧紧地粘结在基体上。
实例ⅩⅢ-SiC+20% TiB2多晶纤维
同实例Ⅰ的αSiC粉末    50.0g
可溶性酚醛树脂（分子量～300）    1.3g
油酸    1.3g
聚乙二醇（分子量20，000）    1.3g
将上述化学品放进一个500ml的球磨缸中，用醇混合并一起研磨2小时。
将在实例Ⅷ制得经烧结的TiB2多晶纤维15.0g置于一个研钵中用杵杆冲碎并且轻轻切成1.5mm至3.0mm长度。
将经研磨后的混合物倒进一个玻璃盘中任其沉降。倾析除去清澈的醇液并将余下的浆液置于一块热板上进一步蒸发去溶剂并且使其稠厚。在搅拌下慢慢将15.0g经切短的TiB2纤维加进该浆液中。任混合物干燥。
将干粉末置于一个63.5mm见方的钢模中并以12000psi（83MPa）进行冷压。然后将经过冷压的板以17，000psi（117MPa）进行各向等压压榨并在氩气中非加压下以2150℃烧结。
所得的复合物密度为2.91g/cc，相当于理论密度的86.1%。微米结构观察显示基质有很少的裂缝。

Claims (19)

1、一种高温多晶陶瓷纤维，其中该纤维包括选自铝、硼、铬、铪、钼、铌、硅、钽、钛、钨、钒和锆不同元素所组成的一种硼化物，碳化物、氮化物或硅化物，并且其中所述纤维的直径在1至200微米之间，所述纤维在温度约1700℃以上在一种惰性气氛中是稳定的，所述的纤维包括一种具有最大粒径小于纤维直径并且平均粒径少于纤维直径的0.2倍的烧结陶瓷粉末，所述的纤维的圆度大于1.15，所述的纤维具有平滑的表面，所述的陶瓷粉末在温度1700℃以上，在一种惰性气氛中是稳定的，所述的陶瓷中至少90%选自B4C，HfC，NbC，SiC，TaC，VC，WC，ZrC，CrB2，HfB2，NbB2，TaB2，TiB2，VB，WB，ZrB2，AiN，HfN，NbN，Si3N4，TaN，TiN，VN，ZrN，Mo5Si3，MoSi2，Zr5Si3和它们的混合物。
2、根据权利要求1的纤维，其中该纤维的横截面平均纵横比至少为1.3∶1。
3、根据权利要求1的陶瓷纤维，其中该陶瓷粉末是二硼化钛、碳化硅、碳化硼或它们的混合物。
4、根据权利要求1的陶瓷纤维，其中该陶瓷粉末是碳化硅粉末。
5、根据权利要求1的高温陶瓷纤维，其中该陶瓷粉末在温度2000℃以上，在一种惰性气体气氛中是稳定的。
6、根据权利要求1的陶瓷纤维，其中该纤维的拉伸强度超过约100，000psi（689MPa）。
7、根据权利要求1q的陶瓷纤维，其中该陶瓷纤维的拉伸强度超过约175，000psi（1200MPa）。
8、根据权利要求1的陶瓷纤维，其中该纤维直径在10至150微米之间。
9、根据权利要求1的纤维，其中该纤维的弹性模量超过2.5×107psi（172GPa）。
10、根据权利要求1的纤维，其中该纤维的弹性模量超过5.0×107psi（345GPa）。
11、一种用权利要求1的纤维增强的结构材料，其中该结构材料是一种金属，陶瓷，玻璃，玻璃陶瓷或聚合物。
12、一种用权利要求1的纤维增强的一种陶瓷产品。
13、根据权利要求1的纤维，其中该陶瓷粉末的平均粒径小于1微米。
14、一种包括含有高温可烧结陶瓷粉末颗粒的屈挠性聚合物基体的一种可纺织和可烧结的单丝，所述颗粒的平均粒径小于所述单丝直径的0.15倍，所述的碳化物陶瓷颗粒是选自另一种不同元素的硼化物、碳化物、氮化物或硅化物，该另一种不同元素是选自铝、硼、铬、铪、钼、铌、硅、钽、钛、钨、钒和锆，所述单丝的直径在2至300微米之间。
15、根据权利要求14的可纺织和可烧结单丝，其中该陶瓷粉末是选自B4C，HfC，NbC，SiC，TaC，VC，WC，ZrC，CrB2，HfB2，NbB2，TaB2，TiB2，VB，WB，ZrB2，AlN，HfN，NbN，Si3N4，TaN，TiN，VN，ZrN，Mo5Si3，MoSi2Zr5Si3和它们的混合物。
16、根据权利要求14的可烧结的单丝，其中该陶瓷颗粒选自TiB2，SiC，B4C和它们的混合物。
17、根据权利要求14的可纺织的单丝，其中该陶瓷颗粒是具有平均粒径小于1微米的碳化硅颗粒，并且该单丝的直径在10至100微米之间，并且其中该聚合物基体是选自一种聚烯烃基体或一种酚醛和聚烯烃树脂的混合物。
18、根据权利要求14的可烧结单丝，其中该单丝含约75至约95%（重量）的陶瓷颗粒，以及约5至25%（重量）包括聚合物在内的有机化合物。
19、一种制备高温烧结陶瓷纤维的方法，包括在温度约为1700°至约3000℃烧结根据权利要求14的单丝，并且其中烧结时间为0.2至少90分钟。
CN88104423A 1987-07-16 1988-07-15 非氧化物烧结的陶瓷纤维 Pending CN1030566A (zh)

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CA1299830C (en) 1992-05-05

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