CN105753493A - 一种抗氧化陶瓷基复合材料及其粉末冶金制备方法 - Google Patents

一种抗氧化陶瓷基复合材料及其粉末冶金制备方法 Download PDF

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CN105753493A
CN105753493A CN201610111131.6A CN201610111131A CN105753493A CN 105753493 A CN105753493 A CN 105753493A CN 201610111131 A CN201610111131 A CN 201610111131A CN 105753493 A CN105753493 A CN 105753493A
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filtering residue
oxidation
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resistant ceramic
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刘莉
王爽
邱晶
刘晓东
黄明明
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Suzhou Netshape Composite Materials Co Ltd
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Abstract

本发明公开了一种抗氧化陶瓷基复合材料及其粉末冶金制备方法，由以下组分按重量份数配比组成：碳化硅13～36份、氮化硅15～30份、二氧化硅12～34份、氧化镧3～9份、氧化铬4～11份、碳纤维7～18份、碳酸氢钠8～12份、无水乙醇13～26份、去离子水30～45份。本发明利用稀有元素与碳化硅、氮化硅及二氧化硅间的协同作用，并通过粉末冶金方法制备获得的抗氧化陶瓷基复合材料具有抗氧化性能好及抗疲劳极限高的优点。

Description

一种抗氧化陶瓷基复合材料及其粉末冶金制备方法
技术领域
本发明涉及一种复合材料，尤其涉及一种抗氧化陶瓷基复合材料及其粉末冶金制备方法。
背景技术
陶瓷基复合材料是以陶瓷为基体与各种纤维复合的一类复合材料。陶瓷基体可为氮化硅、碳化硅等高温结构陶瓷。这些先进陶瓷具有耐高温、高强度和刚度、相对重量较轻、抗腐蚀等优异性能，而其致命的弱点是具有脆性，处于应力状态时，会产生裂纹，甚至断裂导致材料失效。而采用高强度、高弹性的纤维与基体复合，则是提高陶瓷韧性和可靠性的一个有效的方法。纤维能阻止裂纹的扩展，从而得到有优良韧性的纤维增强陶瓷基复合材料。
陶瓷基复合材料具有优异的耐高温性能，主要用作高温及耐磨制品。其最高使用温度主要取决于基体特征。陶瓷基复合材料已实用化或即将实用化的领域有刀具、滑动构件、发动机制件、能源构件等。法国已将长纤维增强碳化硅复合材料应用于制造高速列车的制动件，显示出优异的摩擦磨损特性，取得满意的使用效果。
陶瓷基复合材料中的碳纤维在高温氧化性气氛下易于氧化，其总体性能随着氧化失重的增加而急剧降低，从而限制了其在高温下的应用。为了较为准确地评估陶瓷基复合材料在高温结构部件的潜在应用前景，需要综合分析机械载荷及环境腐蚀对其材料性能的影响。经验证，陶瓷基复合材料在550～650℃温度范围内，其氧化失重严重，造成材料性能丧失。此外，在室温和高温水氧环境下的疲劳极限明显低于其室温疲劳极限。
发明内容
本发明解决的技术问题：为了获得一种抗氧化性能好，抗疲劳极限高的陶瓷基复合材料，本发明提供了一种抗氧化陶瓷基复合材料及其粉末冶金制备方法。
技术方案：一种抗氧化陶瓷基复合材料，由以下组分按重量份数配比组成：碳化硅13～36份、氮化硅15～30份、二氧化硅12～34份、氧化镧3～9份、氧化铬4～11份、碳纤维7～18份、碳酸氢钠8～12份、无水乙醇13～26份、去离子水30～45份。
优选的，所述抗氧化陶瓷基复合材料由以下组分按重量份数配比组成：碳化硅30份、氮化硅25份、二氧化硅28份、氧化镧7份、氧化铬8份、碳纤维14份、碳酸氢钠10份、无水乙醇22份、去离子水38份。
一种抗氧化陶瓷基复合材料的粉末冶金制备方法，包含以下步骤：
(1)将碳酸氢钠溶于去离子水中，制备获得碳酸氢钠溶液；
(2)将碳化硅、氮化硅、二氧化硅、氧化镧、氧化铬和碳纤维同时加入球磨机中，研磨1～3小时，粉末粒径为250～400目，获得粉末混合物；
(3)将步骤(2)获得的粉末混合物加入步骤(1)的碳酸氢钠溶液中，在40～60℃条件下，搅拌反应20～45分钟，过滤去除滤液，获得滤渣；
(4)用去离子水清洗步骤(3)获得的滤渣，滤渣与去离子水的质量比为1:1～1.5，清洗三次；
(5)向经步骤(4)清洗后的滤渣中加入无水乙醇，搅拌反应10～20分钟，吸水两次；过滤去除无水乙醇后，将滤渣置于56～78℃条件下烘干；
(6)将烘干后的滤渣置于混料装置内，利用压力为3.2～4.8MPa的高压气体将上述粉末吹起，5～12分钟后停止通入高压气体，各粉末共同沉积并均匀混合；
(7)将上述均匀混合后的粉末置于电炉中，在氦气的保护氛围中采用3阶段升温的方式进行烧结，3阶段的温度分别为1320℃、1460℃、1630℃，每阶段烧结时间为1～4.5小时，烧结完成后等静压成型，即可获得抗氧化陶瓷基复合材料。
优选的，步骤(2)中将碳化硅、氮化硅、二氧化硅、氧化镧、氧化铬和碳纤维同时加入球磨机中，研磨2.2小时，粉末粒径为300目，获得粉末混合物。
优选的，步骤(3)中将步骤(2)获得的粉末混合物加入步骤(1)的碳酸氢钠溶液中，在56℃条件下，搅拌反应30分钟，过滤去除滤液，获得滤渣。
优选的，步骤(4)中用去离子水清洗步骤(3)获得的滤渣，滤渣与去离子水的质量比为1:1.3，清洗三次。
优选的，步骤(5)中向经步骤(4)清洗后的滤渣中加入无水乙醇，搅拌反应16分钟，吸水两次；过滤去除无水乙醇后，将滤渣置于72℃条件下烘干。
优选的，步骤(6)中将烘干后的滤渣置于混料装置内，利用压力为4.3MPa的高压气体将上述粉末吹起，9分钟后停止通入高压气体，各粉末共同沉积并均匀混合。
优选的，步骤(7)中将上述均匀混合后的粉末置于电炉中，在氦气的保护氛围中采用3阶段升温的方式进行烧结，3阶段的温度分别为1320℃、1460℃、1630℃，每阶段烧结时间为3.2小时，烧结完成后等静压成型，即可获得抗氧化陶瓷基复合材料。
有益效果：本发明利用稀有元素与碳化硅、氮化硅及二氧化硅间的协同作用，并通过粉末冶金方法制备获得的抗氧化陶瓷基复合材料具有抗氧化性能好及抗疲劳极限高的优点。
具体实施方式
实施例1
一种抗氧化陶瓷基复合材料，由以下组分按重量份数配比组成：碳化硅13份、氮化硅15份、二氧化硅12份、氧化镧3份、氧化铬4份、碳纤维7份、碳酸氢钠8份、无水乙醇13份、去离子水30份。
一种抗氧化陶瓷基复合材料的粉末冶金制备方法，包含以下步骤：
(1)将碳酸氢钠溶于去离子水中，制备获得碳酸氢钠溶液；
(2)将碳化硅、氮化硅、二氧化硅、氧化镧、氧化铬和碳纤维同时加入球磨机中，研磨1小时，粉末粒径为250目，获得粉末混合物；
(3)将步骤(2)获得的粉末混合物加入步骤(1)的碳酸氢钠溶液中，在40℃条件下，搅拌反应20分钟，过滤去除滤液，获得滤渣；
(4)用去离子水清洗步骤(3)获得的滤渣，滤渣与去离子水的质量比为1:1，清洗三次；
(5)向经步骤(4)清洗后的滤渣中加入无水乙醇，搅拌反应10分钟，吸水两次；过滤去除无水乙醇后，将滤渣置于56℃条件下烘干；
(6)将烘干后的滤渣置于混料装置内，利用压力为3.2MPa的高压气体将上述粉末吹起，5分钟后停止通入高压气体，各粉末共同沉积并均匀混合；
(7)将上述均匀混合后的粉末置于电炉中，在氦气的保护氛围中采用3阶段升温的方式进行烧结，3阶段的温度分别为1320℃、1460℃、1630℃，每阶段烧结时间为1小时，烧结完成后等静压成型，即可获得抗氧化陶瓷基复合材料。
实施例2
一种抗氧化陶瓷基复合材料，由以下组分按重量份数配比组成：碳化硅30份、氮化硅25份、二氧化硅28份、氧化镧7份、氧化铬8份、碳纤维14份、碳酸氢钠10份、无水乙醇22份、去离子水38份。
一种抗氧化陶瓷基复合材料的粉末冶金制备方法，包含以下步骤：
(1)将碳酸氢钠溶于去离子水中，制备获得碳酸氢钠溶液；
(2)将碳化硅、氮化硅、二氧化硅、氧化镧、氧化铬和碳纤维同时加入球磨机中，研磨2.2小时，粉末粒径为300目，获得粉末混合物；
(3)将步骤(2)获得的粉末混合物加入步骤(1)的碳酸氢钠溶液中，在56℃条件下，搅拌反应30分钟，过滤去除滤液，获得滤渣；
(4)用去离子水清洗步骤(3)获得的滤渣，滤渣与去离子水的质量比为1:1.3，清洗三次；
(5)向经步骤(4)清洗后的滤渣中加入无水乙醇，搅拌反应16分钟，吸水两次；过滤去除无水乙醇后，将滤渣置于72℃条件下烘干；
(6)将烘干后的滤渣置于混料装置内，利用压力为4.3MPa的高压气体将上述粉末吹起，9分钟后停止通入高压气体，各粉末共同沉积并均匀混合；
(7)将上述均匀混合后的粉末置于电炉中，在氦气的保护氛围中采用3阶段升温的方式进行烧结，3阶段的温度分别为1320℃、1460℃、1630℃，每阶段烧结时间为3.2小时，烧结完成后等静压成型，即可获得抗氧化陶瓷基复合材料。
实施例3
一种抗氧化陶瓷基复合材料，由以下组分按重量份数配比组成：碳化硅36份、氮化硅30份、二氧化硅34份、氧化镧9份、氧化铬11份、碳纤维18份、碳酸氢钠12份、无水乙醇26份、去离子水45份。
一种抗氧化陶瓷基复合材料的粉末冶金制备方法，包含以下步骤：
(1)将碳酸氢钠溶于去离子水中，制备获得碳酸氢钠溶液；
(2)将碳化硅、氮化硅、二氧化硅、氧化镧、氧化铬和碳纤维同时加入球磨机中，研磨3小时，粉末粒径为400目，获得粉末混合物；
(3)将步骤(2)获得的粉末混合物加入步骤(1)的碳酸氢钠溶液中，在60℃条件下，搅拌反应45分钟，过滤去除滤液，获得滤渣；
(4)用去离子水清洗步骤(3)获得的滤渣，滤渣与去离子水的质量比为1:1.5，清洗三次；
(5)向经步骤(4)清洗后的滤渣中加入无水乙醇，搅拌反应20分钟，吸水两次；过滤去除无水乙醇后，将滤渣置于78℃条件下烘干；
(6)将烘干后的滤渣置于混料装置内，利用压力为4.8MPa的高压气体将上述粉末吹起，12分钟后停止通入高压气体，各粉末共同沉积并均匀混合；
(7)将上述均匀混合后的粉末置于电炉中，在氦气的保护氛围中采用3阶段升温的方式进行烧结，3阶段的温度分别为1320℃、1460℃、1630℃，每阶段烧结时间为4.5小时，烧结完成后等静压成型，即可获得抗氧化陶瓷基复合材料。
对实施例1～3制备获得的抗氧化陶瓷基复合材料进行性能检测，结果如下表所示：
表1实施例1～3制备获得的抗氧化陶瓷基复合材料性能检测结果

Claims (9)

1.一种抗氧化陶瓷基复合材料，其特征在于，由以下组分按重量份数配比组成：碳化硅13～36份、氮化硅15～30份、二氧化硅12～34份、氧化镧3～9份、氧化铬4～11份、碳纤维7～18份、碳酸氢钠8～12份、无水乙醇13～26份、去离子水30～45份。
2.根据权利要求1所述的一种抗氧化陶瓷基复合材料，其特征在于，由以下组分按重量份数配比组成：碳化硅30份、氮化硅25份、二氧化硅28份、氧化镧7份、氧化铬8份、碳纤维14份、碳酸氢钠10份、无水乙醇22份、去离子水38份。
3.权利要求1所述一种抗氧化陶瓷基复合材料的粉末冶金制备方法，其特征在于，包含以下步骤：
(1)将碳酸氢钠溶于去离子水中，制备获得碳酸氢钠溶液；
(2)将碳化硅、氮化硅、二氧化硅、氧化镧、氧化铬和碳纤维同时加入球磨机中，研磨1～3小时，粉末粒径为250～400目，获得粉末混合物；
(3)将步骤(2)获得的粉末混合物加入步骤(1)的碳酸氢钠溶液中，在40～60℃条件下，搅拌反应20～45分钟，过滤去除滤液，获得滤渣；
(4)用去离子水清洗步骤(3)获得的滤渣，滤渣与去离子水的质量比为1:1～1.5，清洗三次；
(5)向经步骤(4)清洗后的滤渣中加入无水乙醇，搅拌反应10～20分钟，吸水两次；过滤去除无水乙醇后，将滤渣置于56～78℃条件下烘干；
(6)将烘干后的滤渣置于混料装置内，利用压力为3.2～4.8MPa的高压气体将上述粉末吹起，5～12分钟后停止通入高压气体，各粉末共同沉积并均匀混合；
(7)将上述均匀混合后的粉末置于电炉中，在氦气的保护氛围中采用3阶段升温的方式进行烧结，3阶段的温度分别为1320℃、1460℃、1630℃，每阶段烧结时间为1～4.5小时，烧结完成后等静压成型，即可获得抗氧化陶瓷基复合材料。
4.根据权利要求3所述一种抗氧化陶瓷基复合材料的粉末冶金制备方法，其特征在于，步骤(2)中将碳化硅、氮化硅、二氧化硅、氧化镧、氧化铬和碳纤维同时加入球磨机中，研磨2.2小时，粉末粒径为300目，获得粉末混合物。
5.根据权利要求3所述一种抗氧化陶瓷基复合材料的粉末冶金制备方法，其特征在于，步骤(3)中将步骤(2)获得的粉末混合物加入步骤(1)的碳酸氢钠溶液中，在56℃条件下，搅拌反应30分钟，过滤去除滤液，获得滤渣。
6.根据权利要求3所述一种抗氧化陶瓷基复合材料的粉末冶金制备方法，其特征在于，步骤(4)中用去离子水清洗步骤(3)获得的滤渣，滤渣与去离子水的质量比为1:1.3，清洗三次。
7.根据权利要求3所述一种抗氧化陶瓷基复合材料的粉末冶金制备方法，其特征在于，步骤(5)中向经步骤(4)清洗后的滤渣中加入无水乙醇，搅拌反应16分钟，吸水两次；过滤去除无水乙醇后，将滤渣置于72℃条件下烘干。
8.根据权利要求3所述一种抗氧化陶瓷基复合材料的粉末冶金制备方法，其特征在于，步骤(6)中将烘干后的滤渣置于混料装置内，利用压力为4.3MPa的高压气体将上述粉末吹起，9分钟后停止通入高压气体，各粉末共同沉积并均匀混合。
9.根据权利要求3所述一种抗氧化陶瓷基复合材料的粉末冶金制备方法，其特征在于，步骤(7)中将上述均匀混合后的粉末置于电炉中，在氦气的保护氛围中采用3阶段升温的方式进行烧结，3阶段的温度分别为1320℃、1460℃、1630℃，每阶段烧结时间为3.2小时，烧结完成后等静压成型，即可获得抗氧化陶瓷基复合材料。
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Citations (2)

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Publication number Priority date Publication date Assignee Title
WO2013060175A1 (zh) * 2011-10-28 2013-05-02 中国科学院上海硅酸盐研究所 高强度纤维增强陶瓷基复合材料的微区原位反应制备方法
CN105130444A (zh) * 2015-08-27 2015-12-09 苏州莱特复合材料有限公司 一种湿式缸套及其粉末冶金制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013060175A1 (zh) * 2011-10-28 2013-05-02 中国科学院上海硅酸盐研究所 高强度纤维增强陶瓷基复合材料的微区原位反应制备方法
CN105130444A (zh) * 2015-08-27 2015-12-09 苏州莱特复合材料有限公司 一种湿式缸套及其粉末冶金制备方法

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