CN110066176A - 氮化硼纤维增强硅硼氧氮陶瓷基复合材料的制备方法 - Google Patents

氮化硼纤维增强硅硼氧氮陶瓷基复合材料的制备方法 Download PDF

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CN110066176A
CN110066176A CN201910392964.8A CN201910392964A CN110066176A CN 110066176 A CN110066176 A CN 110066176A CN 201910392964 A CN201910392964 A CN 201910392964A CN 110066176 A CN110066176 A CN 110066176A
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boron nitride
oxygen nitrogen
boron
fiber
staple fiber
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吴赟
李鑫
温广武
王鑫昊
仲诚
孙志远
李俐
王洪升
韦其红
邵长涛
孙成功
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Shandong University of Technology
Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Abstract

本发明公开了一种氮化硼纤维增强硅硼氧氮陶瓷基复合材料的制备方法，其特征是：将絮状氮化硼纤维经湿法球磨后得到的氮化硼短纤维加入硅硼氧氮陶瓷粉体中进行均匀混合获得制备陶瓷基复合材料的原料；将原料经干燥、过筛后装模进行热压烧结，之后随炉冷却，出炉脱模后即可获得氮化硼纤维增强硅硼氧氮材料。本发明的制备方法工艺简单，适于工业化操作，生产周期、短成本低。由本发明的方法得到的复合材料性能密度达到1.5~2.5g/cm3，抗弯强度＞90MPa，断裂韧性＞5.2 MPa·m1/2，解决了硅硼氧氮陶瓷的脆性断裂问题，提高了材料的力学性能。

Description

氮化硼纤维增强硅硼氧氮陶瓷基复合材料的制备方法
技术领域
本发明属于陶瓷基复合材料技术领域，涉及一种氮化硼纤维增强硅硼氧氮陶瓷基复合材料的制备方法。
背景技术
硅硼氧氮陶瓷是一种新型耐高温透波陶瓷材料，具有优异的电学、热学及力学性能，但因这种陶瓷材料的本征脆性，限制了该材料在高温结构件上的使用。这种材料陶瓷材料的致命弱点是脆性，根据复合材料的理论，当裂纹扩展遇到纤维时，通过纤维与基体界面的脱离来吸收能量，缓和应力集中；部分纤维在张应力作用下发生断裂而从集体中拔出时，也将吸收较大的能量。因此，纤维增韧陶瓷基复合材料是一种有效解决硅硼氧氮陶瓷材料脆性的途径。而为了保证硅硼氧氮陶瓷的高温透波特性，最适合作为增强相添加的是氮化硼纤维。目前，国内连续氮化硼纤维生产尚不成熟，而非连续氮化硼纤维的生产工艺和产品性能已较为稳定，为本专利技术的实施提供了基础条件。
目前所使用的BN纤维增韧的方法主要有CVD/CVI法[1]，PIP法[2 3 4]，热压烧结[5 6]。中国专利201711312460.8所使用的CVD/CVI法需要先制备氮化硼预制体，然后进行热解沉降，所需周期较长；中国专利201710359001.9所使用PIP法工艺复杂，需要反复浸渍多次，并且所需的设备要求较高；中国专利CN201110005941.0所使用PIP法不仅要反复浸渍，而且要先固化完后热解，所需周期较长；中国专利201710280508.5所使用热压烧结法氮化物粉体和BN短纤维球磨时需要加入纳米SiO2粉和烧结助剂，球磨时间3 - 24 h，需要将BN絮状纤维剪切成长度为5 mm的短纤维，工艺较为复杂且污染较大；中国专利201710039763.0所使用热压烧结法需要使用溶胶凝胶法制备堇青石粉体，加入剪切过的BN短纤维（长度为3 - 5毫米）后需要超声分散，实验步骤繁琐，所需周期长；本专利技术与上述专利技术相比，无需氮化硼纤维预制体，采用球磨的方式对BN絮状纤维进行处理得到BN短纤维，后续经过热压烧结得到氮化硼纤维增强硅硼氧氮陶瓷基复合材料，效率高，所需周期短，工艺简单，易于工程化实施。
[1]西北工业大学.CVD/CVI法制备透波型BN纤维增韧Si-B-N陶瓷基复合材料的方法:CN201711312460.8[P].2017-12-12。
[2]中国航空工业集团公司基础技术研究院.一种纤维增强SiC基复合材料的成型方法:CN201710359001.9[P].2017-05-19。
[3]中材高新材料股份有限公司.氮化物纤维织物增强氮化物陶瓷材料的制备方法:CN201110005941.0[P].2011-01-12。
[4]南京航空航天大学.一种氮化硼纤维增韧的氮化硼-氮化硅基透波复合材料的制备方法:CN201210336410.4[P].2012-09-13。
[5]山东工业陶瓷研究设计院有限公司.氮化硼纤维增强氮化物陶瓷基复合材料的制备方法:CN201710280508.5[P].2017-04-26。
[6]哈尔滨工业大学.一种氮化硼纤维增强堇青石陶瓷基复合材料及其制备方法:CN201710039763.0[P].2017-01-19。
发明内容
本发明的目的是提供一种氮化硼纤维增强硅硼氧氮陶瓷基复合材料的制备方法，从而提高硅硼氧氮陶瓷材料的力学性能。该方法步骤简单，便于工业化操作，本发明采用技术方案如下：
1. 将絮状氮化硼纤维通过湿法球磨的工艺处理成分散性好、尺寸均匀的短纤维，即按照质量比1:2加入正己烷、丙酮等湿法球磨介质，按料球比1:40~1:60、转速200~400转/分钟、球磨时间2~10分钟得到氮化硼短纤维；
2. 按照氮化硼短纤维加入量为所有粉体质量的20％~70％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体置于三维混合机，搅拌混合机或球磨混合机等混合设备中均匀混合，获得制备陶瓷基复合材料的原料；
3. 将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5~10℃/min，烧结温度1400~1800℃，保温时间0.5~2小时，压力15~35MPa；
4. 热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。
与现有技术相比，本发明的优点在于：（1）利用湿法球磨工艺处理絮状团聚氮化硼，获得的氮化硼短纤维分散性好、尺寸均匀，工艺过程简单高效；（2）采用硅硼氧氮粉末与氮化硼纤维直接混合，再进行热压烧结，解决了化学气相沉积、反复浸渍裂解烧结等方法周期长、成本高、资源消耗过大的问题；（3）通过纤维增强的方式显著提高了硅硼氧氮陶瓷材料的性能。
附图说明
图1为通过本发明方法获得的氮化硼短纤维扫描电子显微镜照片；图2为复合材料断口扫描电子显微镜照片；图3为复合材料X射线衍射物相分析图谱；图4为具体实施例获得材料的性能数据。图2和图3表明复合材料中氮化硼纤维形貌完好且均匀分布于基体材料中，物相组成为氮化硼微晶、氮化硅微晶以及非晶态物质构成的硅硼氧氮陶瓷，证明所制得材料为氮化硼纤维增强硅硼氧氮陶瓷复合材料
具体实施方式
为了更好的了解本发明的技术方案，下面结合具体实施例对本发明作进一步说明。
实施例一
将絮状氮化硼纤维置于球磨罐中，按照质量比1:2加入丙酮，按料球比1:45加入氧化锆球，然后在行星式球磨机上以转速200转/分钟、球磨8分钟得到氮化硼短纤维。按照氮化硼短纤维加入量为所有粉体质量的20％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体球磨混合机中均匀混合，获得制备陶瓷基复合材料的原料。将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5℃/min，烧结温度1700℃，保温时间1小时，压力20MPa。热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。复合材料性能为：密度1.99g/cm3，弯曲强度93.2MPa，断裂韧性6.3 MPa·m1/2。
实施例二
将絮状氮化硼纤维置于球磨罐中，按照质量比1:2加入丙酮，按料球比1:45加入氧化锆球，然后在行星式球磨机上以转速200转/分钟、球磨8分钟得到氮化硼短纤维。按照氮化硼短纤维加入量为所有粉体质量的20％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体球磨混合机中均匀混合，获得制备陶瓷基复合材料的原料。将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5℃/min，烧结温度1600℃，保温时间1小时，压力20MPa。热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。复合材料性能为：密度1.97g/cm3，弯曲强度105.7MPa，断裂韧性6.7 MPa·m1/2。
实施例三
将絮状氮化硼纤维置于球磨罐中，按照质量比1:2加入丙酮，按料球比1:45加入氧化锆球，然后在行星式球磨机上以转速200转/分钟、球磨8分钟得到氮化硼短纤维。按照氮化硼短纤维加入量为所有粉体质量的20％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体球磨混合机中均匀混合，获得制备陶瓷基复合材料的原料。将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5℃/min，烧结温度1500℃，保温时间1小时，压力20MPa。热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。复合材料性能为：密度1.94g/cm3，弯曲强度115.3MPa，断裂韧性7.3 MPa·m1/2。
实施例四
将絮状氮化硼纤维置于球磨罐中，按照质量比1:2加入丙酮，按料球比1:45加入氧化锆球，然后在行星式球磨机上以转速200转/分钟、球磨8分钟得到氮化硼短纤维。按照氮化硼短纤维加入量为所有粉体质量的20％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体球磨混合机中均匀混合，获得制备陶瓷基复合材料的原料。将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5℃/min，烧结温度1400℃，保温时间1小时，压力20MPa。热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。复合材料性能为：密度1.89g/cm3，弯曲强度89.4MPa，断裂韧性5.6 MPa·m1/2。
实施例五
将絮状氮化硼纤维置于球磨罐中，按照质量比1:2加入正己烷，按料球比1:45加入氧化锆球，然后在行星式球磨机上以转速300转/分钟、球磨8分钟得到氮化硼短纤维。按照氮化硼短纤维加入量为所有粉体质量的30％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体球磨混合机中均匀混合，获得制备陶瓷基复合材料的原料。将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5℃/min，烧结温度1700℃，保温时间1小时，压力20MPa。热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。复合材料性能为：密度1.98g/cm3，弯曲强度102.4MPa，断裂韧性7.1 MPa·m1/2。
实施例六
将絮状氮化硼纤维置于球磨罐中，按照质量比1:2加入正己烷，按料球比1:45加入氧化锆球，然后在行星式球磨机上以转速300转/分钟、球磨8分钟得到氮化硼短纤维。按照氮化硼短纤维加入量为所有粉体质量的30％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体球磨混合机中均匀混合，获得制备陶瓷基复合材料的原料。将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5℃/min，烧结温度1600℃，保温时间1小时，压力20MPa。热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。复合材料性能为：密度1.97g/cm3，弯曲强度113.9MPa，断裂韧性7.6 MPa·m1/2。
实施例七
将絮状氮化硼纤维置于球磨罐中，按照质量比1:2加入正己烷，按料球比1:45加入氧化锆球，然后在行星式球磨机上以转速300转/分钟、球磨8分钟得到氮化硼短纤维。按照氮化硼短纤维加入量为所有粉体质量的30％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体球磨混合机中均匀混合，获得制备陶瓷基复合材料的原料。将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5℃/min，烧结温度1500℃，保温时间1小时，压力20MPa。热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。复合材料性能为：密度1.94g/cm3，弯曲强度123.1MPa，断裂韧性8.0MPa·m1/2。
实施例八
将絮状氮化硼纤维置于球磨罐中，按照质量比1:2加入正己烷，按料球比1:45加入氧化锆球，然后在行星式球磨机上以转速300转/分钟、球磨8分钟得到氮化硼短纤维。按照氮化硼短纤维加入量为所有粉体质量的30％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体球磨混合机中均匀混合，获得制备陶瓷基复合材料的原料。将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5℃/min，烧结温度1400℃，保温时间1小时，压力20MPa。热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。复合材料性能为：密度1.88g/cm3，弯曲强度96.4MPa，断裂韧性6.4 MPa·m1/2。
实施例九
将絮状氮化硼纤维置于球磨罐中，按照质量比1:2加入正己烷，按料球比1:45加入氧化锆球，然后在行星式球磨机上以转速300转/分钟、球磨8分钟得到氮化硼短纤维。按照氮化硼短纤维加入量为所有粉体质量的40％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体球磨混合机中均匀混合，获得制备陶瓷基复合材料的原料。将原料经干燥、过筛后装模进行热压烧结，热压烧结工艺参数为：升温速率5℃/min，烧结温度1500℃，保温时间1小时，压力20MPa。热压烧结过程结束后随炉冷却，出炉脱模后即获得氮化硼纤维增强硅硼氧氮复合材料。复合材料性能为：密度1.95g/cm3，弯曲强度125.8MPa，断裂韧性8.2 MPa·m1/2。
上述各实施例获得的材料的性能测试数据列于图4中。其中，抗弯强度和断裂韧性分别采用三点弯曲和单边缺口梁三点弯曲法测试；密度由阿基米德排水法测得。

Claims (4)

1.一种氮化硼纤维增强硅硼氧氮陶瓷基复合材料的制备方法，其特征是：所使用的氮化硼短纤维是将絮状氮化硼纤维经湿法球磨后得到的；按照氮化硼短纤维加入量为所有粉体质量的20％-70％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体进行均匀混合获得制备陶瓷基复合材料的原料；将原料经干燥、过筛后装模进行热压烧结，之后随炉冷却，出炉脱模后即可获得氮化硼纤维增强硅硼氧氮材料。
2.如权利要求1所述的制备方法，其特征是：所使用的氮化硼短纤维是将絮状氮化硼纤维按照质量比1:2加入正己烷、丙酮等湿法球磨介质，按照料球比1:40~1:60，转速200~400转/分钟，球磨时间2~10分钟得到。
3.如权利要求1所述的制备方法，其特征是：按照氮化硼短纤维加入量为所有粉体质量的30％-70％比例将氮化硼短纤维、硅硼氧氮陶瓷粉体置于三维混合机，搅拌混合机或球磨混合机等混合设备中均匀混合。
4.如权利要求1所述的制备方法，其特征是：按照升温速率5~10℃/min，烧结温度1400~1800℃，保温时间0.5~2小时，压力15~35MPa工艺参数进行热压烧结。
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