CN112010663B - 一种具有难熔金属碳化物界面的C/SiC陶瓷基复合材料及其制备方法 - Google Patents
一种具有难熔金属碳化物界面的C/SiC陶瓷基复合材料及其制备方法 Download PDFInfo
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- 239000003870 refractory metal Substances 0.000 title claims abstract description 19
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 title claims abstract description 7
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 7
- 238000002360 preparation method Methods 0.000 title abstract description 12
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- 238000000034 method Methods 0.000 claims description 17
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- 239000011812 mixed powder Substances 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- ZRBFEDMQRDRUDG-UHFFFAOYSA-N silicon hexaboride Chemical compound B12B3[Si]45B3B2B4B51 ZRBFEDMQRDRUDG-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
本发明属于超高温陶瓷基复合材料领域，涉及一种具有难熔金属碳化物界面的C/SiC陶瓷基复合材料及其制备方法，即以难熔金属与热解碳界面反应生成难熔金属碳化物，与碳纤维反应结合，结合强度高，碳化硅基体通过化学气相渗透与聚碳硅烷循环浸渍热解制备。本发明的有益效果在于：(1)纤维得到有效保护，提高了纤维的高温抗衰减能力；(2)界面致密、界面强度高、抗裂纹扩展能力强，有效地防止氧气的侵蚀。
Description
技术领域
本发明涉及一种C/SiC陶瓷基复合材料及其制备方法，具体涉及一种具有难熔金属碳化物界面的C/SiC陶瓷基复合材料及其制备方法。
背景技术
国家国防实力的提升离不开航空航天技术的发展以及武器装备的改进，超高音速飞行器正成为各国的研究重点之一。由于飞行器常处于超高温、大热流、强侵蚀、高负载的苛刻工作环境中，热防护部件对于飞行器的保护必不可少，用于制造热防护部件的超高温材料必须具有高强度、耐高温、抗氧化、抗热冲击等优异性能，而普通的碳纤维增强陶瓷基复合材料虽然显著提高了材料的韧性，但是其高温抗氧化性仍然无法达到一些航空领域的需求，而难熔金属碳化物(TaC、HfC、ZrC等)具有高熔点、高硬度和高化学稳定性，耐蚀和耐热冲击，高温抗氧化能力强，是一种具有广阔应用前景的涂层材料。所以用难熔金属碳化物作为碳纤维涂层来大幅度提高陶瓷的高温抗氧化性，使其能够在航空航天领域大放光彩。
中国发明专利(申请号：CN201810586081.6专利名称：一种C/C复合材料的超高温陶瓷涂层及其制备方法)公开了一种C/C复合材料的超高温陶瓷涂层及其制备方法，所述的超高温陶瓷涂层其由抗氧化SiC过渡内层与超高温耐烧蚀陶瓷外层组成；所述的超高温耐烧蚀陶瓷外层为SiC、ZrC、HfC、TaC、TiC、ZrB2、HfB2、TaB2、TiB2涂层中的一种以上。发明了一种C/C复合材料高温抗氧化耐烧蚀用超高温陶瓷涂层的制备方法比较适合工业化生产，该方法具有设备工艺简单、易操作、涂层厚度可控等优点。
中国发明专利(申请号：CN201610346311.2专利名称：一种ZrB2-SiC-SiB6超高温陶瓷及其制备方法)公开了一种ZrB2-SiC-SiB6超高温陶瓷及其制备方法，具体为通过热压烧结方法制备SiB6颗粒和SiC颗粒双相增强ZrB2超高温陶瓷材料的方法，该材料具有优异的高温抗氧化性能，制备工艺过程简单、周期短，属于高温热防护材料技术领域。发明的新型ZrB2-SiC-SiB6超高温陶瓷材料粉体分散方法，针对ZrB2、SiC、SiB6三种陶瓷粉体，通过高速球磨方法将碳化硅粉末、六硼化硅粉末和硼化锆粉末均匀分散和混合，再通过烘干、研磨方法获得混合粉体；发明的新型ZrB2-SiC-SiB6超高温陶瓷材料制备方法，选择高温热压烧结工艺方
有益效果
与现有技术相比，本发明的有益效果在于：(1)纤维得到有效保护，提高了纤维的高温抗衰减能力；(2)界面致密、界面强度高、抗裂纹扩展能力强，有效地防止氧气的侵蚀。
具体实施方式
以下实施例是对本发明的进一步说明，而不是限制本发明的范围。
实施例1：
(1)以碳纤维为预制体，通过化学气相渗透法于900℃沉积热解碳界面，界面相的厚度为2μm；
(2)按一定配比称取NaCl、KCl和KF各20g，置于玛瑙研磨中混合、研磨0.5h，然后加入难熔金属粉钽、铪、锆各5g，所用NaCl、KCl、KF均为分析纯，用前在烘箱中于240℃烘干脱水30h；金属粉粒度为200目，纯度99.9％。
(3)将其混匀后装入平铺有短碳纤维的刚玉坩埚内，盖上盖后放入熔盐反应炉，高纯氩气保护下于900℃保温5h。
(4)待炉温降至室温时取出，用水反复煮洗分离出碳纤维试样，最后将碳纤维放入干燥箱，于120℃干燥5小时后取出。
(5)以三氯甲基硅烷为先驱体通过化学气相渗透法制备碳化硅基体，三氯甲基硅烷(CH3SiCl3，MTS)作为沉积SiC的反应气体，在1200℃发生反应生成SiC。
该复合材料抗弯强度1000MPa，1500℃大气环境中烧蚀失重率-1.2％。
实施例2：
(1)以碳纤维为预制体，通过控制化学气相渗透法于1000℃沉积热解碳界面，界面相的厚度为0.2μm；
(2)按一定配比称取NaCl、KCl和KF各20g，置于玛瑙研磨中混合、研磨0.5h，然后加入难熔金属粉钽、铪各10g，所用NaCl、KCl、KF均为分析纯，用前在烘箱中于240℃烘干脱水30h；钽粉和铪粉粒度为200目，纯度99.9％。
(3)将其混匀后装入平铺有短碳纤维的刚玉坩埚内，盖上盖后放入熔盐反应炉，高纯氩气保护下于1000℃保温5h。
(4)待炉温降至室温时取出，用水反复煮洗分离出碳纤维试样，最后将碳纤维放入干燥箱，于120℃干燥5小时后取出。
(5)制备一定浓度的聚碳硅烷(PCS)溶液，采用循环浸渍裂解工艺制备碳化硅基体，浸渍周期为10个周期。
该复合材料抗压强度520MPa，1500℃大气环境中烧蚀失重率-1.0％。
实施例3：
(1)以碳纤维为预制体，通过化学气相渗透法于1100℃沉积热解碳界面，界面相的厚度为1μm；
(2)按一定配比称取NaCl、KCl和KF各20g，置于玛瑙研磨中混合、研磨0.5h，然后加入难熔金属粉钛15g，所用NaCl、KCl、KF均为分析纯，用前在烘箱中于240℃烘干脱水30h；钛粉粒度为200目，纯度99.9％。
(3)将其混匀后装入平铺有短碳纤维的刚玉坩埚内，盖上盖后放入熔盐反应炉，高纯氩气保护下于1000℃保温5h。
(4)待炉温降至室温时取出，用蒸馏水反复煮洗分离出碳纤维试样，最后将碳纤维放入干燥箱，于120℃干燥5小时后取出。
(5)以三氯甲基硅烷为先驱体通过化学气相渗透法制备碳化硅基体，三氯甲基硅烷(CH3SiCl3，MTS)作为沉积SiC的反应气体，在1100℃发生反应生成SiC。
(6)制备一定浓度的聚碳硅烷(PCS)溶液，采用循环浸渍裂解工艺制备碳化硅基体，浸渍周期为13个周期。
该复合材料具有抗压强度高、抗弯强度高，断裂韧性好的有点，具有类似金属的断裂行为。
上述描述仅是对本发明较佳实施例的描述，并非是对本发明范围的任何限定。任何熟悉该领域的普通技术人员根据上述揭示的技术内容做出的任何变更或修饰均应当视为等同的有效实施例，均属于本发明技术方案保护的范围。
Claims (2)
1.一种具有难熔金属碳化物界面的C/SiC陶瓷基复合材料，该复合材料由40-50％体积分数的碳纤维、40-50％体积分数的碳化硅、3-10％体积分数的难熔金属碳化物界面组成，其特征在于难熔金属碳化物是难熔金属与热解碳界面反应生成，厚度为0.1μm-2μm，结合强度高，所述的难熔金属为钽、铪、锆和钛难熔金属中的一种或几种；碳化硅基体通过化学气相渗透或聚碳硅烷循环浸渍热解制备。
2.一种根据权利要求1所述具有难熔金属碳化物界面的C/SiC陶瓷基复合材料的制备方法，其特征在于包括以下顺序的步骤：
(1)以碳纤维为预制体，通过化学气相渗透法于900-1100℃沉积热解碳界面，界面相的厚度为0.1μm-2μm；
(2)将NaCl、KCl、KF和难熔金属粉混合研磨形成熔盐粉末，所述的难熔金属为钽、铪、锆和钛难熔金属中的一种或几种；
(3)将熔盐粉末包覆在碳纤维表面，高纯氩气保护，在900～1200℃保温1-5h；
(4)待炉温降至室温时取出，用水洗涤碳纤维，然后将碳纤维干燥；
(5)以三氯甲基硅烷为先驱体通过化学气相渗透法制备碳化硅基体；
(6)以聚碳硅烷为先驱体通过循环浸渍热解制备碳化硅基体。
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