CN107879756B - 一种在碳陶复合材料内部在线原位制备氧化硅晶须的方法 - Google Patents
一种在碳陶复合材料内部在线原位制备氧化硅晶须的方法 Download PDFInfo
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Abstract
本发明具体涉及一种在碳陶复合材料内部在线原位制备氧化硅晶须的方法，主要解决了现有方法制备纳米二氧化硅所需的环境温度高、需要有加热过程、反应气体流量大、不适合在陶瓷基复合材料内部反应的问题。方法包括以下步骤：1)将碳化硅陶瓷基复合材料放入化学气相沉积炉内，炉内温度在900～1100℃；2)将制备碳化硅陶瓷基体的先驱体气体与空气的混合气体引入沉积炉内发生反应；3)陶瓷基复合材料内部在线原位形成氧化硅晶须。本发明方法所需环境温度低、反应气体流量小，可有效降低成本。
Description
技术领域
本发明涉及一种氧化硅晶须的制备方法，具体涉及一种在碳陶复合材料内部在线原位制备氧化硅晶须的方法。
背景技术
陶瓷基复合材料作为一种新型的复合材料，不但具有陶瓷材料优异的高温性能，同时克服了陶瓷具有脆性、具有类金属材料断裂行为的缺陷，已成为应用研究的热点材料，在航空航天领域具有广泛的应用潜力。但由于陶瓷基复合材料各组元热膨胀系数不同，导致该材料基体内部存在裂纹，在氧化环境下易氧化而受损。现有技术表明存在于复合材料内部的氧化硅晶须可缓解材料内部不同组元引起的热应力，减少复合材料基体内部的裂纹数量，同时也可减缓材料的氧化。
公开号CN1590292 A公开了一种利用四氯化硅气体可简单高效制备二氧化硅的方法，但该方法所需的环境温度高(反应温度为1600～2100℃)、需要有加热过程、反应气体流量大(惰性载气流速100～150L/min,氧气流速50～80L/min)，不适合在陶瓷基复合材料内部制备纳米二氧化硅。
发明内容
本发明的目的是解决现有方法制备纳米二氧化硅所需环境温度高、需要有加热过程、反应气体流量大，不适合在陶瓷基复合材料内部反应的问题，提供一种在陶瓷基复合材料内部在线原位制备氧化硅晶须的方法。
本发明解决上述问题的技术方案是，一种在碳陶复合材料内部在线原位制备氧化硅晶须的方法，包括以下步骤：
1)将碳化硅陶瓷基复合材料放入化学气相沉积炉内反应，炉内温度在900～1100℃之间；
2)当碳化硅陶瓷基复合材料密度增大后，将制备碳化硅陶瓷基体的先驱体气体与空气的混合气体引入沉积炉内发生反应；
3)在陶瓷基复合材料内部在线原位形成氧化硅晶须。
进一步地，所述碳化硅陶瓷基复合材料为纤维增强的碳化硅陶瓷基体复合材料，密度低于1.3g/cm3。
进一步地，制备碳化硅陶瓷基体的先驱体气体通过以下方法得到，采用气相运输的方法，将载气气体氢气通入MTS液体内，通过鼓泡的形式带出MTS气体，并与稀释气体氩气一起混合形成先驱气体。
进一步地，所述MTS液体的环境温度为室温，压力为常压，可有效降低成本。
进一步地，载气气体氢气的流速为1～3L/min，稀释气体氩气的流速为1～2L/min，空气的流速为0.1～0.3L/min。本发明方法反应气体流量小，可有效降低成本。
进一步地，化学气相沉积炉内的压力为2～5kPa。
本发明的有益效果为：
1.本发明提供了一种在碳陶复合材料内部在线原位制备氧化硅晶须的方法，不但可以缓解不同组元(碳、硅、碳化硅)之间的热应力，减少内部裂纹数量，而且氧化硅晶须也有强化基体的作用。
2.本发明方法所需环境温度低(900～1100℃)、反应气体流量小(氢气的流速为1～3L/min，氩气的流速为1～2L/min，空气的流速为0.1～0.3L/min)，可有效降低成本。
3.本发明工艺方法是在线原位形成氧化硅晶须，可减少复合材料制备过程中升降温环节，从而减少制备所需的工时，提高了制备效率。
4.本发明方法是在制备复合材料碳化硅陶瓷基体的体系上，引入空气，可使复合材料在线原位形成氧化硅晶须，不会引入其他体系，不会影响后续碳化硅基体的制备。
5.本发明可提高陶瓷复合材料的力学性能及抗氧化性能，是一种易操作、低成本、高效率的工艺路线。
附图说明
图1为复合材料内部在线原位形成的氧化硅晶须SEM形貌图；
图2为氧化硅EDS能谱结果。
具体实施方式
以下结合具体实施例对本发明的内容作进一步详细描述：
为了实现在陶瓷基复合材料基体内部形成晶须结构，缓解复合材料各组元不同的热膨胀系数引起的热应力，减少基体中裂纹的数量，本发明公开了一种在陶瓷基复合材料内部在线原位制备氧化硅晶须的方法，
1)前期先按照制备碳化硅陶瓷基体的工艺进行，将碳化硅陶瓷基复合材料放入化学气相沉积炉内反应，炉内温度在900～1100℃之间；
2)当陶瓷基复合材料密度增大后，将制备碳化硅陶瓷基体的先驱体气体与空气的混合气体引入沉积炉内发生反应；
3)在陶瓷基复合材料内部在线原位形成氧化硅晶须。
本发明的方法具体为：先将密度较低(密度低于1.3g/cm3)的碳化硅陶瓷基复合材料放入化学气相沉积炉内，炉内温度在900～1100℃内，炉内压力为2～5kPa，利用鼓泡的方法，将氢气引入到MTS液体内，带出MTS气相并与稀释气体氩气一起汇合形成先驱气体，进入化学气相沉积炉内，在复合材料内部制备碳化硅陶瓷基体，当复合材料到达半致密化状态(密度在1.3～1.8g/cm3)时，在先驱气体中引入空气，并充分混合后进入反应炉内，发生化学反应，空气中的氧元素渗透到复合材料孔隙内部，在碳化硅表面原位发生硅-氧体系的氧化反应，可在复合材料基体内部原位生成氧化硅晶须，半致密化的碳化硅陶瓷基复合材料具体为纤维增强的碳化硅陶瓷基体复合材料。引入空气后，发生氧化反应，形成氧化硅晶须，通过化学气相沉积法，在线原位生长成氧化硅晶须。
制备碳化硅陶瓷基体的先驱气体为三氯甲基硅烷(MTS)，载气为氢气，稀释气体为氩气，采用气相运输的办法，将氢气通入到MTS液体内，通过鼓泡的形式带出MTS气体，然后与空气混为一起；其中，通入MTS液体中载气氢气的流速为1～3L/min，稀释气体氩气的流速为1～2L/min，空气流速为0.1～0.3L/min，MTS液体所处容器的环境温度为室温，压力为常压。
实施例一
先将密度为1.0g/cm3的碳化硅陶瓷基复合材料放入化学气相沉积炉内，设定化学气相沉积炉内的温度为1000℃，压力为5kPa，然后按3L/min的流速将氢气引入到MTS液体内，带出MTS反应气体，再与氩气(流速为2L/min)汇合后统一进入反应炉内，在复合材料内部形成碳化硅基体，当陶瓷基复合材料密度达到1.3～1.5g/cm3后，在原有的反应体系中引入空气，流速为0.1L/min，与MTS等气体混合后统一进入反应炉内，最终在复合材料内部原位形成氧化硅晶须，如图1所示。图2为该晶须的能谱结果，分析表明该工艺可在陶瓷基复合材料原位形成氧化硅晶须。
实施例二
先将密度为1.1g/cm3的碳化硅陶瓷基复合材料放入化学气相沉积炉内，设定化学气相沉积炉内的温度为900℃，压力为2kPa，然后按1L/min的流速将氢气引入到MTS液体内，带出MTS反应气体，再与氩气(流速为1L/min)汇合后统一进入反应炉内，在复合材料内部形成碳化硅基体，当陶瓷基复合材料密度达到1.5～1.8g/cm3后，在原有的反应体系中引入空气，流速为0.3L/min，与MTS等气体混合后统一进入反应炉内，最终在复合材料内部原位形成氧化硅晶须。
实施例三
先将密度为1.2g/cm3的碳化硅陶瓷基复合材料放入化学气相沉积炉内，设定化学气相沉积炉内的温度为1100℃，压力为4kPa，然后按2L/min的流速将氢气引入到MTS液体内，带出MTS反应气体，再与氩气(流速为1.5L/min)汇合后统一进入反应炉内，在复合材料内部形成碳化硅基体，当陶瓷基复合材料密度达到1.8～2.0g/cm3后，在原有的反应体系中引入空气，流速为0.2L/min，与MTS等气体混合后统一进入反应炉内，最终在复合材料内部原位形成氧化硅晶须。
Claims (4)
1.一种在碳陶复合材料内部在线原位制备氧化硅晶须的方法，其特征在于：包括以下步骤，
1)将碳化硅陶瓷基复合材料放入化学气相沉积炉内反应，炉内温度在900～1100℃之间；
2)当碳化硅陶瓷基复合材料密度增大后，将制备碳化硅陶瓷基体的先驱体气体与空气的混合气体引入沉积炉内发生反应；
制备碳化硅陶瓷基体的先驱体气体通过以下方法得到，采用气相运输的方法，将载气气体氢气通入MTS液体内，通过鼓泡的形式带出MTS气体，并与稀释气体氩气一起混合形成先驱体 气体；载气气体氢气的流速为1～3L/min，稀释气体氩气的流速为1～2L/min，空气的流速为0.1～0.3L/min；
3)在陶瓷基复合材料内部在线原位形成氧化硅晶须。
2.根据权利要求1所述的在碳陶复合材料内部在线原位制备氧化硅晶须的方法，其特征在于：所述碳化硅陶瓷基复合材料为纤维增强的碳化硅陶瓷基体复合材料，密度低于1.3g/cm3。
3.根据权利要求2所述的在碳陶复合材料内部在线原位制备氧化硅晶须的方法，其特征在于：所述MTS液体的环境温度为室温，压力为常压。
4.根据权利要求1至3内任一所述的在碳陶复合材料内部在线原位制备氧化硅晶须的方法，其特征在于：化学气相沉积炉内的压力为2～5kPa。
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