CN112174671B - 一种耐高温SiZrBOC五元陶瓷的制备方法 - Google Patents

一种耐高温SiZrBOC五元陶瓷的制备方法 Download PDF

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CN112174671B
CN112174671B CN202011077154.2A CN202011077154A CN112174671B CN 112174671 B CN112174671 B CN 112174671B CN 202011077154 A CN202011077154 A CN 202011077154A CN 112174671 B CN112174671 B CN 112174671B
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sizrboc
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赵广东
张婉莹
韩文波
吕杨
张志新
曲灵犀
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Heilongjiang University
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Abstract

一种耐高温SiZrBOC五元陶瓷的制备方法，本发明涉及有机高分子材料技术领域，具体涉及一种耐高温SiZrBOC五元陶瓷的制备方法。本发明要解决现有方法制备的陶瓷先驱体耐高温性能差的技术问题。方法：采用溶胶凝胶法合成SiZrBOC多元陶瓷先驱体，然后高温热解，得到耐高温SiZrBOC五元陶瓷。本发明在制备SiZrBOC先驱体时，可以将C、O、B、Zr、Si等元素键合为一种大分子网络结构，并且Zr的引入均有效地提高SiBOC陶瓷前驱体的热稳定性。本发明用于制备耐高温SiZrBOC陶瓷材料。

Description

一种耐高温SiZrBOC五元陶瓷的制备方法
技术领域
本发明涉及有机高分子材料技术领域，具体涉及一种耐高温SiZrBOC五元陶瓷的制备方法。
背景技术
先驱体转化陶瓷(polymer-derived ceramics，PDCs)是一类有良好的热机械性能陶瓷材料，具有优异的强度、抗蠕变、抗热震和抗氧化能力。在先驱体转化陶瓷的研究中，与传统陶瓷相比，SiOC陶瓷具有成本低、可设计性和加工性高的特点。然而，SiOC陶瓷在1300℃开始进行碳热还原反应是一个关键问题，因此其高温性能的缺乏也限制了SiOC陶瓷的广泛应用。为了改善这一缺陷，许多学者对SiOC陶瓷进行了改性，引入了一些B、N、Zr、Hf等元素合成了四元陶瓷和五元陶瓷，目前性能较好、比较常用的先驱体有聚碳硅烷、聚硅氮烷、聚硅硼氮碳烷等。目前，在相关领域内已经有科研机构合成出SiBOC、SiZrOC以及SiBCN等陶瓷先驱体，但还没有制备出SiZrBOC陶瓷先驱体的具体方法。
发明内容
本发明要解决现有方法制备的陶瓷先驱体耐高温性能差的技术问题，而提供一种耐高温SiZrBOC五元陶瓷的制备方法。
一种耐高温SiZrBOC五元陶瓷的制备方法，具体按以下步骤进行：
一、将聚甲基氢硅氧烷加入到无水乙醇中，再加入乙二胺进行室温搅拌，得到溶液A；
二、将正丙醇锆和蒸馏水混合，然后加入到步骤一获得的溶液A中，获得溶液B；
三、将硼酸和无水乙醇混合，加入到溶液B中，搅拌并加热至100℃，然后持续搅拌6～6.5h，干燥获得陶瓷先驱体；
四、将步骤三获得的陶瓷先驱体进行高温热解，得到耐高温SiZrBOC五元陶瓷，完成该方法。
本发明用溶胶凝胶法合成了SiZrBOC多元陶瓷先驱体，重点解决在SiZrBOC先驱体交联过程中，关于C、O、B、Zr、Si等元素键合为Si-O-B、Si-O-Si、Si-C、Zr-O-Zr、B-O、Si-O-Zr和陶瓷先驱体最终产率的问题，生成一种性能优异的SiZrBOC陶瓷先驱体制备方法，在整个合成的过程中，需要对元素的摩尔质量进行分析和调整，才能保证得到性能最好的陶瓷先驱体，有利于进行后续的陶瓷制备及其他研究工作。
本发明的有益效果是：
本发明方法在制备得到的SiZrBOC先驱体中，可以将C、O、B、Zr、Si等元素键合为一种大分子网络结构。合成出的SiZrBOC多元陶瓷先驱体中包含Si-O-B、Si-O-Si、Si-C、Zr-O-Zr、B-O、Si-O-Zr等基团，根据加入B/Zr摩尔比的差别可得到不同的陶瓷先驱体和不同的产率，按照本发明方法制备得到高产率SiZrBOC先驱体的陶瓷产率为82～86％。而SiBOC先驱体的陶瓷产率仅为71％，因此Zr的引入可以有效地提高SiBOC陶瓷前驱体的热稳定性。并且本发明制备的陶瓷先驱体在700℃后趋于稳定，1200℃时陶瓷产率在80％以上，说明陶瓷先驱体高温稳定性优异。
本发明用于制备耐高温SiZrBOC陶瓷材料。
附图说明
图1为实施例一所得SiZrBOC陶瓷材料的XRD曲线图片；
图2为实例一所得SiZrBOC陶瓷材料的SEM图片；
图3为实例一所得SiZrBOC陶瓷材料的FT-IR曲线图片；
图4为实例一步骤三获得SiZrBOC陶瓷先驱体的热失重曲线图片。
具体实施方式
本发明技术方案不局限于以下所列举的具体实施方式，还包括各具体实施方式之间的任意组合。
具体实施方式一：本实施方式一种耐高温SiZrBOC五元陶瓷的制备方法，具体按以下步骤进行：
一、将聚甲基氢硅氧烷加入到无水乙醇中，再加入乙二胺进行室温搅拌，得到溶液A；
二、将正丙醇锆和蒸馏水混合，然后加入到步骤一获得的溶液A中，获得溶液B；
三、将硼酸和无水乙醇混合，加入到溶液B中，搅拌并加热至100℃，然后持续搅拌6～6.5h，干燥获得陶瓷先驱体；
四、将步骤三获得的陶瓷先驱体进行高温热解，得到耐高温SiZrBOC五元陶瓷，完成该方法。
具体实施方式二：本实施方式与具体实施方式一不同的是：步骤一中聚甲基氢硅氧烷与无水乙醇的体积比为5:(5.7～6.2)。其它与具体实施方式一相同。
具体实施方式三：本实施方式与具体实施方式一或二不同的是：步骤一中室温搅拌72h。其它与具体实施方式一或二相同。
具体实施方式四：本实施方式与具体实施方式一至三之一不同的是：步骤二中正丙醇锆与蒸馏水的体积比为(14.8～16.8):1。其它与具体实施方式一至三之一相同。
具体实施方式五：本实施方式与具体实施方式一至四之一不同的是：步骤二中正丙醇锆与溶液A中聚甲基氢硅氧烷的体积比为(6.9～7.8):8。其它与具体实施方式一至四之一相同。
具体实施方式六：本实施方式与具体实施方式一至五之一不同的是：步骤三中硼酸和无水乙醇的质量比为3:(11.8～12.5)。其它与具体实施方式一至五之一相同。
具体实施方式七：本实施方式与具体实施方式一至六之一不同的是：步骤三中硼酸和无水乙醇的质量比为3:11.9。其它与具体实施方式一至六之一相同。
具体实施方式八：本实施方式与具体实施方式一至七之一不同的是：步骤三中硼酸与溶液B中正丙醇锆的质量比为2:(7.2～8.3)。其它与具体实施方式一至七之一相同。
具体实施方式九：本实施方式与具体实施方式一至八之一不同的是：步骤三中干燥温度为100℃，干燥时间为12h。其它与具体实施方式一至八之一相同。
具体实施方式十：本实施方式与具体实施方式一至九之一不同的是：步骤四高温热解工艺为：以5℃/min的升温速率升温至1000℃，以3℃/min的升温速率升温至1000～1400℃，保温时间1～2h，随后以3℃/min的降温速率降温至1000℃，再以5℃/min的降温速率降至室温。其它与具体实施方式一至九之一相同。
采用以下实施例验证本发明的有益效果：
实施例一：
本实施例一种耐高温SiZrBOC五元陶瓷的制备方法，具体按以下步骤进行：
一、将聚甲基氢硅氧烷加入到无水乙醇中，再加入乙二胺进行室温搅拌72h，得到溶液A；聚甲基氢硅氧烷与无水乙醇的体积比为5:5.9；
二、将正丙醇锆和蒸馏水混合，然后加入到步骤一获得的溶液A中，获得溶液B；正丙醇锆与蒸馏水的体积比为15.8:1，正丙醇锆与溶液A中聚甲基氢硅氧烷的体积比为6.9:8；
三、将硼酸和无水乙醇混合，硼酸和无水乙醇的质量比为3:11.9，加入到溶液B中，搅拌并加热至100℃，然后持续搅拌6h，干燥获得陶瓷先驱体；干燥温度为100℃，干燥时间为12h；
四、将步骤三获得的陶瓷先驱体进行高温热解，得到耐高温SiZrBOC五元陶瓷，完成该方法。
步骤四高温热解工艺为：以5℃/min的升温速率升温至1000℃，以3℃/min的升温速率升温至1300℃，保温时间1.5h，随后以3℃/min的降温速率降温至1000℃，再以5℃/min的降温速率降至室温。
图1为实例一所得SiZrBOC陶瓷材料的XRD曲线图片；从图中可以看出衍射峰尖锐而强烈，表面其高度结晶性。
图2为实例一所得SiZrBOC陶瓷材料的SEM图片；从图中可以看出陶瓷表面光滑细致，没有缺陷。
图3为实例一所得SiZrBOC陶瓷材料的FT-IR曲线图片；从图中可以看出热解后C-H等部分官能团的消失。
图4为实例一步骤三获得SiZrBOC陶瓷先驱体的热失重曲线图片；从图中可以看出陶瓷先驱体在700℃后趋于稳定，1200℃时陶瓷产率在80％以上，说明陶瓷先驱体高温稳定性优异。
经过管式炉1300℃高温热处理，本实施例制备得到SiZrBOC先驱体的陶瓷产率可达83％，表明其具有优异的耐高温特性。
实施例二：
本实施例一种耐高温SiZrBOC五元陶瓷的制备方法，具体按以下步骤进行：
一、将聚甲基氢硅氧烷加入到无水乙醇中，再加入乙二胺进行室温搅拌72h，得到溶液A；聚甲基氢硅氧烷与无水乙醇的体积比为5:5.7；
二、将正丙醇锆和蒸馏水混合，然后加入到步骤一获得的溶液A中，获得溶液B；正丙醇锆与蒸馏水的体积比为14.8:1，正丙醇锆与溶液A中聚甲基氢硅氧烷的体积比为7.3:8；
三、将硼酸和无水乙醇混合，硼酸和无水乙醇的质量比为3:11.8，加入到溶液B中，搅拌并加热至100℃，然后持续搅拌6h，干燥获得陶瓷先驱体；干燥温度为100℃，干燥时间为12h；
四、将步骤三获得的陶瓷先驱体进行高温热解，得到耐高温SiZrBOC五元陶瓷，完成该方法。
步骤四高温热解工艺为：以5℃/min的升温速率升温至1000℃，以3℃/min的升温速率升温至1300℃，保温时间1.5h，随后以3℃/min的降温速率降温至1000℃，再以5℃/min的降温速率降至室温。
经过管式炉1300℃高温热处理，本实施例制备得到SiZrBOC先驱体的陶瓷产率可达86％。
实施例三：
本实施例一种耐高温SiZrBOC五元陶瓷的制备方法，具体按以下步骤进行：
一、将聚甲基氢硅氧烷加入到无水乙醇中，再加入乙二胺进行室温搅拌72h，得到溶液A；聚甲基氢硅氧烷与无水乙醇的体积比为5:6；
二、将正丙醇锆和蒸馏水混合，然后加入到步骤一获得的溶液A中，获得溶液B；正丙醇锆与蒸馏水的体积比为15.8:1，正丙醇锆与溶液A中聚甲基氢硅氧烷的体积比为7.8:8；
三、将硼酸和无水乙醇混合，硼酸和无水乙醇的质量比为3:12.3，加入到溶液B中，搅拌并加热至100℃，然后持续搅拌6h，干燥获得陶瓷先驱体；干燥温度为100℃，干燥时间为12h；
四、将步骤三获得的陶瓷先驱体进行高温热解，得到耐高温SiZrBOC五元陶瓷，完成该方法。
步骤四高温热解工艺为：以5℃/min的升温速率升温至1000℃，以3℃/min的升温速率升温至1300℃，保温时间1.5h，随后以3℃/min的降温速率降温至1000℃，再以5℃/min的降温速率降至室温。
经过管式炉1300℃高温热处理，本实施例制备得到SiZrBOC先驱体的陶瓷产率可达81％。

Claims (9)

1.一种耐高温SiZrBOC五元陶瓷的制备方法，其特征在于该方法具体按以下步骤进行：
一、将聚甲基氢硅氧烷加入到无水乙醇中，再加入乙二胺进行室温搅拌，得到溶液A；
二、将正丙醇锆和蒸馏水混合，然后加入到步骤一获得的溶液A中，获得溶液B；
三、将硼酸和无水乙醇混合，加入到溶液B中，搅拌并加热至100℃，然后持续搅拌6～6.5h，干燥获得陶瓷先驱体；
四、将步骤三获得的陶瓷先驱体进行高温热解，得到耐高温SiZrBOC五元陶瓷，完成该方法；
步骤二中正丙醇锆与溶液A中聚甲基氢硅氧烷的体积比为(6.9～7.8):8。
2.根据权利要求1所述的一种耐高温SiZrBOC五元陶瓷的制备方法，其特征在于步骤一中聚甲基氢硅氧烷与无水乙醇的体积比为5:(5.7～6.2)。
3.根据权利要求1所述的一种耐高温SiZrBOC五元陶瓷的制备方法，其特征在于步骤一中室温搅拌72h。
4.根据权利要求1所述的一种耐高温SiZrBOC五元陶瓷的制备方法，其特征在于步骤二中正丙醇锆与蒸馏水的体积比为(14.8～16.8):1。
5.根据权利要求1所述的一种耐高温SiZrBOC五元陶瓷的制备方法，其特征在于步骤三中硼酸和无水乙醇的质量比为3:(11.8～12.5)。
6.根据权利要求1所述的一种耐高温SiZrBOC五元陶瓷的制备方法，其特征在于步骤三中硼酸和无水乙醇的质量比为3:11.9。
7.根据权利要求1所述的一种耐高温SiZrBOC五元陶瓷的制备方法，其特征在于步骤三中硼酸与溶液B中正丙醇锆的质量比为2:(7.2～8.3)。
8.根据权利要求1所述的一种耐高温SiZrBOC五元陶瓷的制备方法，其特征在于步骤三中干燥温度为100℃，干燥时间为12h。
9.根据权利要求1所述的一种耐高温SiZrBOC五元陶瓷的制备方法，其特征在于步骤四高温热解工艺为：以5℃/min的升温速率升温至1000℃，以3℃/min的升温速率升温至1000～1400℃，保温时间1～2h，随后以3℃/min的降温速率降温至1000℃，再以5℃/min的降温速率降至室温。
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