CN108546127A - 一种含B/Zr/Si/C复相陶瓷材料的制备方法 - Google Patents

一种含B/Zr/Si/C复相陶瓷材料的制备方法 Download PDF

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CN108546127A
CN108546127A CN201810435181.9A CN201810435181A CN108546127A CN 108546127 A CN108546127 A CN 108546127A CN 201810435181 A CN201810435181 A CN 201810435181A CN 108546127 A CN108546127 A CN 108546127A
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周权
倪礼忠
杨明泽
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East China University of Science and Technology
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Abstract

本发明公开了一类B/Zr/Si/C复相陶瓷材料的制备方法。本方法采用一种在固化过程中可以发生Diels‑Alder反应和Si‑H加成反应的硅炔树脂（PTSA），一种易溶于低沸点有机溶剂、富含硼元素的含硼前驱体（PBS），以及一种溶解性良好、锆含量较高的含锆前驱体（ZMP），由共混法得到锆硅硼炔均相溶液PBZ。该制备方法工艺简单、操作方便，并且改善了共混法的不均一性以及直接合成法的难控制性及异质元素含量低等缺点，制备得到的陶瓷前驱体具备良好的储存稳定性，有助于实现B/Zr/Si/C复相陶瓷材料在耐烧蚀领域的广泛应用。

Description

一种含B/Zr/Si/C复相陶瓷材料的制备方法
技术领域
本发明属于高性能树脂基陶瓷前驱体制备技术领域，特别涉及一种B/Zr/Si/C复相陶瓷材料前驱体的合成方法及其制备。
背景技术
当前，含B、Zr、C等元素的有机陶瓷前驱体树脂一直是研究热点，与传统制备方法相比，利用液态陶瓷前驱体制备陶瓷能够使反应物混合更加均匀（原子尺度或分子尺度均匀混合）从而能够在较低的合成温度下得到纯净的陶瓷材料，很大程度上提高了可操作性。可以适用于制备耐高温聚合物的基体、陶瓷化前驱体、耐烧蚀材料等。
本发明中硼的来源为二十面体笼形结构1,7－碳硼烷（C2B10H12）。
该物质无毒、稳定性好、硼含量高、笼形结构具有非常优异的热稳定性，在空气中于680℃保持稳定，能有效提高先驱体的耐热及热氧化性能。同时热解过程中，原位生成的B4C在高温烧蚀作用下，硼原子被氧化为B2O3形成熔融流动态，可以填补和修复烧蚀形成的微裂纹，具有自愈合抗氧化能力，提高材料的耐烧蚀性能；同时B4C颗粒可提高SiC材料的断裂韧性，当复合材料受到破坏应力时，B4C颗粒大量拔出，防止发生灾难性破坏。因此B原子的引入使得SiC/ZrC/ZrB2/B4C复相陶瓷比仅含SiC/ZrC陶瓷体系表现出更为优异的耐烧蚀和力学性能；同时，原位生成的ZrC、ZrB2、B4C颗粒细小、分布均匀，具有高熔点、高硬度、高化学稳定性和耐烧蚀的特点，并且在高温下具有良好的机械性能，大幅提高B/Zr/Si/C复合材料的耐烧蚀及抗热冲刷性能，抵御超高温烧蚀环境。
本发明采用直接共混法将一种在固化过程中可以发生Diels-Alder反应和Si-H加成反应的硅炔树脂PTSA，一种能发生Si-H加成反应、溶解性良好、硼含量高的含硼前驱体PBS，以及一种溶解性良好、锆含量较高的含锆前驱体ZMP，利用三者在低沸点有机溶剂中优异的溶解性，制备硼锆硅均相前驱体，经过热处理后得到B/Si/Zr/C复相陶瓷材料，其较高的陶瓷转化率和硼锆含量，有望在耐烧蚀材料的研究领域得到进一步发展。
发明内容
将硼、锆元素引入含硅聚合物中制备B/Zr/Si/C复相陶瓷材料，可以很大程度提高材料的耐烧蚀性能。本发明利用合成的硅炔树脂PTSA作为硅源，以富含硼且溶解性良好的含硼聚合物PBS作为硼源，以溶解性良好的含锆聚合物ZMP作为锆源，利用三者的良好溶解性，以质量比1:1:1.2、1:1:1.5、1:1:2 共混得到硼锆硅均相前驱体PBZ。将其置于高纯氩气气氛下1600～1800℃热处理3～5h，即得到B/Zr/Si/C复相陶瓷材料。
本发明所述硅炔树脂PTSA为一类分子主链结构中含有C≡C和Si-H基团的杂化聚合物，其固化过程中可发生交联反应变为三维网络结构，其结构式见说明书附图1，图1为硅炔树脂PTSA的结构式。
本发明所述含硼聚合物PBS，易溶于低沸点有机溶剂，具有较高的硼含量以及Si-H基团，其固化过程中可发生交联反应变为三维网络结构，其结构式见说明书附图2，图2为含硼前驱体PBS的结构式。
本发明采用了一种含锆聚合物ZMP，其具有良好的溶解性和较高的锆含量，其结构见说明书附图3，图3为含锆前驱体ZMP的结构式。
本发明的目的是制备B/Zr/Si/C复相陶瓷材料的方法，其特征如下:
（1）将PBS、ZMP与PTSA分别溶解于四氢呋喃中，将两者以不同的质量比1：（1~4）：（1~5）共混，得到澄清透明溶液，旋蒸除溶剂后即得PBZ。
（2）氩气保护下，1600～1800℃保温3～5h，得到B/Zr/Si/C复相陶瓷。
（3）该硼锆硅前驱体具有较高的陶瓷转化率，且复相陶瓷中硼锆硅含量较高。
本发明通过将硼元素、锆元素引入到主链含有大量C≡C和Si-H基团的硅炔树脂中，利用它们的良好溶解性，通过物理共混即可得到均一体系，操作方便，比例易于控制；另外该前驱体在很好保留了硅炔树脂性能的基础上，又能发挥硼、锆元素的耐烧蚀优势，具备较高的陶瓷产率，有助于实现B/Zr/Si/C复相陶瓷材料在耐高温烧蚀领域的广泛应用。
具体实施方式：
结合实施例对该复相陶瓷的制备方法进行进一步说明，但其并不限制本发明的保护范围：
实施例1：
取2gPBS、2gZMP和2.4gPTSA分别溶解于四氢呋喃中，共混得到淡黄色澄清溶液，60℃下旋蒸除溶剂，得蜡状固体PBZ。将其置于高纯氩气气氛保护下的管式炉内，按照5℃/min的升温速率升至1600℃，保温3h。即得复相陶瓷。陶瓷转化率为76.98%，硼、锆、硅质量含量分别为35.52%、30.02%,、11.05%。
实施例2：
取2gPBS、2gZMP和3gPTSA分别溶解于四氢呋喃中，共混得到淡黄色澄清溶液，60℃下旋蒸除溶剂，得蜡状固体PBZ。将其置于高纯氩气气氛保护下的管式炉内，按照5℃/min的升温速率升至1800℃，保温3h。即得复相陶瓷。陶瓷转化率为78.02%，硼、锆、硅质量含量分别为32.47%、27.43%、12.63%。
实施例3：
取2gPBS、2gZMP和4gPTSA分别溶解于四氢呋喃中，共混得到淡黄色澄清溶液，60℃下旋蒸除溶剂，得蜡状固体PBZ。将其置于高纯氩气气氛保护下的管式炉内，按照5℃/min的升温速率升至1800℃，保温5h。即得复相陶瓷。陶瓷转化率为79.82%，硼、锆、硅质量含量分别为28.42%、24.09%、14.73%。
综上所述可见，本发明提供的B/Zr/Si/C复相陶瓷材料的制备方法，操作简单况且锆硅比例可调，其良好的互溶性有助于该复相陶瓷材料在耐烧蚀领域的应用。
以上所述仅是本发明的实施方式的具体举例，应当指出，对于本领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进，这些改进也应视为本发明的保护范围。

Claims (6)

1.一类B/Zr/Si/C复相陶瓷材料的制备方法，其特征在于：采用一种在固化过程中可以发生Diels-Alder反应和Si-H加成反应的硅炔树脂PTSA，一种溶解性良好、含硼量高、具有Si-H的含硼前驱体PBS，以及一种溶解性良好、锆含量较高的且具有活性基团碳碳双键的含锆前驱体ZMP，将两者按不同的质量比共混得到锆硅均相溶液PBZ。
2.权利要求1所述的B/Zr/Si/C复相陶瓷材料的制备方法，其特征在于：所述的硅炔树脂PTSA为一类分子主链结构中含有C≡C和Si-H基团的杂化聚合物，其结构式见说明书附图1。
3.权利要求1所述的B/Zr/Si/C复相陶瓷材料的制备方法，其特征在于：所述的含硼前驱体PBS，其结构式见说明书附图2。
4.利要求1所述的B/Zr/Si/C复相陶瓷材料的制备方法，其特征在于：所述的含锆前驱体ZMP，其结构式见说明书附图3。
5.利要求1所述的B/Zr/Si/C复相陶瓷材料的制备方法，其特征在于：将PBS、ZMP与PTSA分别溶解于低沸点有机溶剂中，按质量比1：（1~4）：（1~5）共混，得到澄清透明溶液，除去溶剂后，即得PBZ。
6.利要求1所述的B/Zr/Si/C复相陶瓷材料的制备方法，其特征在于：氩气保护下，1600~1800℃管式炉内保温3~5h，得到B/Zr/Si/C复相陶瓷。
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