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含锆、硅有机陶瓷前驱体的制备及其陶瓷化研究    

PREPARATION AND CERAMIZATION OF ZIRCONIUM AND SILICON CONTAINING ORGANIC PRECURSORS

文献类型:期刊文献

中文题名:含锆、硅有机陶瓷前驱体的制备及其陶瓷化研究

英文题名:PREPARATION AND CERAMIZATION OF ZIRCONIUM AND SILICON CONTAINING ORGANIC PRECURSORS

作者:杨明泽[1];周权[1];彭峥强[1];宋宁[1];倪礼忠[1]

机构:[1]华东理工大学材料科学与工程学院特种功能高分子材料及相关技术教育部重点实验室,上海200237

年份:2019

期号:3

起止页码:43

中文期刊名:玻璃钢/复合材料

外文期刊名:Fiber Reinforced Plastics/Composites

收录:北大核心:【北大核心2017】;

基金:国家自然科学基金资助项目(51573044)

语种:中文

中文关键词:陶瓷前驱体;后聚合;陶瓷化

外文关键词:precursor;post polymerization;ceramization

摘要:以正丙醇锆、乙酰丙酮,1,2-丙二醇为原料,制备主链为-Zr-O-CH2-CH-,侧链含有不饱和基团的含锆聚合物(ZMP)并作为锆源。将主链为-Si H、-C≡C-的硅炔树脂(PTSA)作为硅源。将二者以质量比2∶5进行复配,制得陶瓷前驱体(PMS)。采用FT-IR和NMR对ZMP结构进行表征,EDS分析了ZMP的元素组成;利用原位红外分别探讨了PMS的固化行为,运用TGA研究了PMS的耐热性能; TGA测试表明,陶瓷前驱体具有良好的耐热及热稳定性能,在氮气和空气气氛下1000℃时的质量保留率分别为90. 24%和88. 53%。通过XRD、SEM、TEM和Raman研究了PMS的陶瓷化演变。陶瓷化演变结果表明,PMS在1600℃下的陶瓷转化率高达57. 4%,且陶瓷产物中含高结晶度的Zr C、Si C晶体。
Zirconium-containing polymer( ZMP) with a main chain of-Zr-O-CH2-CH-and an unsaturated group in the side was prepared by using zirconium n-propoxide,acetylacetone and 1,2-propanediol as raw materials of zirconium source. A silicon alkyne resin( PTSA) with a main chain of-Si H,-C≡C-was used as a silicon source. The two were reconstituted at a mass ratio of 2 ∶ 5 to obtain a ceramic precursor( PMS). The ZMP structure was characterized by FT-IR and NMR. The elemental composition of ZMP was analyzed by EDS. The curing behavior of PMS was investigated by DSC and in-situ infrared,and the heat resistance of PMS was studied by TGA.The TGA test shows that the precursor has good heat and thermal stability,and the mass retention rates at 1000 ℃under nitrogen and air atmosphere are 90. 24% and 88. 53%,respectively. The ceramization evolution of PMS was studied by XRD,SEM,TEM and Raman. The ceramization evolution results show that the ceramic conversion rate of PMS at 1600 ℃ is as high as 57. 4%,and the ceramic products contain high crystallinity Zr C and SiC crystals.

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