SiCN前驱体炔丙基聚硅氮烷的制备与性能  

Preparation and properties of the propargyl polysilazane as SiCN precursors

作　　者：王欢 王卓 任鹏刚 王明存 WANG Huan;WANG Zhuo;REN Peng-gang;WANG Ming-cun(Faculty of Printing, Packaging Engineering and Digita Media Technology,Xian University of Technology,Xi'an 710048, China;School of Chemistry,Beihang University, Beijing 100191, China)

机构地区：[1]西安理工大学印刷包装与数字媒体学院,陕西西安710048 [2]北京航空航天大学化学学院,北京100191

出　　处：《热固性树脂》2019年第4期49-56,共8页Thermosetting Resin

基　　金：北京分子科学国家实验室基金(201637749501)

摘　　要：由液体聚硅氮烷(LSZ)和溴丙炔在三乙胺缚酸剂促进下的缩合反应制备了炔丙基聚硅氮烷(PPSZ),作为SiCN陶瓷前驱体。通过控制溴丙炔的用量可以得到炔基含量不同的前驱体。采用傅里叶变换红外光谱、凝胶渗透色谱、示差扫描量热分析和动态流变测试等研究了PPSZ及其固化产物的分子结构和固化性能。采用扫描电子显微镜、X-射线衍射仪和热重分析等研究了前驱体陶瓷化过程和陶瓷材料的性能。结果表明:PPSZ在热固化过程中具有理想的流变性,但固化温度较高(>275℃)。PPSZ具有较高的陶瓷化产率,陶瓷化过程的体积膨胀得到抑制。在相对较低的热解温度下SiCN陶瓷的结晶性不高,但有明显的SiC衍射峰。PPSZ树脂热解后陶瓷具有较好的高温抗氧化性能。The propargyl polysilazane(PPSZ)for precursor of SiCN ceramics was prepared by the condensation reaction of liquid polysilazane(LSZ)and propargylbromide in the promotion of triethylamine de-acid agent. The precursors with different propargyl contents could be obtained by controlling the amount of propargylbromide. The molecular structure and curing properties of PPSZ and its cured products were studied by Fourier transform infrared spectroscopy,gel permeation chromatography,differential scanning calorimetry and dynamic rheological testing. The precursor ceramization process and properties of the ceramic materials were studied by scanning electron microscopy,X-ray diffractometry and thermogravimetric analysis. The results showed that the PPSZ had ideal rheological properties during thermal curing, but the curing temperature was higher than 275 ℃. The PPSZ had high ceramization yields,and the volume expansion of the ceramization process was suppressed. The crystallinity of SiCN ceramics was not high at relatively low pyrolysis temperatures,but there were significant Si C diffraction peaks. After pyrolysis of PPSZ resin,the ceramic had good high temperature oxidation resistance.

关 键 词：炔丙基聚硅氮烷 制备 SiCN陶瓷 前驱体 

分 类 号：TB325[一般工业技术—材料科学与工程]