| 紫外光固化乙烯基硅氮烷-巯基共聚物热裂解产物的表征 |
| Characterization of Pyrolysate for UV Curable Polysilazane-Vinyl-Thiol Copolymer |
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| 摘要: 采用热失重与热分析联用(TGA-DTA)、X射线衍射(XDR)，场发射扫描电镜(FE-SEM)、透射电镜(TEM)、能谱仪及排水法对紫外光固化乙烯基硅氮烷-巯基共聚体系裂解产物进行了分析和表征。结果表明：在300～500 ℃的范围内出现了相吻合的质量损失速率峰和热量吸收峰；最终质量保持率约为55wt%；体系表观密度出现先下降后上升的趋势，保温时间提高可使热解产物进一步密实化，密度最终达到2.458 g·cm-3；在保温2 h的条件下，共聚系在1 400 ℃下生成少量Si3N4晶体，在1 600 ℃下，热解物晶体组成为nSiO2∶nSi3N4∶nSiC=3∶26∶71，结晶度达91.25%；延长保温时间即可提高体系的结晶度，也可降低结晶温度。在1 400 ℃保温24 h，观察到热解物内生成大量不规则的晶须。 |
| 关键词: 乙烯基硅氮烷-巯基共聚体系 紫外光固化 热裂解 |
| 基金项目: |
| Abstract: The pyrolysate of UV curable polysilazane-vinyl-thiol copolymer was analyzed and characterized by TGA-DTA, XRD, FE-SEM, Energy-dispersive X-ray spectroscopy and TEM. It is found that two distinct weight loss peaks at 358 ℃ and 450 ℃ in TGA curve are identical with two DTA endothermic peaks. The total weight loss is 45wt%. At the beginning the apparent density drops down, then enhances progressively, and finally gets to 2.458 g·cm-3. Si3N4 crystal can be formed at 1 400 ℃ for 2 h and the crystalline degree can reach 91.25% at 1 600 ℃ with the composition of nSiO2∶nSi3N4∶nSiC=3∶26∶71. Extending the holding time not only does the crystalline degree increase, but also the crystalline temperature decreases. Irregular whisker of Si3N4 was observed by SEM after pyrolyating at 1 400 ℃ for 24 h. |
| Keywords: polysilazane-vinyl-thiol UV-curing pyroylsis |
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| 摘要点击次数: 1485 |
| 全文下载次数: 1959 |
| 陈立新,王亚洲,宋家乐,张教强.紫外光固化乙烯基硅氮烷-巯基共聚物热裂解产物的表征[J].无机化学学报,2009,25(1):37-41. |
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