含ZrC炭气凝胶的合成及其表征叶丽.pdfVIP

含 ZrC 炭气凝胶的合成及其表征 叶丽 冀志宏 赵爱军 邱文丰 赵彤 (中国科学院化学研究所 北京 100190) 文 摘 本文利用碳热还原原理，以聚乙酰丙酮锆（PZO ）为锆源，2, 4-二羟基苯甲酸（DA ） 和甲醛为C源，制备了一种含ZrC 的C气凝胶。制备方法如下：首先，将聚乙酰丙酮锆与 2, 4- 二羟基苯甲酸在乙醇中进行配体交换反应，然后加入甲醛原位聚合形成溶胶和醇凝胶，超临 界二氧化碳干燥得到含Zr有机气凝胶；所得有机气凝胶在氩气保护下热解，即得到含Zr 的C 气凝胶，通过调节PZO/DA大的质量比可以方便的调节C气凝胶中Zr 的含量。对不同温度的 热解产物进行研究表明，如果Zr完全以ZrO2 的形式存在，所得气凝胶的抗氧化性比纯的炭气 凝胶有所降低，而当提高热解温度，使气凝胶发生碳热还原生成部分ZrC可以提高气凝胶的 抗氧化性，且在 1300 °C热解所得的气凝胶具有最高的比表面积和最好的耐氧化性。 关键词 ZrC ，C 气凝胶，碳热还原，抗氧化性 Preparation and Characterization of ZrC-Containing Carbon Aerogels Ye Li, Ji Zhihong, Zhao Aijun, Qiu Wenfeng, Zhao Tong (Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190) Abstract ZrC-containing carbon aerogels were prepared by sol-gel method using 2, 4-dihydroxybenzoic acid (DA) and formaldehyde (F) as carbon precursor and polyzirconoxone (PZO) as zirconium precursor. First, DA and PZO were dissolved in EtOH and suffered a ligand-exchange reaction, and then F was added. And the resulting alcogels were then dried directly using supercritical CO2, followed by carbonization under an argon atmosphere. Study suggested that when Zr existed as ZrO2 absolutely, the oxidation resistance of the carbon aerogels will be decreased, however, when Zr partly existed as ZrC, the oxidation resistance of the carbon aerogels will be improved. Especially, the samples pyrolyzed at 1300 °C exhibit the best oxidation resistance and have the largest specific surface areas. Key words ZrC ，C aerogel，carbothermal reduction，oxidation resistance 作者简介：叶丽，博士研究生，主要从事气凝胶材料的研究工作。 E-mail ： yeli@iccas.ac.cn, 联系电话：010