高等学校化学学报 ›› 2012, Vol. 33 ›› Issue (09): 1908.doi: 10.3969/j.issn.0251-0790.2012.09.006

• 研究论文: 无机化学 • 上一篇    下一篇

高温水热合成具有超低介电常数的规则介孔氧化硅材料

刘福建2, 韩冰1, 曹洋1, 邹永存1, 孟祥举3, 肖丰收3   

  1. 1. 吉林大学无机合成与制备化学国家重点实验室, 长春 130012;
    2. 绍兴文理学院应用化学研究所, 绍兴 312000;
    3. 浙江大学化学系催化研究所, 杭州 310007
  • 收稿日期:2011-10-26 出版日期:2012-09-10 发布日期:2012-08-14
  • 通讯作者: 邹永存,男,高级工程师,主要从事介孔材料的合成与应用研究.E-mail:zouyc@jlu.edu.cn E-mail:zouyc@jlu.edu.cn
  • 基金资助:

    国家自然科学基金(批准号: 20973079)资助.

Hydrothermal Synthesis of Ordered Mesoporous Silicas with Extraordinarily Ultra-low Dielectric Constants

LIU Fu-Jian2, HAN Bing1, CAO Yang1, ZOU Yong-Cun1, MENG Xiang-Ju3, XIAO Feng-Shou3   

  1. 1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changchun 130012, China;
    2. Institute of Applied Chemistry, Shaoxing University, Shaoxing 312000, China;
    3. Key Laboratory of Applied Chemistry of Zhejiang Province, Department of Chemistry, Zhejiang University, Hangzhou 310028, China
  • Received:2011-10-26 Online:2012-09-10 Published:2012-08-14

摘要:

分别以高分子三嵌段共聚物P123(PEO20-PPO70-PEO20)和F127(PEO106-PPO70-PEO106)为模板剂, 通过高温水热法制备了具有超低介电常数的规则介孔氧化硅材料(OMSs). 当合成温度达到200℃时, 得到的产物仍可保持规则的介孔结构. X射线衍射和氮气吸附结果表明, OMSs系列材料具有规则的二维六方或体心立方介孔结构、 大的比表面积和孔容及均一的孔径分布. 29Si MAS NMR分析表明, OMSs与低温(100℃)合成产物相比具有更高的骨架缩合度, 从而具有优异的水热稳定性. 由于具有大的孔容和高的骨架缩合度, OMSs表现出了超低的介电常数. 以P123为模板剂, 200℃下合成的OMS的介电常数可达1.31. OMSs作为一类稳定的超低介电常数材料, 对于绝缘材料的发展具有潜在的应用价值.

关键词: 规则介孔材料, 高温合成, 氧化硅, 介电常数, 缩合度

Abstract:

Ordered mesoporous silica samples with extraordinarily ultra-low dielectric constants(k) were hydrothermally synthesized at different temperatures(150—200℃) via soft-templates including amphiphilic triblock polymers of P123(PEO20-PPO70-PEO20) and F127(PEO106-PPO70-PEO106). The characterizations of XRD and N2 adsorption-desorption isotherms show that these samples have ordered mesostructure, high BET surface area, large pore volume and uniform pore size.29Si MAS NMR spectra show that the samples have much higher silica condensation degree than the ones synthesized at relatively low temperatures. More importantly, these samples exhibit extraordinarily ultra-low dielectric constant(k). For example, ordered mesoporous silica of SBA-15 synthesized at 200℃ gives k value as low as 1.31, which is interpreted by a collaborative effect of large pore volume with high silica condensation degree. These samples with extraordinarily ultra-low dielectric constants would be potentially important for applications of superior insulators in electronic industry.

Key words: Ordered mesoporous material, High temperature synthesis, Silica, Dielectric constant, Condensation degree

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