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制备条件对有机-无机杂化凝胶结构性能的影响

Effect of Preparation Parameters on the Textural Characteristics of Methyl-modified Xerogels
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摘要 以含氢聚甲基硅氧烷(PMHS)和正硅酸乙酯(TEOS)作为前驱体,在室温、无模板剂条件下采用溶胶-凝胶法制备了系列甲基化凝胶材料,并借助N2-吸附/脱附等温线、高分辨透射电镜(TEM)、热分析(TG-DTG)、傅立叶红外光谱(FT-IR)及固体硅核磁(29Si MAS NMR)等测试方法对凝胶材料的结构特征及骨架稳定性进行了系统表征。详细考察了溶胶-凝胶体系PMHS用量、碱量及水量等制备参数对凝胶材料结构性能的影响。结果表明:PMHS/TEOS质量比介于1/10~1/8、NaOH用量介于0.04~0.12和H2O用量为2 mL时所得凝胶材料具有发达的孔道结构和优异的骨架稳定性。 Template-free methyl-modified xerogels have been prepared with polymethylhydrosiloxane (PMHS) and tetraethoxysilane (TEOS) as co-precursors employing mild sol-gel synthesis pathway; and the dependence of textural characteristics on the preparation parameters were detailed investigated by using N2- adsorption-desorption isotherms, transmission electron microscopy (TEM), thermogravimetric analysis (TG-DTG), Fourier transform infrared spectroscopy (FF-IR) and solid state 29Si magic angle spinning nuclear magnetic resonance spectroscopy (29Si MAS NMR). It was demonstrated that highly developed and stable framework of exrogel materials could be prepared under an optimum synthesis conditions, i.e. PMHS/TEOS mass ratios between 1/10-1/8, NaOH dosage of 0.04-0.12 g and H20 amount of 2 mL.
出处 《硅酸盐通报》 CAS CSCD 北大核心 2012年第4期1031-1034,1038,共5页 Bulletin of the Chinese Ceramic Society
关键词 凝胶材料 甲基化 制备条件 表征 xerogel methyl modified preparation conditions characterization
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参考文献8

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