以锆酸四丁酯为锆源,采用溶胶-凝胶法结合化学液相沉积(CLD),即在凝胶老化过程中用部分水解的锆酸四丁酯和正硅酸四乙酯进行液相修饰,经过乙醇超临界干燥(SCFD)制备耐高温ZrO_2/SiO_2块体复合气凝胶。采用透射电子显微镜(TEM)、傅里叶红外光谱仪(FT-IR)、X线衍射仪(XRD)、N_2吸附分析仪等仪器表征了ZrO_2/SiO_2复合气凝胶的形貌、表面基团、晶相和孔结构,着重研究其耐热性能。结果表明:制备的ZrO_2/SiO_2复合气凝胶具有优秀的耐温性能,1 000℃处理2 h后,仍为四方相,线收缩率仅为12%,比表面积高达186 m2/g。
Heat-resistant monolithic zirconia / silica composite aerogels were prepared by using zirconium n-butoxide as precursor via sol-gel route combined with chemical liquid deposition( CLD),and supercritical fluid drying( SCFD). Zirconia wet gels were modified with partially hydrolyzed zirconium nbutoxide and tetraethoxysilane during aging. Transmission electron microscope( TEM),Fourier transform infrared spectroscope( FT-IR),X-ray diffraction( XRD),and N_2 adsorption analyzer were used to characterize the morphology,surface groups,phases,pore structure,and thermal properties. The obtained composite aerogel exhibited excellent heat resistance remained in the tetragonal phase at 1 000 ℃ for 2h. Its linear shrinkage was about 12% and the specific surface area was as high as 186 m~2/ g.