摘要
以石油生焦为原料 ,硫酸和硝酸的混合酸为氧化剂 ,通过化学氧化制得炭质水性中间相。将炭质水性中间相于丙酮溶剂中浸泡 7d形成炭质溶胶 ,然后用乙醇洗涤脱出其中的丙酮溶剂得到炭质醇溶胶。再将炭质醇溶胶与锆醇溶胶进行混合制得二元醇溶胶 ,随后进行超临界流体干燥得到二元气凝胶。二元气凝胶具有疏松的表观结构 ,由尺寸为 3～ 15nm的颗粒组成。采用二元炭质 -二氧化锆气凝胶前驱体 ,经氩气气氛下的碳热还原合成了Zr(C ,O)纳米粉体 .并采用XRD和TEM等分析测试技术和化学分析对二元气凝胶和由其制得的Zr(C ,O)纳米粒子的表面形貌和结构进行了表征 .结果表明 ,前驱体制备工艺中 ,合成温度对Zr(C ,O)的结构和化学组成性能有较大的影响 .
The aqua-mesophase can be obtained by the chemical oxidization of petroleum green coke using the mixture of sulfuric acid and nitric acid as an oxidization agent. The aqua-mesophases are dissolved in the acetone solvent at room temperature for one week to form carbonaceous gel. The carbonaceous gel is washed with absolute ethanol to take out acetone to form carbonaceous alcosol. The carbonaceous alcosol and zirconia alcosol are mixed to obtain binary carbonaceous-zirconia alcosol, then dried by sol-gel supercritical fluid drying to prepare the binary aerogel. The binary aerogel with loose appearance is composed of 3-15 nm particles. Using the binary aerogel as a precursor, Zr(C,O) nanosized powders are synthesized by the carbothermal reduction reaction under argon atmosphere. The morphology and structure of binary aerogels and the Zr (C,O) powders prepared from them are characterized by XRD and TEM analyses. The results show that the preparing conditions of binary aerogel precursors and the synthesis temperature have an obvious influence on the structure and the chemical composition of Zr(C,O) solid solutions.
出处
《硅酸盐学报》
EI
CAS
CSCD
北大核心
2001年第2期123-127,共5页
Journal of The Chinese Ceramic Society
基金
煤转化国家重点实验室基金!资助项目 (9919)
