摘要
以无机铜盐CuCl2的醇溶液为前驱体,采用聚丙烯酸(PAA)为分散剂,环氧丙烷为凝胶促进剂,通过溶胶-凝胶工艺(sol-gel process)制备了铜基醇凝胶,再经CO2超临界流体干燥工艺得到浅绿色块状初始铜基气凝胶,最后经过热处理获得黑色块状纯氧化铜气凝胶样品,其平均密度约为300mg/cm^3。用扫描电子显微镜(SEM)对气凝胶的微结构进行分析可知,最终获得的气凝胶样品主要由百纳米级的矩体颗粒堆砌而成。X射线衍射(XRD)分析表明初始样品具有典型的无定形结构,其主要的结晶成份为斜方晶Cu^2+ 2 Cl(OH)3,而X射线荧光光谱(XRF)测试结果表明其Cu与Cl的元素比为3.55:1,高于Cu^2 +2 Cl(OH)3中两元素的化学计量比,结合化学原理分析可知,其未结晶成分主要为水合氢氧化铜。而XRD的测试结果表明,经过500℃热处理后的样品成分主要为单斜晶氧化铜。
Monolithic copper oxide aerogels were prepared from copper chloride, propylene oxide and polyacrylic acid. Firstly, by using of polyacrylic acid as a dispersant and propylene oxide as an accelerator, the copper-contained alcogel could be made via the sol-gel process. Then the initial light-green monolithic sample could be obtained by the process of aging and supercritical drying. Finally, the black monolithic sample with density of about 300 mg/cm^3 could be obtained by the thermal treatment at 500℃. SEM studies indicated that the final sample being a kind of porous materials consisted of nearly rectangular, submicron particles. In term of XRD, it indicated that the crystal part of initial aerogels was mostly orthorhombic copper chloride hydroxide (Cu^2+ 2 CI(OH)3), while the non-crystal part was Cu(OH)2, taken analysis of chemical principle and XRF result (Cu:C1 equal to 3.55 : 1, which is greater than 2 : 1 in Cu^2+2CI(OH)3) as consideration. And the final sample was monoclinic copper oxide.
出处
《功能材料》
EI
CAS
CSCD
北大核心
2007年第A06期2150-2154,共5页
Journal of Functional Materials
基金
基金项目:上海市科技启明星计划资助项目(05QMx1454)