大孔钙铝石块体材料的制备及表征  

Preparation and Characterization of Macroporous Mayenite Monoliths

作　　者：郭兴忠[1] 蔡晓波[1] 宋杰[1] 杨辉[1] 

机构地区：[1]浙江大学材料科学与工程学院,杭州310027

出　　处：《无机材料学报》2015年第2期141-146,共6页Journal of Inorganic Materials

基　　金：国家自然科学基金(51372225);浙江省自然科学基金(LY13B010001)~~

摘　　要：以无机盐二水氯化钙（Ca Cl2·2H2O）和六水氯化铝（Al Cl3·6H2O）为原料,1,2-环氧丙烷（PO）为凝胶促进剂,粘均分子量Mw=100000的聚氧化乙烯（PEO）为相分离诱导剂,乙二醇为络合剂,甲酰胺为干燥控制化学添加剂（DCCA）,采用溶胶-凝胶伴随相分离制备了大孔钙铝石块体。利用扫描电镜（SEM）、压汞、X射线衍射（XRD）等测试技术对所得的块体进行了表征。结果表明：加入PEO能诱导体系发生相分离;PEO用量和溶剂中醇水比会对多孔结构产生明显影响;在合适凝胶温度下,当加入适量PEO和溶剂时,可以获得共连续大孔结构的钙铝石块体;1000℃热处理后,干凝胶由无定型转变为钙铝石晶型Ca12Al14O32Cl2,块体的共连续大孔结构在热处理后被完整保留,其大孔孔径分布在1~2μm,孔隙率为73.0%;热处理前后的钙铝石块体均能保持光滑且致密的骨架。Macroporous mayenite monoliths were successfully prepared via Sol-Gel process accompanied by phase separation using calcium chloride dihydrate and aluminum chloride hexahydrate as raw materials, propylene oxide （PO） as a gelation agent, and poly （ethylene oxide） with average molecular weight of 100,000 as a phase separation inducer. In addition, glycol was used as a chelating agent and formamide as a drying control chemical additive. Macroporous monoliths were characterized by scanning electron microscope（SEM）, mercury porosimetry, and X-ray diffraction （XRD）. The result shows that the addition of PEO induces phase separation; the amount of PEO and the ratio of etha- nol to water have an important effect on porous structure, and monolithic mayenite with co-continuous marcoporous structure is obtained at appropriate addition of PEO and solvent as well as gelation temperature. The dried gels are amorphous, and transform to Ca12Al14O32Cl2 after heat-treatment at 1000℃ in air, while the co-continuous macro- pores are retained. The monolith after heat-treatment has narrow pore size distribution of 1-2 p.m and porosity of 73.0%. The monoliths before and after beat-treatment oossess smooth and dense skeletons.

关 键 词：大孔块体 钙铝石 溶胶–凝胶 相分离 

分 类 号：TQ174[化学工程—陶瓷工业]