杉木粉/ZrO2网络互穿杂化材料的制备、形态、结构与性能

Preparation,morphology,structure and properties of fir flour/ZrO_2 hybrid material with interpenetrating network

用20%NaOH溶液处理一定尺寸的杉木粉,以ZrOCl2·8 H2O为无机前驱体,采用水热法将无机物组装在处理后的杉木粉的网络微孔结构中,制备了ZrO2/杉木粉杂化材料。将杂化材料在空气中经过热处理得到多孔ZrO2陶瓷。用FESEM、FTIR、XRD和TGA研究了杉木粉和杂化材料的形态、化学与结晶结构和热稳定性。结果表明：处理后的杉木粉显现出清晰的管胞与纹孔的网络微孔结构,纤维素中的部分氢键被破坏,结晶度下降,反应活性得以提高;在水热条件下,无机前驱体渗透到了杉木粉的微孔结构中,氧氯化锆水解后的羟基与杉木粉中的羟基发生了缩合反应,最终形成了无机/有机垂直互穿网络结构。杂化材料的热稳定性优于杉木粉,热分解温度从282℃提高到298℃。多孔ZrO2陶瓷材料具有笼状结构,孔径约在10-20μm之间。

A specific size of fir flour was treated with 20% NaOH solution,and fir flour/ZrO2 hybrid material was prepared by the hydrothermal method using ZrOCl2·8H2O as inorganic precursor.Porous ZrO2 ceramics was obtained after the hybrid material was treated at 800℃ in air.The morphology,micro structure and properties of the alkaline treated fir flour,hybrid material and ZrO2 ceramics were analyzed by FESEM,FTIR,XRD and TGA.The results showed that cross-porous network structure of the tracheid and pit of fir flour were clear.The hydrogen bonds in cellulose were broken partly and the crystallinity of cellulose decreased,which caused an increase in reaction activity of cellulose.Under the hydrothermal condition,inorganic precursor was infiltrated into the tracheid and pit of fir flour.The hydroxyl groups from the hydrolysis of ZrOCl2 reacted with the hydroxyl groups of the fir flour and interpenetrating network micro structure of the hybrid material was lastly formed.The decomposition temperature increased from 282℃ for fir flour to 298℃ for the hybrid material.The porous ZrO2 ceramics had cage-like structure and the diameter of the pore was about 10—20 μm.