模板浸渍法制备ZrO_(2)纤维研究  

Preparation of ZrO_(2) fibers by template impregnation method

作　　者：张雷 闫森旺 李虹屿 孙小飞[1] 王刚[1] 张一帆 王守业[1] Zhang Lei;Yan Senwang;Li Hongyu;Sun Xiao-fei;Wang Gang;Zhang Yifan;Wang Shouye

机构地区：[1]中钢集团洛阳耐火材料研究院有限公司先进耐火材料国家重点实验室,河南洛阳471039

出　　处：《耐火材料》2022年第2期101-106,共6页Refractories

基　　金：国家重点研发计划资助项目(2018YFB0605904)。

摘　　要：将15 cm×15 cm×1 cm的粘胶纤维模板放入浓度为1、2及3 mol·L^(-1)的ZrOCl_(2)溶液,分别在20、40、60℃下浸渍20 h,经过洗涤、离心、干燥得到ZrO_(2)纤维前驱体,再对前驱体进行600、800、1000、1200℃保温2 h热处理制得ZrO_(2)纤维。研究浸渍温度、浸渍液浓度、热处理温度对ZrO_(2)纤维形貌和相组成的影响。结果表明,随着浸渍温度由20℃提高到60℃,浸渍液浓度由1 mol·L^(-1)提高到3 mol·L^(-1),纤维横截面微观形貌由扁平状向圆柱状变化,同时纤维的平均直径逐渐增大,说明提高浸渍温度和浸渍液浓度有利于粘胶纤维模板对Zr^(4+)的吸附。ZrO_(2)纤维经过热处理后,主要是以单斜相ZrO_(2)存在。随着热处理温度的增加,ZrO_(2)纤维晶粒变大,结晶程度增加,同时纤维表面经历由光滑到小晶粒出现再到裂纹出现的转变。Viscose fiber templates(15 cm×15 cm×1 cm)were put into ZrOCl_(2) solutions of different concentrations(1,2 and 3 mol·L^(-1))and impregnated at 20,40 and 60℃for 20 h,respectively.After washing,centrifugation and drying,ZrO_(2)fiber precursors were obtained.ZrO_(2)fibers were prepared by heat treatment of the precursors at 600,800,1000 and 1200℃for 2 h.The effects of the impregnation temperature,the impregnation solution concentrations and the heat treatment temperature on the microstructure and the phase composition of the ZrO_(2) fibers were studied.The results show that with the increase of the impregnation temperature from 20℃to 60℃and the impregnation solution concentration increases from 1 mol·L^(-1)to 3 mol·L^(-1),the microstructure of fiber cross section changes from flat to cylindrical,and the average fiber diameter increases,indicating that the increase of the impregnation solution concentration and the impregnation temperature is beneficial to increasing the adsorption capacity of Zr^(4+) on viscose fiber templates.After heat treatment,ZrO_(2) fiber mainly exists in monoclinic ZrO_(2) phase.With the increase of the heat treatment temperature,the grains in ZrO_(2) fibers become larger and the crystallinity degree increases,meanwhile the fiber surface undergoes a transition from smooth to small grains and then to cracks.

关 键 词：ZrO_(2)纤维 模板浸渍法 显微形貌 直径 

分 类 号：TQ175[化学工程—硅酸盐工业]