模板浸渍法制备ZrO2纤维研究

doi:10.3969/j.issn.1001-1935.2022.02.002

耐火材料 ›› 2022, Vol. 56 ›› Issue (2): 101-106.DOI: 10.3969/j.issn.1001-1935.2022.02.002

模板浸渍法制备ZrO₂纤维研究

张雷(), 闫森旺, 李虹屿, 孙小飞(), 王刚, 张一帆, 王守业

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

收稿日期:2021-08-17 出版日期:2022-04-15 发布日期:2022-04-21
通讯作者: 孙小飞,男,1981年生,博士,教授级高级工程师。E-mail: sunxiaofei0217@163.com
作者简介:张雷:男,1994年生,硕士研究生。E-mail: 937268721@qq.com
基金资助:
国家重点研发计划资助项目(2018YFB0605904)

Preparation of ZrO₂ fibers by template impregnation method

Zhang Lei(), Yan Senwang, Li Hongyu, Sun Xiao-fei(), Wang Gang, Zhang Yifan, Wang Shouye

State Key Laboratory of Advanced Refractories,Sinosteel Luoyang Institute of Refractories Research Co.,Ltd.,Luoyang 471039,Henan,China

Received:2021-08-17 Online:2022-04-15 Published:2022-04-21
Contact: Sun Xiao-fei

摘要/Abstract

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ZrOCl₂溶液,分别在20、40、60 ℃下浸渍20 h,经过洗涤、离心、干燥得到ZrO₂纤维前驱体,再对前驱体进行600、800、1 000、1 200 ℃保温 2 h热处理制得ZrO₂纤维。研究浸渍温度、浸渍液浓度、热处理温度对ZrO₂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Zr⁴⁺的吸附。ZrO₂纤维经过热处理后,主要是以单斜相ZrO₂存在。随着热处理温度的增加,ZrO₂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。

关键词: ZrO₂纤维, 模板浸渍法, 显微形貌, 直径

Abstract:

Viscose fiber templates (15 cm×15 cm×1 cm) were put into ZrOCl₂ 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,ZrO₂ fiber precursors were obtained.ZrO₂ fibers were prepared by heat treatment of the precursors at 600,800,1 000 and 1 200 ℃ 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 ZrO₂ 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 Zr⁴⁺ on viscose fiber templates.After heat treatment,ZrO₂ fiber mainly exists in monoclinic ZrO₂ phase.With the increase of the heat treatment temperature,the grains in ZrO₂ fibers become larger and the crystallinity degree increases,meanwhile the fiber surface undergoes a transition from smooth to small grains and then to cracks.

Key words: zirconia fiber, template impregnation method, micro-morphology, diameter

中图分类号:

TQ175

张雷, 闫森旺, 李虹屿, 孙小飞, 王刚, 张一帆, 王守业. 模板浸渍法制备ZrO₂纤维研究[J]. 耐火材料, 2022, 56(2): 101-106.

Zhang Lei, Yan Senwang, Li Hongyu, Sun Xiao-fei, Wang Gang, Zhang Yifan, Wang Shouye. Preparation of ZrO₂ fibers by template impregnation method[J]. Refractories, 2022, 56(2): 101-106.

图/表 6

图1 不同浸渍温度制备的ZrO2纤维的SEM照片

Fig.1 SEM images of ZrO2 fibers prepared at different impregnation temperatures

图2 不同浸渍温度制备的ZrO2纤维直径频率分布的直方图

Fig.2 Histogram of the frequency distribution of diameter of ZrO2 fibers prepared at different impregnation temperatures

图3 采用不同浓度浸渍液制备的ZrO2纤维的SEM照片

Fig.3 SEM images of ZrO2 fibers prepared with different impregnation solution concentrations

图4 采用不同浓度浸渍液制备的ZrO2纤维直径频率分布的直方图

Fig.4 Histogram of frequency distribution of diameter of ZrO2 fibers prepared at different impregnation solution concentrations

图5 不同温度热处理后ZrO2纤维的XRD图谱

Fig.5 XRD patterns of ZrO2 fibers heat treated at different temperatures

图6 不同温度热处理后的ZrO2纤维的SEM照片

Fig.6 SEM images of ZrO2 fibers heat treated at different temperatures

参考文献 15

[1]	陈代荣, 韩伟健, 李思维, 等. 现代技术陶瓷[J]. 2018, 39(3):195-196.
[2]	刘贵双. 氧化锆纤维及纤维板的制备与性能研究[D]. 南京: 南京理工大学, 2012.
[3]	朱玉龙. 氧化锆基陶瓷纤维和纤维板的制备及性能研究[D]. 南京: 南京理工大学, 2015.
[4]	孙亚娟. 溶胶法连续氧化锆纤维制备工艺研究[D]. 北京: 中国科学院大学, 2018.
[5]	DAS R N, NAD S, PRAMANIK P. Nanocrystalline yttria-stabilized zirconia fibers from plant fibers and their polymer composites[J]. Journal of the American Ceramic Society, 2008, 91(3):1034-1036. DOI URL
[6]	贾光耀. 氧化锆纤维隔膜及其制备方法:CN101029451[P]. 2007-09-05.
[7]	HARTRIDGE A, TAYLOR M D, BHATTACHARYA A K. Synthesis and characterization of partially and fully stabilized zirconia fibers made from an inorganic precursor[J]. Journal of materials research, 2001, 16(8):2384-2390. DOI URL
[8]	LI L P, ZHANG P G, LIANG J D, et al. Phase transformation and morphological evolution of electrospun zirconia nanofibers during thermal annealing[J]. Ceramics International, 2010, 36(2):589-594. DOI URL
[9]	SUN G X, DU X Y, ZHANG M X, et al. Fabrication of zirconia fibers by a sol-gel combined rotational centrifugal spinning technique[J]. Transactions of the Indian Ceramic Society, 2014, 73(3):228-232. DOI URL
[10]	LIU H Y, CHEN Y, LIN G S, et al. Preparation of high-quality zirconia fibers by super-high rotational centrifugal spinning of inorganic sol[J]. Advanced Manufacturing Processes, 2013, 28(2):133-138.
[11]	孙国勋. 溶胶纺丝法制备氧化锆纤维[D]. 济南: 济南大学, 2014.
[12]	刘贵双, 刘和义, 裴石光, 等. 热处理气氛对制备氧化锆连续纤维的影响[J]. 材料导报, 2011, 25(24):15-19.
[13]	徐培珮, 徐建峰, 关克田. ZrO₂纤维隔热板的制备[J]. 耐火材料, 2015, 49(3):175-177.
[14]	尹衍升, 陈守刚, 刘英才. 氧化锆陶瓷的掺杂稳定及生长动力学[M]. 北京: 化学工业出版社, 2004:1-2.
[15]	LIN Y C, GAN D, SHEN P, et al. Phase transformation of ZrO₂ in MnZn-ferrite under magnetic field[J]. Journal of the American Ceramic Society, 1996, 79(2):559-561. DOI URL

模板浸渍法制备ZrO₂纤维研究

Preparation of ZrO₂ fibers by template impregnation method

RichHTML

PDF

可视化

摘要/Abstract

引用本文

使用本文

图/表 6

参考文献 15

相关文章 1

编辑推荐

Metrics

本文评价