摘要
针对纤维多孔陶瓷存在有机硅树脂黏结剂耐温性差,以及压力浸渍法导致样品内部纤维呈定向层状排布问题,采用正丙醇锆改性有机硅树脂制备锆硅杂化树脂黏结剂,通过抽滤法将杂化树脂与通过冷冻干燥法制备的莫来石纤维三维骨架复合,并在管式炉中高温裂解,制得莫来石纤维多孔陶瓷;采用傅里叶变换红外光谱、X射线光电子能谱、扫描电子显微镜以及X射线衍射仪对锆硅杂化树脂的结构、形貌和物相组成进行表征。通过X射线衍射仪、阿基米德排水法、万能试验机、热常数分析仪、红外热成像仪和扫描电子显微镜对莫来石纤维多孔陶瓷性能和微观结构进行表征。结果表明:与未掺锆(Zr)元素的有机硅树脂相比,Zr元素的引入使有机硅树脂的耐热性显著提高,锆硅摩尔比为1∶10的锆硅杂化树脂在1000℃氩气环境下的残余质量分数由原来的61.13%提高到77.15%;制备的莫来石纤维多孔陶瓷具有低密度(0.325~0.339 g/cm^(3))、高孔隙率(81.8%~85.2%)、低热导率(0.063~0.070 W/mK)特点;该陶瓷的抗压强度随着处理温度的升高呈先升高后降低的变化趋势,1200℃时样品的抗压强度最高为0.73 MPa;当处理温度升高至1400℃时,样品内部莫来石纤维晶粒长大,纤维强度下降。该研究可为制备结构均匀且高温热稳定性良好的莫来石纤维多孔陶瓷提供参考。
Aiming at the problems existing in fibrous porous ceramics,such as the poor temperature resistance of silicone resin binders and the directional layered arrangement of fibers inside the samples caused by the pressure impregnation method,zirconium-silicon hybrid resin binder was prepared by modifying organosilicon resin with n-propanol zirconium.The hybrid resin was combined with the three dimensional framework of mullite fiber prepared by freeze-drying method through suction filtration,and then subjected to high-temperature cracking in a tube furnace to obtain mullite fiber porous ceramics.The structure,morphology and phase composition of zirconium-silicon hybrid resin were characterized by Fourier transform infrared spectroscopy,X-ray photoelectron spectroscopy,scanning electron microscopy and X-ray diffractometer.The properties and microstructure of mullite fiber porous ceramics were characterized by X-ray diffractometer,Archimedes displacement method,universal testing machine,thermal constant analyzer,infrared thermal imager and scanning electron microscope.The results showed that compared with the silicone resin without zirconium(Zr)doping,the introduction of Zr significally improved the heat resistance of the silicone resin.Specifically,the residual mass fraction of the zirconiumsilicone hybrid resin with a zirconium-silicone ratio of 1:10 in the argon gas environment at 1,o0o C increased from the original 61.13% to 77.15%.The mullite fiber porous ceramics prepared by this method had the characteristics of low density(0.325-0.339 g/cm^(3)),high porosity(81.8%-85.2%),and low thermal conductivity(0.O63—0.O70 W/mK).The compressive strength of the ceramic first increased and then decreased with the rise in processing temperature.The sample reached its highest compressive strength of O.73 MPa at 1,200℃.When the sintering temperature rose to 1,400℃,the mullite fiber grained inside the sample grow,and the fiber strength decreased.This study can provide reference for the preparation of mullite fiber porous ceramics with uniform structure and good high-temperature thermal stability.
作者
易舒政
陈建军
YI Shuzheng;CHEN Jianjun(School of Materials Science&Engineering,Zhejiang Sci-Tech University,Hangzhou 310018,China)
出处
《浙江理工大学学报(自然科学版)》
2025年第6期786-794,共9页
Journal of Zhejiang Sci-Tech University(Natural Sciences)
基金
浙江省自然科学基金重点项目(LZ23E020003)
国家自然科学基金项目(51872262)。
关键词
锆硅杂化树脂
莫来石纤维
纤维多孔陶瓷
聚硅氧烷
隔热材料
hybrid zirconium-silicone resin
mullite fiber
fibrous porous ceramics
polysiloxane
thermal insulation material
