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氧化锆基陶瓷纤维和纤维板的制备及性能研究

发布时间:2018-11-16 18:54
【摘要】:本文采用溶胶-凝胶法以氧化钇为稳定剂,通过乙酸与碱式碳酸锆反应,制备出了乙酸聚锆前驱体溶胶和氧化锆前驱体凝胶纤维。通过研究加入H+/Zr4+的比例可知,当加入的比例为1.8~1.9时,可以得到稳定性较好并具有可纺性的溶胶,通过粘度测试确定最佳的甩丝粘度为20~30Pa-S;采用FT-IR和TG-DTA测试分析,推断出前驱体凝胶纤维中存在乙酸聚锆的链式结构,并以此为根据制定出了合理的热处理制度。采用XRD、 SEM等测试手段对不同煅烧温度得到的TZP陶瓷纤维和10wt%氧化铝掺杂的AL2O3-3Y-TZP陶瓷纤维的纤维直径、晶粒大小以及纤维强度进行了研究,结果发现纤维直径大约为10~12μm,晶粒大小大约为80~300nm,同时表明Al2O3的加入有抑制ZrO2晶粒长大的作用,可增加其纤维的抗拉强度,并且最大抗拉强度可以达到1.2GPa。采用湿法成型制备氧化锆基陶瓷纤维板,研究采用真空吸滤和加压整平的工艺方法,将自制的Al2O3-3Y-TZP陶瓷连续纤维切成短纤维后加入成型剂,通过施加不同压力制备出密度不同的纤维板湿坯,再经烘干和1600℃高温煅烧得到厚度均匀、表面平整的陶瓷纤维板。研究陶瓷纤维板1600℃下重烧的热线收缩,厚度方向永久线收缩较大,大约为10~12%,长度方向和宽度方向较小,大约为2~4%;陶瓷纤维板的抗弯强度和抗压强度随密度升高而提高,当密度达到0.55g/cm3时,抗弯强度可以达到2.386MPa,抗压强度可以达到0.353MPa。通过测试不同密度陶瓷纤维板1000℃下的导热系数,发现当纤维板密度较低孔隙率较大时,热对流占主导地位,此时随孔隙率增大,导热系数增大;当密度增大孔隙率降低时,热传导占主导地位,此时随密度增大,导热系数增大;.最佳的密度范围为0.4-0.8g/cm3。此时1000℃下的陶瓷纤维板导热系数最低,大约为0.20~0.25W/m·K。通过添加不同比例的Al2O3-3Y-TZP陶瓷短纤维到氧化锆泡沫陶瓷中,发现添加的纤维含量越高,其泡沫陶瓷的抗弯强度也越高;当添加的短纤维含量为30wt%时,抗弯强度为37.95MPa。
[Abstract]:In this paper, polyzirconium acetate precursor sol and zirconia precursor gel fiber were prepared by using yttrium oxide as stabilizer and acetic acid reacted with basic zirconium carbonate by sol-gel method. By studying the ratio of H / Zr4, the sol with good stability and spinnability can be obtained when the proportion of H / Zr4 is 1.8-1.9, and the optimum viscosity of the spun wire is 20 ~ 30Pa-S by viscosity test. The chain structure of polyzirconium acetate in the precursor gel fiber was inferred by means of FT-IR and TG-DTA, and a reasonable heat treatment system was worked out on the basis of it. The diameter, grain size and strength of TZP ceramic fibers and AL2O3-3Y-TZP ceramic fibers doped with 10 wt% alumina at different calcination temperatures were studied by means of XRD, SEM. The results show that the diameter of the fiber is about 10 ~ 12 渭 m and the grain size is about 80 ~ 300 nm. It is also shown that the addition of Al2O3 can inhibit the growth of ZrO2 grain and increase the tensile strength of the fiber, and the maximum tensile strength can reach 1.2 GPA. Zirconia based ceramic fiberboard was prepared by wet molding. Vacuum filtration and pressure leveling were used to cut the Al2O3-3Y-TZP ceramic continuous fiber into short fibers and then to add molding agent. The wetted board with different density and density was prepared by applying different pressure. Then the ceramic fiberboard with uniform thickness and flat surface was obtained by drying and calcining at 1600 鈩,

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