多孔碳化硅(SiC)陶瓷兼备碳化硅材料和多孔陶瓷材料的优点,比重小、高温强度高、抗氧化性强、耐腐蚀性强,是近年来多孔陶瓷领域的研究热点。本文以包混工艺为基础,选取金属硅粉为硅源、钡酚醛树脂为炭源、碳化硅晶须(SiCw)为增强体、Al2O3、SiO2和Y2O3为烧结助剂,经过先驱体粉体制备、复合添加、成型、炭化、烧结和脱炭等工序制备出多孔SiCw/SiC陶瓷材料;研究了SiCw添加工艺和添加量对样品物相组成、抗弯强度、热膨胀系数和抗热震性等性能的影响。论文的主要内容和结论如下:(1)采用湿法添加SiCw工艺制备了一组梯度SiCw浓度的多孔SiCw/SiC陶瓷材料样品(W系,wet group)并测试了其综合性能。结果表明:W系多孔SiCw/SiC陶瓷样品的物相为较纯的β-SiC;材料的抗弯强度随SiCw相对浓度的提高先增大后减小;SiCw的添加对样品的孔隙率影响不大,平均孔径随SiCw添加量的增大先增大后减小;SiCw的添加对样品的热膨胀系数影响不大,但抗热震性在SiCw含量大时下降明显。(2)研究发现:W系样品中部分SiCw与骨架结合,通过载荷转移等机理对基体产生增强作用;部分SiCw穿插在孔隙中形成了新的孔结构;碳硅比随SiCw的添加发生变化,导致SiCw浓度高时抗弯强度和抗热震性不高。(3)采用干法添加SiCw工艺制备了一组梯度SiCw浓度的多孔SiCw/SiC陶瓷材料样品(D系,dry group)并测试了其综合性能。结果表明:D系多孔SiCw/SiC陶瓷样品的物相为较纯的β-SiC;SiCw的添加对样品增强作用明显,抗弯强度随SiCw添加量的增大单调提高;SiCw的添加对孔隙率和平均孔径影响不大,骨架密度随SiCw添加量的增大略有上升;样品的热膨胀系数、抗热震性受SiCw添加的影响不大。(4)研究发现:D系样品中SiCw主要作用于骨架结构,通过裂纹桥联、裂纹偏转、晶须拔出等机制对基体产生增强作用,而对孔隙性质影响较小;采用干法工艺添加SiCw不影响碳硅比,制备出的样品综合性能良好。(5)对比W系和D系多孔SiCw/SiC陶瓷样品的综合性能,发现干法工艺能在有效增强材料的同时更好地保持基体的高温性能,是一种更具优势的添加工艺。(6)设计了一种以多孔SiCw/SiC陶瓷材料为滤芯的柴油机尾气颗粒捕集器模拟装置。滤芯材料炭化后径向尺寸收缩率为3.254±0.436%,失重率为12.283±0.104%;烧结后径向尺寸收缩率率0.639±0.435%,失重率为24.076±4.113%;气体渗透率为10.50×10-10m2,基本可以达到柴油机尾气过滤器滤芯材料对该项指标的要求。
Porous silicon carbide (SiC) is a perfect blend of porous ceramics and silicon carbide material, possessing advantages of the two, such as low density, outstanding high-temperature strength, considerable antioxidation stability and corrosion resistance. Attempting for a step forward, the trial of strengthening porous SiC ceramics with silicon carbide whiskers (SiCw) through coat-mix method was practiced, with silicon powder as silicon (Si) donator, barium phenolic resin as carbon (C) donator and the composite of Al2O3, SiO2 and Y2O3 as additives. The route consists of preparation of core-shell structure precursor powder, addictives mixing, molding, carbonization, sintering and carbon removing, and porous SiCw/SiC compound was produced successfully, whose overall properties, including chemical composition, bending strength, thermal expansion coefficient and thermal shock resistance were tested. Effects of introducing SiCw through “dry method” and “wet method” was studied respectively and the effects of addictive amount on final products were analyzed. The study could be generally described as follows:(1) A set of porous SiCw/SiC ceramic examples were produced through coat-mix method in way of introducing SiCw in the liquid state, which was marked “W group”, and their overall properties were tested. Results show that the examples were consisted of pure β-SiC; the matrix was enhanced by SiCw in certain concentration interval, but the enhancement drops with further raise in relative SiCw content; the introducing of SiCw has not evident influence on porosity, while the average pore diameter first rises then falls with the increase of SiCw adding amount; thermal coefficient was not sensitive to the introducing of SiCw, while the thermal shock resistance showed a setback when large amount of SiCw was added. (2) For the W group examples, it is indicated that part of SiCw combines with the skeleton and the other exists in interspaces creating smaller pores, depending on which structure the matrix was strengthened and the average pore diameter was decreased. Because the silicon to carbon ratio rises with the addition of SiCw, negative effects cannot be neglected.(3) A set of porous SiCw/SiC ceramic examples were produced through coat-mix method in way of introducing SiCw in the dry state, which was marked “D group”, and their overall properties were tested. Results show that the examples were consisted of pure β-SiC; the matrix was enhanced by SiCw significantly; the introducing of SiCw has not evident influence on porosity and average pore diameter, while the density of skeleton rise with the increase of SiCw amount; high-temperature properties, represented by thermal coefficient and thermal shock resistance, was not sensitive to the introducing of SiCw. (4) For the D group examples, it is indicated that SiCw combines mainly with the skeleton and reinforces the composite in accordance with some toughening mechanism such as whisker bridge, whisker rupture and whisker pull out.(5) Compared to W group examples, those of D group showed a monotonous increase in bending strength and a maintenance in aspects like pore properties and high-temperature properties, so the dry adding method is recommended as a better choice.(6) A simulator of diesel particulate filter was designed and a set of experimental facility was assembled with commercial widgets and porous SiCw/SiC ceramic produced through coat-mix method. The filter cartridge has a radial dimension shrinkage of 3.254±0.436% and a weight loss rate of 12.283±0.104% in carbonization and a radial dimension shrinkage of 0.639±0.435% and a weight loss rate of 24.076±4.113% in sintering,the permeability of the cartridge is 10.50×10-10m2. The basic properties finely meet the requirements for usage as filter cartridge.