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以碳化硅粉为主要原料、硅粉和炭黑为碳化硅自结合相粉体、AlF3·3H_2O为添加剂,采用发泡结合反应烧结法制备了碳化硅晶须自增强多孔陶瓷。研究了AlF3·3H_2O添加量(质量分数)对碳化硅晶须自增强多孔陶瓷的物相组成、显微结构和力学性能等的影响。结果表明:添加适量的AlF3·3H_2O可以促进碳化硅晶须的形成,并提高多孔陶瓷样品的强度。当AlF3·3H_2O添加量为2%时,所制备孔隙率为76.9%的碳化硅晶须自增强多孔陶瓷样品的常温抗折强度和耐压强度分别为2.6 MPa和3.7 MPa,样品中生成的SiCw晶须的长度约为4 μm,直径约为62 nm,其生长是由气–固反应机理控制。
Abstract：Introduction Silicon carbide porous ceramics are widely used in many fields because of their corrosion resistance, good thermal shock resistance, large specific surface area and superior mechanical properties. Silicon carbide porous ceramics are mainly prepared by different methods(i.e., pore-forming agent method, organic foam impregnation method, freeze–drying method, and foaming method). Among these, the foaming method with simple operation and controllable density and shape of the products is a common approach to prepare silicon carbide porous ceramics with a high porosity. However, silicon carbide porous ceramics still have the disadvantage of low mechanical properties. The In-situ generation of SiC whiskers can greatly improve the mechanical properties of the materials. Therefore, in this paper, silicon carbide whiskers self-reinforced porous ceramics were prepared by foaming method and reactive sintering with silicon carbide powder of 70%(in mass fraction) as a raw material, 30% silicon powder and carbon black as a self-bonding phase, AlF3·3H_2O as an additive. In addition, the effect of AlF3·3H_2O content on the phase composition, microstructure and mechanical properties of silicon carbide whiskers self-reinforced porous ceramics was also investigated. Methods In this work, silicon carbide powders were used as raw materials. Silicon powders and carbon black were used as self-bonding phase materials. AlF3·3H_2O was selected as an additive. Triethanolamine dodecyl sulfate was used as a blowing agent. The ground powders were slowly added to a solution containing 0.5% Isobam 104 and 0.15% sodium carboxymethylcellulose, which was vigorously stirred in a mechanical stirrer to produce a slurry containing 50%(in volume fraction) of ground powders. Subsequently, 1.0%(in volume fraction) triethanolamine dodecyl sulphate was added to the obtained slurry and then vigorously stirred to prepare a homogeneous wet foam, which was rapidly poured into moulds with the dimensions of 160 mm×80 mm×40 mm and dried at ambient temperature for 48 h. Afterwards, the demoulded foam green bodies were dried at 40–100 ℃. Finally, the dried foam green bodies were fired in argon atmosphere furnace at 1600 ℃ for 2 h to obtain porous ceramics. Results and discussion, The average large spherical pore size and annular pore size in as-prepared silicon carbide whiskers self-reinforced porous ceramics both firstly decrease and then increase with increasing the content of AlF3·3H_2O from 0 to 4%. These results are due to the minimum surface free energy of the slurry with 2% AlF3·3H_2O, leading to the stable bubbles existing in the slurry. Adding an appropriate amount of AlF3·3H_2O can promote the formation of silicon carbide whiskers and improve the strength of as-prepared silicon carbide whiskers self-reinforced porous ceramics. At AlF3·3H_2O content of 2%, the flexural and compressive strengths of porous ceramic samples with a porosity of 76.9% are 2.6 MPa and 3.7 MPa, respectively, which are significantly higher than those of the porous ceramic samples prepared without AlF3·3H_2O(i.e., 1.1 MPa and 1.4 MPa). The enhanced mechanical properties can be related to the microstructure of the porous samples. The more uniform pore distribution and smallest average spherical pores and annular pores in porous sample with AlF3·3H_2O addition of 2% are formed, resulting in improved mechanical properties of porous sample. Also, a large number of silicon carbide whiskers with the largest length are generated, which act as a reinforcing phase for further improving the mechanical properties of porous samples. Conclusions Adding an appropriate amount of AlF3·3H_2O could promote the formation of silicon carbide whiskers and improve the strength of porous ceramic specimens. At AlF3·3H_2O content of 2%, the flexural and compressive strengths of as-prepared silicon carbide whisker self-reinforced porous ceramic samples with a porosity of 76.9% were 2.6 MPa and 3.7 MPa, respectively. The length and the diameter of SiCw whiskers generated in the samples were 4 μm and 62 nm, respectively, and their growth was controlled due to the gas-solid reaction mechanism.
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基本信息:
DOI：10.14062/j.issn.0454-5648.20250103
中图分类号:TQ174.1
引用信息:
[1]时义红,曹荣,余王志,等.AlF_3·3H_2O添加量对碳化硅晶须自增强多孔陶瓷性能的影响[J].硅酸盐学报,2025,53(09):2577-2585.DOI:10.14062/j.issn.0454-5648.20250103.
基金信息:
安徽省教育厅自然科学基金项目(2023AH051130); 安徽省大学生创新创业训练计划(S202410360186,S202410360195)