硅酸盐学报

AlF₃·3H₂O添加量对碳化硅晶须自增强多孔陶瓷性能的影响

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时义红 ¹ , 曹荣 ¹ , 余王志 ¹ , 邓先功 ¹ , 刘翔 ¹ , 陈玥 ¹ , 丁祥 ¹ , 葛雪祥 ¹ , 张毅 ¹ , 冉松林 ¹ , 张海军 ²

硅酸盐学报 | 碳中和与耐火材料专题—研究论文 2025,53(9): 2577-2585

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硅酸盐学报 |碳中和与耐火材料专题—研究论文 2025 , 53 (9) : 2577 -2585

AlF₃·3H₂O添加量对碳化硅晶须自增强多孔陶瓷性能的影响

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时义红¹, 曹荣¹, 余王志¹, 邓先功¹, 刘翔¹, 陈玥¹, 丁祥¹, 葛雪祥¹, 张毅¹, 冉松林¹, 张海军²

作者信息

^1．安徽工业大学材料科学与工程学院先进陶瓷研究中心，安徽马鞍山 243002

^2．武汉科技大学省部共建耐火材料与冶金国家重点实验室，武汉 430081

通讯作者:

邓先功（1980—），男，博士，讲师。

作者简介:

时义红（2000—），男，硕士。

Effect of AlF₃·3H₂O Content on Properties of Silicon Carbide Whiskers Self-Reinforced Porous Ceramics

Yihong SHI¹, Rong CAO¹, Wangzhi YU¹, Xiangong DENG¹, Xiang LIU¹, Yue CHEN¹, Xiang DING¹, Xuexiang GE¹, Yi ZHANG¹, Songlin RAN¹, Haijun ZHANG²

Affiliations

^1.Advanced Ceramics Research Center, School of Materials Science and Engineering, Anhui University of Technology, Ma'anshan 243002, Anhui, China

^2.The State Key Laboratory of Refractories and Metallurgy, Wuhan University of Science and Technology, Wuhan 430081, China

Corresponding Author:

DENG Xiangong (1980-), male, Ph.D., Lecturer. E-mail: dengxg@ahut.edu.cn

SHI Yihong (2000-), male, Master. E-mail: 965271340@qq.com

出版时间: 2025-09-20 doi: 10.14062/j.issn.0454-5648.20250103

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摘要

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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、AlF₃·3H₂O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AlF₃·3H₂O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AlF₃·3H₂O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AlF₃·3H₂O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SiC_w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。

关键词

碳化硅多孔陶瓷 / 碳化硅晶须 / 三水氟化铝 / 力学性能

Abstract

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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, AlF₃·3H₂O as an additive. In addition, the effect of AlF₃·3H₂O 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. AlF₃·3H₂O 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 AlF₃·3H₂O from 0 to 4%. These results are due to the minimum surface free energy of the slurry with 2% AlF₃·3H₂O, leading to the stable bubbles existing in the slurry. Adding an appropriate amount of AlF₃·3H₂O can promote the formation of silicon carbide whiskers and improve the strength of as-prepared silicon carbide whiskers self-reinforced porous ceramics. At AlF₃·3H₂O 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 AlF₃·3H₂O (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 AlF₃·3H₂O 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 AlF₃·3H₂O could promote the formation of silicon carbide whiskers and improve the strength of porous ceramic specimens. At AlF₃·3H₂O 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 SiC_w whiskers generated in the samples were 4 μm and 62 nm, respectively, and their growth was controlled due to the gas-solid reaction mechanism.

Key words

silicon carbide porous ceramics / silicon carbide whiskers / aluminum fluoride trihydrate / mechanical properties

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时义红, 曹荣, 余王志, 邓先功, 刘翔, 陈玥, 丁祥, 葛雪祥, 张毅, 冉松林, 张海军. AlF₃·3H₂O添加量对碳化硅晶须自增强多孔陶瓷性能的影响. 硅酸盐学报, 2025 , 53 (9) : 2577 -2585 . DOI: 10.14062/j.issn.0454-5648.20250103

Yihong SHI, Rong CAO, Wangzhi YU, Xiangong DENG, Xiang LIU, Yue CHEN, Xiang DING, Xuexiang GE, Yi ZHANG, Songlin RAN, Haijun ZHANG. Effect of AlF₃·3H₂O Content on Properties of Silicon Carbide Whiskers Self-Reinforced Porous Ceramics[J]. Journal of the Chinese Ceramic Society, 2025 , 53 (9) : 2577 -2585 . DOI: 10.14062/j.issn.0454-5648.20250103

基金

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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)

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2025年第53卷第9期

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文章信息

doi: 10.14062/j.issn.0454-5648.20250103

接收时间：2025-02-18
首发时间：2026-10-21
出版时间：2025-09-20

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收稿日期：2025-02-18
修回日期：2025-03-15

基金

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)

作者信息

^1．安徽工业大学材料科学与工程学院先进陶瓷研究中心，安徽马鞍山 243002

^2．武汉科技大学省部共建耐火材料与冶金国家重点实验室，武汉 430081

通讯作者:

邓先功（1980—），男，博士，讲师。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20250103

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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