硅酸盐学报

成分设计对Al₂O₃-Ti₃Si（Al）C₂-C耐火材料结构与性能的影响

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辛亚楼 ¹ , 简云铃 ¹ , 尹洪峰 ¹ , 袁蝴蝶 ¹ , 汤云 ¹ , 任小虎 ¹ , 刘宇驰 ¹ , 刘国齐 ²^,³

硅酸盐学报 | 碳中和与耐火材料专题—研究论文 2025,53(9): 2559-2567

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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) : 2559 -2567

成分设计对Al₂O₃-Ti₃Si（Al）C₂-C耐火材料结构与性能的影响

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辛亚楼¹, 简云铃¹, 尹洪峰¹, 袁蝴蝶¹, 汤云¹, 任小虎¹, 刘宇驰¹, 刘国齐²^,³

作者信息

^1．西安建筑科技大学材料科学与工程学院，西安 710055

^2．中钢集团洛阳耐火材料研究院有限公司，河南洛阳 471039

^3．上海大学材料科学与工程学院，上海 200444

通讯作者:

尹洪峰（1965—），男，教授。

刘国齐（1975—），男，正高级工程师。

作者简介:

辛亚楼（1992—），男，讲师。

Effect of Composition Design on Structure and Properties of Al₂O₃-Ti₃Si(Al)C₂-C Refractories

Yalou XIN¹, Yunling JIAN¹, Hongfeng YIN¹, Hudie YUAN¹, Yun TANG¹, Xiaohu REN¹, Yuchi LIU¹, Guoqi LIU²^,³

Affiliations

^1.College of Materials Science and Engineering, Xi'an University of Architecture & Technology, Xi'an 710055, China

^2.State Key Laboratory of Advanced refractory Materials, Luoyang 471039, Henan, China

^3.School of Materials Science and Engineering, Shanghai University, Shanghai 200444, China

Corresponding Author:

YIN Hongfeng (1965-), male, Professor. E-mail: yinhf01@163.com;

LIU Guoqi (1975-), male, Senior Engineer. liuguoqi@shu.edu.cn

XIN Yalou (1992-), male, Lecturer. E-mail: xinyalou@xauat.edu.cn

出版时间: 2025-09-20 doi: 10.14062/j.issn.0454-5648.20240818

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摘要

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采用反应熔融浸渗法将硅铝合金渗透到Al₂O₃-TiC-C预制体中，经过高温反应获得了与Ti₃Si（Al）C₂结合的低碳Al₂O₃-Ti₃Si（Al）C₂-C耐火材料。研究了石墨添加量和熔渗介质对Al₂O₃-Ti₃Si（Al）C₂-C耐火材料相组成、显微结构以及性能的影响。结果表明，预制体中的石墨对合金的润湿性较差，不利于合金向预制体内部渗透，最终影响预制体中Ti₃Si（Al）C₂的原位生成。当耐火材料遭受破坏时，由于Ti₃Si（Al）C₂层状结构引发的扭结、分层等多种变形机制，可以在裂纹传播过程中消耗大量能量从而赋予材料优异的力学性能。尤其是在热震过程中，新形成的Al₂O₃和TiO₂等氧化物在耐火材料中形成致密氧化层，有助于恢复甚至增强耐火材料的强度，当预制体中不含石墨，使用Al₅₀Si₅₀合金在1500 ℃熔渗后，所制备的Al₂O₃-Ti₃Si（Al）C₂-C耐火材料的常温抗折强度为75.5 MPa，在热震后提升到110.5 MPa。

关键词

成分设计 / 铝-钛硅铝碳-碳质耐火材料 / 反应熔融浸渗法 / 力学性能 / 抗热震性

Abstract

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Introduction

Recent development on low-carbon/ultra-low carbon refractories with superior properties for the rapid development of green low-carbon economy and high-quality clean steel is a research hotspot. The structure and properties of low-carbon refractories in a variety of ways are optimized to solve the problem of deterioration of high- temperature properties caused by simple reduction of graphite content. The introduction of carbon nanomaterials can significantly reduce the overall carbon content of the material. Also, the mechanical strength and thermal shock resistance of carbon-containing refractories are improved simultaneously because the nanostructures absorb and buffer the thermal stress generated by a large number of thermal shocks. In addition, reinforcement phases such as carbides, borides and nitrides are also applied to improve the organizational structure and properties of low-carbon refractories to solve the long-standing problem of carbon source oxidation. However, the poor dispersion of nanomaterials in the matrix is a significant technical problem, and the synthesis process of composite powders is complex and challenging. High production costs and the difficulty of achieving large-scale application restrict the industrial development of these materials. The structural degradation at high temperatures leads to a decline in the strength of refractories and even deterioration of comprehensive performance, which cannot guarantee the stability of long-term service of refractories

Methods

The MAX phase materials were expected to achieve the balance between low carbonization and service performance of carbon-containing refractories due to their graphite-like layered structure, high thermal conductivity, high damage tolerance and good oxidation resistance and thermal shock resistance. In this work, in-situ Ti₃Si(Al)C₂ reaction bonded low carbon Al₂O₃-C refractory was prepared by a reactive melt infiltration method based on the preparation process of ceramic matrix composite materials. The effects of the amount of TiC/graphite in the prefabricated material and the type of Si-Al alloy as the infiltration medium on the phase composition, microstructure, physical properties, mechanical properties and thermal shock resistance of the refractories were investigated.

Results and discussion

The phase composition and performance (i.e., the apparent porosity, bulk density and flexural strength) are different at different compositions of the preforms. Corundum, Ti₃Si(Al)C₂ and TiC phases appear in all the samples, and trace amounts of SiC, TiAl_xSi_y and residual Al also occur. When the preform does not contain graphite, the content of Ti₃Si(Al)C₂ in the sample is higher, and the apparent porosity is much lower. The flexural strength of the sample increases from 9.0 MPa and 23.4 MPa to 79.4 MPa and 82.2 MPa, respectively, when the graphite removes from the raw material. Also, the bulk density of refractories is higher. This is due to the poor wettability of graphite and alloy, which prevents the infiltration of alloy melt into the preform. Graphite reacts with Si to form SiC phase and consumes Si element, which affects the growth of subsequent Ti₃Si(Al)C₂ phase. The content of titanium carbide in the raw material also affects the generation of Ti₃Si(Al)C₂, increasing the content of titanium carbide is beneficial to generating more Ti₃Si(Al)C₂, which causes a lower porosity and a higher bulk density of Al₂O₃-Ti₃Si(Al)C₂-C efractories. The overall apparent porosity of samples Al₅₀Si₅₀ and Al₉₅Si₅ is lower than that of sample Al₅Si₉₅, and the bulk density is relatively high. This is related to a fact that the presence of Al promotes the infiltration of alloy melt into the precast and is conducive to the formation of Ti₃Si(Al)C₂. The flexural strength of the sample T25@Al₅₀Si₅₀ using Al₅₀Si₅₀ alloy as a penetration medium increases from 75.5 MPa to 110.5 MPa after thermal shock. The rich toughening mechanism of Ti₃Si(Al)C₂ helps to improve the thermal shock resistance of the refractory, and the oxidation products generated after the oxidation of Ti₃Si(Al)C₂ can make the structure of the refractory more dense. The presence of whiskers in the refractory is also beneficial for better thermal shock resistance.

Conclusions

Low carbon Al₂O₃-Ti₃Si(Al)C₂-C refractory could be prepared after the preform was infiltrated with Al₅₀Si₅₀ alloy. The presence of graphite in the preform obstructed the penetration of Si-Al alloy and ultimately affected the mechanical properties of the sample. The flexural strength of the preform without graphite was up to 82.2 MPa after the infiltration reaction at 1550 ℃. The content of Al in the infiltration medium had an effect on the production of Ti₃Si(Al)C₂ in the refractory. The presence of Al was conducive to the reduction of twinning grain boundary energy between TiC grains, effectively promoting the formation of TiCx twins. Ti₃Si(Al)C₂ phase was also easy to nucleate from the TiCx twin and grow in the Ti-Si-Al liquid phase. The Ti₃Si(Al)C₂ phase consumed energy through various deformation mechanisms, thus increasing the flexural strength of the refractory material at room temperature. Also, Ti₃Si(Al)C₂ could form a continuous and dense oxide layer during the thermal shock process, effectively preventing the Ti₃Si(Al)C₂ inside the sample from being further oxidized. The formation of the dense layer could restore or even strengthen the mechanical properties of the refractory after thermal shock. The flexural strength of sample T25@Al₅₀Si₅₀ increased from 75.5 MPa to 110.5 MPa after thermal shock.

Key words

composition design / alumina-titanium silicon aluminum carbon-carbon refractory / reactive melt infiltration method / mechanical properties / thermal shock resistance

引用本文

辛亚楼, 简云铃, 尹洪峰, 袁蝴蝶, 汤云, 任小虎, 刘宇驰, 刘国齐. 成分设计对Al₂O₃-Ti₃Si（Al）C₂-C耐火材料结构与性能的影响. 硅酸盐学报, 2025 , 53 (9) : 2559 -2567 . DOI: 10.14062/j.issn.0454-5648.20240818

Yalou XIN, Yunling JIAN, Hongfeng YIN, Hudie YUAN, Yun TANG, Xiaohu REN, Yuchi LIU, Guoqi LIU. Effect of Composition Design on Structure and Properties of Al₂O₃-Ti₃Si(Al)C₂-C Refractories[J]. Journal of the Chinese Ceramic Society, 2025 , 53 (9) : 2559 -2567 . DOI: 10.14062/j.issn.0454-5648.20240818

基金

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陕西省自然科学基础研究计划(2024JC-YBQN-0593)
先进耐火材料国家重点实验室开放课题(SKLAR202301)

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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.0454-5648.20240818

接收时间：2024-12-24
首发时间：2026-10-21
出版时间：2025-09-20

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出版历史

收稿日期：2024-12-24
修回日期：2025-01-23

基金

陕西省自然科学基础研究计划(2024JC-YBQN-0593)

先进耐火材料国家重点实验室开放课题(SKLAR202301)

作者信息

^1．西安建筑科技大学材料科学与工程学院，西安 710055

^2．中钢集团洛阳耐火材料研究院有限公司，河南洛阳 471039

^3．上海大学材料科学与工程学院，上海 200444

通讯作者:

尹洪峰（1965—），男，教授。

刘国齐（1975—），男，正高级工程师。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20240818

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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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