Mo<sub>2</sub>C-TiN<sub>0.3</sub>复合材料的高温高压制备及性能

邹芹; 王宽; 李艳国; 戴伟绩; 罗永安

doi:10.13394/j.cnki.jgszz.2023.0157

Mo₂C-TiN_0.3复合材料的高温高压制备及性能

doi: 10.13394/j.cnki.jgszz.2023.0157

邹芹^{1, 2,},
王宽¹,
李艳国^1, ,,
戴伟绩²,
罗永安¹

1.
燕山大学机械工程学院, 河北秦皇岛066004
2.
燕山大学亚稳材料制备技术与科学国家重点实验室, 河北秦皇岛066004

基金项目: 河北省高校科研重点项目（ZD2021099）。

详细信息

作者简介:
邹芹，女，1978年生，教授、博士生导师。主要研究方向：超硬工具。E-mail：zq@ysu.edu.cn

通讯作者:
李艳国，男，1978年生，副研究员、硕士生导师。主要研究方向：陶瓷及其复合材料。E-mail：lyg@ysu.edu.cn

中图分类号: TB332
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- 被引次数: 0
出版历程
- 收稿日期: 2023-08-03
- 修回日期: 2023-10-27
- 录用日期: 2023-11-22
- 网络出版日期: 2024-09-25
- 刊出日期: 2024-08-20

Preparation and properties of Mo₂C-TiN_0.3 composite materials at high temperature and high pressure

ZOU Qin^{1, 2
,},
WANG Kuan¹,
LI Yanguo^{1
, ,},
DAI Weiji²,
LUO Yongan¹

1.
School of Mechanical Engineering, Yanshan University, Qinhuangdao 066004, Hebei, China
2.
State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004, Hebei, China

摘要

摘要: 将Mo₂C和TiN_0.3粉体采用机械合金化和高温高压烧结相结合的方法进行分层烧结，并制备30% Mo₂C-70%TiN_0.3的烧结体复合材料，分析Mo₂C-TiN_0.3烧结体的物相组成、微观组织结构及力学性能。结果表明：Mo₂C和TiN_0.3 间存在明显的相互扩散，且形成了2层不同的扩散层；随着烧结温度不断升高，Mo₂C-TiN_0.3烧结体的晶粒尺寸逐渐变大，会导致烧结体的机械性能变差；在烧结过程中有高硬高脆的MoC生成，能够维持Mo₂C-TiN_0.3烧结体的硬度在19.0～20.0 GPa，但会降低其断裂韧性。
- TiN_0.3 /
- Mo₂C /
- 扩散 /
- 高温高压烧结 /
- 机械合金化
Abstract: Objectives: This study aims to prepare sintered bodies of Mo₂C and TiN_0.3 and explore their phase compositions, microstructures, and mechanical properties. Using a combined approach of mechanical alloying and high-temperature high-pressure sintering, the research investigates the stratified sintering process of Mo₂C and TiN_0.3 powders, analyzes the influence of different sintering temperatures on the sintered body performances, and aims to optimize the preparation process to enhance the comprehensive properties of the sintered bodies. Methods: This experiment employed a combination of mechanical alloying and high-temperature high-pressure sintering to prepare the sintered bodies. Initially, Mo₂C and TiN_0.3 powders were mechanically alloyed in a 7:3 volume ratio. The powders were thoroughly mixed using a high-energy ball mill to ensure uniform mixing. Subsequently, the mixed powders were subjected to high-temperature and high-pressure sintering using a six-sided top press under various temperature conditions to obtain sintered bodies with different sintering parameters. During the sintering process, the temperature and pressure were strictly controlled to study their effects on the microstructure and mechanical properties of the sintered bodies. The phase composition of the sintered bodies was analyzed using X-ray diffraction (XRD) to identify the presence and changes of various phases. The microstructure of the sintered bodies was observed using a scanning electron microscope (SEM) to analyze the grain size and morphology. To evaluate the mechanical properties of the sintered bodies, Vickers hardness tests and fracture toughness tests were conducted. These test methods were used to comprehensively analyze the overall performance of Mo₂C and TiN_0.3 sintered bodies under different sintering conditions. Results: The experimental results indicate significant mutual diffusion between Mo₂C and TiN_0.3 during the sintering process, forming two distinct diffusion layers. The formation of these diffusion layers markedly affects the phase composition and microstructure of the sintered body. As the sintering temperature increases, the grain size of the Mo₂C-TiN_0.3 sintered body gradually enlarges, leading to a deterioration in mechanical properties. Specifically, at lower sintering temperatures, the sintered body exhibits higher hardness, but as the temperature rises, the grain size increases, resulting in decreased hardness. Additionally, the formation of a highly hard and brittle MoC phase was detected during high-temperature sintering. In addition, MoC phase formation with high hardness and brittleness was detected during high temperature sintering. The presence of the MoC phase helps maintain the hardness of the sintered body within the range of 19.0 to 20.0 GPa, but also leads to a reduction in fracture toughness. The microstructure of the sintered body varies significantly with different sintering temperatures. Under low-temperature sintering conditions, the grains of the sintered body are small and evenly distributed, and the phase composition is relatively stable. However, with the increase of sintering temperature, the grains gradually grow, and the phase distribution becomes uneven, which leads to a decline in the mechanical properties of the sintered body. Furthermore, SEM analysis reveals the presence of numerous pores and cracks on the surface of the high-temperature sintered body, which are crucial factors affecting its mechanical performance. Conclusions: Through the study of 30% Mo₂C-TiN_0.3 sintered bodies, it is found that: (1) The mutual diffusion between Mo₂C and TiN_0.3 plays a crucial role in the formation of the sintered body, directly impacting its phase composition and microstructure. (2) As the sintering temperature increases, the grain size of the sintered body enlarges, leading to a decline in its mechanical properties, particularly in its hardness and fracture toughness. (3) The MoC phase generated in the sintering process helps to maintain the high hardness of the sintered body, but also reduces fracture toughness. Therefore, in practical applications, it is necessary to find a balance between hardness and toughness to optimize the overall performance of the sintered body. (4) Different sintering temperatures significantly affect the microstructure of the sintered body, highlighting the importance of optimizing sintering process parameters to enhance the performance of the sintered body. Others: The mechanical alloying and high-temperature and high-pressure sintering methods used in this study demonstrate the potential for producing high-performance Mo₂C and TiN_0.3 sintered bodies. By optimizing sintering process parameters, the performance of the sintered bodies can be further enhanced. Furthermore, future research could explore the effects of other additives on the performance of Mo₂C-TiN_0.3 sintered bodies to obtain higher performance hard and brittle materials.
- TiN_0.3 /
- Mo₂C /
- diffusion /
- high-temperature high-pressure sintering /
- mechanical alloying(MA)

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图 1 维氏硬度的压痕及裂纹图

Figure 1. Indentation and crack diagram of Vickers hardness

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图 2 TiN_0.3与Mo₂C分层烧结的SEM图和EDS线扫描图

Figure 2. SEM and EDS line scan of layered sintering of TiN_0.3 and Mo₂C

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图 3 不同温度下Mo₂C-TiN_0.3复合烧结体的XRD图谱

Figure 3. XRD pattern of Mo₂C-TiN_0.3 composite sintered body at different temperatures

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图 4 不同烧结温度下Mo₂C-TiN_0.3复合烧结体的断口SEM形貌

Figure 4. SEM fracture morphology of Mo₂C-TiN_0.3 composite sintered body at different sintering temperatures

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图 5 不同烧结温度下Mo₂C-TiN_0.3复合烧结体的力学性能

Figure 5. Mechanical properties of Mo₂C-TiN_0.3 composite sintered body at different sintering temperatures

下载: 全尺寸图片幻灯片

表 1 TiN_0.3制备原料

Table 1. TiN_0.3 preparation raw materials

构成	取值
Ti∶CH₄N₂O 摩尔比 R₁	6∶1
Ti∶N 原子比 R₂	3∶1
Ti 质量 m₁ / g	33.08
CH₄N₂O质量 m₂ / g	6.92

下载: 导出CSV

表 2 1 500 ℃下Mo₂C-TiN_0.3复合烧结体断口的点能谱分析结果

Table 2. Point energy spectrum analysis results of Mo₂C-TiN_0.3 composite sintered body at 1 500 ℃

位置	质量分数 ω / %
位置	Ti	N	C	Mo
Point 1	3.64	1.62	51.29	43.45
Point 2	28.56	50.94	11.22	9.28

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表 3 TiN基陶瓷的机械性能对比

Table 3. Comparison of mechanical properties of TiN based ceramics

性能			来源
	Mo₂C-TiN_0.3	TiN-TiB₂	TiN-HfC	TiN-Al₂O₃	未增强 TiN基陶瓷
	本实验	文献[21]	文献[35]	文献[36]	文献[34]
维氏硬度 H_v / GPa	19.9	14.8	17.9	18.9	12.5
断裂韧性 K_IC / (MPa·m^1/2)	3.2	5.8	5.2	4.5	3.4

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