自蔓延高温合成氮化硅多孔陶瓷的研究进展

doi:10.15541/jim20220019

无机材料学报 ›› 2022, Vol. 37 ›› Issue (8): 853-864.DOI: 10.15541/jim20220019

所属专题：【结构材料】超高温结构陶瓷

自蔓延高温合成氮化硅多孔陶瓷的研究进展

张叶¹^,²(), 曾宇平¹()

1.中国科学院上海硅酸盐研究所高性能陶瓷和超微结构国家重点实验室, 上海 200050
2.中国科学院大学材料科学与光电工程中心, 北京 100049

收稿日期:2022-01-13 修回日期:2022-04-12 出版日期:2022-08-20 网络出版日期:2022-04-26
通讯作者: 曾宇平, 研究员. E-mail: yuping-zeng@mail.sic.ac.cn
作者简介:张叶(1994-),男,博士研究生. E-mail: zhangyezn@student.sic.ac.cn
基金资助:
中国科学院重点部署项目(ZDRW-CN-2019-3);国家自然科学基金青年项目(51902327)

Progress of Porous Silicon Nitride Ceramics Prepared via Self-propagating High Temperature Synthesis

ZHANG Ye¹^,²(), ZENG Yuping¹()

1. State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
2. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2022-01-13 Revised:2022-04-12 Published:2022-08-20 Online:2022-04-26
Contact: ZENG Yuping, professor. E-mail: yuping-zeng@mail.sic.ac.cn
About author:ZHANG Ye (1994-), male, PhD candidate. E-mail: zhangyezn@student.sic.ac.cn
Supported by:
Key Project of CAS(ZDRW-CN-2019-3);National Natural Science Foundation of China(51902327)

摘要/Abstract

摘要：

多孔氮化硅陶瓷兼具有高气孔率和陶瓷的优异性能, 在吸声减震、过滤等领域具有非常广泛的应用。然而, 目前常规的制备方法如气压/常压烧结、反应烧结-重烧结以及碳热还原烧结存在烧结时间长、能耗高、设备要求高等不足, 导致多孔Si₃N₄陶瓷的制备成本居高不下。因此, 探索新的快速、低成本的制备方法具有重要意义。近年来, 采用自蔓延高温合成法直接制备多孔氮化硅陶瓷展现出巨大潜力, 其可以利用Si粉氮化的剧烈放热同时完成多孔氮化硅陶瓷的烧结。本文综述了自蔓延反应的引发以及所制备多孔氮化硅陶瓷的微观形貌、力学性能和可靠性。通过组分设计和工艺优化, 可以制备得到氮化完全、晶粒发育良好、力学性能与可靠性优异的多孔氮化硅陶瓷。此外还综述了自蔓延合成多孔Si₃N₄陶瓷晶界相性质与高温力学性能之间的关系, 最后展望了自蔓延高温合成多孔Si₃N₄陶瓷的发展方向。

关键词: 自蔓延高温合成, 氮化硅, 微观形貌, 力学性能, 综述

Abstract:

Porous silicon nitride (Si₃N₄) ceramics can be widely used in various fields, such as sound and shock absorption, filtration and so on, due to its high porosity and outstanding properties of ceramics. However, conventional preparation methods, such as gas-pressure/pressureless sintering, sintering reaction-bonded sintering and carbothermal reduction sintering, perform long sintering time, high energy consumption and high equipment requirements, which makes the preparation of porous Si₃N₄ ceramics expensive. Therefore, it is of great importance to explore a rapid and low-cost preparation method. In recent years, the direct preparation of porous Si₃N₄ ceramics by self-propagating high temperature synthesis (SHS) has showed great potential of which the heat released from the nitridation of Si powder could be used for the in-situ sintering of porous Si₃N₄ ceramics. In present paper, researches relating to the initiation of the SHS reaction, and microstructural evolution, mechanical properties, and reliability of the fabricated Si₃N₄ ceramics are summerized systematically. Porous Si₃N₄ ceramics with complete nitridation, excellent grain morphology and outstanding mechanical properties and reliability are obtained by adjusting raw materials and process parameters. Furthermore, the relationship between properties of grain boundary phase and high-temperature mechanical properties of SHS-fabricated porous Si₃N₄ ceramics is reviewed. Finally, the development direction of the self-propagating high temperature synthesis of porous Si₃N₄ ceramics is prospected.

Key words: self-propagating high-temperature synthesis, silicon nitride, microstructure, mechanical property, review

中图分类号:

TQ174

张叶, 曾宇平. 自蔓延高温合成氮化硅多孔陶瓷的研究进展[J]. 无机材料学报, 2022, 37(8): 853-864.

ZHANG Ye, ZENG Yuping. Progress of Porous Silicon Nitride Ceramics Prepared via Self-propagating High Temperature Synthesis[J]. Journal of Inorganic Materials, 2022, 37(8): 853-864.

图/表 13

图1 溶胶-凝胶结合自蔓延合成多孔Si3N4陶瓷光学的照片(a)及放大微观结构图(b~d)[32]

Fig. 1 Optical picture (a) and amplified microstructures (b-d) of the porous Si3N4 ceramics prepared by gel-casting and SHS[32]

图2 自蔓延反应合成多孔Si3N4陶瓷示意图[47]

Fig. 2 Schematic illustration of the fabrication of porous Si3N4 ceramics by SHS[47]

表1 样品配方、自蔓延反应参数及样品性能汇总

Table 1 Composition of raw materials, parameters of SHS process and properties of the fabricated samples

Si/g	Si₃N₄/g	Y₂O₃/g	Combustion temperature/℃	Reaction time/s	Open porosity/%	Shrinkage/%	Ref.
30-45	70-55	2	1870-2050	30-13	40.5-45.8	/	[47]
30-70	70-30	5	1820-1982	/	50.0-60.0	2.8-3.4	[48]

图3 不同工艺参数制备多孔Si3N4陶瓷的微观形貌(p为N2气压力, d50为Si粉粒度)[46]

Fig 3 Microstructures of the porous Si3N4 ceramics fabricated by different (p) pressures of N2 gas (p) and average particle sizes of Si powder (d50)[46] (a) p=3 MPa, d50=2.7 μm; (b) p=5 MPa, d50=2.7 μm; (c) p=7 MPa, d50=2.7μm; (d) p=9 MPa, d50=2.7 μm; (e) p=5 MPa, d50=1.3 μm; (f) p=5 MPa, d50=2.7 μm; (g) p=5 MPa, d50=4.5 μm; (h) p=5 MPa, d50=8.7 μm

图4 不同粒度Si粉制备的多孔Si3N4形成机理示意图[46]

Fig. 4 Schematic of the formation mechanism of porous Si3N4 starting from Si with different particle sizes[46]

图5 自蔓延合成Si3N4陶瓷不同区域显微结构[59]

Fig. 5 Microstructures of different areas of the SHS-fabricated Si3N4 ceramics[59]

图6 不同种类稀释剂和成型压力制备样品弯曲强度的韦伯分布拟合[59]

Fig. 6 Weibull plots of flexural strength for samples prepared with different types of Si3N4 diluent and shaping pressures[59] (Sample ST uses Si3N4 diluent with coarse particle size and high β phase while sample SA uses Si3N4 diluent with fine particle size and high α phase, -X represents the shaping pressure)

表2 使用两种不同Si3N4稀释剂和不同成型压力制备样品的相关系数和Weibull模量[59]

Table 2 Correlation coefficient and Weibull modulus of samples obtained with two different Si3N4 powders and varied shaping pressures[59]

	SA-50	SA-100	SA-150	SA-200	ST-50	ST-100	ST-150	ST-200	Ref.[63-64]
R²	0.99	0.96	0.99	0.97	0.96	0.90	0.96	0.99	-
m	11.4	9.3	8.8	5.7	11.4	16.0	17.2	11.0	10.6-20.9

图7 不同烧结方法制备Si3N4陶瓷的弯曲强度与孔隙率之间的关系

Fig. 7 Relationship between flexural strength and porosity of ceramics prepared by different methods SSN represents sintering Si3N4 by pressureless or gas pressure sintering[10,65⇓⇓⇓⇓⇓⇓⇓⇓-74]; SRBSN represents sintering reaction-bonded Si3N4 [75⇓⇓⇓⇓⇓⇓⇓-83]; CRS represents Si3N4 fabricated by carbothermal reduction sintering[16,84⇓-86]; SHS represents Si3N4 fabricated by self-propagating high temperature synthesis[46⇓-48,56,59-60]

图8 不同烧结助剂制备的多孔Si3N4陶瓷的室温和高温弯曲强度[56]

Fig. 8 Room-temperature and high-temperature flexural strength of the fabricated porous Si3N4 ceramics with different sintering additives[56]

图9 不同烧结助剂制备的多孔Si3N4陶瓷在1400 ℃下断裂时的应力-应变曲线[56]

Fig. 9 Stress-strain curves of the obtained porous Si3N4 ceramics during fracture at 1400 ℃[56]

图10 采用不同质量分数Y2O3作为烧结助剂自蔓延合成Si3N4陶瓷的显微结构和平均晶粒尺寸[62]

Fig. 10 Microstructures and average grain sizes of the SHS-fabricated Si3N4 ceramics prepared with different Y2O3 mass content as sintering additive[62] (a) 0; (b) 0.4%; (c) 0.8%; (d) 1.2%; (e) 1.6%. L, D, AR represents average grain length, average grain diameter, and average aspect ratio respectively

图11 多孔Si3N4陶瓷室温和高温弯曲强度与烧结助剂添加量的关系[62]

Fig. 11 Room-temperature and high-temperature flexural strength of the fabricated porous Si3N4 ceramics as function of sintering additives addition[62]

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自蔓延高温合成氮化硅多孔陶瓷的研究进展

Progress of Porous Silicon Nitride Ceramics Prepared via Self-propagating High Temperature Synthesis

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