氮气压力对多孔氮化硅陶瓷显微组织和力学性能的影响

doi:10.3724/SP.J.1077.2014.13531

无机材料学报 ›› 2014, Vol. 29 ›› Issue (7): 701-705.DOI: 10.3724/SP.J.1077.2014.13531 CSTR: 32189.14.SP.J.1077.2014.13531

氮气压力对多孔氮化硅陶瓷显微组织和力学性能的影响

张俊禧¹, 徐照芸¹, 王波¹, 秦毅¹, 杨建锋¹, 赵中坚², 胡伟², 施志伟²

(1. 西安交通大学金属材料强度国家重点实验室, 西安 710049; 2. 上海玻璃钢研究院有限公司, 上海 201404)

收稿日期:2013-10-17 修回日期:2013-11-27 出版日期:2014-07-20 网络出版日期:2014-06-20
作者简介:张俊禧(1986–), 男, 硕士研究生. E-mail: xzy0030@163.com
基金资助:
国家自然科学基金(51272205,51072157);A3前瞻计划(51161140399)

Effects of Nitrogen Pressure on Microstructure and Mechanical Performance of Porous Silicon Nitride Ceramics

ZHANG Jun-Xi¹, XU Zhao-Yun¹, WANG Bo¹, QIN Yi¹, YANG Jian-Feng¹, ZHAO Zhong-Jian², HU Wei², SHI Zhi-Wei²

(1. State Key Laboratory for Mechanical Behavior of Materials, Xi’an Jiaotong University, Xi’an 710049, China; 2. Shanghai FRP Research Institute CO., Ltd., Shanghai 201404, China)

Received:2013-10-17 Revised:2013-11-27 Published:2014-07-20 Online:2014-06-20
About author:ZHANG Jun-Xi. E-mail: xzy0030@163.com
Supported by:
National Natural Science Foundation of China (51272205,51072157);A3 Foresight Program (51161140399)

摘要/Abstract

摘要：

以α-Si₃N₄为原料, Y₂O₃为烧结助剂, 在三种不同的氮气压力(0.12、0.32和0.52 MPa)下烧结制备了多孔氮化硅陶瓷。研究了氮气压力对氮化硅的烧结行为、显微组织和力学性能的影响, 分别通过SEM观察显微组织并统计晶粒的长径比, 通过XRD对物相进行分析, 并对烧结试样进行三点弯曲强度测试。随着氮气压力的提高, 多孔陶瓷的线收缩率降低、气孔率提高, 这是由于低熔点的液相中N含量随氮气压力的提升而增加, 导致了液相粘度提高, 抑制陶瓷致密化。随着氮气压力的提高, 组织中的棒状β-Si₃N₄生长良好, 晶粒长径比增大, 其原因是高的液相粘度抑制了β-Si₃N₄形核, 有利于β-Si₃N₄生长。由于β-Si₃N₄棒状晶的作用, 陶瓷弯曲强度随氮气压力的升高得到改善, 但是气孔率的升高降低陶瓷的强度。在0.52 MPa的氮气压力下烧结的多孔陶瓷气孔率达58%, 弯曲强度为140 MPa。

关键词: 氮化硅, 氮气压力, 长径比

Abstract:

Porous silicon nitride ceramic was fabricated by using α-Si₃N₄ as raw material and Y₂O₃ as a sintering additive, with nitrogen pressure of 0.12 MPa, 0.32 MPa and 0.52 MPa. Effects of the nitrogen pressure on grain morphology and mechanical properties of the resultant porous Si₃N₄ ceramics were characterized by SEM, XRD and flexural strength. With the increasing of nitrogen pressure, sintering shrinkage decreased, with a corresponding increased porosity. Due to the increase of nitrogen pressure, the viscosity of liquid phase increased due to increased N solubility, leading to the low densification in the sintering. Fibrous β-Si₃N₄ grains were developed in the porous microstructure and the grain morphology and aspect ratio were greatly affected by the nitrogen pressures. The high viscosity of the liquid phase in nitrogen at high pressure led to restraining of the β-Si₃N₄ nucleation, and preferential growth of β-Si₃N₄. Due to the formation of elongated β-Si₃N₄, flexural strength of the porous Si₃N₄ ceramic was improved by the increase of nitrogen pressure, while decreased with the increase of porosity. The porous Si₃N₄ ceramics with porosity of 58% and flexural strength of 140 MPa were obtained at the nitrogen pressure of 0.52 MPa.

Key words: Si3N4 nitrogen pressure, aspect ratio

中图分类号:

TQ174

张俊禧, 徐照芸, 王波, 秦毅, 杨建锋, 赵中坚, 胡伟, 施志伟. 氮气压力对多孔氮化硅陶瓷显微组织和力学性能的影响[J]. 无机材料学报, 2014, 29(7): 701-705.

ZHANG Jun-Xi, XU Zhao-Yun, WANG Bo, QIN Yi, YANG Jian-Feng, ZHAO Zhong-Jian, HU Wei, SHI Zhi-Wei. Effects of Nitrogen Pressure on Microstructure and Mechanical Performance of Porous Silicon Nitride Ceramics[J]. Journal of Inorganic Materials, 2014, 29(7): 701-705.

图/表 7

图1 多孔Si3N4陶瓷烧结升温曲线

Fig. 1 Heating curves of sinter porous Si3N4 ceramics

图2 试样线收缩率和气孔率随氮气压力的变化关系

Fig. 2 Shrinkage and porosity of porous Si3N4 ceramic as a function of N2 pressure

图3 烧结温度1750 ℃、2 h、0.32MPa N2压力下烧结的多孔Si3N4陶瓷的XRD图谱

Fig. 3 XRD patterns of porous Si3N4 ceramic sintered at 1750 ℃for 2 h with N2 pressure of 0.32 MPa

图4 1750 ℃不同氮气压力烧结试样断口SEM照片

Fig. 4 SEM images of porous Si3N4 ceramic sintered at 1750 ℃ with different N2 pressures (a) 0.12 MPa; (b) 0.32 MPa; (c) 0.52 MPa

图5 不同氮气压力烧结氮化硅陶瓷晶粒尺寸分布

Fig. 5 Grain size distribution of porous Si3N4 ceramic sintered at 1750 ℃ with different N2 pressures

图6 1750 ℃不同氮气压力烧结试样的晶粒长径比

Fig. 6 Respect ratio of porous Si3N4 ceramic grain sintered at 1750 ℃ with different N2 pressures

图7 不同氮气压力下烧结试样强度

Fig. 7 Relation between flexural strength and different N2 pressure for porous Si3N4 ceramics

参考文献 14

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氮气压力对多孔氮化硅陶瓷显微组织和力学性能的影响

Effects of Nitrogen Pressure on Microstructure and Mechanical Performance of Porous Silicon Nitride Ceramics

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