碳热还原-反应烧结法制备多孔氮化硅陶瓷

doi:10.3724/SP.J.1077.2013.12381

无机材料学报 ›› 2013, Vol. 28 ›› Issue (5): 469-473.DOI: 10.3724/SP.J.1077.2013.12381 CSTR: 32189.14.SP.J.1077.2013.12381

碳热还原-反应烧结法制备多孔氮化硅陶瓷

鲁元^1,2, 杨建锋³, 李京龙^1,2

(1. 西北工业大学凝固技术国家重点实验室, 西安 710072; 2. 西北工业大学陕西省摩擦焊接重点实验室, 西安 710072; 3. 西安交通大学金属材料强度国家重点实验室, 西安 710049)

收稿日期:2012-06-15 修回日期:2012-08-18 出版日期:2013-05-10 网络出版日期:2013-04-22
作者简介:鲁元(1980–), 男, 博士研究生. E-mail: luyuan19801104@163.com
基金资助:
国家自然科学基金(50772086, 50821140308);国家863项目(2007AA03Z558)

Fabrication of Porous Silicon Nitride with High Porosity by Carbothermal Reduction-reaction Bonding

LU Yuan^1,2, YANG Jian-Feng³, LI Jing-Long^1,2

(1. State Key Laboratory of Solidification Processing, Northwestern Polytechnical University, Xi’an 710072, China; 2. Shaanxi Key Laboratory of Friction Welding Technologies, Northwestern Polytechnical University, Xi’an 710072, China; 3. State Key Laboratory for Mechanical Behavior of Materials, Xi'an Jiaotong University, Xi’an 710049, China)

Received:2012-06-15 Revised:2012-08-18 Published:2013-05-10 Online:2013-04-22
About author:LU Yuan. E-mail: luyuan19801104@163.com
Supported by:
National Natural Science Foundation of China (50772086, 50821140308);The High-Tech R & D Program of China (2007AA03Z558)

摘要/Abstract

摘要：

以廉价的二氧化硅、炭黑和硅粉为起始原料, 利用碳热还原-反应烧结法制备了高气孔率、孔结构均匀的多孔氮化硅陶瓷, 考察了原料中硅粉含量对多孔氮化硅陶瓷微观组织和力学性能的影响。XRD分析表明烧结后的试样成分除了少量的α-Si₃N₄相和晶间相Y₂Si₃O₃N₄外, 其余都是β-Si₃N₄相; SEM分析显示微观组织由棒状β-Si₃N₄晶粒和均匀的孔组成。通过改变硅粉的含量, 制备了不同气孔率, 力学性能优异的多孔氮化硅陶瓷。

关键词: 碳热还原-反应烧结法, 多孔氮化硅陶瓷, 气孔率

Abstract:

By using cheaper Si, SiO₂ and carbon black as starting material, the porous silicon nitride ceramics with high porosity and uniform pore structure were prepared by carbothermal reduction-reaction bonding method. The influences of Si content on the microstructure and mechanical properties of the samples were investigated. Microstructures and mechanical properties of porous silicon nitride ceramics were studied by XRD, SEM and three-point bending measurement. XRD analysis showed that only β-Si₃N₄ phase, minor of α-Si₃N₄phase and glass phase Y₃Si₃O₃N₄ were detected in the samples. SEM analysis showed that porous silicon nitride ceramics obtained were composed of rod-like β-Si₃N₄ grains and uniform pores. Porous silicon nitride ceramics with different porosities and good mechanical properties were fabricated by changing the Si content.

Key words: carbothermal reduction-reaction bonding, porous silicon nitride ceramics, porosity

中图分类号:

TQ171

鲁元, 杨建锋, 李京龙. 碳热还原-反应烧结法制备多孔氮化硅陶瓷[J]. 无机材料学报, 2013, 28(5): 469-473.

LU Yuan, YANG Jian-Feng, LI Jing-Long. Fabrication of Porous Silicon Nitride with High Porosity by Carbothermal Reduction-reaction Bonding[J]. Journal of Inorganic Materials, 2013, 28(5): 469-473.

图/表 5

Table 1 Composition of the starting powders with different Si contents

Samples	Composition/wt%
Samples	SiO₂	C	Y₂O₃	Si
S0	67.9	27.1	5	-
S10	60.7	24.3	5	10
S20	53.6	21.4	5	20
S30	46.4	18.6	5	30
S40	39.3	15.7	5	40
S50	32.1	12.9	5	50
S60	25.0	10.0	5	60
S70	17.9	7.1	5	70
S80	10.7	4.3	5	80
S95	-	-	5	95

图1 硅粉含量不同的起始粉料的差热分析

Fig. 1 Thermogravimetry-differential thermal analysis of the starting powders with different Si contents

Table 2 Change of linear shrinkage, weight loss, porosity and flexural strength of the samples with Si content

Sample	Weight loss/%	Linear shrinkage/%	Porosity/%	Flexural strength/M?a
S0	45.72	17.24	79.59	17.66
S10	34.61	11.19	74.88	18.54
S20	31.29	0.87	70.05	17.91
S30	16.57	1.16	66.23	22.91
S40	-4.55	1.41	58.11	37.12
S50	-11.32	0.15	53.17	82.11
S60	-15.42	1.19	51.16	101.99
S70	-25.84	0.37	49.77	116.55
S80	-36.92	0.76	46.32	155.87
S95	-50.14	1.29	44.53	188.98

图2 不同硅粉含量试样的XRD 图谱

Fig. 2 XRD patterns of the samples with different Si contents

图3 不同硅粉含量的试样断面的SEM照片

Fig. 3 Fracture surface SEM images of the samples with different Si contents

参考文献 18

[1]	LU Yuan, YANG Jian-Feng, LU Wei-Zhong, et al. Porous silicon nitride ceramics prepared by carbothermal reduction-pressureless sintering method. Journal of The Chinese Ceramic Society, 2009, 37(8): 6-10.
[2]	Yang J, Yang J F, Shan S Y, et al. Effect of sintering additives on microstructure and mechanical properties of porous silicon nitride ceramics. J. Am. Ceram. Soc., 2006, 89(12): 3843-3845.
[3]	Yoshiaki Inagaki, Naoki Kondo, Tatsuki Ohji. High performance porous silicon nitrides. J. Eur. Ceram. Soc., 2002, 22: 2489-2494.
[4]	Chen D Y, Zhang B L, Zhuang H R, et al. Combustion synthesis of network silicon nitride porous ceramics. Ceram. Int., 2003, 29: 363-364.
[5]	LIU Xue-Jian, HUANG Zhi-Yong, HUANG Li-Ping, et al. Mechanical properties and micro structure of silicon sitride ceramies by pressureless sintering. Journal of Inorganic Materials, 2004, 19(6): 1282-1286.
[6]	SHAN Shao-Yun, YANG Jian-Feng, GAO Ji-Qiang, et al. Porous silicon nitride ceramics prepared by carbothermal reduction
[7]	method.Journal of Inorganic Materials, 2006, 21(4): 913-918.
[8]	Hideki H, Katsumi Y, Naoki K, et al. Nitridation enhancing effect of ZrO2 on silicon powder. Mater. Lett., 2008, 62: 3475-3477.
[9]	YAO Dong-Xu, ZENG Yu-Ping. High flexural strength porous silicon nitride prepared via nitridation of silicon powder. Journal of Inorganic Materials, 2011, 26(4): 422-426.
[10]	Yang J F, Shan SY, Janssen R, et al. Synthesis of fibrous β-Si3N4 structured porous ceramics using carbothermal nitridation of silica. Acta Mater., 2005, 53(10): 2981-2990.
[11]	Toru W, Hiromasa Y, Junichi T, et al. In situ measurement of shrinkage during postreaction sintering of reaction-bonded silicon nitride. J. Am. Ceram. Soc., 2008, 91(10): 3413-3415.
[12]	Lee B T, Yoo J H, Kim H D, et al. Size effect of raw Si powder on microstructures and mechanical properties of RBSN and GPSed-RBSN bodies. Mater. Sci. Eng. A, 2002, 333: 306-313.
[13]	Lee JS, Mun J H, Han B D, et al. Effect of β-Si3N4 seed particles on the property of sintered reaction-bonded silicon nitride. Ceram. Int., 2003, 29: 897-905.
[14]	YIN Shao-Wu, WANG li, LIU Chuan-Ping, et al. The study on the preparation of silicon nitride powders by direct nitridationat normal pressure. Bulletin of The Chinese Ceramic Society, 2007, 27(2): 230-235.
[15]	Weimer A W, Eisman G A, Susnitzky D W, et al. Mechanism and kinetics of the carbothermal nitridation synthesis of α-silicon nitride. J. Am. Ceram. Soc., 1997, 80(11): 2853-2863.
[16]	ZHANG Yu-Dong, SU Xun-Jia, HOU Gen-Liang, et al. Research progress on reactive sintering of silicon nitride. Inorganic Chemicals Industry, 2007, 39(2): 10-12.
[17]	Park D S, Kim H D, Lim K T, et al. Microstructure of reaction- bonded silicon nitride fabricated under static nitrogen pressure. Mater. Sci. Eng. A, 2005, 405: 158-162.
[18]	Lee J S, Mun J H, Han B D, et al. Effect of raw-Si particle size on the properties of sintered reaction-bonded silicon nitride. Ceram. Int., 2004, 30(6): 965-976.

碳热还原-反应烧结法制备多孔氮化硅陶瓷

Fabrication of Porous Silicon Nitride with High Porosity by Carbothermal Reduction-reaction Bonding

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