多孔SiCO陶瓷中SiC纳米线的原位合成及生长机理

doi:10.3724/SP.J.1077.2013.12353

无机材料学报 ›› 2013, Vol. 28 ›› Issue (5): 474-478.DOI: 10.3724/SP.J.1077.2013.12353 CSTR: 32189.14.SP.J.1077.2013.12353

多孔SiCO陶瓷中SiC纳米线的原位合成及生长机理

潘建梅, 程晓农, 严学华, 张成华, 徐桂芳

(江苏大学材料科学与工程学院, 镇江 212013)

收稿日期:2012-05-28 修回日期:2012-07-30 出版日期:2013-05-10 网络出版日期:2013-04-22
作者简介:潘建梅(1985–), 女, 博士研究生. E-mail: jmpanc@163.com
基金资助:
江苏省材料摩擦学重点实验室开放基金(kjsmcx07005);江苏省高校自然科学基金(08KJD430010);江苏省普通高校研究生科研创新计划(CXZZ11_0558);江苏大学高级专业人才科研启动基金(09jdg033);常熟市科技发展规划项目(CG201005)

In situ Synthesis and Growth Mechanism of SiC Nanowires in SiCO Porous Ceramics

PAN Jian-Mei, CHENG Xiao-Nong, YAN Xue-Hua, ZHANG Cheng-Hua, XU Gui-Fang

(School of Materials Science and Engineering, Jiangsu University, Zhenjiang 212013, China)

Received:2012-05-28 Revised:2012-07-30 Published:2013-05-10 Online:2013-04-22
About author:PAN Jian-Mei. E-mail: jmpanc@163.com
Supported by:
Materials Tribology Key Laboratory of Jiangsu Opening Foundation (kjsmcx07005);Natural Science Foundation of the Jiangsu High Education (08KJD430010);Postgraduate Innovation Project of Jiangsu Province (CXZZ11_0558);Talent Foundation of Jiangsu University (09jdg033);Changshu Research Project (CG201005)

摘要/Abstract

摘要：

采用聚氨酯海绵为多孔模板, 浸渍有机硅树脂后在Ar气氛中原位合成了SiC纳米线。采用TG、XRD、SEM和TEM等分析测试手段对样品进行了表征, 研究了保温时间对合成SiC纳米线的影响, 并探讨了SiC纳米线的生长机理。研究结果表明: SiC纳米线生长在多孔陶瓷中, 纳米线长度达几十微米, 单根纳米线的直径不均一。SiC纳米线的生长机理为VS生长模式。随着保温时间的延长, 纳米线的数量增加, 形貌发生了变化, 且多孔陶瓷的比表面积明显增大, 体积电阻率降低。

关键词: SiC纳米线, 聚合物先驱体, 多孔陶瓷, 原位合成

Abstract:

SiC nanowires were in situ prepared in Ar atmosphere using polyurethane sponge as a porous template infiltrated with silicone resin. Characterizations of the samples were carried out by TG, XRD, SEM and TEM. The effects of the holding time on the synthesis of SiC nanowires were observed. The growth mechanism of SiC nanowires was discussed. The experimental results show that SiC nanowires were grown directly within the pores of the porous ceramics. The lengths of these nanowires are up to several tens of micrometers and single nanowire has a districtive diameter. The growth mechanism of the nanowires is supported by VS growth model. With the increase of the holding time, the amount of the nanowires increases and these nanowires present different morphologies. Furthermore, the specific surface area of the porous ceramics increases significantly and the volume resistivity decreases.

Key words: SiC nanowires, polymeric precursors, porous ceramics, in-situ synthesis

中图分类号:

TQ174

潘建梅, 程晓农, 严学华, 张成华, 徐桂芳. 多孔SiCO陶瓷中SiC纳米线的原位合成及生长机理[J]. 无机材料学报, 2013, 28(5): 474-478.

PAN Jian-Mei, CHENG Xiao-Nong, YAN Xue-Hua, ZHANG Cheng-Hua, XU Gui-Fang. In situ Synthesis and Growth Mechanism of SiC Nanowires in SiCO Porous Ceramics[J]. Journal of Inorganic Materials, 2013, 28(5): 474-478.

图/表 7

图1 固化后的海绵/有机硅树脂在Ar气氛中的TG曲线

Fig. 1 TG curve of the cured sponge/silicone resin in Ar atmosphere

图2 1400℃不同保温时间制备样品的XRD图谱

Fig. 2 XRD patterns of the samples holding at 1400℃ for different time

图3 1400℃保温1 h制备样品的SEM照片和EDS分析

Fig. 3 SEM images and EDS analysis of the sample holding at 1400℃ for 1 h

图4 1400℃保温2 h样品的SEM照片

Fig. 4 SEM images of the sample holding at 1400℃ for 2 h

图5 1400℃保温3 h的样品的SEM照片

Fig. 5 SEM images of the sample holding at 1400℃ for 3 h

图6 SiC纳米线的TEM照片: (a~c) 不同形貌的SiC纳米线及对应的纳米线的SEAD照片(c中的插图); (d)纳米线的HRTEM照片

Fig. 6 TEM images of SiC nanowires: (a-c) different morphologies of SiC nanowires and the corresponding SEAD pattern (see insert in Fig. 6(c)) of the nanowire, and (d) HRTEM image of the nanowire

Table 1 Porosity, specific surface area and volume resistivity of the samples holding at 1400℃ for different time

Holding time/h	Porosity/%	Specific surface area /(m²·g^-1)	Volume resistivity /(Ω·cm)
1	82.3	32	0.135
2	84.5	37	0.092
3	85.4	45	0.065

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多孔SiCO陶瓷中SiC纳米线的原位合成及生长机理

In situ Synthesis and Growth Mechanism of SiC Nanowires in SiCO Porous Ceramics

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