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[1]崔艺,吴晓栋,崔升,等.新型块状氮化硅气凝胶的制备及表征[J].南京工业大学学报(自然科学版),2020,42(04):508-515.[doi:10.3969/j.issn.1671-7627.2020.04.009]
 CUI Yi,WU Xiaodong,CUI Sheng,et al.Preparation and characterization of novel bulk silicon nitride aerogels[J].Journal of NANJING TECH UNIVERSITY(NATURAL SCIENCE EDITION),2020,42(04):508-515.[doi:10.3969/j.issn.1671-7627.2020.04.009]
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新型块状氮化硅气凝胶的制备及表征()
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《南京工业大学学报(自然科学版)》[ISSN:1671-7627/CN:32-1670/N]

卷:
42
期数:
2020年04期
页码:
508-515
栏目:
出版日期:
2020-07-17

文章信息/Info

Title:
Preparation and characterization of novel bulk silicon nitride aerogels
文章编号:
1671-7627(2020)04-0508-08
作者:
崔艺吴晓栋崔升沈晓冬
1.南京工业大学 材料科学与工程学院 材料化学工程国家重点实验室 江苏先进无机功能复合材料协同创新中心,江苏 南京 211800
Author(s):
CUI Yi WU Xiaodong CUI Sheng SHEN Xiaodong
Jiangsu Collaborative Innovation Center for Advanced Inorganic Function Composites, State Key Laboratory of Materials-Oriented Chemical Engineering, College of Materials Science and Engineering, Nanjing Tech University, Nanjing 211800,China
关键词:
溶胶凝胶 碳热还原 块状Si3N4 高比表
Keywords:
sol-gel carbothermal reduction bulk Si3N4 heat treatment
分类号:
TQ138.1
DOI:
10.3969/j.issn.1671-7627.2020.04.009
文献标志码:
A
摘要:
以尿素为氮源,通过溶胶-凝胶法并结合超临界干燥、惰性氛围碳化、碳热还原和空气除碳等工艺制备块状氮化硅(Si3N4)气凝胶。通过不同温度热处理,研究Si3N4气凝胶的形成过程及机制。采用X线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X线光电子能谱仪(XPS)、N2吸附-脱附仪分析材料的相组成、微观结构和孔结构等。结果表明:当热处理温度为1 500 ℃时,体系中以Si3N4相为主,继续升高热处理温度至1 600 ℃时,Si3N4相转化为SiC相。Si3N4气凝胶中Si3N4相和SiO2相分别占74.4%和25.6%。Si3N4气凝胶以Si3N4纳米颗粒的形式存在,其粒径为20~40 nm,孔径为20~40 nm,比表面积高达519.58 m2/g。Si3N4气凝胶的室温热导率为0.045 W/(m·K),其形成机制是基于C、SiO2和N2之间的气-固(VS)生长。
Abstract:
The bulk Si3N4 aerogel was prepared by sol-gel method, using urea as nitrogen source, combined with supercritical drying technique, followed by carbonization, carbothermal reduction and air combustion processes. The formation process and mechanism of silicon nitride aerogel were studied by heat treatment at different temperatures. X-ray diffraction(XRD), scanning electron microscopy(SEM), transmission electron microscopy(TEM), X-ray photoelectron spectroscopy(XPS), N2 adsorption-desorption measurement were carried out for testing the phases, microstructures and pore structures. Results showed that Si3N4 was the dominant phase in the composite when the heat treatment temperature was increased to 1 500 ℃. Si3N4 phase was transformed into SiC phase with further heat treatment at 1 600 ℃. The Si3N4 phase and SiO2 phase accounted for 74.4% and 25.6% of the composite aerogels, respectively. Si3N4 aerogels existed in the form of Si3N4 nanoparticles, with particle sizes of about 20-40 nm and pore diameters of about 20-40 nm, as well as specific surface areas of up to 519.58 m2/g. The thermal conductivity of silicon nitride aerogel at room temperature was 0.045 W/(m·K), and its formation mechanism was based on the growth of vapor-solid(VS)mechanism between C, SiO2 and N2.

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备注/Memo

备注/Memo:
收稿日期:2019-11-15
基金项目:江苏省博士后科研资助计划(2019K005); 江苏省高等学校自然科学基金面上项目(19KJB430023); 南京市留学人员科技创新项目; 中国博士后基金面上项目(2019M661781)
作者简介:崔艺(1997—),女,E-mail:18351806506@163.com; 吴晓栋(联系人),讲师,E-mail:wuxiaodong@njtech.edu.cn; 崔升(联系人),教授,E-mail:scui@njtech.edu.cn.
引用格式:崔艺,吴晓栋,崔升,等.新型块状氮化硅气凝胶的制备及表征[J].南京工业大学学报(自然科学版),2020,42(4):508-515.
CUI Yi, WU Xiaodong, CUI Sheng, et al. Preparation and characterization of novel bulk silicon nitride aerogels[J].Journal of Nanjing Tech University(Natural Science Edition),2020,42(4):508-515..
更新日期/Last Update: 2020-07-30