Catalytic preparation of α-silicon nitride single-crystalline nanowires by layered double hydroxides

doi:10.11949/j.issn.0438-1157.20180760

CIESC Journal ›› 2018, Vol. 69 ›› Issue (10): 4471-4478.DOI: 10.11949/j.issn.0438-1157.20180760

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Catalytic preparation of α-silicon nitride single-crystalline nanowires by layered double hydroxides

LEI Chao, LI Kefeng, WANG Jian, MAO Xinhua, ZOU Liming, XIE Huanwen

Guangdong Institute of Materials and Processing, Guangdong Academy of Sciences, Guangzhou 510650, Guangdong, China

Received:2018-07-09 Revised:2018-07-26 Online:2018-10-05 Published:2018-10-05
Supported by:
supported by the Project for Research Environment and Capacity Building of Guangdong Academy of Sciences (2016GDASPT-0209, 2016GDASPT-0321), the Innovation Driven Development Capacity Building of Guangdong Academy of Sciences (2018GDASCX-0964), the Guangdong Academy of Sciences Project (2017 GDASCX-0117), the Guangzhou Science and Technology Planning Project (ZWY201704003), the Guangdong Institute of Materials and Processing Innovation Capacity Building Project (2017A070701029) and the Project for Public Welfare Research and Capacity Building of Guangdong Province (2017A070702019).

LDH催化制备单晶a-Si₃N₄纳米线研究

雷超, 李克峰, 王健, 毛新华, 邹黎明, 谢焕文

广东省科学院广东省材料与加工研究所, 广东广州 510650

通讯作者: 雷超
基金资助:
广东省科学院科研平台环境与能力建设专项项目（2016GDASPT-0209，2016GDASPT-0321）；广东省科学院实施创新驱动发展能力建设专项项目（2018GDASCX-0964）；广东省科学院院属骨干科研机构创新能力建设专项项目（2017GDASCX-0117）；广州市科技计划项目（ZWY201704003）；广东省材料与加工研究所创新能力建设项目（2017A070701029）；广东省公益研究与能力建设专项（2017A070702019）。

Abstract

Abstract:

α-Silicon nitride single-crystalline nanowires were prepared by direct nitridation of nano-Si powders in N₂-H₂ mixture gas under the catalysis of layered double hydroxide (LDH) flakes. The results show that when the H₂ content is less than 0.5%, the as-prepared Fe/Mg/Al LDH catalyst has excellent high temperature thermal stability, and can maintain its structural integrity and catalytic activity after calcination and reduction at 1250℃. Through decreasing the size and increasing the density of nano Fe particles on LDHs, via reducing the temperature, Fe content in LDHs and adding Mo element into LDHs, the diameter of as prepared a-Si₃N₄ nanowires can be decreased to 30-50 nm, with the aspect ratio higher than 1000. Further study shows that the growth of nanowires was controlled by the vapor-liquid-solid (VLS) mechanism.

Key words: Si₃N₄ nanowires, LDH catalyst, chemical vapor deposition, thermal stability, VLS mechanism

摘要：

提出了一种以LDH （水滑石类化合物）为催化剂，纳米硅粉为原料，在N₂-H₂混合气氛下制备单晶a-Si₃N₄纳米线的CVD （化学气相沉积）方法。研究结果表明：当H₂含量小于0.5%时，所制备的Fe/Mg/Al LDH催化剂具有优良的高温热稳定性，在1250℃下煅烧与还原后仍可保持自身结构完整与催化活性。通过降低还原温度与LDH中Fe含量、在LDH中引入Mo元素等手段，有效地降低金属Fe纳米晶粒直径、增大成核密度，所制备单晶a-Si₃N₄纳米线面密度可达5×10¹⁴～9×10¹⁴ m^-2，直径为30～50 nm，长度达20～80 μm （长径比>1000）。进一步研究表明本实验中纳米线为VLS （气液固）生长机制。

关键词: 氮化硅纳米线, LDH催化剂, 化学气相沉积, 热稳定性, VLS机制

CLC Number:

TB32

LEI Chao, LI Kefeng, WANG Jian, MAO Xinhua, ZOU Liming, XIE Huanwen. Catalytic preparation of α-silicon nitride single-crystalline nanowires by layered double hydroxides[J]. CIESC Journal, 2018, 69(10): 4471-4478.

雷超, 李克峰, 王健, 毛新华, 邹黎明, 谢焕文. LDH催化制备单晶a-Si₃N₄纳米线研究[J]. 化工学报, 2018, 69(10): 4471-4478.

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Catalytic preparation of α-silicon nitride single-crystalline nanowires by layered double hydroxides

LDH催化制备单晶a-Si₃N₄纳米线研究

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Catalytic preparation of α-silicon nitride single-crystalline nanowires by layered double hydroxides

LDH催化制备单晶a-Si3N4纳米线研究

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LDH催化制备单晶a-Si₃N₄纳米线研究