氧气辅助法制备氮化硼纳米管

doi:10.15541/ji.m.2013.0629

无机材料学报 ›› 2014, Vol. 29 ›› Issue (8): 880-884.DOI: 10.15541/ji.m.2013.0629 CSTR: 32189.14.10.15541/ji.m.2013.0629

氧气辅助法制备氮化硼纳米管

李娟^1,2,3, 吴浩⁴, 陈拥军², 徐盛明¹

(1. 清华大学核能与新能源技术研究院, 北京100084; 2. 海南大学材料与化工学院, 海口570228; 3. 广西大学化学化工学院, 南宁530004; 4. 清华大学材料学院, 北京电子显微镜中心, 北京 100084)

收稿日期:2013-12-03 修回日期:2014-02-24 出版日期:2014-08-20 网络出版日期:2014-07-15
基金资助:
国家自然科学基金(51162001) National Natural Science Foundation of China (51162001)

Oxygen Gas-assisted Synthesis of Boron Nitride Nanotubes

LI Juan^1,2,3, WU Hao⁴, CHEN Yong-Jun², XU Sheng-Ming¹

(1. Institute of Nuclear and New Energy Technology, Tsinghua University, Beijing 100084, China; 2. College of Materials and Chemical Engineering, Hainan University, Haikou 570228, China; 3. College of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China; 4. Beijing National Center for Electron Microscopy, Key Laboratory of Advanced Materials of Ministry of Education of China and State Key Laboratory of New Ceramics and Fine Processing, School of Materials Science and Engineering, Tsinghua University, Beijing 100084, China)

Received:2013-12-03 Revised:2014-02-24 Published:2014-08-20 Online:2014-07-15

摘要/Abstract

摘要：

将无定形硼粉于流动氨气(50 mL/min)和不同氧气流量(10、15、20、40 mL/min)的混合气氛下高温(1300℃)处理后, 在不锈钢基片上收集到白色棉花状产物。研究结果表明, 微量的氧气可将硼粉氧化成气态的B₂O₂中间体, 为BN纳米管的生长提供活性较高的硼源。当氧气流量适中时, 所得纳米管的平均直径为80 nm, 长度可达几百微米。氧气流量对BN纳米管的直径和产量影响较大, 纳米管直径随着氧气流量的增大而增大, 产量则出现先升高后降低的趋势。氮化硼纳米管的生长机理属于气-液-固模型。

关键词: 氮化硼纳米管, 氧气辅助法, 气-液-固生长机理

Abstract:

Wool-like products were fabricated on the stainless-steel substrates by directly heating amorphous B powder at high temperature (1300℃) at 50 mL/min ammonia gas with different flow of oxygen gas (10, 15, 20, 40 mL/min). It was found that B powder could be oxidized by trace oxygen gas to form the intermediate B₂O₂ vapor, which can act as highly active boron source for the growth of BN nanotubes. When an appropriate amount of oxygen was introduced, the obtained nanotubes had an average diameter of about 80 nm and the lengths of several hundred micrometer. Both the diameter and the yield of BN nanotubes could be influenced dramatically by the flow rate of oxygen. With the increase of oxygen flow, the diameter of nanotubes was gradually increased, and the yield of nanotubes was improved obviously at first and then turned down. The formation mechanism of these nanotubes is governed by a vapor-liquid- solid (VLS) growth model.

Key words: boron nitride nanotubes, oxygen gas-assisted, vapor-liquid-solid growth model

中图分类号:

TQ174

李娟, 吴浩, 陈拥军, 徐盛明. 氧气辅助法制备氮化硼纳米管[J]. 无机材料学报, 2014, 29(8): 880-884.

LI Juan, WU Hao, CHEN Yong-Jun, XU Sheng-Ming. Oxygen Gas-assisted Synthesis of Boron Nitride Nanotubes[J]. Journal of Inorganic Materials, 2014, 29(8): 880-884.

图/表 6

图1 氧气流量为10 mL/min、反应温度为1300℃所得产物的 XRD 图谱

Fig. 1 XRD pattern of the product synthesized at 1300℃ and oxygen flow of 10 mL/min

图2 在氧气流量为10 mL/min、反应温度为1300℃下产物的低倍(a)和高倍(b) SEM照片

Fig. 2 Low- (a) and high- (b) magnification SEM images of the product synthesized at 1300℃ and oxygen flow of 10 mL/ min. Inset is the high-magnification image of a particle attached at the end of the 1 D nanostructure

图3 BN纳米管TEM照片(a)(插图为头部带有颗粒的BN纳米管的TEM照片)和管壁的HRTEM照片(b)及其相应的EDX图谱(c, d)

Fig. 3 TEM image (inset TEM image showing a particle attached at the end of a BN nanotube) (a) and HRTEM image (b) of BN nanotube wall, and their EDX patterns (c,d), respectively

图4 BN纳米管的光致发光图谱

Fig. 4 Photoluminescence spectrum of the BN nanotubes

图5 1300℃不同氧气流量下所得BN纳米管的低倍和高倍SEM照片

Fig. 5 Low- and high-magnification SEM images of BN nanotubes synthesized at 1300℃ and different flow rates of oxygen (a) and (b): 15 mL/min; (c) and (d) : 20 mL/min; (e) and (f): 40 mL/min

图6 在氧气流量为10 mL/min、1200℃(a)和1350℃(b)下所得产物的SEM照片

Fig. 6 SEM images of the nanotubes synthesis at 1200℃ (a), 1350℃(b) and oxygen flow of 10 mL/min

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氧气辅助法制备氮化硼纳米管

Oxygen Gas-assisted Synthesis of Boron Nitride Nanotubes

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