第24卷第1期 2009年1月
文章编号：1000-324X(2009)01-0013-05
无机材料学报
Joumal of Inorganic Materials
先驱体热解制备富硼、氨氮BCN化合物及其发光性能研究
杨建，丘泰，沈春英，潘丽梅
（南京工业大学材料科学与工程学院，南京210009）
Vol.24.No.1 Jan.，2009
摘要：以三案氰胺和硼酸为原料，在水溶液中反应合成出纤维状C,NH（H，BO、），先驱体，通过使其在高温氢气氨下热解制备出了高确、氢BCN化合物.利用XRD、FT-IR、XPS、SEM、HRTEM等对热解产物进行了表征，采用FS测量了热解产物的室温光致发光光谱，研究了热解温度对产物及其光致发光性能的影响.结果表明，1000℃以上热解均可制备出乱层石墨结构富硼、氮BCN化合物.随热解温度的升高，BCN化合物中的B、N含量逐渐增大，C含量逐渐减小,BCN 化合物的晶体形状为棒状或纤维状，由相互交织的平均直径在2nm左右的纳米纤维构成.这些BCN化合物均为宽带隙半导体，在340~450nm和670~705nm出现了两个很强的呈明显宽化的光致发光峰，且随热解温度的升高，短波长的发射峰波长基本呈逐减小的变化趋势。
关键词：BCN化合物；富硼、氮；热解；光致发光
中图分类号：0613；0482；075
文献标识码：A
Photoluminescence of (Boron and Nitrogen)-rich BCN Compounds Pyrolysed from Precursor
YANG Jian, QIU Tai, SHEN Chun-Ying, PAN Li-Mei
(College of Materials Science and Engineering, Nanjing University of Technology, Nanjing 210009, China)
Abstract: C,N,H,(H,BO, )2 precursor was synthesized with C,N,H, and H,BO, as raw materials in aqueous solution,which was followed by pyrolysis at high temperature in flowing N, atmosphere to prepare (boron and nitrogen)-rich BCN compounds. The pyrolysis products were characterized by FTIR, XRD, XPS, SEM and HRTEM. The room-temperature photoluminescence(PL) spectra of the pyrolysis products were meas-ured by fluorescence spectrometry. Effect of pyrolysis temperature on the pyrolysis products and their photo luminescencewere investigated.The results indicate that （(boron and nitrogen)-rich BCN compounds with turbostratic graphite structure can be obtained when the pyrolysis temperature is above 1000. With the in-crease of pyrolysis temperature, the contents of B and N in the BCN compounds increase whereas the content of C decreases. These BCN compounds show bar-like or fibrous morphologies similar to the precursor. HR TEM analysis reveals that these BCN compounds are composed of interweaved nanofibers with average diame-ter of ca. 2nm. PL results indicate that these BCN compounds are semiconductors with two strong and broad PL peaks centered at 340-450nm and 670-705nm. With the increase of pyrolysis temperature, the wave-length of the peak centered in the shorter wavelength range decreases due to the variation of the chemical composition.
Key words: BCN compounds; (boron and nitrogen)-rich; pyrolysis; photoluminescence
三元硼碳氮（BCN)化合物具有与BN和C相似的结构和介于两者之间的随成分可调的物理、化学特性，其特殊的电学、光学、热学、力学等性质以及潜在的应用前景引起了人们的极大兴趣(",2).新型BCN化合物的制备、表征和性能研究已成为研究热点.研究人员依据理论计算选取各种不同的原料，采用多种合
成方法制备出了各种成分和结构的BCN化合物（薄膜、纳米棒、粉末).制备方法有先驱体氮化法(3]、固相热解法[4]、化学气相沉积法（CVD)[5]、物理气相沉积法(PVD)[6)、高温高压法(7)]、冲击合成（机械球磨）法["]等，但目前得到的多为富碳的BCN化合物，尤其对BC,N化合物的理论和实验研究较广泛，而对富硼、
收稿日期：2008-04-01，收到修改稿日期：2008-07-01
杨建（1976-），男，博士，教授，E-mail；yangjian1976@163.com
作者简介：万方数据