摘要
以三聚氰胺和硼酸为原料在水溶液中反应合成出了C3N6H6(H3BO3)2先驱体,利用热重-差示扫描量热-质谱(TG-DSC-MS)联用技术及FT-IR,XRD,SEM等对由C3N6H6(H3BO3)2热解制备BCN化合物的过程进行了表征研究.结果表明,先驱体C3N6H6(H3BO3)2是由C3N6H6分子和H3BO3分子通过分子间氢键作用形成的三维超分子结构化合物.随热解温度的升高,先驱体中的H3BO3和C3N6H6结构单元逐渐发生分解,同时依次放出H2O,NH3,CO2,NO2等气体.1000℃之后热解过程基本结束,产物中形成B-N,B-C和C-N化学键,得到B,C,N原子级化合的具有乱层石墨结构的BCN化合物.XPS分析结果表明,1900℃热解得到了组成近似为B3CN3的新型富氮BCN化合物.SEM观察表明,B3CN3具有与先驱体相同的棒状或纤维状形貌,但晶体尺寸较先驱体减小.
C3N6H6（H3BO3）2 was synthesized with C3N6H6 and H3BO3 as raw materials in aqueous solution, which was then used as the precursor for preparation of a BCN compound by pyrolysis in flowing N2 atmosphere. The pyrolysis process was investigated by means of TG-DSC-MS coupling technique, FT-IR, XRD and SEM. The results indicate that the precursor C3N6H6（H3BO3）2 is a 3D supramolecular compound which is constructed by different hydrogen-bonding interactions between C3N6H6 and H3BO3 molecules. With the increase of pyrolysis temperature, C3N6H6 and H3BO3 unit in the precursor is gradually decomposed, accompanied by the release of H2O, NH3, CO2, and NO2 gases. After 1000℃, the pyrolysis process has completed and B-N, B-C, and C-N chemical bonds established in the products, which means the formation of turbostratic-structure BCN compounds with atomic-level hybrid of B, C, and N elements. A novel nitrogen-rich BCN compound with an approximate composition of B3CN3 was obtained from the pyrolysis at 1 900 ℃. The B3CN3 compound shows bar-like or fibrous morphology similar to the precursor, but there is an obvious reduction in its crystal size compared with the precursor.
出处
《过程工程学报》
EI
CAS
CSCD
北大核心
2006年第3期466-471,共6页
The Chinese Journal of Process Engineering
基金
国防化工新材料重点科研基金资助项目
关键词
BCN
热解
合成
先驱体
化学键
BCN
pyrolysis
synthesis
precursor
chemical bond
