炸药爆轰法制备的纳米石墨粉的拉曼光谱

Raman Spectrum of Nano-Graphite Synthesized by Explosive Detonation

负氧平衡炸药爆轰法合成的纳米石墨粉,是一种新型的具有良好实用前景的纳米粉体材料。采用负氧平衡炸药梯恩梯(TNT),在分别充有氮气、氩气、二氧化碳等保护性气体、压力为025～2atm的密闭容器内爆轰制备了纳米石墨粉。用激光拉曼光谱对制备的样品进行了测试,结果表明样品为石墨结构。纳米石墨粉的Raman峰与块体石墨相比,其峰位向高波数方向偏移了约5cm-1。纳米石墨粉Raman峰的半高宽约为22cm-1,由此可计算出纳米石墨粉的颗粒大小为297～397nm。与高纯石墨Raman峰相比,纳米石墨粉的Raman峰由于尺寸效应出现了蓝移现象,并对此现象进行了讨论。用X射线衍射仪(XRD)和透射电子显微镜(TEM)测定了纳米石墨粉的物相,并对其颗粒粒径进行了估算,其结果为258nm(酸处理前)和186nm(酸处理后),与Raman光谱的结果基本吻合。

The nano-graphite powder synthesized by the detonation of explosives with negative oxygen balance is a new powder material with potential applications. In this work, the preparation of nano-graphite powder in steel chamber by pure TNT (trinitrotoluene) explosives has been introduced. In the synthesis process, the protective gases in the steel chamber are N-2, CO2 and At, and the pressure is 0.25-2 atm. Raman spectrum of the nano-graphite was measured. The characteristic Raman band assigned to sp(2) of graphite has been observed at about 1 585 cm(-1) with half-peak width of 22 cm(-1). The peak shifted to a higher frequency by 5 cm(-1) compared with that of bulk graphite. The authors explain this blue shift phenomenon by size effect. The average size of nanographite from Raman measurement is 2.97-3.97 nm. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to measure the structure and particle size of the nano-graphite. The crystallite size of nano-graphite estimated from XRD and TEM are 2.58 nm(acid untreated) and 1.86 nm(acid treated) respectively, which is in accord with the results of the measurement approximately.