以0.10、0.15、0.18、0.30 mm 4种不同粒径的石墨为原料,采用密闭氧化、氨-水合胼还原法,经过2个控温阶段制备了10~20 μm大粒径氧化石墨(GO)与石墨烯,并通过正交实验、单因素实验优化了制备条件. 测定了GO与石墨烯的傅里叶红外光谱、拉曼光谱及热稳定性.用扫描电镜、X线衍射光谱、原子力显微镜测试了产品的结构与石墨烯片层厚度. 实验结果表明:石墨粒径越小,片层剥离程度越高, GO的产率、热稳定性也均有提高. 石墨烯在800 ℃下残炭率高于80%,剥离层厚度约为1 nm. 本实验研究为制备大粒径GO与石墨烯提供了一种可行的实验方法.
With different size of 0.10、0.15、0.18、0.30 mm of natural graphiteas raw material,graphite oxide(GO)and graphene with a size of 10~20 μm were prepared by pressurized oxidation, ammonia-hydrazine-based multiplex reduction through two different temperature stages. The reaction conditions were optimized by orthogonal test and single factor test. The Fourier transform infrared spectroscopy, Raman spectrometer, thermal stability of the GO and graphene were investigated. Morphology, structure and layer thickness of GO and graphene were investigated by Scanning electron microscopy, X-ray diffraction photometer, atomic force spectroscopy. Results show that GO yield, sheet peeling degree and thermal stability are improved with the decreasing graphite size. The residue yields of the prepared graphene at 800 ℃ are all above 80%, and it presents a thickness of about 1.0 nm. The study provides a practical method for the preparation of GO and graphene with large size.
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