少层石墨烯的微波辐照法快速制备及表征(英文)

以可膨胀石墨为原料制备少层石墨烯,通过初次微波辐照3 min、混酸(浓硫酸与浓硝酸的体积比为1:1)浸泡处理24 h及二次微波辐照剥离3 min的工艺流程,得到了少层石墨烯。用扫描电镜(SEM)、X射线衍射(XRD)、拉曼光谱(Raman)、原子力显微镜(AFM)、X射线光电子能谱(XPS)、红外光谱(FTIR)和燃烧法元素分析对实验产物进行表征。结果表明:经过初次微波辐照处理,伴随闪光及爆裂声,可膨胀石墨层片结构被剥离,迅速形成疏松、多孔的蠕虫形貌。通过混酸浸泡、二次微波辐照和超声分散等后续处理,可快速制得厚度约为4.7 nm的约十几层的石墨烯,且石墨烯未被严重氧化,纯度高,结晶度高。

Rapid microwave irradiation fast preparation and characterization of few-layer graphenes

Few-layer graphenes were fabricated from expandable graphite by rapid microwave exfoliation. Expandable graphite was irradiated in a domestic microwave in full power for 3 min, then soaked in mixed strong hydrogen nitrate and sulfuric acid with volume ratio of 1：1 for 24 h and re-irradiated, thus few-layer graphene sheets were obtained. Specimens gained from every step were selectively characterized by different techniques, such as SEM, XRD, Raman, AFM, XPS, FTIR and combustion elemental analysis. The results show that expandable graphite with loose, porous and worm-like morphology forms instantaneously in microwave irradiation with crackling sound and sparkles, which manifests physical exfoliation of graphene sheets. Few-layer graphene sheets with a dozen or more layers and average thickness of about 4.7 nm are obtained eventually after sequential treatment of microwave irradiation, mixed acid soaking and second microwave irradiation. The as-prepared few-layer graphenes still have high crystallinity and high purity with traces of oxide groups and without serious unrecoverable oxidation damage.