Jeong Hae-Kyung, Lee Yun Pyo, Lahaye Rob J W E, Park Min-Ho, An Kay Hyeok, Kim Ick Jun, Yang Cheol-Woong, Park Chong Yun, Ruoff Rodney S, Lee Young Hee
BK21 Physics Division, Institute of Basic Science, Center for Nanotubes and Nanostructured Composites, Sungkyunkwan University, Suwon 440-746, Korea.
J Am Chem Soc. 2008 Jan 30;130(4):1362-6. doi: 10.1021/ja076473o. Epub 2008 Jan 8.
Graphite oxide (GO) samples were prepared by a simplified Brodie method. Hydroxyl, epoxide, carboxyl, and some alkyl functional groups are present in the GO, as identified by solid-state 13C NMR, Fourier-transform infrared spectroscopy, and X-ray photoemission spectroscopy. Starting with pyrolytic graphite (interlayer separation 3.36 A), the average interlayer distance after 1 h of reaction, as determined by X-ray diffraction, increased to 5.62 A and then increased with further oxidation to 7.37 A after 24 h. A smaller signal in 13C CPMAS NMR compared to that in 13C NMR suggests that carboxyl and alkyl groups are at the edges of the flakes of graphite oxide. Other aspects of the chemical bonding were assessed from the NMR and XPS data and are discussed. AB stacking of the layers in the GO was inferred from an electron diffraction study. The elemental composition of GO prepared using this simplified Brodie method is further discussed.
氧化石墨烯（GO）样品采用简化的Brodie法制备。通过固态¹³C核磁共振、傅里叶变换红外光谱和X射线光电子能谱鉴定，GO中存在羟基、环氧基、羧基和一些烷基官能团。以热解石墨（层间距3.36 Å）为起始原料，经X射线衍射测定，反应1小时后的平均层间距增加到5.62 Å，进一步氧化24小时后，层间距增至7.37 Å。¹³C交叉极化魔角旋转核磁共振（¹³C CPMAS NMR）中的信号比¹³C NMR中的信号小，这表明羧基和烷基位于氧化石墨烯薄片的边缘。根据核磁共振和X射线光电子能谱数据评估了化学键合的其他方面，并进行了讨论。通过电子衍射研究推断出GO中层的AB堆叠结构。进一步讨论了使用这种简化的Brodie法制备的GO的元素组成。
