Department of Chemistry, and the Smalley Institute for Nanoscale Science and Technology, Rice University, MS 222, 6100 Main Street, Houston, Texas 77005, USA.
ACS Nano. 2010 Aug 24;4(8):4806-14. doi: 10.1021/nn1006368.
An improved method for the preparation of graphene oxide (GO) is described. Currently, Hummers' method (KMnO(4), NaNO(3), H(2)SO(4)) is the most common method used for preparing graphene oxide. We have found that excluding the NaNO(3), increasing the amount of KMnO(4), and performing the reaction in a 9:1 mixture of H(2)SO(4)/H(3)PO(4) improves the efficiency of the oxidation process. This improved method provides a greater amount of hydrophilic oxidized graphene material as compared to Hummers' method or Hummers' method with additional KMnO(4). Moreover, even though the GO produced by our method is more oxidized than that prepared by Hummers' method, when both are reduced in the same chamber with hydrazine, chemically converted graphene (CCG) produced from this new method is equivalent in its electrical conductivity. In contrast to Hummers' method, the new method does not generate toxic gas and the temperature is easily controlled. This improved synthesis of GO may be important for large-scale production of GO as well as the construction of devices composed of the subsequent CCG.
一种改进的氧化石墨烯(GO)制备方法。目前,Hummers 法(KMnO4、NaNO3、H2SO4)是制备氧化石墨烯最常用的方法。我们发现,不添加 NaNO3,增加 KMnO4 的用量,并在 H2SO4/H3PO4(9:1)混合液中进行反应,可以提高氧化过程的效率。与 Hummers 法或添加额外 KMnO4 的 Hummers 法相比,这种改进的方法提供了更多的亲水性氧化石墨烯材料。此外,尽管我们的方法制备的 GO 比 Hummers 法制备的 GO 氧化程度更高,但当它们在同一腔室中用联氨还原时,由这种新方法制备的化学转化石墨烯(CCG)在电导率方面是等效的。与 Hummers 法不同的是,新方法不会产生有毒气体,并且温度容易控制。这种改进的 GO 合成方法对于大规模生产 GO 以及由后续 CCG 构建器件可能非常重要。