(制备石墨烯方法)Chemical route to Graphene Kaner.pdf

Supporting Information to Accompany: A Chemical Route to Graphene for Device Applications Scott Gilje?, Song Han?, Minsheng Wang?, Kang Wang?, Ric Kaner? ? Department of Chemistry and Biochemistry, University of California Los Angeles, Los Angeles, California, 90095, ? Department of Electrical Engineering, University of California at Los Angeles, Los Angeles, California, 90095 Graphite oxide synthesis: Graphite oxide is synthesized from graphite powder (SP-1 grade 325 mesh, Bay Carbon Inc.) by a modified Hummers method as originally presented by Kovtyukhova, et al.1,2 The graphite is first pretreated in order to fully oxidize it to graphite oxide (GO). To accomplish this concentrated H2SO4 (50 ml) is heated to 90 °C in a 300 ml beaker with K2S2O8 (10 g) and with P2O5 (10 g) added with stirring until all of the reactants are completely dissolved. The mixture is then cooled to 80 °C. Graphite powder (12 g) is then added to the H2SO4 solution resulting in bubbling which subsides within 30 minutes. The mixture is kept at 80 °C for 4.5 hours using a hotplate after which the heating is stopped and the mixture diluted with 2 L of DI water and left overnight. The following day the mixture is filtered and washed using a 0.2 micron Nylon Millipore filter to remove all traces of acid. The solid is transferred to a drying dish and allowed to dry in air overnight. For the oxidation step of the synthesis, H2SO4 (460 ml) is placed into a 2 L Erlenmeyer flask and chilled to 0 °C using an ice bath. The pretreated graphite is then added to the acid and stirred. KMnO4 (60 g) is added slowly and allowed to dissolve with the aid of stirring, while the temperature is closely monitored so as not to allow the mixture to go above 10 °C. This mixture is then allowed to react at 35 °C for 2 hours after which distilled water (920 ml) is added, initially in 20-30 ml aliquots. Since the addition of the water causes the temperature of the mixture to rise rapidly, water addit