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Method and characterisation 3.7.1 Preparation of Graphene Oxide Graphene oxide was prepared by a modified Hummer’s method [103]. The preparation was carried out by mixing (5.0 g) graphite flakes (Graphite Trading Company) with sodium nitrate (4.5g, KNO3) and concentrated sulfuric acid (169 ml, H2SO4). The mixture was cooled in ice bath and potassium permanganate (22.5g, KMnO4) was slowly added (over 1hr) then left stirred to warm to room temperature for seven days. A dark mixture formed and was then dispersed into 550 ml of 5 wt% H2SO4 in water and stirred for a further three hours. After adding hydrogen peroxide (15 g, H2O2, 30 vol) a yellow/gold mixture was found and left stirred for two more hours. An additional dilution was made to the golden mixture with 500 ml of 3wt% of H2SO4 and 0.5wt% of H2O2 and left to stir overnight for washing purposes. The mixture was then centrifuged at 11000 rpm for 15 mins until a thick dark yellow viscous liquid was obtained. The washing process was repeated 12 times with same recipe (3wt% of H2SO4 and 0.5wt% of H2O2) as well as with a pure DI water until the mixture became neutral (pH 7). As a result of the washing process, a brawny-orange viscous liquid (GO) was obtained with concentration around 3.0 mg/ml. Figure 3.38 Modified Hummer’s method of graphene oxide Sirhan AL-Batty Page 122PDF Image | Membrane Electrode Assembly Modification by Zeolite and Graphene Oxide
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