本實驗使用天然石墨以改良Hummers方法製備石墨烯氧化物(graphene oxide, GO),利用硼氫化鈉還原成石墨烯(reduced graphene oxide, rGO),與利用熱剝離方式還原的商業用石墨烯(Commercial graphene, CG)為基材,以不同無電鍍參數於石墨烯上沉積鐵鎳磷奈米顆粒形成鐵鎳磷/石墨烯奈米複合材料,探討無電鍍參數及不同製備方法合成的石墨烯對Fe-Ni-P/Graphene微觀結構與性質的影響。 由XRD分析發現天然石墨經過氧化後,層間距離由0.338nm增加到0.785nm,以硼氫化鈉方法還原後發現C軸平面峰消失,顯示出石墨不再沿著C軸排列而導致結晶性變差。 無電鍍鐵鎳參數為固定鍍液溫度50℃、析鍍時間3min,改變鐵鎳離子比、鍍液pH值,隨著鐵鎳離子比增加,鐵含量跟著提高,在鐵鎳離子比(Fe2+/Ni2+)為9時最高鐵含量高達34.23%。 本實驗於石墨烯氧化還原過程以及無電鍍沉積鐵鎳金屬都是在溶液中進行,雖然CG在微觀結構觀察下比rGO更薄,但由於石墨烯為疏水性的緣故,為減少接觸面積,在溶液中會因此產生堆疊、團聚的現象,而表面皺褶則是因要減少表面能而產生,所以嘗試將CG經改良Hummers方法氧化增加親水性、讓石墨烯分散於水溶液中,試著讓CG趨近於單層、減少皺褶、面積展延的狀態。 將鐵鎳金屬沉積在氧化CG上,以微觀結構觀察其表面形貌以及金屬粒子分布狀況可發現,金屬粒子均勻分佈在石墨烯上,石墨烯比較不易堆疊、且金屬粒子分佈較均勻。
Graphene is a subject of great interest due to their unique structure and excellent properties, such as superior electronic conductivity, extremely high specific surface area, large surface to volume ratio and high stability. The excellent properties of graphene enable them to be a suitable catalyst support. In this study, Fe-Ni particles are deposited on surface of two kinds of graphene which was prepared by chemical method, one was fabricated f by using modified Hummers method first, and then was reduced to Graphene (rGO) by sodium borohydride, the other is commercial graphene (CG) that was exfoliated by thermal energy. According to the last experimental results, the Fe content of Fe-Ni-P nanoparticles deposited on rGO increases with ratio of Fe2+/Ni2+ (1~7 ), and the highest content of Fe is 29.3at%. In this study, the electroless Fe-Ni plating on rGO was at pH10, Fe2+/Ni2+=1~9, 50℃, for 3 minuteudys and in Ar atmosphere. And the composition of deposits are analyzed by EDS and listed in Table 1. The highest content of Fe rises to 34.23at%. The XRD results reveal that Crystal Ni (111) phase is evident for Fe2+/Ni2+=1 and gradually decays with ratio of Fe2+/Ni2+. CG could turning hydrophobic into hydrophilic by using oxidizadation to attach functional group by modified Hummer’s method, and then after electoless Fe-Ni plating, oxidized CG was deposited many uniform Fe-Ni nano particles on the surface of oxidized CG.