Composites of graphene (oxide) (GO) and first-row transition-metal cations( Co 2 + ,N i 2 + ,M n 2 + ,F e 2 + )a re prepared by mixingG Oa nd aqueous metal salt solutions. The amount of metal cation bound to GO nanosheets is calculated by using inductively coupled plasma mass spectrometry (ICP-MS) andt he possible binding sites of the metalsa re investigated by meanso fa ttenuated total reflectance infrared (ATR-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS) measurements. Electrodes loaded with the metal/GO composites are prepared by as imple drop-casting technique without any binderso rc onductive additives.T he effect of electrochemical reduction on the structure of the composite electrodes is investigated by Raman spectroscopy, XPS, X-ray diffraction (XRD) analysis, and field emission scanninge lectron microscopy (FESEM). Ad etailed electrochemical characterization is performed for the utilization of the composite electrodes for electrochemical capacitors and possible oxygen reduction reactione lectrocatalysts by cyclic voltammetry (CV) and rotatingd isk electrode measurements. The highest areal capacitance is achieved with the as-deposited Fe/GO composite (38.7 mF cm À2 at 20 mV s À1 ). In the cyclic stabilitym easurements, rCo/GO, rNi/GO, rMn/GO, and rFe/ GO exhibit ac apacitance retention of 44, 1.1, 73, and 87 % after 3000cycles of CV at 100 mV s À1 ,r espectively.[a] Dr.