High performance supercapacitors have taken their place in the world as one of the research areas emerging in order to feed increasing energy consumption. By using metal oxides in electrode structures, supercapacitors have become advantageous products and have shed light on electrochemistry as low-cost materials. In this study, it was aimed to obtain nanocomposite materials as anode electrodes (FeCo2O4/Co3O4/Co3V2O8/Ni =FeCoVN) by using hydrothermal method for low cost, high storage capacity electrodes and synthesis of direct transition metal oxide (FeCo2O4) and cobalt vanadate (Co3V2O8) on nickel foam (Ni). A number of structures such as hetero-structures and hierarchical nanosphere with nanowire, nanorod, nanoflake, nanoplate structures were obtained. The relationship between temperature, reaction time and FeCl3 amount (g) parameters and changing electrochemical performances of the samples were interpreted by cyclic voltammetry (CV), galvanostatic charge-discharge measurements (GCD) and electrochemical impedance spectroscopy (EIS). Among anode electrodes, it was determined that the sample (the sample named 072–5 h) with a reaction time of 5 h at 120 °C and containing 0.72 g FeCl3 had the largest area in the CV (5 mV/s and from −0.3 to +0.6 V analysis. It has also been found that this sample has the largest capacitance value (3.5 F/cm2). When the GCD analysis results (for 1 A/cm2 current density) of 072–5 h nanocomposite material are evaluated, it can be said that it is the sample that preserves symmetry and linearity best and has the longest charge-discharge time. This shows that the 072–5 h nanocomposite material is promising for anode supercapacitors compared to other synthesized samples.