Electrochemical energy storage devices have attracted considerable attention because of their ability to supply high energy and power in energy management systems. In this work, we synthesized highly electrochemically active nickel boride/nickel borate (NixB/NiBxOy) composite materials using a chemical coprecipitation method. The variation of precursor solution’s concentration controlled the chemical, morphological, surface area and structural properties of composite material. The electrochemical measurements of NixB/NiBxOy material display a high charge storage capacity of ~201.5 mAh/g at 5 mV s-1 scan rate amongst the different concentration. The charge storage capacity, rate capability and cycle stability of NixB/NiBxOy materials were effectively controlled by the material composition, structure, size, surface area and porosity feature through the charge kinetics, surface and diffusive capacity contribution and the battery–type charge storage mechanism. These findings provide an important insight to control electrochemical properties by optimizing the physical and chemical features of battery–type material.