The current article reports a preparation method of nano-petal nickel hydroxide, which was synthesized using urea as a precipitator by hydrothermal method. Nickel hydroxide samples with different microstructural characteristics were prepared by changing molar ratio of nickel/urea and reaction time. The prepared nickel hydroxide samples were characterized using X-ray diffraction(XRD) and scanning electron micrography(SEM).Electrochemical performances of the samples were then determined under charging–discharging rate of 0.2C. The influences of different conditions of the hydrothermal synthesis method on microstructure parameters of nickel hydroxide were analyzed, while relationships between microstructural characteristics parameters of nickel hydroxide and the electrochemical performances of nickel electrode were also explored. The current article reports a preparation method of nano-petal nickel hydroxide, which was synthesized using urea as a precipitator by hydrothermal method. Nickel hydroxide samples with different microstructural characteristics were prepared by changing molar ratio of nickel / urea and reaction time. The prepared nickel hydroxide samples were characterized using X-ray diffraction (XRD) and scanning electron micrography (SEM). Electrochemical performances of the samples were then determined at charging-discharging rate of 0.2C. The influences of different conditions of the hydrothermal synthesis method on microstructure parameters of nickel hydroxide were analyzed, while relationships between microstructural characteristics parameters of nickel hydroxide and the electrochemical performances of nickel electrode were also explored.