Sonochemical degradation of urea was employed to synthesize alpha-nickel hydroxide from different nickel salts. Utilization of ultrasound yielded products with properties significantly different than the products obtained by thermal degradation of urea. The effect of intercalating chloride, nitrate, acetate, and sulfate anions on morphology and electrochemical performance was studied. The sulfate-intercalated sample had the smallest interlayer spacing when obtained by the sonochemical method, contradicting all the previous thermal synthesis results. The specific capacitance trend also differed from the literature values, and the value for the sulfate-intercalated sample was larger than that of acetate- and nitrate-intercalated samples. Ultrasonic synthesis increased the specific capacitance of the sulfate-intercalated sample significantly. This sample was also the most reversible and had the highest charge efficiency.