Nickel nanoparticles supported on metal oxides were prepared by a modified electroless nickel-plating method. The process and mechanism of electroless plating were studied by changing the active metal (Ag) loading, acidity, and surface area of metal oxides and were characterized by UV–vis spectroscopy, transmission electron microscopy, scanning electron microscopy, and H 2 chemisorption. The results showed that the dispersion of nickel nanoparticles was dependent on the interface reaction between the metal oxide and the plating solution or the active metal and the plating solution. The Ag loading and acidity of the metal oxide mainly affected the interface reaction to change the dispersion of nickel nanoparticles. The use of ultrasonic waves and microwaves and the change of solvents from water to ethylene glycol in the electroless plating could affect the dispersion and size of nickel nanoparticles.