Belonging to the technical field of inorganic nano-materials, the invention specifically relates to a preparation method of a hollow Ni-Zn ferrite microsphere. The method comprises: taking 6g of glucose and dissolving it totally in 60ml of deionized water; shifting the solution into a high pressure reactor of 100ml in volume, and leaving the solution to react at a temperature of 180DEG C for 8h, then subjecting a prepared turbid solution to 5min of centrifugation by a high speed centrifuge at a speed of 16000rpm; dissolving 0.268g of NiCl3.6H2O, 0.045g of ZnCl2.6H2O, and 0.079g of FeCl3.6H2O in 60ml of ethylene glycol, and conducting magnetic stirring at a temperature of 25DEG C for 30min; then adding 0.6g-3g of urea into the turbid solution; weighing 0.3g-0.6g of a prepared microsphere which is then added into the turbid solution, carrying out ultrasonic treatment for 2min and magnetic stirring for 10min so as to obtain a black suspending liquid, then drying the liquid at a temperature of 60DEG C. The method of the invention provides a good approach and idea for synthesizing hollow inorganic nano-microspheres.