In order to identify changes in the nature of the particles due to changes in the inflow rate of the raw material solution, the present study was intended to prepare nano-sized cobalt oxide (Co3O4) powder with an average particle size of 50 nm or less by spray pyrolysis reaction using raw cobalt chloride solution. As the inflow rate of the raw material solution increased, droplets formed by the pyrolysis reaction showed more divided form and the particle size distribution was more uneven. As the inflow rate of the solution increased from 2 to 10 ml/min, the average particle size of the formed particles increased from about 25 nm to 40 nm, while the average particle size did not show significant changes when the inflow rate increased from 10 to 50 ml/min. XRD analysis showed that the intensity of the XRD peaks increased remarkably when the inflow rate of the solution increased from 2 to 10 ml/min. On the other hand, the peak intensity stayed almost constant when the inflow rate increased from 10 to 50 ml/min. With the increase in the inflow rate from 2 to 10 ml/min, the specific surface area of the particles decreased by approximately 20 %. On the contrary, the specific surface area stayed constant when the inflow rate increased from 10 to 50 ml/min.