The work aims to determine the optimal spraying process parameters and analyze the mechanism of coatings deposition behavior by studying phase structure and microstructure of the coatings with different spraying process parameters. Nano-Yb2O3 stabilized ZrO2 (YbSZ) coating was prepared by solution precursor plasma spraying (SPPS). On the basis of tradi-tional plasma spraying, liquid atomizing device was added. The atomizing nozzle injected solution into plasma flame. The coating phase structure, crystallinity, grain size and microstructure were studied by controlling the spraying distance and spraying power, and the deposition mechanism was discussed in combination with microscopic morphology. The coating exhibited three microscopic morphologies: agglomerated large particles, nano-sized particles and uniform pores, and the large particles were stacked. When the spray power was 30 kW, the coating exhibited m-ZrO2 and the average grain size reached 669 nm. As the spraying distance and the spraying power increased, a single t-ZrO2 phase was detected in the sample, and the number of nano-sized particles greatly increased, and the pore diameter became small. As the spray distance increased from 60 mm to 100 mm, the average grain size was first reduced from 429 nm to 177 nm and then increased to 319 nm. The spraying parameters affect the crystallinity, grain size, and microscopic morphology of the coatings, and the coatings obtained at low power has a paste-like uncrystallized structure. Increasing the spraying power can effectively increase the crystallinity and grain size. As the spraying distance increases, the grain size decreases first and then increases. The atomized droplets in plasma flame generally undergo the process of concentration, saturation, solidification, nucleation and growth, particle melting and flattening. The higher the spraying power and the temperature zone are, the more complete the droplet evolution is. By optimizing the process parameters, functional coatings with different structural properties can be obtained.