The work aims to investigate the effects of different particle sizes of micron agglomerated powders on the properties of GYbZ thermal barrier coatings prepared by plasma spray-physical vapor deposition (PS-PVD). With micron agglomerated (Gd0.9Yb0.1)2Zr2O7 (GYbZ) powder as raw material, the thermal barrier coating of GYbZ was prepared on the surface of nickel-based superalloy by PS-PVD process with three agglomerated powders with different particle sizes. The average particle size of the powder was 2-3 μm. A planetary ball mill was used to mix the two powders. The molar ratio of Gd2Zr2O7 to Yb2O3 was 9:1. The agglomerated powder obtained by spray granulation was sieved and dried in a constant temperature oven at 70℃ until taken out before spraying. In this paper, the preparation of the coating was divided into two stages:the preparation of the bonding layer and the preparation of the ceramic layer. Both the bonding layer and the ceramic layer were prepared by plasma spraying physical vapor deposition (PS-PVD). In this work, double-ceramic layer material system was adopted. In the GYbZ/YSZ double-ceramic layer thermal barrier coating system, the YSZ layer was located between the GYbZ and the metal bonding layer. YSZ can improve the thermal expansion coefficient mismatch between the GYbZ and the metal bonding layer. A YSZ layer with a thickness of about 200 μm was prepared on the surface of the adhesive layer by PS-PVD technology, and then a GYbZ coating was prepared on the YSZ coating, and the thickness of the GYbZ coating was about 100 μm. The total thickness of the ceramic layer was about 300 μm. X-ray diffractometer (XRD) was used to analyze the phase of the sprayed agglomerated powder and sprayed coating; the surface and cross-section of the agglomerated powder and coating samples were observed by scanning electron microscope (SEM); The bonding strength of the coating was tested by the electronic testing machine; the thermal shock resistance of the coating was tested by an automatic water quenching machine. Results showed that with the decrease of the powder particle size, powders of spherical degree became worse, and the porosity of the powder increased gradually, The smaller the powder particle size, the higher the gasification rate of spraying, the less unmelted particles in the coating, and the more obvious the coating plume-columnar structure. However, when the powder with D50 of 13 μm was sprayed, due to the too small particle size and poor fluidity of the powder, part of the powder cannot pass through the nozzle smoothly and reach the center of the plasma flame during the powder feeding process. The deposition rate of the coating was slightly reduced. The GYbZ agglomerated powder diffraction pattern showed the stacking of Gd2Zr2O7 and Yb2O3 phases, while the GYbZ coating diffraction pattern showed a single defect fluorite structure. At the same time, with the reduction of the particle size of the agglomerated powder, the mechanical properties and thermal shock resistance of the corresponding coatings were significantly improved. The conclusion of this paper is that the coating prepared with the agglomerated powder with D50 of 13 μm has a complete feather-column structure with the highest bonding strength and the best thermal shock resistance.