Air plasma spray technique (APS) is widely used in the biomedical industry for the development of HA-based biocoatings. The present study focuses on the influence of powder homogenization treatment by high-energy ball milling (HEBM) in developing a novel hydroxyapatite-barium titanate (HA/BT) composite coating deposited by APS; in order to compare the impact of the milling process, powders were homogenized by mechanical stirring homogenization (MSH) too. For the two-homogenization process,

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... weight percent ratios were studied; 10%, 30%, and 50% w/w of BT in the HA matrix. The phase and crystallite size were analyzed by X-ray diffraction patterns (XRD); the BT-phase distribution in the coating was analyzed by backscattered electron image (BSE) with a scanning electron microscope (SEM); the energy-dispersive X-ray spectroscopy (EDS) analysis was used to determinate the Ca/P molar ratio of the coatings, the degree of adhesion (bonding strength) of coatings was determinate by pull-out test according to ASTM C633, and finally the nanomechanical properties was determinate by nanoindentation. In the results, the HEBM powder processing shows better efficiency in phase distribution, being the 30% (w/w) of BT in HA matrix that promotes the best bonding strength performance and failure type conduct (cohesive-type), on the other hand HEBM powder treatment promotes a slightly greater crystal phase stability and crystal shrank conduct against MSH; the HEBM promotes a better behavior in the nanomechanical properties of (i) adhesive strength, (ii) cohesive/adhesive failure-type, (iii) stiffness, (iv) elastic modulus, and (v) hardness properties.