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Thick titanium coatings were prepared by the warm spraying (WS) and cold spraying (CS) processes to investigate the oxidation and microstructure of the coating layers. Prior to the coating formations, the temperature and velocity of in-flight titanium powder particles were numerically calculated. Significant oxidation occurred in the WS process using higher gas temperature conditions with low nitrogen flow rate, which is mixed to the flame jet of a high velocity oxy-fuel (HVOF) spray gun in order to control the temperature of the propellant gas. Oxidation, however, decreased strikingly as the nitrogen flow rate increased. In the CS process using nitrogen or helium as a propellant gas, little oxidation was observed. Even when scanning electron microscopy or an x-ray diffraction method did not detect oxides in the coating layers produced by WS using a high nitrogen flow rate or by CS using helium, the inert gas fusion method revealed minor increases of oxygen content from 0.01 to 0.2 wt.%. Most of the cross-sections of the coating layers prepared by conventional mechanical polishing looked dense. However, the cross-sections prepared by an ion-milling method revealed the actual microstructures containing small pores and unbounded interfaces between deposited particles.

Warm spraying has been developed by NIMS, in which powder particles are accelerated and simultaneously heated, and deposited onto a suitable substrate in thermally softened solid state. In this study, commercially available titanium powder was sprayed onto steel substrate by the spraying process. Microstructural developments and deposition behaviors from a deposited single particle to a thick coating layer were observed by high resolution electron microscopes. A single titanium particle sprayed onto the substrate was severely deformed and grain-refined mainly along the interfacial boundary of particle/substrate by the impact of the sprayed particle. A successive impact by another particle further deformed the previously deposited particle and induced additional grain refinement of the remaining part. In a thick coating layer, the severe deformation and grain refinement were also observed. The results have demonstrated the complex deposition behavior of sprayed particles in the warm spraying using thermally softened metallic powder particles.

High-resolution observations by electron microscopy have revealed the existence of nanoscale amorphous oxide film along the interfacial regions of kinetically sprayed titanium particles. The oxide was formed as the surface of feedstock particles was dynamically oxidized during the flight of several milliseconds. In spite of the severe plastic deformation associated with the impacts of these particles onto the substrate, as well as onto the previously deposited particles, some portion of the oxide remained, providing a bond between the particles.

Thermally softened titanium powder particles were impacted at about 760 m/s onto three substrate materials, i.e., titanium, aluminum, and zirconia, at the same time. In spite of the very different physicochemical properties of these substrate materials, most of particles were bonded to the substrate. However, their microstructures suggested different dynamic deformation behaviors and interface features. On titanium or zirconia substrate, particles showed shear instability and direct metallurgical bonding or metal-ceramic bonding that resulted from the removal of oxide covered on them, while on aluminum, although the particle was not heavily deformed and its oxide remained it was also bonded to the substrate due to the instability of substrate and the removal of aluminum oxide. The results have demonstrated the complex and material dependent nature of bonding formation in kinetic spraying using thermally softened metallic powder particles.

Titanium powder particles accelerated and simultaneously heated by the supersonic gas flow were deposited onto steel substrate by the warm spraying process. The sprayed particles were heavily deformed and bonded to the substrate in solid state. Especially, all the deposited particles showed jetting-out of materials out of the particle-substrate interface triggered by the adiabatic shear instability known to occur under such shock impact conditions. High-magnified images showed that grain refinement occurred in the jetting-out region by dynamic recrystallization. Furthermore, the elemental analysis using the electron energy loss spectrum showed jetting-outs of the substrate as well as the particle. Numerical simulation based on the Johnson-Cook plastic deformation model showed that the jetting-out phenomenon commences about 10 ns after the initial contact of the particle with the substrate and at a position away from the center bottom of particle, where the highest compressive stress is experienced.

Micron-sized titanium particles were deposited on steel substrates by the warm spraying, which is a modified high velocity oxy-fuel (HVOF) spraying technique. In the process, nitrogen gas is mixed with the HVOF flame jet to lower the temperature of injected powder particles. Detailed observations of splats formed on polished substrates by using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were conducted to investigate the effects of particle temperature on the bonding of splats with the substrate and the microstructure within the splats. At lower nitrogen flow rates, the particles observed were heavily deformed and exhibited diverse splat morphologies and microstructures. At higher nitrogen flow rates, most of the particles were impacted in the solid state and the oxidation of particles was remarkably less. The TEM observation revealed distinctively different microstructures within the splats as well as the splat/substrate interfaces depending on whether the particle was molten or solid before the impact.

A modification of high-velocity oxy-fuel (HVOF) thermal spray process named as warm spray (WS) has been developed. By injecting room temperature inert gas into the combustion gas jet of HVOF, the temperature of the propellant gas can be controlled in a range approximately from 2300 to 1000 K so that many powder materials can be deposited in thermally softened state at high impact velocity. In this review, the characteristics of WS process were analyzed by using gas dynamic simulation of the flow field and heating/acceleration of powder particles in comparison with HVOF, cold spray (CS), and high-velocity air-fuel (HVAF) spray. Transmission electron microscopy of WS and CS titanium splats revealed marked differences in the microstructures stemming from the different impact temperatures. Mechanical properties of several metallic coatings formed under different WS and CS conditions were compared. Characteristics of WC-Co coatings made by WS were demonstrated for wear resistant applications.