Spray pyrolysis-based synthesis of pure molybdenum powder with nanoscale primary particles and its sintering characteristics

Molybdenum (Mo) is a refractory metal with exceptional high-temperature stability, resistance to creep, and low coefficient of thermal expansion, it thus has great potential for various high-temperature applications. Nevertheless, conventional methods of synthesizing Mo powder, such as mechanical milling and wet chemical processing, have encountered limitations in producing sintered bodies with high relative density and a fine grain structure while maintaining a low sintering temperature. Therefore, it is crucial to develop an efficient powder synthesis method that enables precise and uniform control over the powder's size and shape while minimizing contamination. Such an approach would contribute to achieving excellent formability and sinterability for the resulting Mo sintered body. In this study, we successfully demonstrated the ultrasonic spray pyrolysis (USP) technique in combination with hydrogen reduction for synthesizing pure Mo powder. The resulting Mo powder exhibited micro-sized secondary particles composed of nanoscale primary particles, leading to improved formability and sinterability, essential for fabricating high-quality sintered bodies. In order to comprehensively understand the properties of the as-prepared molybdenum oxide and hydrogen-reduced Mo powder, we employed various methods to analyze its physicochemical characteristics systematically. Subsequently, the fine Mo particles were subjected to a pressureless sintering process after a conventional uniaxial powder molding. Due to its excellent formability and sinterability, we achieved a Mo sintered body with a grain size of approximately 3 μm while maintaining a relatively high sintering density of 98.3% at a comparatively low sintering temperature of 1400 °C. The resulting microstructure contributed to a relatively high hardness of around 234 Hv. These results indicate the successful synthesis of pure Mo powder with desirable properties and highlight its potential in various applications, particularly those requiring high-quality sintered bodies with enhanced hardness.