Synthesis of high-purity and defined oxide nanopowders using pulsating spray pyrolysis
BEGAND S. 1, FRICKEL A. 1, DRESCHER V. 2
1 Fraunhofer IKTS, Hermsdorf, Germany; 2 Glatt Ingenieurtechnik GmbH, Weimar, Germany
The production of transparent and optoceramics but also active materials for battery storage or oxide ceramics for medical technology products increasingly requires powder materials that are characterized by nanoscale grain sizes, high purity and a defined phase composition. Fraunhofer IKTS and Glatt Ingenieurtechnik are pursuing the synthesis of oxide nanopowders based on pulsed spray pyrolysis in the project "PulsON". The new synthesis plant can realize a process gas from room temperature up to 1300° C, depending on the product requirements. This flexibility is realized by an electric heater that prevents contamination of the product by combustion residues, which is mandatory for high purity products like the optoceramics used in this project. In addition, this kind of heat source allows highest flexibility regarding process gases (oxidizing, inert or reducing) and raw materials (solutions, suspensions, emulsions or powders). The unique feature of the technology is a pulsator unit which creates an oscillating process gas stream with frequencies up to 400 Hz and amplitudes of up to 60 mbar. As a result, a high amount of turbulences is created within the gas flow, which proved to be very beneficial on the interaction between gas and spray droplets: Primary droplets will be further atomized and heat and mass transfer rates will be increased significantly. This allows decomposition, precipitation, and the subsequent crystallization to take place in very short process times. A major goal in this project is to determine the interrelationship between the precursors, the process parameters, and the powder properties. Among others, the influence of different pulsation states and the use of precursor additives promises the controlled adjustment of particle morphology and primary crystallite sizes. The material system selected for this purpose is Mg-Al-Spinel. For the first time, the process engineering advantages of high-temperature synthesis can be exploited, since the target stoichiometries and phases of the powders can be precisely controlled based on the very short heating times, the highly effective, homogeneous heat input and controllable residence times in the synthesis plant. These experimental results are supported by computer-based simulations. They give a deeper insight into the interaction between plant geometry, gas stream and particle movement to understand the interrelationship between these parameters and lead to process guidelines to move on from lab-scale to production-scale.