A Study of Parameters and Properties Influencing the Size, Morphology and Oxygen Content of Water Atomized Metal Powders
Time: Mon 2021-12-20 10.00
Subject area: Materials Science and Engineering
Doctoral student: Fredrik Persson , Processer
Opponent: Professor emeritus Lauri Holappa, Aalto University, Finland
Supervisor: Professor Pär Jönsson, Processer; Assistant Professor Christopher Neil Hulme,
The production of metal powders by water atomization is a well-established process, which can be used to produce a wide range of particle sizes for different applications. In general, there is a lack of detailed knowledge about what process parameters that affect the powder properties for water atomized metal powders. More specifically, this thesis focuses on the particle size, morphology and oxygen content of water atomized iron powders. A careful control of the particle size distribution is necessary to atomize powders with a high quality and at a low production cost. Demands on the particle morphologies vary depending on the application for the final product. It is important to control both the melt properties and atomizing parameters, to produce powders with an even particle shape and sintered steel components with tight tolerances. The oxidation of the liquid metal should also be as low as possible during the water atomization, to avoid a large amount of harmful oxide forming in the final powder. Pores are generally considered as defects in metal powders. Therefore, the powder porosity should be as low as possible.
The main objective of this thesis is to obtain a more in-depth knowledge of water atomization of metal powders, by investigating some fundamental parts of the process. The study investigates how the median particle size (d50 value) for iron powders is influenced by the water pressure, the melt stream diameter, the jet angle, the water level in the atomizing tank, changed configurations of the water jets, superheat of the melt, and the carbon and sulfur content in the liquid steel. Similarly, the thesis also investigates factors that influence the particle shape, porosity and oxidation of water atomized iron powders.
Laboratory and pilot experiments show that the effect on the d50 value was large for the water pressure, medium for the viscosity, surface tension and water to metal ratio, and small for the melt stream diameter. Calculations indicate that the water jet angle has a large effect on the d50 value. In practice, this effect cannot be exploited beyond certain limits caused by instabilities in the atomizing system, which occur if the jet angle is too large.
The particle size decreases when the carbon and sulfur contents in the liquid iron are increased. This is attributed to decreased viscosities and surface tensions, respectively. An alternative explanation could be that the superheats at increased carbon contents result in a longer time spent in the molten state before the atomization is completed. This may also lead to a decrease in the particle size. Calculations using a developed d50 model estimate that a decreased viscosity from 6.8 mPa s to 4.3 mPa s leads to a reduction in the d50 value by 33%. Similarly, a decreased surface tension from 1840 mN/m to 900 mN m-1 reduces the d50 value by 27%.
The distribution of oxides in pilot water atomized Fe-Mn-C powders was determined by using optical and scanning electron microscopy, combined with energy dispersive X-ray microanalysis. The oxygen in the atomized powders was mainly present as thin surface oxide layers, which increase in thickness from 10 nm to 50 nm as the particle sizes increase from 10 microns to 750 microns. Manganese oxides were observed to be unevenly distributed at the surface of several particles, when the alloy contained 0.3 wt.% manganese. Experimental data indicate that between 10 - 20% of the manganese was present as oxides in the powders. However, equilibrium calculations at 1550 °C estimate that only 4% of the initial manganese content remained in the steel after a completed atomization.
The sphericity of the atomized powders decreases as the particle size increases. One feasible explanation is that some larger particles are irregular, since they are formed by collisions of smaller particles. Conversely, smaller particles are formed directly from breakups of the melt and are not the product of collisions between droplets. The sphericity of the size fraction 20-45 microns increases as the carbon content in the iron increases from 0.2 wt.% to 4.2 wt.%. The atomized droplets with larger carbon contents spend a longer time in the molten state, which allows them more time to form a spherical shape during the atomization process. The porosity of iron-carbon powders increases with increasing carbon contents in the melt. Dissociation of steam to hydrogen at the melt surface and precipitation of hydrogen pores in the melt were the most likely mechanisms to cause a pore formation in the powders.
Keywords: water atomization; metal powder: particle size; oxygen content; particle shape; porosity; steelmaking