Liquid phase sintering of W-Ni-Fe composites liquid penetration, agglomerate separation and tungsten particle growth

University dissertation from Stockholm : KTH

Abstract: The initial stage of liquid phase sintering, involving liquid penetration, agglomerate separation, particle spreading and growth has been investigated in experiments using tungsten heavy alloys. The particle composites used were produced by hot isostatic pressing (HIP) of pure powder mixtures of W-Ni-Fe-(Co). By using different HIP temperatures, volume fractions of tungsten, alloying elements like Cobalt and Sulphur or excluding Iron from the matrix, liquid penetration, agglomerate separation and particle growth conditions were affected. The investigations were performed mainly under microgravity (sounding rockets or parabolic trajectories by airplanes) but at high tungsten particle fractions, short sintering times or at infiltration of solid pure tungsten, they were performed at normal gravity. The liquid penetration of the tungsten agglomerates is explained by initial wetting under non-equilibrium conditions, due to the reaction between the liquid matrix and the particles, and a decrease of interfacial energy. The dissolving of tungsten gives a pressure drop in the penetrating liquid and a driving force for the liquid movement by a suggested parabolic penetration model. For cold worked tungsten, a penetration theory was proposed, where an internal stress release in the penetrated tungsten grains creates space for the advancing liquid.The spreading of the tungsten agglomerates is explained by an interagglomerate melt swelling due to a Kirkendall effect. The liquid matrix undergoes a volume increase since the diffusion rates of Ni-Fe are higher than for W and initial concentration gradients of W and Ni, Fe exists. The suggested model by Kirkendall are also used for an analysis of the interaction behaviour between solid particles and a solidification front and inclusion behaviour in iron base alloys during teeming and deoxidation.The average tungsten particles size decrease initially since part of the tungsten particles is dissolved when the non-equilibrium matrix phase is melting. When equilibrium is reached, the tungsten particles grow in accordance with the Ostwald ripening process by an approximately 1/3 power law. Larger particle fraction of particles showed a higher growth rate, due to shorter diffusion distances between the particles. Cobalt, Sulphur and absence of iron in the matrix were found to increase the growth rate of the tungsten particles due to a higher surface tension between the solid tungsten particles and the matrix melt.