Coupling in-situ X-ray micro- and nano-tomography and discrete element method for investigating high temperature sintering of metal and ceramic powders

¹ Univ. Grenoble Alpes, CNRS, SIMAP, 38000 Grenoble, France
² Universidad Michoacana de San Nicolás de Hidalgo, IIMM and INICIT, Fco. J. Mujica S/N, Ed. C-2 C.U., Morelia, Michoacán, C.P. 58060, Mexico
³ ESRF The European Synchrotron, CS 40220, 38043 Grenoble Cedex 9, France
⁴ Forschungszentrum Jülich Institute of Energy and Climate Research, D-52425 Jülich, Germany

^* e-mail: christophe.martin@grenoble-inp.fr
^** e-mail: didier.bouvard@grenoble-inp.fr

Published online: 30 June 2017

Abstract

The behaviour of various powder systems during high temperature sintering has been investigated by coupling X-ray microtomography and discrete element method (DEM). Both methods are particularly relevant to analyse particle interactions and porosity changes occurring during sintering. Two examples are presented. The first one deals with a copper powder including artificially created pores which sintering has been observed in situ at the European synchrotron and simulated by DEM. 3D images with a resolution of 1.5 μm have been taken at various times of the sintering cycle. The comparison of the real displacement of particle centers with the displacement derived from the mean field assumption demonstrates significant particle rearrangement in some regions of the sample. Although DEM simulation showed less rearrangement, it has been able to accurately predict the densification kinetics. The second example concerns multilayer ceramic capacitors (MLCCs) composed of hundreds of alternated metal electrode and ceramic dielectric layers. The observation of Ni-based MLCCs by synchrotron nanotomography at Argon National Laboratory with a spatial resolution between 10 and 50 nm allowed understanding the origin of heterogeneities formed in Ni layers during sintering. DEM simulations confirmed this analysis and provided clues for reducing these defects.