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In situ Probing of Interfacial Roughness and Transient Phases During Ceramic Cold Sintering Process



Fan Zhang, Russell Maier, Igor Levin, Andrew J. Allen, Jun-Sang Park, Peter Kenesei, Ivan Kuzmenko, Jan Ilavsky, Pete Jemian


The ceramic cold sintering process (CSP) offers an eco-friendly approach to producing fully dense ceramics at low temperatures. However, an incomplete mechanistic understanding hinders its optimization and widespread adoption. In this study, we analyze the microstructural and structural changes in ZnO, a model CSP system, using in situ synchrotron-based high-energy small-angle X-ray scattering and X-ray diffraction techniques. Our results reveal the time evolution of ZnO particles' surface area and roughness, reflecting the dissolution and re-precipitation processes that enable densification. The in situ measurements supply valuable kinetic data for these stages of CSP. Alongside microstructural changes and densification, we observed the evolution of secondary phases representing reaction products between ZnO and acetic acid, the solvent used. The initial ZnO/solvent mixture's dominant secondary phase is attributed to zinc acetate, which is gradually replaced by a zinc soap-type structure during CSP. This structure has a large (≈21 Å) lattice parameter and is assumed to have a layered nature. The formation of this soap phase appears to be a signature of successful cold sintering, as it facilitates mass transport, leading to densification. This soap phase is retained in the sintered sample as an intergranular component. This study underscores the potential of in situ synchrotron characterization for revealing microstructural and phase evolution details during CSP. These findings, which would be challenging to obtain through ex situ measurements, provide crucial data to guide and validate theoretical models, ultimately enhancing CSP's effectiveness and adoption.
ACTA Materialia


synchrotron, in situ, ceramics, processing, cold sintering


Zhang, F. , Maier, R. , Levin, I. , Allen, A. , Park, J. , Kenesei, P. , Kuzmenko, I. , Ilavsky, J. and Jemian, P. (2023), In situ Probing of Interfacial Roughness and Transient Phases During Ceramic Cold Sintering Process, ACTA Materialia, [online],, (Accessed May 21, 2024)


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Created October 15, 2023, Updated September 5, 2023