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Volume 112
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3D particle aggregation in consolidated clay systems: Insights from phase-contrast nano-holo-tomography
Angela Casarella a b *, Gustavo Pinzón c, Vijayshree Sadasivan a, Olga Stamati d, Julie Villanova c, Bratislav Lukić c e, Jelke Dijkstra a
a Chalmers University of Technology, Department of Architecture and Civil Engineering, Gothenburg, 43218, Sweden
b Imperial College London, Department of Civil and Environmental Engineering, London, SW72AZ, UK
c ESRF – The European Synchrotron, Grenoble, 38043, France
d Univ. Grenoble Alpes, CNRS, Grenoble INP, 3SR, Grenoble, 38000, France
e Institut Laue-Langevin, Grenoble, France
10.1016/j.partic.2026.02.002
Volume 112, May 2026, Pages 271-283
Received 15 October 2025, Revised 25 January 2026, Accepted 1 February 2026, Available online 9 February 2026, Version of Record 27 March 2026.
E-mail: a.casarella@imperial.ac.uk
Highlights

• First-ever non-destructive 3D imaging of saturated kaolin clay fabric.

• Face-to-face clay platelet stacks form in consolidated clay regardless of fluid.

• Pore fluid pH controls aggregates arrangement: edge-to-face (acidic) vs face-to-face (alkaline).

• Autocorrelation and local orientation methods quantify anisotropy without segmentation.

• Findings enable particle-scale evidence to inform and validate DEM.


Abstract

The microstructural arrangement of clay platelets governs their macroscopic properties, yet 3D observations at the particle scale remain limited. This study employs radiation-based X-ray phase-contrast nano-holo-tomography (nano-CT) to achieve an unprecedented three-dimensional (3D) characterisation of clay particle fabric in saturated kaolin clay samples subjected to one-dimensional (1D) compression. Two samples were prepared with acidic (pH = 4.1) and alkaline (pH = 9.1) pore fluids to examine the influence of electrochemical conditions on the association of clay particle. Phase-contrast nano-CT resolves individual kaolin platelets and their spatial arrangement, enabling quantitative analysis of fabric. Autocorrelation function analyses are used to study the alignment of a macroscopically isotropic, yet locally anisotropic structure for the acidic sample, where the edge-to-face (EF) associations of stacks of particles (i.e., aggregates) dominate. In contrast, the alkaline sample exhibits a highly anisotropic, face-to-face (FF) aligned aggregate configuration. These findings contribute to a deeper understanding of clay fabric characterisation and highlight the potential of non-destructive synchrotron X-ray 3D nano-imaging techniques for advancing clayey materials characterisation.

Graphical abstract
Keywords
Clay microstructure; X-ray nano-tomography; Fabric; Kaolin; Pore fluid pH; Orientation
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