Cryo‐FIB‐nanotomography for quantitative analysis of particle structures in cement suspensions

Abstract

SummaryCryo-FIB-nanotomography is a novel high-resolution 3D-microscopy technique, which opens new possibilities for the quantitative microstructural analysis of complex suspensions. In this paper, we describe the microstructural changes associated with dissolution and precipitation processes occurring in a fresh cement paste, which has high alumina and sulphate contents. During the first 6 min, precipitation of ettringite leads to a general decrease of the particle size distribution. In the unhydrated cement paste almost no particles smaller than 500 nm are present, whereas after 6 min this size class already represents 9 vol%. The precipitation of ettringite also leads to a significant increase of the particle number density from 0.294 * 10 9 /mm 3 at t 0min to 20.55 * 10 9 /mm 3 at t 6min . Correspondingly the surface area increases from 0.75 m 2 /g at t 0min to 2.13 m 2 /g at t 6min . The small ettringite particles tend to form agglomerates, which strongly influence the rheological properties. The particular strength of cryo-FIB-nt is the potential to quantify particle structures in suspension and thereby also to describe higher-order topological features such as the particle-particle interfaces, which is important for the study of agglomeration processes.

Variations in the morphology of porosity in the Boom Clay Formation: insights from 2D high resolution BIB-SEM imaging and Mercury injection Porosimetry

“…Recent developments in the field of micro-focus X-ray computed tomography (μ-CT) (Bésuelle et al, 2006;Jin, 2007;Bugani et al, 2009;Sok et al, 2009;Bell et al, 2011;Cnudde et al, 2011) allow describing the 3D fabrics of clay materials and its evolution under load, but the resolutions achieved are not good enough to resolve porosity. The emergence of ion-beam milling tools, like focussed (FIB) and broad-ion-beam (BIB) cross-sectioning (Holzer et al, 2006(Holzer et al, , 2007(Holzer et al, , 2010Loucks et al, 2009;Desbois et al, 2010a, b;2011a, b;Holzer & Cantoni, 2012) led to an important progress in imaging microstructures and porosity in argillaceous materials, down to the nm-scale resolution. FIB serial cross-sectioning allows reconstructing 3D microstructures (Van Geet et al, 2008;Heath et al, 2011;Keller et al, 2011).…”

Imaging pore space in tight gas sandstone reservoir: insights from broad ion beam cross-sectioning

“…Focussed Ion Beam (FIB) technique was also demonstrated to be able to prepare high quality polished cross-sections in clay-rich geomaterials ( [4], [6]). However, this technique induces potentially more damage to the surface since it uses mainly Gallium source ( [7]) and typical areas produced by FIB (about µm 2 ) are much smaller than those prepared by BIB (about mm 2 ).…”

“…Consequently, image analysis and structural-geometrical interpretation has been of limited confidence ( [1], [2]). The recent development of Argon ion source milling tools which allow producing polished cross-sections of exceptionally high quality offer now a new technical milestone of surface preparation suitable for high resolution porosity SEM imaging at nano-scale ( [3], [4], [5], [6]). …”

Toward Reproducible Three-Dimensional Microstructure Analysis of Granular Materials and Complex Suspensions

“…For this purpose the solution can be vitrified with high pressure freezing~Bachmann & Mayer, 1987;Moor, 1987;Monaghan et al, 1998!. Because it is beyond the scope of this article to discuss the details of high pressure freezing and of cryoimaging, we are referring to previous publications about cryo-FIB applications on cement suspensions Holzer et al, 2007;Zingg et al, 2008!. With the present case study, we intend to evaluate the methodological reproducibility of particle analysis based on cryo-FIB-nt.…”

“…FIB-nt is a rather novel 3D microscopy technique that was successfully applied in various materials science disciplines during the last few years~Inkson et al, 2001;Holzer et al, 2004Holzer et al, , 2006Holzer et al, , 2007Konrad et al, 2006;Uchic et al, 2006Uchic et al, , 2007Wilson et al, 2006;Holzapfel et al, 2007;McGrouther & Munroe, 2007;Velichko et al, 2007!. FIB-nt is based on a serial sectioning procedure with a dual beam FIB-scanning electron microscopy~SEM!…”