Roman Loser

Analysis of cement-bonded materials by multi-cycle mercury intrusion and nitrogen sorption.

The pore systems of cement-based materials are studied by N(2) sorption and mercury intrusion porosimetry (MIP). Pore size distributions and internal surfaces are derived. Especially in materials with a broad pore size distribution, these (and other) methods generally do not lead to coincident results. It is shown here, how the interpretation of the experimental data of the two methods may be modified in order to obtain coincident pore size distributions from both methods. The studied pore systems are described as array of chambers which are connected by smaller throats. N(2) adsorption is used to calculate the size of the pores, whereby no distinction between throat or chamber type is possible with this method. Assuming mercury entrapping in ink-bottle type pores (pores that are connected to an external surface through smaller pores only) being the dominant process for mercury snap-off during extrusion and applying multi-cycle MIP, the calculation of the size of the entrances of these ink-bottles is possible. It is shown that similar results also may be derived from mercury extrusion data by applying a contact angle correction for the retracting mercury meniscus. A good agreement of the pore size distribution of the connected, non-ink-bottle type pores derived from either N(2) sorption or mercury intrusion is obtained. Samples of cement paste and mortar are analysed. A significant difference between cement paste and mortar regarding the neck entrances of ink-bottle type pores is found and attributed to the coarse pore space around the aggregates, the interfacial transition zone.

Focussed ion beam nanotomography reveals the 3D morphology of different solid phases in hardened cement pastes

Due to the development of integrated low‐keV back‐scattered electron detectors, it has become possible in focussed ion beam nanotomography to segment not only solid matter and porosity of hardened cement paste, but also to distinguish different phases within the solid matter. This paper illustrates a method that combines two different approaches for improving the contrast between different phases in the solid matrix of a cement paste. The first approach is based on the application of a specially developed 3D diffusion filter. The second approach is based on a modified data‐acquisition procedure during focussed ion beam nanotomography. A pair of electron images is acquired for each slice in the focussed ion beam nanotomography dataset. The first image is captured immediately after ion beam milling; the second image is taken after a prolonged exposure to electron beam scanning. The acquisition of complementary focussed ion beam nanotomography datasets and processing the images with a 3D anisotropic diffusion filter allows distinguishing different phases within the hydration products.