RT Journal Article
T1 Mix and measure II: joint high-energy laboratory powder diffraction and microtomography for cement hydration studies
A1 Fernández-Sánchez, Jaime
A1 Cuesta, Ana
A1 Shirani, Shiva
A1 Redondo-Soto, Cinthya
A1 Torre, Ángeles G. de la
A1 Santacruz-Cruz, María Isabel
A1 Salcedo, Inés R.
A1 León-Reina, Laura
A1 García-Aranda, Miguel Ángel
K1 Cemento Portland -- Análisis
AB Portland cements (PCs) and cement blends are multiphase materials of differentfineness, and quantitatively analysing their hydration pathways is very chal-lenging. The dissolution (hydration) of the initial crystalline and amorphousphases must be determined, as well as the formation of labile (such as ettringite),reactive (such as portlandite) and amorphous (such as calcium silicate hydrategel) components. The microstructural changes with hydration time must also bemapped out. To address this robustly and accurately, an innovative approach isbeing developed based on in situ measurements of pastes without any sampleconditioning. Data are sequentially acquired by Mo K�1 laboratory X-raypowder diffraction (LXRPD) and microtomography (mCT), where the samevolume is scanned with time to reduce variability. Wide capillaries (2 mm indiameter) are key to avoid artefacts, e.g. self-desiccation, and to have excellentparticle averaging. This methodology is tested in three cement paste samples: (i)a commercial PC 52.5 R, (ii) a blend of 80 wt% of this PC and 20 wt% quartz, tosimulate an addition of supplementary cementitious materials, and (iii) a blendof 80 wt% PC and 20 wt% limestone, to simulate a limestone Portland cement.LXRPD data are acquired at 3 h and 1, 3, 7 and 28 days, and mCT data arecollected at 12 h and 1, 3, 7 and 28 days. Later age data can also be easilyacquired. In this methodology, the amounts of the crystalline phases are directlyobtained from Rietveld analysis and the amorphous phase contents are obtainedfrom mass-balance calculations. From the mCT study, and within the attainedspatial resolution, three components (porosity, hydrated products and unhy-drated cement particles) are determined. The analyses quantitatively demon-strate the filler effect of quartz and limestone in the hydration of alite and thecalcium aluminate phases. Further hydration details are discussed.
PB Wiley
YR 2024
FD 2024
LK https://hdl.handle.net/10630/32038
UL https://hdl.handle.net/10630/32038
LA eng
NO Fernandez-Sanchez, J., Cuesta, A., Shirani, S., Redondo-Soto, C., De la Torre, A. G., Santacruz, I., Salcedo, I. R., Leon-Reina, L. & Aranda, M. A. G. (2024). Mix and measure II: joint high-energy laboratory powder diffraction and microtomography for cement hydration studies. J. Appl. Cryst. 57.
NO Funding for open access charge: Universidad de Málaga / CBUA.
DS RIUMA. Repositorio Institucional de la Universidad de Málaga
RD 20 ene 2026