RT Journal Article
T1 Mix and measure - Combining in situ X-ray powder diffraction and microtomography for accurate hydrating cement studies.
A1 Shirani, Shiva
A1 Cuesta-García, Ana María
A1 Gómez-de-la-Torre, María de los  Ángeles
A1 Santacruz-Cruz, María Isabel
A1 Koufany, Imane
A1 Redondo-Soto, Cinthya
A1 Salcedo, Inés R.
A1 León-Reina, Laura
A1 García-Aranda, Miguel Ángel
K1 Cemento Portland
K1 Rayos X - Difracción
K1 Sistemas de imágenes
AB It is reported an innovative methodology based on in situ MoKα1 laboratory X-ray powder diffraction (LXRPD)and microtomography (μCT) avoiding any sample conditioning. The pastes are injected in 2.0 mm capillaries andthe extremes are just sealed. The measurements take place in the same region of the hydrating paste. Thickcapillaries are key to avoiding self-desiccation, which dictates the need of high-energy X-ray radiation for thediffraction study. This approach has been tested with a PC 42.5 R paste having w/c = 0.50. μCT data werecollected at 12 h and 1, 3, 7 and 79 days. LXRPD data were acquired at 1, 3, 7 and 77 days. In this proof-ofprincipleresearch, the same paste was also cured ex situ. Portlandite contents obtained by thermal analysis,ex situ powder diffraction, in situ mass balance calculation and in situ powder diffraction were 13.8, 13.1, 13.1and 12.5 wt%, respectively. From the μCT study, the grey value histogram evolution with time showed a crossingpoint which allowed us to distinguish (appearing) hydrated products from (dissolving) unhydrated cementparticles. Segmentations were carried out by global thresholding and the random forest approach (one type ofsupervised Machine Learning). The comparison of the segmented results for the unhydrated cement fraction andthe Rietveld quantitative phase analysis outputs gave an agreement of 2 %. The potential of this methodology todeal with more complex binders is also presented.
PB Elsevier
YR 2023
FD 2023-11-14
LK https://hdl.handle.net/10630/28312
UL https://hdl.handle.net/10630/28312
LA eng
NO S. Shirani, A. Cuesta, A.G. De la Torre, I. Santacruz, A. Morales-Cantero, I. Koufany, C. Redondo-Soto, I.R. Salcedo, L. León-Reina, M.A.G. Aranda, Mix and measure - Combining in situ X-ray powder diffraction and microtomography for accurate hydrating cement studies, Cement and Concrete Research, Volume 175, 2024, 107370, ISSN 0008-8846, https://doi.org/10.1016/j.cemconres.2023.107370
NO This research was partly supported by the research grant PID2020-114650RB-I00 of Agencia Estatal de Investigacion which is co-funded byERDF.
DS RIUMA. Repositorio Institucional de la Universidad de Málaga
RD 19 ene 2026