RT Journal Article
T1 Rietveld Quantitative Phase Analysis of Oil Well Cement: in Situ Hydration Study at 150 Bars and 150 °C
A1 Fraga, Edmundo
A1 Cuesta-García, Ana María
A1 Zea-Garcia, Jesus D.
A1 Gómez-de-la-Torre, María de los  Ángeles
A1 Yañez-Casal, Armando
A1 García-Aranda, Miguel Ángel
AB Oil and gas well cements are multimineral materials that hydrate under high pressureand temperature. Their overall reactivity at early ages is studied by a number of techniquesincluding through the use of the consistometer. However, for a proper understanding of theperformance of these cements in the field, the reactivity of every component, in real‐worldconditions, must be analysed. To date, in situ high energy synchrotron powder diffraction studiesof hydrating oil well cement pastes have been carried out, but the quality of the data was notappropriated for Rietveld quantitative phase analyses. Therefore, the phase reactivities werefollowed by the inspection of the evolution of non‐overlapped diffraction peaks. Very recently, wehave developed a new cell specially designed to rotate under high pressure and temperature. Here,this spinning capillary cell is used for in situ studies of the hydration of a commercial oil wellcement paste at 150 bars and 150 °C. The powder diffraction data were analysed by the Rietveldmethod to quantitatively determine the reactivities of each component phase. The reaction degreeof alite was 90% after 7 hours, and that of belite was 42% at 14 hours. These analyses are accurate,as the in situ measured crystalline portlandite content at the end of the experiment, 12.9 wt%,compares relatively well with the value determined ex situ by thermal analysis, i.e., 14.0 wt%. Thecrystalline calcium silicates forming at 150 bars and 150 °C are also discussed.
PB MDPI - Publisher of Open Access Journals
YR 2019
FD 2019-06
LK https://hdl.handle.net/10630/17816
UL https://hdl.handle.net/10630/17816
LA eng
NO Materials 2019, 12, 1897
NO This research was funded by Spanish MINECO, grant number BIA2017‐82391‐R which is co‐fundedby FEDER.We thank Marc Malfois for his help during the experiment performed at NCD‐SWEETbeamline at ALBA synchrotron. We also thank Marcus Paul (Dyckerhoff GmbH) for providing the OWCsample with its characterization and helpful discussions.
DS RIUMA. Repositorio Institucional de la Universidad de Málaga
RD 11 abr 2026