RT Journal Article
T1 High pressure and temperature spinning capillary cell for in-situ synchrotron X-ray powder diffraction
A1 Fraga, Edmundo
A1 Yáñez, Armando
A1 Zea-Garcia, Jesus D.
A1 Gómez-de-la-Torre, María de los  Ángeles
A1 Cuesta-García, Ana María
A1 Valcárcel-Fernández, Ricardo
A1 Farré-París, Francesc
A1 Malfois, Marc
A1 García-Aranda, Miguel Ángel
K1 Materiales a altas presiones
K1 Resistencia de materiales
K1 Pozos petrolíferos - Materiales
K1 Cemento
AB In situ research of materials under moderate pressures (hundreds of bar) is essential in many scientific fields. These range from gas sorption to chemical and biological processes. One industrially important discipline is the hydration of oil well cements. Existing capillary cells in this pressure range are static as they are easy to design and operate. This is convenient for the study of single-phase materials; however, powder diffraction quantitative analyses for multiphase systems cannot be performed accurately as a good powder average cannot be attained. Here, the design, construction and commissioning of a cost-effective spinning capillary cell for in situ powder X-ray diffraction is reported, for pressures currently up to 200 bar. The design addresses the importance of reducing the stress on the capillary by mechanically synchronizing the applied rotation power and alignment on both sides of the capillary while allowing the displacement of the supports needed to accommodate different capillaries sizes and to insert the sample within the tube. This cell can be utilized for multiple purposes allowing the introduction of gas or liquid from both ends of the capillary. The commissioning is reported for the hydration of a commercial oil well cement at 150 bar and 150°C. The quality of the resulting powder diffraction data has allowed in situ Rietveld quantitative phase analyses for a hydrating cement containing seven crystalline phases.
YR 2019
FD 2019
LK https://hdl.handle.net/10630/21575
UL https://hdl.handle.net/10630/21575
LA eng
NO The design, production and commissioning of this cellwas carried out at the ALBA synchrotron as part ofEdmundo Fraga’s PhD project. This work wasfinancially supported by the Spanish Ministry ofEconomy and Competitiveness through GrantsBIA2014-57658-C2-1-R and BIA2017-82391-R whichare co-funded by FEDER. We are grateful to Prof.Angus Wilkinson, Georgia Institute of TechnologyAtlanta, for sharing his knowledge and details on thehigh pressure cell developed by his team. We alsothank Dr. Marcus Paul, Dyckerhoff-Lengerich,Germany, for fruitful discussion on Oil Well Cements.The cell was commissioned at BL11-NCD-SWEETbeamline.
DS RIUMA. Repositorio Institucional de la Universidad de Málaga
RD 21 ene 2026