High-pressure and -temperature spinning capillary cell for in situ synchrotron X-ray powder diffraction.
J Synchrotron Radiat
; 26(Pt 4): 1238-1244, 2019 Jul 01.
Article
em En
| MEDLINE
| ID: mdl-31274449
ABSTRACT
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 200â
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 150â
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.
Palavras-chave
Texto completo:
1
Base de dados:
MEDLINE
Assunto principal:
Pressão
/
Temperatura
/
Síncrotrons
/
Difração de Pó
Idioma:
En
Ano de publicação:
2019
Tipo de documento:
Article