Next Article in Journal
Design of Low RCS Circularly Polarized Patch Antenna Array Using Metasurface for CNSS Adaptive Antenna Applications
Previous Article in Journal
A Review of The Lesser-Studied Microemulsion-Based Synthesis Methodologies Used for Preparing Nanoparticle Systems of The Noble Metals, Os, Re, Ir and Rh
Article Menu

Export Article

Open AccessArticle

Rietveld Quantitative Phase Analysis of Oil Well Cement: In Situ Hydration Study at 150 Bars and 150 °C

1
ALBA Synchrotron, Carrer de la Lum, 2-26, Cerdanyola del Vallès, 08290 Barcelona, Spain
2
Departamento de Ingeniería Industrial, Universidade da Coruña, Ferrol, 15403 A Coruña, Spain
3
Departamento de Química Inorgánica, Cristalografía y Mineralogía, Universidad de Málaga, 29071 Málaga, Spain
*
Author to whom correspondence should be addressed.
Materials 2019, 12(12), 1897; https://doi.org/10.3390/ma12121897
Received: 9 May 2019 / Revised: 28 May 2019 / Accepted: 6 June 2019 / Published: 12 June 2019
(This article belongs to the Special Issue In Situ Diffraction, Spectroscopy and Scattering)
  |  
PDF [3901 KB, uploaded 14 June 2019]
  |     |  

Abstract

Oil and gas well cements are multimineral materials that hydrate under high pressure and temperature. Their overall reactivity at early ages is studied by a number of techniques including through the use of the consistometer. However, for a proper understanding of the performance of these cements in the field, the reactivity of every component, in real-world conditions, must be analysed. To date, in situ high energy synchrotron powder diffraction studies of hydrating oil well cement pastes have been carried out, but the quality of the data was not appropriated for Rietveld quantitative phase analyses. Therefore, the phase reactivities were followed by the inspection of the evolution of non-overlapped diffraction peaks. Very recently, we have 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 well cement paste at 150 bars and 150 °C. The powder diffraction data were analysed by the Rietveld method to quantitatively determine the reactivities of each component phase. The reaction degree of alite was 90% after 7 h, and that of belite was 42% at 14 h. 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%. The crystalline calcium silicates forming at 150 bars and 150 °C are also discussed. View Full-Text
Keywords: high-pressure equipment; powder diffraction; synchrotron radiation; cement hydration; reactivity; oil well cement high-pressure equipment; powder diffraction; synchrotron radiation; cement hydration; reactivity; oil well cement
Figures

Figure 1

This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).

Supplementary materials

  • Supplementary File 1:

    PDF-Document (PDF, 1478 KB)

  • Externally hosted supplementary file 1
    Doi: 10.5281/zenodo.2565904
    Link: http://dx.doi.org/10.5281/zenodo.2565904
    Description: All raw powder diffraction data has been deposited at zenodo and they are freely available.
SciFeed

Share & Cite This Article

MDPI and ACS Style

Fraga, E.; Cuesta, A.; Zea-Garcia, J.D.; De la Torre, A.G.; Yáñez-Casal, A.; Aranda, M.A.G. Rietveld Quantitative Phase Analysis of Oil Well Cement: In Situ Hydration Study at 150 Bars and 150 °C. Materials 2019, 12, 1897.

Show more citation formats Show less citations formats

Note that from the first issue of 2016, MDPI journals use article numbers instead of page numbers. See further details here.

Related Articles

Article Metrics

Article Access Statistics

1

Comments

[Return to top]
Materials EISSN 1996-1944 Published by MDPI AG, Basel, Switzerland RSS E-Mail Table of Contents Alert
Back to Top