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

Materials ◽  
2019 ◽  
Vol 12 (12) ◽  
pp. 1897 ◽  
Author(s):  
Edmundo Fraga ◽  
Ana Cuesta ◽  
Jesus Zea-Garcia ◽  
Angeles De la Torre ◽  
Armando Yáñez-Casal ◽  
...  
Keyword(s):  
High Pressure ◽  
Powder Diffraction ◽  
High Energy ◽  
Ex Situ ◽  
Oil Well ◽  
High Pressure And Temperature ◽  
Quantitative Phase ◽  
Oil Well Cement ◽  
Well Cement

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.

scholarly journals High-pressure and -temperature spinning capillary cell for in situ synchrotron X-ray powder diffraction

2019 ◽  
Vol 26 (4) ◽  
pp. 1238-1244 ◽  
Author(s):  
Edmundo Fraga ◽  
Jesus D. Zea-Garcia ◽  
Armando Yáñez ◽  
Angeles G. De la Torre ◽  
Ana Cuesta ◽  
...  
Keyword(s):  
Powder Diffraction ◽  
Cost Effective ◽  
Oil Well ◽  
X Ray Diffraction ◽  
High Pressure And Temperature ◽  
X Ray ◽  
Quantitative Analyses ◽  
Well Cement

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.

Behavior of oil well cement slurry systems aged in CO2-saturated water under high pressure and temperature

2020 ◽  
Author(s):  
Jonathan Dias Nascimento ◽  
Camila Aparecida Abelha Rocha ◽  
Cristina Aiex Simão ◽  
Romildo Dias Toledo Filho
Keyword(s):  
High Pressure ◽  
Oil Well ◽  
Cement Slurry ◽  
High Pressure And Temperature ◽  
Saturated Water ◽  
Oil Well Cement ◽  
Well Cement

scholarly journals The Viscosity and Atomic Structure of Volatile-Bearing Melilititic Melts at High Pressure and Temperature and the Transport of Deep Carbon

Minerals ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 267 ◽  
Author(s):  
Vincenzo Stagno ◽  
Veronica Stopponi ◽  
Yoshio Kono ◽  
Annalisa D’Arco ◽  
Stefano Lupi ◽  
...  
Keyword(s):  
Experimental Data ◽  
High Pressure ◽  
Atomic Structure ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
High Pressure And Temperature ◽  
X Ray ◽  
Falling Sphere ◽  
Basaltic Melts

Understanding the viscosity of mantle-derived magmas is needed to model their migration mechanisms and ascent rate from the source rock to the surface. High pressure–temperature experimental data are now available on the viscosity of synthetic melts, pure carbonatitic to carbonate–silicate compositions, anhydrous basalts, dacites and rhyolites. However, the viscosity of volatile-bearing melilititic melts, among the most plausible carriers of deep carbon, has not been investigated. In this study, we experimentally determined the viscosity of synthetic liquids with ~31 and ~39 wt% SiO2, 1.60 and 1.42 wt% CO2 and 5.7 and 1 wt% H2O, respectively, at pressures from 1 to 4.7 GPa and temperatures between 1265 and 1755 °C, using the falling-sphere technique combined with in situ X-ray radiography. Our results show viscosities between 0.1044 and 2.1221 Pa·s, with a clear dependence on temperature and SiO2 content. The atomic structure of both melt compositions was also determined at high pressure and temperature, using in situ multi-angle energy-dispersive X-ray diffraction supported by ex situ microFTIR and microRaman spectroscopic measurements. Our results yield evidence that the T–T and T–O (T = Si,Al) interatomic distances of ultrabasic melts are higher than those for basaltic melts known from similar recent studies. Based on our experimental data, melilititic melts are expected to migrate at a rate ~from 2 to 57 km·yr−1 in the present-day or the Archaean mantle, respectively.

In Situ Growth Studies of Artificial Layered (BA,SR,CA)CUO2 on Quasi-Ideal SrTiO3 Substrates by High Pressure Rheed

1999 ◽  
Vol 569 ◽  
Author(s):  
Gertjan Koster ◽  
Guus J.H.M. Rijnders ◽  
Dave H.A. Blank ◽  
Horst Rogalla
Keyword(s):  
High Pressure ◽  
Thin Film Deposition ◽  
High Energy ◽  
Layer Growth ◽  
Film Deposition ◽  
Perovskite Oxide ◽  
Ex Situ ◽  
Layer By Layer ◽  
Substrate Surfaces

ABSTRACTThe layered structure of oxides, like the high-T, cuprates, has been topic of research for some years now. The possibility to control thin film deposition on an atomic level has made fabrication of artificial structures and junctions accessible by depositing atomic layers or molecular blocks sequentially. Perfectly smooth substrate surfaces are hereby a prerequisite.Using Pulsed Laser Deposition (PLD), different perovskite oxide materials have been deposited on SrTiO3 substrates. With in situ high pressure Reflection High Energy Electron Diffraction we studied growth at different temperatures and oxygen pressures. Ex situ XRD and AFM have been used to study the morphology after deposition.Here we applied a new approach in obtaining layer-by-layer growth implied by the way of depositing the material, almost regardless of the deposition conditions. By alternating intervals of high supersaturation depositing one unit cell layer with intervals of lower supersaturation, one is able to force a layer-by-layer growth mode, which is in principle only feasible with PLD. We applied this technique to fabricate the layered infinite structure (Ba,Sr,Ca)CuO2 with artificial layered modulation, which have been characterized by XRD and AFM.

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