In situmonitoring of powder reactions in percolating solution by wet-cell X-ray diffraction techniques

2003 ◽  
Vol 36 (3) ◽  
pp. 948-949 ◽  
Author(s):  
Laurence N. Warr ◽  
Heiko Hofmann
Keyword(s):  
Open Systems ◽  
Reaction Chamber ◽  
Solution Chemistry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Standard Powder ◽  
Flow Through ◽  
Kinetics Of

This note describes how the kinetics of powder reactions in percolating solution can be studied by X-ray diffraction using a wet-cell flow-through reaction chamber. The device can be routinely moved between diffractometer and controlled laboratory (pressure, temperature) conditions with the ease of a standard powder holder. Short-termin situmeasurements and long-termquasiin situmonitoring of dissolution and crystallization reactions are possible with a minimum of sample preparation and little disturbance of the system. Measuring time-dependent changes in the concentration of crystalline reactants and products provides information for quantifying reaction kinetics and for determining dissolution and crystal growth mechanisms. Results can be compared with changes in solution chemistry of the collected eluate, enabling a more complete reconstruction of heterogeneous crystal–solution reactions in open systems.

In-Situ Diffraction Studies of Gas Storage Materials on a Laboratory X-Ray System

2013 ◽  
Vol 1544 ◽  
Author(s):  
Marco Sommariva ◽  
Harald van Weeren ◽  
Olga Narygina ◽  
Jan-André Gertenbach ◽  
Christian Resch ◽  
...  
Keyword(s):  
Large Scale ◽  
Fossil Fuels ◽  
Reaction Chamber ◽  
Hydrogen Gas ◽  
Gas Pressure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structural Modifications ◽  
Model Studies

ABSTRACTThe sorption processes for hydrogen and carbon dioxide are of considerable, and growing interest, particularly due to their relevance to a society that seeks to replace fossil fuels with a more sustainable energy source. X-ray diffraction allows a unique perspective for studying structural modifications and reaction mechanisms that occur when gas and solid interact. The fundamental challenge associated with such a study is that experiments are conducted while the solid sample is held under a gas pressure. To date in-situ high gas pressure studies of this nature have typically been undertaken at large-scale facilities such as synchrotrons or on dedicated laboratory instruments. Here we report high-pressure XRD studies carried out on a multi-purpose diffractometer. To demonstrate the suitability of the equipment, two model studies were carried out, firstly the reversible hydrogen cycling over LaNi5, and secondly the structural change that occurs during the decomposition of ammonia borane that results in the generation of hydrogen gas in the reaction chamber. The results have been finally compared to the literature. The study has been made possible by the combination of rapid X-ray detectors with a reaction chamber capable of withstanding gas pressures up to 100 bar and temperatures up to 900 °C.

scholarly journals In situ monitoring of hydrothermal reactions by X-ray diffraction with Bragg–Brentano geometry

2020 ◽  
Vol 53 (4) ◽  
pp. 1163-1166
Author(s):  
Karsten Mesecke ◽  
Winfried Malorny ◽  
Laurence N. Warr
Keyword(s):  
Quantitative Information ◽  
In Situ Monitoring ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
X Ray ◽  
Saturated Vapour Pressure ◽  
Concrete Production ◽  
Aerated Concrete ◽  
Kinetics Of

This note describes an autoclave chamber developed and constructed by Anton Paar and its application for in situ experiments under hydrothermal conditions. Reactions of crystalline phases can be studied by successive in situ measurements on a conventional laboratory X-ray diffractometer with Bragg–Brentano geometry at temperatures <483 K and saturated vapour pressure <2 MPa. Variations in the intensity of X-ray diffraction reflections of both reactants and products provide quantitative information for studying the reaction kinetics of both dissolution and crystal growth. Feasibility is demonstrated by studying a cementitious mixture used for autoclaved aerated concrete production. During a period of 5.7 h at 466 K and 1.35 MPa, the crystallization of torbermorite and the partial consumption of quartz were monitored.

Kinetics of Multi-Step Redox Processes by Time-Resolved In Situ X-ray Diffraction

2016 ◽  
Vol 88 (11) ◽  
pp. 1684-1692 ◽  
Author(s):  
Lukas C. Buelens ◽  
Vladimir V. Galvita ◽  
Hilde Poelman ◽  
Christophe Detavernier ◽  
Guy B. Marin
Keyword(s):  
Redox Processes ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Kinetics Of

In situ high temperature X-ray diffraction study of the kinetics of phase separation in the uranium-plutonium mixed oxide (U0.55Pu0.45)O2-x

2014 ◽  
Vol 1645 ◽  
Author(s):  
Romain VAUCHY ◽  
Renaud.C. BELIN ◽  
Anne-Charlotte ROBISSON ◽  
Fiqiri HODAJ
Keyword(s):  
Phase Separation ◽  
Room Temperature ◽  
Mixed Oxides ◽  
Oxygen Stoichiometry ◽  
X Ray Diffraction ◽  
Fundamental Interest ◽  
X Ray ◽  
Uranium Plutonium ◽  
Kinetics Of

ABSTRACTUranium-plutonium mixed oxides incorporating high amounts of plutonium are considered for future nuclear reactors. For plutonium content higher than 20%, a phase separation occurs, depending on the temperature and on the oxygen stoichiometry. This phase separation phenomenon is still not precisely described, especially at high plutonium content. Here, using an original in situ fast X-ray diffraction device dedicated to radioactive materials, we evidenced a phase separation occurring during rapid cooling from 1773 K to room temperature at the rate of 0.05 and 2 K per second for a (U0.55Pu0.45)O2-x compound under a reducing atmosphere. The results show that the cooling rate does not impact the lattice parameters of the obtained phases at room temperature but their fraction. In addition to their obvious fundamental interest, these results are of utmost importance in the prospect of using uranium-plutonium mixed oxides with high plutonium content as nuclear fuels.

A flow-through reaction cell that couples time-resolved X-ray diffraction with stable isotope analysis

2011 ◽  
Vol 44 (2) ◽  
pp. 429-432 ◽  
Author(s):  
Andrew J. Wall ◽  
Peter J. Heaney ◽  
Ryan Mathur ◽  
Jeffrey E. Post ◽  
Jonathan C. Hanson ◽  
...  
Keyword(s):  
Stable Isotope ◽  
Stable Isotope Analysis ◽  
Isotope Fractionation ◽  
Isotope Analysis ◽  
X Ray Diffraction ◽  
Reaction Cell ◽  
Time Resolved ◽  
X Ray ◽  
Flow Through

A non-metallic flow-through reaction cell is described, designed forin situtime-resolved X-ray diffraction coupled with stable isotope analysis. The experimental setup allows the correlation of Cu isotope fractionation with changes in crystal structure during copper sulfide dissolution. This flow-through cell can be applied to many classes of fluid–mineral reactions that involve dissolution or ion exchange.

Grain-Growth Kinetics of Nanocrystalline Iron Studied In Situ by Synchrotron Real-Time X-ray Diffraction

2000 ◽  
Vol 104 (11) ◽  
pp. 2467-2476 ◽  
Author(s):  
H. Natter ◽  
M. Schmelzer ◽  
M.-S Löffler ◽  
C. E. Krill ◽  
A. Fitch ◽  
...  
Keyword(s):  
Real Time ◽  
Grain Growth ◽  
Growth Kinetics ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nanocrystalline Iron ◽  
Grain Growth Kinetics ◽  
Kinetics Of

scholarly journals A Flow-Through Reaction Cell for Studying Minerals Leaching by In-Situ Synchrotron Powder X-ray Diffraction

Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 990
Author(s):  
Fatemeh Nikkhou ◽  
Fang Xia ◽  
Xizhi Yao ◽  
Idowu A. Adegoke ◽  
Qinfen Gu ◽  
...  
Keyword(s):  
Flow Rate ◽  
Pressure Leaching ◽  
X Ray Diffraction ◽  
Reaction Cell ◽  
Time Resolved ◽  
X Ray ◽  
Ore Minerals ◽  
Flow Through ◽  
Diffraction Patterns

A flow-through reaction cell has been developed for studying minerals leaching by in-situ time-resolved powder X-ray diffraction, allowing for a better understanding of the leaching mechanisms and kinetics. The cell has the capability of independent control of temperature (up to 95 °C) and flow rate (>0.5 mL min−1) for atmospheric pressure leaching. It was successfully tested at the powder diffraction beamline at the Australian Synchrotron. Galena powder was leached in a citrate solution under flow-through condition at a flow rate of 0.5 mL min−1, while diffraction patterns were collected during the entire leaching process, showing rapid galena dissolution without the formation of secondary mineral phases. The flow-through cell can be used to study leaching processes of other ore minerals.

A Model for Formation and Consumption of Transient Phase

2011 ◽  
Vol 172-174 ◽  
pp. 646-651 ◽  
Author(s):  
Gamra Tellouche ◽  
Khalid Hoummada ◽  
Dominique Mangelinck ◽  
Ivan Blum
Keyword(s):  
Differential Scanning Calorimetry ◽  
Phase Formation ◽  
Transient Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Proposed Model ◽  
Transient Phases ◽  
Kinetics Of

The phase formation sequence of Ni silicide for different thicknesses is studied by in situ X ray diffraction and differential scanning calorimetry measurements. The formation of a transient phase is observed during the formation of δ-Ni2Si; transient phases grow and disappear during the growth of another phase. A possible mechanism is proposed for the transient phase formation and consumption. It is applied to the growth and consumption of θ-Ni2Si. A good accordance is found between the proposed model and in situ measurement of the kinetics of phase formation obtained by x-ray diffraction and differential scanning calorimetry for higher thickness.

Rechargeable nonaqueous lithium/Mo6S8 battery

1984 ◽  
Vol 62 (6) ◽  
pp. 527-531 ◽  
Author(s):  
P. J. Mulhern ◽  
R. R. Haering
Keyword(s):  
Discharge Rate ◽  
Active Material ◽  
Rate Capability ◽  
Constant Current ◽  
Electrochemical Cells ◽  
X Ray Diffraction ◽  
X Ray ◽  
Long Cycle Life

Electrochemical cells based on the intercalation of lithium into Mo6S8 were examined by derivative constant current chronopotentiometry, in situ X-ray diffraction, and long-term cycling. About three-quarters of the capacity of such cells oeeurs between 2.0 and 2.1 V with most of the remainder near 2.45 V. Li/Mo6S8 cells have a long cycle life, good discharge rate capability, and an energy density of at least 260 W∙h/kg (1 W∙h = 3.6 kJ) of active material. Such cells can be made by starting with cathodes made from ternary Chevrel phase compounds. AyMo6S8 (A = Cu, Fe, Ni), and electrochemically converting these materials to form LixMo6S8.

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