Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis

2016 ◽  
Vol 52 (96) ◽  
pp. 13865-13868 ◽  
Author(s):  
Saul J. Moorhouse ◽  
Yue Wu ◽  
Hannah C. Buckley ◽  
Dermot O'Hare
Keyword(s):  
High Temperature ◽  
Molten Salt ◽  
Powder Diffraction ◽  
High Energy ◽  
Chemical Processes ◽  
Molten Salt Synthesis ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray

We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses.

Probing Molten Salt Flux Reactions Using Time-Resolved in Situ High-Temperature Powder X-ray Diffraction:  A New Synthesis Route to the Mixed-Valence NaTi2O4

2004 ◽  
Vol 16 (6) ◽  
pp. 1153-1159 ◽  
Author(s):  
Margret J. Geselbracht ◽  
Liam D. Noailles ◽  
Lien T. Ngo ◽  
Jessica H. Pikul ◽  
Richard I. Walton ◽  
...  
Keyword(s):  
High Temperature ◽  
Molten Salt ◽  
Mixed Valence ◽  
Salt Flux ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Synthesis Route ◽  
New Synthesis

scholarly journals Probing Molten Salt Flux Reactions Using Time-Resolved in situ High-Temperature Powder X-Ray Diffraction: A New Synthesis Route to the Mixed-Valence NaTi2O4.

ChemInform ◽  
2004 ◽  
Vol 35 (23) ◽  
Author(s):  
Margret J. Geselbracht ◽  
Liam D. Noailles ◽  
Lien T. Ngo ◽  
Jessica H. Pikul ◽  
Richard I. Walton ◽  
...  
Keyword(s):  
High Temperature ◽  
Molten Salt ◽  
Mixed Valence ◽  
Salt Flux ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Synthesis Route ◽  
New Synthesis

A furnace and environmental cell for thein situinvestigation of molten salt electrolysis using high-energy X-ray diffraction

2011 ◽  
Vol 19 (1) ◽  
pp. 39-47 ◽  
Author(s):  
Mark J. Styles ◽  
Matthew R. Rowles ◽  
Ian C. Madsen ◽  
Katherine McGregor ◽  
Andrew J. Urban ◽  
...  
Keyword(s):  
Molten Salt ◽  
Inert Anode ◽  
High Energy ◽  
X Ray Diffraction ◽  
Molten Salt Electrolysis ◽  
X Ray ◽  
Quantitative Measurements ◽  
Materials Used ◽  
Characterization Of Materials

This paper describes the design, construction and implementation of a relatively large controlled-atmosphere cell and furnace arrangement. The purpose of this equipment is to facilitate thein situcharacterization of materials used in molten salt electrowinning cells, using high-energy X-ray scattering techniques such as synchrotron-based energy-dispersive X-ray diffraction. The applicability of this equipment is demonstrated by quantitative measurements of the phase composition of a model inert anode material, which were taken during anin situstudy of an operational Fray–Farthing–Chen Cambridge electrowinning cell, featuring molten CaCl2as the electrolyte. The feasibility of adapting the cell design to investigate materials in other high-temperature environments is also discussed.

In situsynchrotron powder diffraction study of active belite clinkers

2007 ◽  
Vol 40 (6) ◽  
pp. 999-1007 ◽  
Author(s):  
Ángeles G. De la Torre ◽  
Khadija Morsli ◽  
Mohammed Zahir ◽  
Miguel A.G. Aranda
Keyword(s):  
High Temperature ◽  
High Resolution ◽  
Powder Diffraction ◽  
Polymorphic Transformation ◽  
High Energy ◽  
Dicalcium Silicate ◽  
Polymorphic Transformations ◽  
X Ray ◽  
High Temperature Reactions

The clinkerization processes to form belite clinkers, with theoretical compositions close to 60 wt% of Ca2SiO4, have been studiedin situby high-resolution high-energy (λ = 0.30 Å) synchrotron X-ray powder diffraction. In order to obtain active belite cements, different amounts of K2O, Na2O and SO3have been added. The existence range of the high-temperature phases has been established and, furthermore, Rietveld quantitative phase analyses at high temperature have been performed for all patterns. The following high-temperature reactions have been investigated: (i) polymorphic transformations of dicalcium silicate, \alpha_{\rm L}'-Ca2SiO4↔ \alpha_{\rm H}'-Ca2SiO4from 1170 to 1230 K, and \alpha_{\rm H}'-Ca2SiO4↔ α-Ca2SiO4from 1500 to 1600 K; (ii) melting of the aluminates phases, Ca3Al2O6and Ca4(Al2Fe2)O10, above ∼1570 K; and (iii) reaction of Ca2SiO4with CaO to yield Ca3SiO5above ∼1550 K. Moreover, in all the studied compositions the temperature of the polymorphic transformation \alpha_{\rm H}'-Ca2SiO4↔ α-Ca2SiO4has decreased with the addition of activators. Finally, active belite clinkers were produced as the final samples contained α-belite phases.

A furnace for the in situ study of the formation of inorganic solids at high temperature using time-resolved energy-dispersive x-ray diffraction

2000 ◽  
Vol 71 (11) ◽  
pp. 4177 ◽  
Author(s):  
Margret J. Geselbracht ◽  
Richard I. Walton ◽  
E. Sarah Cowell ◽  
Franck Millange ◽  
Dermot O’Hare
Keyword(s):  
High Temperature ◽  
Energy Dispersive ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Inorganic Solids ◽  
In Situ Study
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