Design and development of a controlled pressure/temperature set-up forin situstudies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station

2015 ◽  
Vol 22 (1) ◽  
pp. 42-48 ◽  
Author(s):  
Eduardo Salas-Colera ◽  
Álvaro Muñoz-Noval ◽  
Catherine Heyman ◽  
Conchi O. Ania ◽  
José B. Parra ◽  
...  
Keyword(s):  
Powder Diffraction ◽  
Gas Adsorption ◽  
Processes And Reactions ◽  
X Ray ◽  
Experimental Station ◽  
Transmission Geometry ◽  
Gas Reactions ◽  
In Operando ◽  
Set Up

A novel set-up has been designed and used for synchrotron radiation X-ray high-resolution powder diffraction (SR-HRPD) in transmission geometry (spinning capillary) forin situsolid–gas reactions and processes in an isobaric and isothermal environment. The pressure and temperature of the sample are controlled from 10−3to 1000 mbar and from 80 to 1000 K, respectively. To test the capacities of this novel experimental set-up, structure deformation in the porous material zeolitic imidazole framework (ZIF-8) by gas adsorption at cryogenic temperature has been studied under isothermal and isobaric conditions. Direct structure deformations by the adsorption of Ar and N2gases have been observedin situ, demonstrating that this set-up is perfectly suitable for direct structural analysis underin operandoconditions. The presented results prove the feasibility of this novel experimental station for the characterization in real time of solid–gas reactions and other solid–gas processes by SR-HRPD.

Monitoring Polymer-Assisted Mechanochemical Cocrystallisation Through in Situ X-Ray Powder Diffraction

2020 ◽  
Author(s):  
Luzia S. Germann ◽  
Sebastian T. Emmerling ◽  
Manuel Wilke ◽  
Robert E. Dinnebier ◽  
Mariarosa Moneghini ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Powder Diffraction ◽  
Reaction Rate ◽  
Polymer Additives ◽  
Time Resolved ◽  
X Ray

Time-resolved mechanochemical cocrystallisation studies have so-far focused solely on neat and liquid-assisted grinding. Here, we report the monitoring of polymer-assisted grinding reactions using <i>in situ</i> X-ray powder diffraction, revealing that reaction rate is almost double compared to neat grinding and independent of the molecular weight and amount of used polymer additives.<br>

Structural evolution of NASICON-type Li1+xAlxGe2−x(PO4)3 using in situ synchrotron X-ray powder diffraction

2016 ◽  
Vol 4 (20) ◽  
pp. 7718-7726 ◽  
Author(s):  
Dorsasadat Safanama ◽  
Neeraj Sharma ◽  
Rayavarapu Prasada Rao ◽  
Helen E. A. Brand ◽  
Stefan Adams
Keyword(s):  
Solid Electrolyte ◽  
Diffraction Study ◽  
Powder Diffraction ◽  
Structural Evolution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nasicon Type ◽  
Precursor Glass

In situ synchrotron X-ray diffraction study of the synthesis of solid-electrolyte Li1+xAlxGe2−x(PO4)3 (LAGP) from the precursor glass reveals that an initially crystallized dopant poor phase transforms into the Al-doped LAGP at 800 °C.

Applications of High-Resolution Powder X-Ray Diffraction

2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch
Keyword(s):  
High Resolution ◽  
Synchrotron Radiation ◽  
Powder Diffraction ◽  
X Rays ◽  
X Ray Diffraction ◽  
Crystalline Materials ◽  
X Ray ◽  
Structural Characterisation ◽  
Pdf Analysis

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.

scholarly journals Exploration of the NaxMoO2phase diagram for low sodium contents (x≤ 0.5)

2018 ◽  
Vol 6 (30) ◽  
pp. 14651-14662 ◽  
Author(s):  
Laura Vitoux ◽  
Marie Guignard ◽  
Jacques Darriet ◽  
Claude Delmas
Keyword(s):  
Phase Diagram ◽  
Powder Diffraction ◽  
X Ray ◽  
Low Sodium

Phase diagram in the NaxMoO2system (x≤ 0.5) determined using electrochemistry andin situX-ray powder diffraction.

An In-situ X-ray Powder Diffraction Study of the Adsorption of Hydrofluorocarbons in Zeolites

2001 ◽  
Vol 105 (13) ◽  
pp. 2604-2611 ◽  
Author(s):  
Michael F. Ciraolo ◽  
Jonathan C. Hanson ◽  
Poul Norby ◽  
Clare P. Grey
Keyword(s):  
Diffraction Study ◽  
Powder Diffraction ◽  
X Ray

Determination of the crystal structure of magnesium perchlorate hydrates by X-ray powder diffraction and the charge-flipping method

2010 ◽  
Vol 66 (6) ◽  
pp. 579-584 ◽  
Author(s):  
Kevin Robertson ◽  
David Bish
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Fundamental Parameter ◽  
Magnesium Perchlorate ◽  
Space Group ◽  
X Ray ◽  
Partial Pressures ◽  
Dehydration Reactions

X-ray powder diffraction (XRD) data were used to solve the crystal structures of phases in the magnesium perchlorate hydrate system, Mg(ClO4)2·nH2O (n = 4, 2). A heating stage and humidity generator interfaced to an environmental cell enabled in-situ XRD analyses of dehydration reactions under controlled temperatures and partial pressures of H2O (P_{{\rm H}_2{\rm O}}). The crystal structures were determined using an ab initio charge-flipping method and were refined using fundamental-parameter Rietveld methods. Dehydration of magnesium perchlorate hexahydrate to tetrahydrate (348 K) results in a decrease in symmetry (space group = C2), where isolated Mg2+ cations are equatorially coordinated by four H2O molecules with two [ClO4]− tetrahedra at the apices. Further dehydration to the dihydrate (423 K) leads to bridging of the isolated packets to form double corner-sharing chains of octahedra and polyhedra (space group = C2/m).

scholarly journals Mechanisms of mechanochemical salt formation by in situ real time X-ray powder diffraction

2016 ◽  
Vol 72 (a1) ◽  
pp. s394-s394
Author(s):  
Adam A. L. Michalchuk ◽  
Ivan A. Tumanov ◽  
Simon A. J. Kimber ◽  
Elena V. Boldyreva ◽  
Colin R. Pulham
Keyword(s):  
Real Time ◽  
Powder Diffraction ◽  
Salt Formation ◽  
X Ray
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