scholarly journals A compact low-power infrared tube furnace for in situ and in operando X-ray powder diffraction

2018 ◽  
Vol 74 (a1) ◽  
pp. a458-a458
Author(s):  
Andrew Doran ◽  
Martin Kunz ◽  
Christine M. Beavers
2017 ◽  
Vol 88 (1) ◽  
pp. 013903 ◽  
Author(s):  
A. Doran ◽  
L. Schlicker ◽  
C. M. Beavers ◽  
S. Bhat ◽  
M. F. Bekheet ◽  
...  

2015 ◽  
Vol 22 (1) ◽  
pp. 42-48 ◽  
Author(s):  
Eduardo Salas-Colera ◽  
Álvaro Muñoz-Noval ◽  
Catherine Heyman ◽  
Conchi O. Ania ◽  
José B. Parra ◽  
...  

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.


2020 ◽  
Author(s):  
Luzia S. Germann ◽  
Sebastian T. Emmerling ◽  
Manuel Wilke ◽  
Robert E. Dinnebier ◽  
Mariarosa Moneghini ◽  
...  

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>


2016 ◽  
Vol 4 (20) ◽  
pp. 7718-7726 ◽  
Author(s):  
Dorsasadat Safanama ◽  
Neeraj Sharma ◽  
Rayavarapu Prasada Rao ◽  
Helen E. A. Brand ◽  
Stefan Adams

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.


2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch

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.


2018 ◽  
Vol 6 (30) ◽  
pp. 14651-14662 ◽  
Author(s):  
Laura Vitoux ◽  
Marie Guignard ◽  
Jacques Darriet ◽  
Claude Delmas

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


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

2010 ◽  
Vol 66 (6) ◽  
pp. 579-584 ◽  
Author(s):  
Kevin Robertson ◽  
David Bish

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).


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

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