Characterization of Gas‐Solid Reactions using In Situ Powder X‐ray Diffraction

Møller, Kasper T.; Hansen, Bettina; Dippel, Ann‐Christin; Jørgensen, Jens-Erik; Jensen, Torben R.

doi:10.1002/zaac.201400262

Cited by 35 publications

(23 citation statements)

References 126 publications

(189 reference statements)

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“…The activation energies extracted for the air-exposed samples may be assumed to be maximum values, which may be relevant to know for practical applications. This work also illustrates that in situ synchrotron radiation powder X-ray diffraction (SR-PXD) is a useful technique for investigation of kinetic properties [40,41]. These results indicate that the presence of either Mg 2 Cu or MgCu 2 in MgH 2 has a pronounced positive effect on the dehydrogenation kinetics of air-exposed samples.…”

Section: Coppermentioning

confidence: 66%

Mg-based compounds for hydrogen and energy storage

Crivello

Denys

Dornheim³

et al. 2016

Appl. Phys. A

155

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Magnesium-based alloys attract significant interest as cost-efficient hydrogen storage materials allowing the combination of high gravimetric storage capacity of hydrogen with fast rates of hydrogen uptake and release and pronounced destabilization of the metalhydrogen bonding in comparison with binary Mg-H systems. In this review, various groups of magnesium compounds are considered, including (1) RE-Mg-Ni hydrides (RE = La, Pr, Nd); (2) Mg alloys with p-elements (X = Si, Ge, Sn, and Al); and (3) magnesium alloys with d-elements (Ti, Fe, Co, Ni, Cu, Zn, Pd). The hydrogenation-disproportionation-desorption-recombination process in the Mg-based alloys (LaMg 12 , LaMg 11 Ni) and unusually high-pressure hydrides synthesized at pressures exceeding 100 MPa (MgNi 2 H 3 ) and stabilized by Ni-H bonding are also discussed. The paper reviews interrelations between the properties of the Mg-based hydrides and p-T conditions of the metal-hydrogen interactions, chemical composition of the initial alloys, their crystal structures, and microstructural state.

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Section: Coppermentioning

confidence: 66%

Mg-based compounds for hydrogen and energy storage

Crivello

Denys

Dornheim³

et al. 2016

Appl. Phys. A

155

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“…They are chosen with individual bias and focus on utilizing information from reaction pathways in synthesis planning and optimization of synthesis protocols. Instrumental aspects on developments of in situ diffraction and spectroscopy techniques including available condition parameters for gas pressure and gas flow systems can be found in recent reviews …”

Section: Introductionmentioning

confidence: 99%

Looking into the Black Box of Solid‐State Synthesis

Kohlmann

2019

Eur J Inorg Chem

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The rational planning of solid-state synthesis is hampered by the fact that in general little is known on reaction processes and thus they cannot be utilized in an efficient way. This is in stark contrast to molecular chemistry, where retrosynthesis is a very powerful tool for the development of new compounds. Time-dependent in situ studies of solid-state synthesis reactions by thermal analysis, diffraction and spectroscopy techniques can unravel reaction pathways. Examples for the synthesis of metal hydrides, nitrides, oxides, by solid gas, electrochemical and ball-milling methods show that the identification and characterization of reaction intermediates is often key to reaction control. Knowledge of their behavior helps avoiding [a] Chemistry -Functional Materials. His research focuses on solid state chemistry, metal hydrides, neutron diffraction and the elucidation of reaction pathways of solids by in situ methods.

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“…Typically, an experimental parameter such as temperature is varied and measured whilst X-ray diffraction data are collected. This technique enables the study of complex reactions between solids and high-pressure hydrogen (Pitt et al, 2011;Møller et al, 2014), carbon dioxide (Capobianco et al, 2014;Jensen et al, 2014), ammonia (Sedlmaier et al, 2013), diborane (Remhof et al, 2014), liquids (Madsen et al, 2005), supercritical fluids (Schaef et al, 2012) etc. under dynamic conditions.…”

Section: Introductionmentioning

confidence: 99%

In situ X-ray diffraction environments for high-pressure reactions

et al. 2015

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New sample environments and techniques specifically designed for in situ powder X‐ray diffraction studies up to 1000 bar (1 bar = 105 Pa) gas pressure are reported and discussed. The cells can be utilized for multiple purposes in a range of research fields. Specifically, investigations of gas–solid reactions and sample handling under inert conditions are undertaken here. Sample containers allowing the introduction of gas from one or both ends are considered, enabling the possibility of flow‐through studies. Various containment materials are evaluated, e.g. capillaries of single‐crystal sapphire (Al2O3), quartz glass (SiO2), stainless steel (S316) and glassy carbon (Sigradur K), and burst pressures are calculated and tested for the different tube materials. In these studies, high hydrogen pressure is generated with a metal hydride hydrogen compressor mounted in a closed system, which allows reuse of the hydrogen gas. The advantages and design considerations of the in situ cells are discussed and their usage is illustrated by a case study.

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Characterization of Gas‐Solid Reactions using In Situ Powder X‐ray Diffraction

Cited by 35 publications

References 126 publications

Mg-based compounds for hydrogen and energy storage

Mg-based compounds for hydrogen and energy storage

Looking into the Black Box of Solid‐State Synthesis

In situ X-ray diffraction environments for high-pressure reactions

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