Sample environment issues relevant to the acquisition of inelastic neutron scattering measurements of heterogeneous catalyst samples

Warringham, Robbie; Bellaire, Daniel; Parker, Stewart F.; Taylor, J. W.; Ewings, R. A.; Goodway, Chris; Kibble, Mark; Wakefield, S.; Jura, Marek; Dudman, Michael; Tooze, Robert P.; Webb, Paul B.; Lennon, David

doi:10.1088/1742-6596/554/1/012005

Cited by 28 publications

(39 citation statements)

References 25 publications

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“…Two Inconel reactors [29] were charged with the catalyst pellets. The first reactor was attached to a gas manifold apparatus [27] and the catalyst dried by the following procedure: whilst continually maintaining a flow of helium over the catalyst (1000 sccm, CK Gas, [99.0 %), the sample was heated to 623 K at a heating rate of 10 K min -1 and then maintained at that temperature for 2 h. The heating was stopped and the sample allowed to cool to ambient temperature in a continuous flow of He. The reactor was then isolated and transferred to an argonfilled glove box (MBraun UniLab MB-20-G, […”

Section: Methodsmentioning

confidence: 99%

“…For example, following on from the work of Silverwood et al who used INS to examine alumina-supported nickel catalysts applied to the dry [18-21] and steam [22] reforming of methane, Warringham and co-workers have used a combination of indirect [23] and direct [24][25][26] geometry INS spectrometers to investigate iron based FischerTropsch synthesis (FTS) catalysts. Moreover, Warringham et al [27] recently reported on sample environment details relevant to the acquisition of INS spectra of heterogeneous catalysts.…”

Section: Introductionmentioning

confidence: 99%

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Application of Inelastic Neutron Scattering to the Methanol-to-Gasoline Reaction Over a ZSM-5 Catalyst

et al. 2016

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Inelastic neutron scattering (INS) is used to investigate a ZSM-5 catalyst that has been exposed to methanol vapour at elevated temperature. In-line mass spectrometric analysis of the catalyst exit stream confirms methanol-to-gasoline chemistry, whilst ex situ INS measurements detect hydrocarbon species formed in/on the catalyst during methanol conversion. These preliminary studies demonstrate the capability of INS to complement infrared spectroscopic characterisation of the hydrocarbon pool present in/on ZSM-5 during the MTG reaction. Graphical Abstract& David Lennon

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Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Application of Inelastic Neutron Scattering to the Methanol-to-Gasoline Reaction Over a ZSM-5 Catalyst

et al. 2016

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“…The time is given by experimental and technical details such as size and materials properties (heat conductivity) of the cell used. [18]. Reduction and methanation takes place at 300 °C in this cell at indicated conditions.…”

Section: Experimental Boundary Conditions Of Drifts and Insmentioning

confidence: 97%

“…→ CO * + H2O * + 6H * CO − formation (4) [18]. Reduction and methanation takes place at 300 • C in this cell at indicated conditions.…”

Section: Co2 + 4h2mentioning

confidence: 99%

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Volatile Hydrogen Intermediates of CO2 Methanation by Inelastic Neutron Scattering

et al. 2020

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Despite vast research efforts, the detection of volatile intermediates of catalytic reactions remains a challenge: in addition to the compatibility of the technique to the harsh reaction conditions, a molecular understanding is hampered by the difficulty of extracting meaningful information from operando techniques applied on complex materials. Diffusive reflectance infrared Fourier transform spectroscopy (DRIFTS) is a powerful method, but it is restricted by optical selection rules particularly affecting the detection of hydrogen. This gap can be filled by inelastic neutron scattering (INS). However, INS cannot be used on hydrogenated systems at temperatures higher than 20 K. We demonstrate how its use as a post-mortem method gives insights into the crucial intermediates during CO2 methanation on Ni/alumina-silica catalysts. We detect a variety of H–, O–, and C-based intermediates. A striking outcome is that hydrogen and oxygen are concurrently chemisorbed on the catalysts, a result that needs the combined effort of DRIFTS and INS.

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Neutron Vibrational Spectroscopy

Parker

2020

Encyclopedia of Analytical Chemistry

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Neutron vibrational spectroscopy ( inelastic neutron scattering ( INS )) is a form of vibrational spectroscopy that is complementary to infrared and Raman spectroscopies. It has a very wide spectral range of zero to several thousand cm −1 , there are no selection rules so all modes are allowed and comparison with ab initio calculations is straightforward. The disadvantages are that it is relatively insensitive and restricted to the solid state. It is particularly sensitive to modes involving hydrogen and in hydrogenous materials, these dominate the spectra. In this article, the history, theory, and practice of the technique are briefly reviewed. The extensive range of applications of this form of spectroscopy is illustrated with examples in the areas of hydrogen storage, catalysis, soft condensed matter, ice, carbons, and magnetism.

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Sample environment issues relevant to the acquisition of inelastic neutron scattering measurements of heterogeneous catalyst samples

Cited by 28 publications

References 25 publications

Application of Inelastic Neutron Scattering to the Methanol-to-Gasoline Reaction Over a ZSM-5 Catalyst

Application of Inelastic Neutron Scattering to the Methanol-to-Gasoline Reaction Over a ZSM-5 Catalyst

Volatile Hydrogen Intermediates of CO2 Methanation by Inelastic Neutron Scattering

Neutron Vibrational Spectroscopy

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