Each month we post a new edition to the SES ‘Spotlight On…’ series, showcasing equipment at our institutions, providing information and case studies for interested researchers/industries, and promoting better use of already available equipment.

The DRIFTS Spectrometer is used for insitu studies of species formed at the surface of a material (e.g. a catalysis) during a reaction. The set up of the spectrometer allows researcher to perform reactuins under operando conditions (heat, gas flow) to preform reactons under realistic conditions and get real data.THE DRIFTS Spectrometer is used for insitu studies of species formed at the surface of a material (e.g. a catalysit) during a reaction. The set up of the spectrometer allows researcher to perform reactuins under operando conditions (heat, gas flow) to preform reactons under realistic conditions and get real data.

X-ray absorption fine structure (XAFS) is a specific structure observed in X-ray absorption spectroscopy. On a synchrotron X-ray source this can be coupled with information on the metal coordination and oxidation state in the material (e.g

Catalyst) providing a powerful understanding of what is occurring in real reactions. The DRIFTS spectrometer is a powerful tool for studying inset chemical reactions and when coupled with XAFS can provide insight into reaction mechanisms and active site behavior and characteristics.

The spectrometer can be used for the study of reactions over metal and metal oxide surfaces under operando (real) conditions to enhance our understand of how catalysis activate/deactivate, and the nature and changes in the active site of catalysis as reactions progress. This is of interest to anyone studying reactions over surfaces in chemistry, materials science and catalysis.

Name of Equipment

Rapid scanning FT-IR with combined XAFS/DRIFTS accessory

Current High-level Research:

  • The uses of in-situ and operando spectroscopic methods
    Techniques and measurements that are performed in real time (during an ongoing reaction) and under realistic conditions are important for investigating, understanding and developing improved catalyst materials. This project aimed to develop a combined XAFS/DRIFTS system where the local structure and oxidation state information was provided by X-ray Absorption fine structure (XAFS) and surface sensitive information obtained from FTIR.  This powerful combination of techniques is now available for use by the wider UK Catalysis Hub network, and has already been used by several groups to study a variety of catalytic systems.
  • Further Developments in Advanced In Situ and Operando Spectroscopy
    This project is aimed at the developments of spatially resolved XAFS techniques for gas phase investigation as well as high temperature/pressure batch reactor that allows for operando XAFS investigations. The technique (SpaciFB, Figure 1) has already undergone three phases of testing. 1) investigation of the hydrogen effect promotion of the CO oxidation. 2) The first ever operando structure-activity investigations of Non-Thermal Plasma enhanced catalysts. 3) The spatially resolved investigation of kinetic oscillations during CO oxidation. The results of phase 1 & 2 are being summarised in two high impact publications (in-preparation).

The XAFS DRIFTS facility provides the UK Catalysis Hub and its network with a unique cutting edge resource for the investigation and understanding of real catalytic systems: what the active species is, how it is activate and importantly deactivates so that we can develop our knowledge of catalytic mechanisms and develop new catalysts with increased activity and productively, to promote new and more efficient reactions of relevance to global challenges and industrial processes.

Dr. Josie Goodall, Project Manager (UK Cataysis Hub)

Who has access?

Catalysis Hub network and academics in collaboration with Hub researchers.

Is there preferential access given to a particular type of researcher? E.g. Based on institution, field of research

Members of the UK catalysis hub ( industrial or academic)

Any SLAs or standards (eg ISO, ..) associated with the facility?

None

Additional Technical Details

Cary 680 Agilent Fourier transform Infra red spectrometer combined with Praying mantis optics and a Harrick DaVinci Arm to allow combined XAFS /DRIFTS experiments ( combined XAFS / DRIFTS spectrometer )

Does it require an on-site visit to use the facility/equipment?

Yes/No. The facility is situated at the Harwell campus, however regular experiments can be taken to beamlines (e.g diamond light source, ESRF etc).

Are there costs associated/fees? Please explain.

Free at the point of use however costs (travel, substance, consumables, chemicals) are incurred by collaborators and other costs may be incurred during beam times at synchrotrons. Users are expected to provide their own consumables and chemicals.

Can it be bought as a service with access to a team of experts?

No, however the hub is pleased to collaborate. An understanding of the techniques used (IR and XAS would be needed to understand the data produced). Users would be expected to get training and learn how to use the machine or collaborate scientifically with researchers as part of he UK catalysis Hub.

 One of the remits of the UK Catalysis Hub is to maximise the opportunity presented by having a physical research base on the RAL campus. The ability to develop bespoke sample environments, in conjunction with Diamond, that the entirety of the UK Catalysis Hub have access to is a unique situation and strategic advantage for UK catalytic science.

Related publications and articles

  • E. K. Gibson, E. M. Crabb, D. Gianolio, A. E. Russell, D. Thompsett, P. P. Wells, Understanding the role of promoters in catalysis: operando XAFS/DRIFTS study of CeOx/Pt/Al2O3 during CO oxidation, Catalysis, Structure & Reactivity (2017) 3, 5
  • Emma K. Gibson, Andrew M. Beale, C. Richard A. Catlow, Arunabhiram Chutia, Diego Gianolio, Anna Gould, Anna Kroner, Khaled M. H. Mohammed, Michal Perdjon, Scott M. Rogers, Peter P. Wells, Restructuring of AuPd nanoparticles studied by a combined XAFS/DRIFTS approach, Chem. Mater, 27 (10), pp 3714– 3720, DOI: 10.1021/acs.chemmater.5b00866

Where is it located?

Harwell research complex
68 Maxwell Ave
Didcot
OX11 0FA

Schematic of the cell showing the beam and IR 

“The XAFS DRIFTS set up is a popular instrument in our laboratory used by many researchers for various applications. This combined technique allows real time analysis of the changes taking place on a catalyst surface and oxidation state changes of the metals, allowing a deeper understanding of reaction pathways crucial to the chemical industry”

– June Callison, Research Technician (UCL)

Main contact & applications:

UK Catalysis Hub
Dr. Josie Goodall (Project Manager)
E: josie.goodall@rc-harwell.ac.uk

Potential relevant disciplines:

EXAFS, catalysis, chemistry , material science

Links: 

Watch: in situ DRIFTS setup

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