Versatile x-ray spectroscopy facility

X-ray photoelectron and emission spectroscopies (XPS and XES) are fundamental tools for characterizing the chemical composition of materials at their surfaces. Conventional instrumentation can only probe samples under vacuum conditions, and hence volatile or aqueous samples must be frozen prior to measurement.  This can change the sample behaviour and makes it difficult to monitor evolution over time.

Through funding from the Royce Institute, we are developing a bespoke instrument that will establish the world’s first multi-technique X-ray core level spectroscopy facility for the characterization of materials under natural environmental conditions. This will enable measurement of samples and devices containing volatile components (e.g. solvents, adsorbed gases, biological and biomaterials, pastes and suspensions) without cryogenic cooling for the first time. 

It will also allow investigation of electrically insulating samples, studies of whole devices and dynamic processes, and depth profiling of molecular materials, all under environmental conditions. The facility will link directly with the Leeds beam-line at the Diamond Light Source - the UK’s national synchrotron facility. 

Equipment

Combining hard and soft X-ray photoelectron (XPS) with X-ray emission spectroscopy (XES), researchers will be able to characterise the nature of chemical bonding and chemical composition. Environmental control will allow users to characterise materials under conditions relevant for manufacture and application.

The instrument suite also interfaces seamlessly with the Multifunctional Heterostructured Materials Facility and our cleanroom facility.

  • Bespoke XPS system, configured around a Specs EnviroESCA system
  • Ar cluster source
  • Charge neutralisation
  • UHV XPS module with Al (monochromatic)
  • Zr and Cr Kα sources and noble gas ion etching
  • EasyXES 100
  • High pressure sample preparation chamber for sample transfer to UHV
  • Sample transport devices (‘suitcases’), linking to UHV, glovebox and cleanroom environments
  • In-situ and operando cells for synchrotron XAS, including environmental chambers for electron-yield and optical luminescence yield NEXAFS
  • Crystallisers and liquid jet devices for probing of liquids with synchrotron X-ray absorption, X-ray Raman scattering, X-ray scattering and X-ray Pair Distribution Function measurements

Researchers can perform measurements such as:

  • Characterisation of samples and devices containing volatile components (e.g. solvents, adsorbed gases, biological and biomaterials, pastes and suspensions), without cryogenic cooling
  • Investigations of electrically insulating samples
  • Studies of whole devices and dynamic processes
  • Depth profiling of molecular materials by controlled erosion with a noble gas cluster source
  • Rapid XPS characterisation of sample libraries under environmental conditions.

The facility is linked to the Diamond Leeds collaboration with a view to supporting users in design, application and preparation of experimental programmes with advanced X-ray characterisation at the UK’s synchrotron facility, Diamond.

Partners and sponsors

The Henry Royce Institute, which is the UK's National Centre for Research and Innovation of Advanced Materials. It operates as a hub and spoke model, with the hub at The University of Manchester, and spokes at the founding partners, initially comprising the universities of Sheffield, Leeds, Liverpool, Cambridge, Oxford and Imperial College London, as well as UKAEA and NNL.

Diamond Light Source is the UK’s national synchrotron. Diamond is one of the most advanced scientific facilities in the world, and its pioneering capabilities are helping to keep the UK at the forefront of scientific research.

Members of staff

Professor Sven Schroeder, Royal Academy of Engineering Bragg Centenary Chair in Engineering Applications of Synchrotron Radiation

Research Interests: In situ process monitoring in microreactors, state-of-the-art spectroscopies and microscopies, Interface and colloid science, surface and solid state physics, instrument development and synchrotron radiation experiments (in situ X-ray spectroscopy, scattering and fluorescence). 

Dr Elizabeth Willneff, Senior Research Fellow, School of Design

Research Interests: colloid and interface science – microemulsions, surfactants, X-ray spectroscopy – XPS, XAS (NEXAFS, XANES, EXAFS), synchrotron analytical methods, chemistry of synthetic organic pigments and quantum chemical calculations.