A Facility for Ambient Pressure Photoelectron Spectroscopy (APPES) (R)
Lead Research Organisation:
Imperial College London
Department Name: Materials
Abstract
For over 50 years, x-ray photoelectron spectroscopy (XPS) has demonstrated itself as an invaluable technique in the study of filled electronic states of solids, as well helping to determine the nature of interactions between solid surfaces and molecular species. Unfortunately there is one main drawback in the technique, that being that typical XPS measurements are performed in ultra high vacuum (UHV) conditions (10-10 mbar), due to the need of minimising the chances of unfavourable collisions occurring before the excited photoelectrons reach the energy analyser. Due to this restraint, studying the surfaces of technologically important materials occurs at a pressure many orders of magnitude lower than the operational conditions of the systems themselves (1-50 bar). Bridging this so-called "Pressure Gap" has remained a significant technological challenge. Very recent developments in electron energy analyser and sample holder design have for the first time allowed photoelectron spectroscopic measurements to be performed in ambient pressures of up to 25 mbar. The opportunity to study "real" surfaces in-situ and in-operando is a step change in the field of photoelectron spectroscopy, and opens a new and vital chapter in the area of surface science.
The ambient pressure photoelectron spectroscopy (APPES) system is a state-of-the-art laboratory-based instrument with capabilities of performing high-energy resolution, low signal-to-noise photoemission measurements in up to 25 mbar ambient pressure with a number of different gases (O2, N2, H2, ethylene, acetylene). The instrument is equipped with a monochromated x-ray source and a high transmission, differentially pumped electron energy analyser. The system is fitted with an in-situ sample cell, which can provide a temperature range of 80 - 1100 K in the ambient atmospheres, permitting in-operando measurements. This specially designed modular in-situ cell, which is fully retractable from the analysis chamber, also allows standard UHV XPS comparative measurements to be performed with ease.
The APPES instrument based at the Department of Materials, Imperial College London will be highly multidisciplinary, covering five broad research themes (i) Energy; (ii) Catalysis; (iii) Electronic Materials; (iv) Biomaterials; (v) Environmental and Heritage Science. The instrument, while hosted at Imperial is engaged in highly collaborative research at a regional, national (including the Diamond Light Source) and international level, with access arrangements also provided through coordination the National XPS Facility (NEXUS) at the University of Newcastle. This new approach to providing wide- reaching access will allow the APPES technique to be fully exploited and generate world-leading cutting edge scientific output.
The ambient pressure photoelectron spectroscopy (APPES) system is a state-of-the-art laboratory-based instrument with capabilities of performing high-energy resolution, low signal-to-noise photoemission measurements in up to 25 mbar ambient pressure with a number of different gases (O2, N2, H2, ethylene, acetylene). The instrument is equipped with a monochromated x-ray source and a high transmission, differentially pumped electron energy analyser. The system is fitted with an in-situ sample cell, which can provide a temperature range of 80 - 1100 K in the ambient atmospheres, permitting in-operando measurements. This specially designed modular in-situ cell, which is fully retractable from the analysis chamber, also allows standard UHV XPS comparative measurements to be performed with ease.
The APPES instrument based at the Department of Materials, Imperial College London will be highly multidisciplinary, covering five broad research themes (i) Energy; (ii) Catalysis; (iii) Electronic Materials; (iv) Biomaterials; (v) Environmental and Heritage Science. The instrument, while hosted at Imperial is engaged in highly collaborative research at a regional, national (including the Diamond Light Source) and international level, with access arrangements also provided through coordination the National XPS Facility (NEXUS) at the University of Newcastle. This new approach to providing wide- reaching access will allow the APPES technique to be fully exploited and generate world-leading cutting edge scientific output.
Planned Impact
Since the first development of x-ray photoelectron spectroscopy (XPS) over 50 years ago, the technique has formed the basis of numerous scientific breakthroughs providing vast economic and societal benefits. The proposed APPES technique, has the potential to have an even greater impact, due to the fact that the surface electronic structure of a wide array of different materials, each with their own technological applications will be be studied under conditions close to which they operate.
The obvious beneficiary of APPES measurements is in the commercial private sector, with emphasis on businesses operating in all the identified research themes. For example, Johnson-Matthey who work within the area of catalysis, could utilise the technique for understanding how catalysts behave in near-operational conditions. This could lead to significant improvements in reactor design and lowering catalyst cost, thereby the technique will have a direct economic impact.
The impact to the planned VERSOX beamline at the Diamond Light Source is important to stress. This proposal seeks to help to coordinate and develop the national capability, and strategy, in the APPES technique at a personnel, instrumentation and scientific output level.
There are a number of government agencies who would benefit from this research including the Health Protection Agency (HPA - Biosafety Unit, Decontamination Studies and Molecular Identification Services), the Environment Agency (National Laboratory Service). We would also seek to liaise and seek collaborative research efforts with the National Physical Laboratory (NPL). Understanding how pathogens behave in contact with surgical instruments, without exposing the samples to extreme UHV environments would have great national and international health benefits. One experiment could look at the growth of pathogens under aerobic and anaerobic conditions within a specially designed in-situ high pressure cell.
The APPES technique would also have a great impact on the area of conservation and heritage science, where we have already sought interest in the study of paint pigments from a colleague at Tate Britain. As the instrument is hosted geographically close to many museums (Natural History, Science Museum, V&A) we would seek to establish collaborative research with those institutions. We would also use the Institute of Conservation as a point of contact for planned heritage science research.
At a more specific project level, the Lead Co-I will develop a range of skills including public communication (training by the Royal Society), a well as opportunities to interact with government and policy makers at a national level (again through the Royal Society MP-Scientist pairing scheme).
The obvious beneficiary of APPES measurements is in the commercial private sector, with emphasis on businesses operating in all the identified research themes. For example, Johnson-Matthey who work within the area of catalysis, could utilise the technique for understanding how catalysts behave in near-operational conditions. This could lead to significant improvements in reactor design and lowering catalyst cost, thereby the technique will have a direct economic impact.
The impact to the planned VERSOX beamline at the Diamond Light Source is important to stress. This proposal seeks to help to coordinate and develop the national capability, and strategy, in the APPES technique at a personnel, instrumentation and scientific output level.
There are a number of government agencies who would benefit from this research including the Health Protection Agency (HPA - Biosafety Unit, Decontamination Studies and Molecular Identification Services), the Environment Agency (National Laboratory Service). We would also seek to liaise and seek collaborative research efforts with the National Physical Laboratory (NPL). Understanding how pathogens behave in contact with surgical instruments, without exposing the samples to extreme UHV environments would have great national and international health benefits. One experiment could look at the growth of pathogens under aerobic and anaerobic conditions within a specially designed in-situ high pressure cell.
The APPES technique would also have a great impact on the area of conservation and heritage science, where we have already sought interest in the study of paint pigments from a colleague at Tate Britain. As the instrument is hosted geographically close to many museums (Natural History, Science Museum, V&A) we would seek to establish collaborative research with those institutions. We would also use the Institute of Conservation as a point of contact for planned heritage science research.
At a more specific project level, the Lead Co-I will develop a range of skills including public communication (training by the Royal Society), a well as opportunities to interact with government and policy makers at a national level (again through the Royal Society MP-Scientist pairing scheme).
People |
ORCID iD |
David Payne (Principal Investigator) |
Publications
Kahk J
(2015)
A study of the pressure profiles near the first pumping aperture in a high pressure photoelectron spectrometer
in Journal of Electron Spectroscopy and Related Phenomena
Eriksson SK
(2014)
A versatile photoelectron spectrometer for pressures up to 30 mbar.
in The Review of scientific instruments
Edwards M
(2015)
Increased photoelectron transmission in High-pressure photoelectron spectrometers using "swift acceleration"
in Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment
Kerherve G
(2017)
Laboratory-based high pressure X-ray photoelectron spectroscopy: A novel and flexible reaction cell approach.
in The Review of scientific instruments
García-Trenco A
(2018)
PdIn intermetallic nanoparticles for the Hydrogenation of CO2 to Methanol
in Applied Catalysis B: Environmental
Tetzner K
(2017)
The impact of post-deposition annealing on the performance of solution-processed single layer In 2 O 3 and isotype In 2 O 3 /ZnO heterojunction transistors
in Journal of Materials Chemistry C
Regoutz A
(2018)
The influence of oxygen on the surface interaction between CO2 and copper studied by ambient pressure X-ray photoelectron spectroscopy
in Surface Science
Description | This grant has allowed the development of the world-leading laboratory-based high-pressure photoelectron spectrometer. We have developed a unique system that allows the measurement of chemistry and physics of surfaces under a gaseous environment - compared to traditional vacuum measurements. The unique high-pressure reaction cell allows precision control of sample environment, thereby allowing controlled and reproducible measurements to be performed. The system has been performing above expectation is is the focal point of 3 EPSRC awards -studying the surface chemistry of solid oxide fuel cells and carbon dioxide reduction catalysts. In 2020 the system was upgraded to incorporate an angle-resolved photoelectron spectrometer (ARPES), coupled to a high pressure XPS system. This is the first system of its type in the world. |
Exploitation Route | There are a number of publications in the process of being published based on this work. We have done extensive research to understand the behaviour of gas flow near the sample surface - which is very important to the high-pressure XPS community as knowing exactly the pressure of the surface at the point of measurement, is critical to understanding the surface chemistry. We have implemented a number of upgrades to the system, which will increase the signal-to-noise of spectra and also reducing the time taken to perform experiments, as well as currently attaching a new chamber to the system for preparation of single crystal surfaces (work done in collaboration with Royal Dutch Shell. All of these activities will be used by the wider (global) photoemission community We are now currently measuring the O2 interaction with haemoglobin. The first demonstration of this technique on biologically critical proteins. |
Sectors | Chemicals Electronics Energy Environment Healthcare Manufacturing including Industrial Biotechology Culture Heritage Museums and Collections Pharmaceuticals and Medical Biotechnology |
Description | We are happy to begin delivering significant impact in each of the 5 research themes (catalysis, energy materials, electronic materials, biomaterials, environment and heritage science). The theme of catalysis has already secured an EPSRC award to study CO2 reduction catalysts using high-pressure XPS, and two more on SOFCs (energy materials). We discovered the need to use an in-line gas purifier to lower contamination to the ppb levels. This was published in Review of Scientific Instruments in 2017. |
Sector | Chemicals,Energy,Environment,Manufacturing, including Industrial Biotechology,Culture, Heritage, Museums and Collections |
Impact Types | Economic |
Description | EPSRC Strategic Advisory Team for Capital Equipment |
Geographic Reach | National |
Policy Influence Type | Participation in a guidance/advisory committee |
URL | http://www.epsrc.ac.uk/research/ourportfolio/themes/researchinfrastructure/strategy/ |
Description | Oral evidence for the report on Scientific Infrastructure to the House of Lords Select Committee for Science and Technology |
Geographic Reach | National |
Policy Influence Type | Contribution to a national consultation/review |
URL | http://www.publications.parliament.uk/pa/ld201314/ldselect/ldsctech/76/7602.htm |
Description | Roadmap for Photoelectron Spectroscopy |
Geographic Reach | National |
Policy Influence Type | Contribution to a national consultation/review |
URL | https://www.epsrc.ac.uk/funding/calls/capitalroadmapspectroscopy/ |
Description | Energy Resilient Manufacturing |
Amount | £295,230 (GBP) |
Funding ID | EP/M013839/1 |
Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
Sector | Public |
Country | United Kingdom |
Start | 01/2015 |
End | 06/2016 |
Description | Experimental Equipment Call |
Amount | £1,461,911 (GBP) |
Funding ID | EP/M028291/1 |
Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
Sector | Public |
Country | United Kingdom |
Start | 03/2015 |
End | 03/2016 |
Description | Industrial Funding |
Amount | £620,000 (GBP) |
Organisation | Total E & P |
Sector | Private |
Country | United Kingdom |
Start | 04/2017 |
End | 04/2019 |
Description | Regenerative Medicine Capital June 2013 |
Amount | £29,500 (GBP) |
Funding ID | MR/L012677/1 |
Organisation | Medical Research Council (MRC) |
Sector | Public |
Country | United Kingdom |
Start | 08/2013 |
End | 08/2017 |
Description | SUPERGEN Fuel Cells Challenge |
Amount | £1,076,043 (GBP) |
Funding ID | EP/M014142/1 |
Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
Sector | Public |
Country | United Kingdom |
Start | 03/2015 |
End | 03/2019 |
Description | SUPERGEN Fuel Cells Challenge |
Amount | £1,229,672 (GBP) |
Funding ID | EP/M014304/1 |
Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
Sector | Public |
Country | United Kingdom |
Start | 01/2015 |
End | 12/2017 |
Description | Scienta Omicron |
Organisation | Scienta Omicron GmbH |
Country | Germany |
Sector | Private |
PI Contribution | Scienta Omicron are the manufacturers of the high pressure XPS instrument, and have provided support in attempting some exciting new experiments. |
Collaborator Contribution | They have promised to underpin any unintentional damage to the spectrometer caused by the experiments we wish to perform. |
Impact | We have so far published 4 papers together, with another 2 in preparation. |
Start Year | 2014 |
Description | Shell |
Organisation | Shell Global Solutions International BV |
Department | Shell Global Solutions UK |
Country | Netherlands |
Sector | Private |
PI Contribution | We are currently still designing the new chamber to be added to the high pressure XPS system |
Collaborator Contribution | Shell have provided funding to allow me to build a new chamber for preparing surfaces for high pressure XPS measurements. The research will be focused on corrosion research of pipeline materials. |
Impact | Too early for any outputs |
Start Year | 2015 |
Description | University of Oxford |
Organisation | University of Oxford |
Department | Inorganic Chemistry |
Country | United Kingdom |
Sector | Academic/University |
PI Contribution | We are working in collaboration with Charlotte Williams (University of Oxford). At Imperial we will be performing high pressure XPS on industrially relevant catalysts for CO2 reduction to methanol. |
Collaborator Contribution | Our collaborator in Oxford will be synthesising and testing the performance of these new catalysts. |
Impact | The publication outputs have been captured in the other submission (EP/M013839/1) for the specific collaborative work on catalysis. |
Start Year | 2015 |