NANOESCA - ELECTRON SPECTROSCOPY FOR CHEMICAL ANALYSIS IMAGED AT THE NANOSCALE.

Lead Research Organisation: University of Bristol
Department Name: Chemistry

Abstract

The NanoESCA is an Ultra High Vacuum (UHV) photoemission spectroscopy system with sub-micron spatial resolution for real-space and k-space (reciprocal space) mapping from areas of a few microns of flat material surfaces, and the capability to perform quantitative chemical state mapping at the nanoscale. The system is designed for installation on a synchrotron beam line end-station or in a Nano Science Laboratory.
The system has various modes of operation. UV photon sources are used for Ultra-violet Photoemission Spectroscopy (UPS), Angle Resolved UPS, and Photo Emission Electron Microscopy (PEEM), soft X-rays are used for X-ray Photoemission Spectroscopy (XPS). UPS gives energy filtered information on weakly bound states and the valence band structure in real space and the surface electronic band structure in k-space. XPS is used to probe core level spectra to obtain quantitative information on the chemical composition of a surface. In contrast to the high resolution Scanning Electron Microscope, PEEM directly images surface areas emitting photoelectrons in real time without scanning. By energy filtering PEEM images it is possible to obtain quantitative maps of surface work function. The field of view is adjustable from millimetres to microns allowing high resolution imaging of features as small as 30nm (UPS modes) and 480nm (XPS mode).
The NanoESCA machine being requested represents the next generation in imaging and spectroscopic PEEM. It uses an extension of the established parallel imaging technique, to simultaneously image and filter photoelectrons, by using a double hemispherical (aberration corrected) electron analyser in combination with high photon flux VUV and X-ray sources, to realise nano scale imaging and spectroscopy in real space and in k-space; the latter mode allows information on the electronic band structure of materials to be visualised and compared directly with theoretical models. Uniquely, this capability to obtain nanoscale spectroscopy using either X-ray or VUV sources is obtained by parallel imaging through the same PEEM 'column' which also acts as the entrance lens of the imaging spectrometer.

Planned Impact

The impact of the NanoESCA on University of Bristol (UoB) research themes will be transformative due to new insights expected into the properties of materials at the nanoscale impacting: Nanoscience and Quantum Information (Nanostructured devices for photon/electron confinement in Diamond and Silicon); Electronic and Photonic Materials (Functional complex oxides for solar fuels, Organic Spintronics, Diamond thermionics); Advanced Composites and Intelligent Structures (Next Generation GaN-on-Diamond RF Power Amplifier Devices, Bone and tissue engineering). Each of these themes supports research over a wide range of EPSRC-funded activities ensuring high demand for NanoESCA on existing and future grants.
 
Description Materials discovery due to unique visualisation of material properties.
A new photoemission technique has been developed that allows the unoccupied levels of a crystalline material to be visualised. This technique is applicable to materials being researched for applications in valleytronics, spintronics, voltaics and phononics.
Exploitation Route Bristol NanoESCA has been made a University Facility providing a service to materials researchers located at SW region universities including Bath, Cardiff, Exeter, Oxford, and a basis for international collaborations with researchers in Norway, Denmark, Italy, Germany, France, USA and Japan.
Sectors Aerospace, Defence and Marine,Education,Electronics,Energy

URL http://www.bristol.ac.uk/physics/facilities/nanoesca/
 
Description Have completed impact acceleration KTS project to demonstrate that samples pre analysed in the Bristol NanoESCA may be transported under ultra high vacuum to a synchrotron beam line (I05 at Diamond Light Source) and further high resolution analysis performed on the end station without any sample preparation. In 2020 we have also demonstrated that this preanalysis technique may be used in conjunction with national synchrotron facilities overseas. For this trial beamtime was successfully completed at Elettra in Trieste, Italy, on the Spectromicroscopy beamline. Diamond Light Source has been funded by EPSRC to evaluate laser PEEM capability linked to I06 beamline. Bristol are supporting this project providing lab beam time analysis of selected 2D materials and have also been training beam line scientists to operate the NanoESCA. Samples have been exchanged between Bristol and Diamond by UHV suitcase.
First Year Of Impact 2019
Sector Energy
 
Title Data from AlO diamond termination paper in PSSB 
Description This is the data repository for the paper 'Experimental Studies of Electron Affinity and Work Function from Aluminium on Oxidised Diamond (100) and (111) Surfaces' by Michael C. James, Mattia Cattelan, Neil A. Fox, Rui F. Silva, Ricardo M. Silva and Paul W. May. Physica Status Solidi B (2021). 
Type Of Material Database/Collection of data 
Year Produced 2021 
Provided To Others? Yes  
URL https://data.bris.ac.uk/data/dataset/3ohhlefvl13zr23pcl9u55a21f/
 
Title Data from photoluminescence spectroscopy, admittance spectroscopy, photoelectron emission microscopy, current-voltage characteristics, and spectral response of quantum efficiency measurements on Cu2ZnZnSnS4 (CZTS) films and solar cells as a function of... 
Description This is the dataset used in the journal article to be published in American Chemical Society's Applied Energy Materials. Article Title: Mapping the Energetics of Defect States in Cu2ZnSnS4 films and the Impact of Sb DopingAuthors: Devendra Tiwari, Michael V. Yakushev, Tristan Koehler, Mattia Cattelan, Neil Fox, Robert W. Martin, Reiner Klenk and David J FerminDOI: https://10.1021/acsaem.1c03729 The dataset was produced in collaboration with colleagues from University of Bristol, Strathclyde University and Helmholtz Zentrum Berlin. The dataset contains .csv files and can be accessed can be using any text editor or any spreadsheet software. 
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://figshare.northumbria.ac.uk/articles/dataset/Data_from_photoluminescence_spectroscopy_admitta...
 
Title Data from photoluminescence spectroscopy, admittance spectroscopy, photoelectron emission microscopy, current-voltage characteristics, and spectral response of quantum efficiency measurements on Cu2ZnZnSnS4 (CZTS) films and solar cells as a function of... 
Description This is the dataset used in the journal article to be published in American Chemical Society's Applied Energy Materials. Article Title: Mapping the Energetics of Defect States in Cu2ZnSnS4 films and the Impact of Sb DopingAuthors: Devendra Tiwari, Michael V. Yakushev, Tristan Koehler, Mattia Cattelan, Neil Fox, Robert W. Martin, Reiner Klenk and David J FerminDOI: https://10.1021/acsaem.1c03729 The dataset was produced in collaboration with colleagues from University of Bristol, Strathclyde University and Helmholtz Zentrum Berlin. The dataset contains .csv files and can be accessed can be using any text editor or any spreadsheet software. 
Type Of Material Database/Collection of data 
Year Produced 2022 
Provided To Others? Yes  
URL https://figshare.northumbria.ac.uk/articles/dataset/Data_from_photoluminescence_spectroscopy_admitta...
 
Title Mapping Shunting Paths at the Surface of Cu2ZnSn(S,Se)4 Films via Energy-Filtered Photoemission Microscopy 
Description This deposition includes the data of the experiments and calculations used and presented in the article published in the Cell press journal: iScience titled:"Mapping Shunting Paths at the Surface of Cu2ZnSn(S,Se)4 Films via Energy-Filtered Photoemission Microscopy" authored by Devendra Tiwari, Mattia Cattelan, Robert L. Harniman, Andrei Sarua, Ali Abbas, Jake W. Bowers, Neil A. Fox, David J. Fermin. DOI: 10.1016/j.isci.2018.10.004 
Type Of Material Database/Collection of data 
Year Produced 2018 
Provided To Others? Yes  
 
Title The Impact of Sb and Na Doping on the Surface Electronic Landscape of Cu2ZnSnS4 Thin-Films 
Description This deposition includes the data of the experiments and calculations used and presented in the article published in the Journal: ACS energy letters, Authors: Devendra Tiwari, Mattia Cattelan, Robert L. Harniman, Andrei Sarua, Neil Fox, Tristan Koehler, Reiner Klenk and David J Fermin, DOI: https://10.1021/acsenergylett.8b02081 
Type Of Material Database/Collection of data 
Year Produced 2018 
Provided To Others? Yes  
 
Description Aarhus University 
Organisation Aarhus University
Country Denmark 
Sector Academic/University 
PI Contribution NanoESCA training for PhDs from Department of Physics and Astronomy at Aarhus University.
Collaborator Contribution Preparation of sample materials for analysis.
Impact Physics, Chemistry
Start Year 2019
 
Description Eindhoven University of Technology 
Organisation Eindhoven University of Technology
Country Netherlands 
Sector Academic/University 
PI Contribution NanoESCA Materials Analysis
Collaborator Contribution Complimentary Materials analysis and sample preparation.
Impact None to date.
Start Year 2016
 
Description Humboldt-Universität zu Berlin 
Organisation Humboldt University of Berlin
Country Germany 
Sector Academic/University 
PI Contribution NanoESCA Beamtime analysis of materials
Collaborator Contribution Provision of material samples.
Impact Physics, Chemistry
Start Year 2018
 
Description Laser PEEM facility at Diamond Light Source 
Organisation Diamond Light Source
Country United Kingdom 
Sector Private 
PI Contribution Provided NanoESCA training and pre-characterisation of samples for Laser PEEM project.
Collaborator Contribution Installation and commissioning of Laser PEEM.
Impact Publication is planned.
Start Year 2021
 
Description Linkoping University (Dr. Vagin) 
Organisation Linkoping University
Department Department of Physics, Chemistry and Biology (IFM)
Country Sweden 
Sector Academic/University 
PI Contribution NanoESCA materials analysis
Collaborator Contribution Complimentary materials analysis.
Impact Publication in preparation.
Start Year 2016
 
Description NPL (Dr. Kazakova) 
Organisation National Physical Laboratory
Country United Kingdom 
Sector Academic/University 
PI Contribution NanoESCA Materials Analysis.
Collaborator Contribution Material preparation.
Impact None to date.
Start Year 2017
 
Description Norwegian University of Science and Technology (NTNU) 
Organisation Norwegian University of Science and Technology (NTNU)
Country Norway 
Sector Academic/University 
PI Contribution Training for NTNU staff on the NanoESCA instrument platform.
Collaborator Contribution Technical advice on angle resolved photoemission of diamond.
Impact Physics, Chemistry
Start Year 2018
 
Description University of Bath (Dr. Da Como) 
Organisation University of Bath
Department Department of Physics
Country United Kingdom 
Sector Academic/University 
PI Contribution NanoESCA Material Analysis
Collaborator Contribution Sample preparation and complimentary analysis
Impact Publication in preparation.
Start Year 2017
 
Description University of Bath (Dr. Nogaret) 
Organisation University of Bath
Department Department of Physics
Country United Kingdom 
Sector Academic/University 
PI Contribution NanoESCA Materials Analysis
Collaborator Contribution Complimentary Materials analysis and sample synthesis.
Impact Publication in preparation.
Start Year 2017
 
Description University of Padova (Prof. Agnoli) 
Organisation University of Padova
Country Italy 
Sector Academic/University 
PI Contribution NanoESCA materials analysis
Collaborator Contribution Complimentary material analysis.
Impact Publication in press.
Start Year 2016
 
Description Aberration-Corrected PEEM Workshop 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Workshop on the upgrade of IO-6 beamline at Diamond Light Source to incorporate Aberration-Corrected PEEM. Discussions about sample transfer between IO6 and Bristol NanoESCA with attendees.
Year(s) Of Engagement Activity 2019
 
Description UKSAF 2018 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Industry/Business
Results and Impact Invited talk on the NanoESCA facility.
Year(s) Of Engagement Activity 2018