A pEek on the lab
national physical laboratory (uk)
LAB and RESEARCH
ELECTROCHEMISYRY & RAMAN SPECTROSCOPY LABORATORY
This is a chemistry laboratory suited to performing electrochemical and spectroscopic measurements. The laboratory is equipped with several potentiostats and houses the confocal Raman microscope used for ex situ, in situ and operando Raman spectroscopy measurements.
SURFACE CHAMICAL ANALYSIS LABORATORY
The surface chamical analysis laboratory is set up to allow surface chemical analysis measurements on a variety of samples including energy storage materials. A suite of techniques including XPS, HAXPES, SIMS, and OrbiSIMS allow the determination of elemental and chemical composition of the surface region of materials (i.e. within several nanometres depth), both in depth and spatially resolved. Other techniques include AFM for imaging the topography of sample surfaces, and ellipsometry for characterizing the dielectric properties of thin films.
GLOVE BOX LABORATORY
This chemistry laboratory is housing an MBraun LabMaster Pro glovebox that is used for storage of air sensitive chemicals as well as assembly/disassembly of battery cells for spectroelectrochemistry as well as battery metrology research. The glove box is fitted with an additional solvent trap (LMF) that allows us to handle small volumes of liquid electrolytes within the box.
Renishaw inViaTM QontorTM confocal microscope
The confocal Raman microscope used by the Electrochemistry Group at NPL is a Renishaw inViaTM QontorTM system equipped with two 50 mW lasers (532 nm and 660 nm). The system includes Rayleigh filters, two exchangeable gratings (600 lines mm-1 and 1800 lines mm-1) and a Peltier-cooled CCD detector. The microscope optics include 5×, 20× and 50× long working distance objective lenses, mounted on a high speed encoded motorized XYZ stage.
Kratos AXIS Supra+ X-ray photoelectron spectrometer
The X-ray photoelectron spectrometer used by the Surface Technology Group at NPL is an AXIS Supra+ instrument from Kratos Analytical Ltd. The instrument is equipped with a monochromated dual-anode X-ray source (Al Kα / Ag Lα) for XPS and hard X-ray photoelectron spectroscopy (HAXPES). A gas cluster ion source (GCIS) is attached to the analysis chamber to allow surface cleaning and depth profiling of samples using monoatomic Ar+ ions or Ar-clusters. Air-sensitive samples can be transferred into the instrument without exposure to ambient atmosphere using an inert atmosphere sample holder.
OrbiSIMS ION TOF
OrbiSIMS (Hybrid-SIMS, IONTOF, GmbH, Germany) consists of a time-of-flight secondary ion mass spectrometer (ToF SIMS) platform and an Orbitrap Q ExactiveTM mass analyser. This dual analyser approach provides mutually synergistic benefits; the high-speed of the ToF analyser, necessary for 3D imaging, supports the slower speed of the Orbitrap (up to 20 Hz) and conversely the high mass accuracy and mass resolving power of the Orbitrap compensates for the more limited performance of the ToF analyser. The instrument is equipped with a Bi analysis gun, and sputter guns of Ar (gas cluster ion beam), O2 and Cs. There is also a Leica chamber to allow inert sample transfer.
Principal Research Scientist, NPL
Andy Wain is a principal research scientist in the Electrochemistry Group at NPL and leads the theme of Interfacial Chemistry and Catalysis, which aims to support industry through a suite of cutting-edge tools for characterising electrochemically active materials. His research interests include electrochemical energy conversion and storage, nanoelectrochemistry, heterogeneous catalysis, corrosion and electrochemical sensing.
Andy received a Master’s degree in Chemistry from Oxford University in 2003 and was awarded his doctorate in spectroelectrochemistry in 2006 from the same institution. He then spent two years as a postdoctoral research associate at California State University Los Angeles, where he focused on novel electrochemical approaches to studying bio-molecule modified interfaces. Andy has worked at NPL since 2008.
Andy has worked on a range of projects at NPL, most notably in establishing a capability for electrochemical imaging over multiple length scales. A more recent focus has been the development and application of novel approaches to operando molecular vibrational spectroscopy (FTIR and Raman spectroelectrochemistry). Andy has published over 70 peer-reviewed papers, 3 book chapters and an edited volume on Nanoscale Electrochemistry. In 2013 he achieved chartered chemist (CChem) status and is now a Fellow of the Royal Society of Chemistry (FRSC) and a Fellow of the Institute of Materials, Minerals & Mining (FIMMM).
Higher Research Scientist, NPL
Rudra Samajdar is a higher research scientist at the Electrochemistry Group in NPL, working in the Interfacial Chemistry and Catalysis theme, supporting NPL research in batteries, hydrogen, and biosensors in commercial and Government contracts. Rudra’s research interests primarily include developing spectroscopic methods for studying (electro)chemical phenomena at different time and length scales, aimed towards understanding energy storage and harvesting, sensing, and fundamental physical chemistry.
Rudra received an integrated MS-PhD from the Solid State and Structural Chemistry Unit, Indian Institute of Science, Bangalore, India in 2019, working on physical chemistry of haem proteins. Subsequently he continued as a post-doc during 2019 at the Indian Institute of Science, working on biomolecular redox mediation in lithium-oxygen batteries, and electron transfer over bio-functionalized electrodes. In 2020, he moved to the University of Strathclyde as a post-doc to study electrolytes for magnesium electrolytes using vibrational spectroscopy. Rudra has worked at NPL since August 2021.
Rudra’s work at NPL currently involves using vibrational spectroscopy to understand electrochemical interfaces in operando. Some of his recent work has involved developing an efficient spectro-electrochemical methodology for studying organic electrolytes, and using Raman/FTIR spectroscopy to understand complex mass transport effects at electrode surfaces. An ongoing area of interest is developing set-ups for multi-modal/hyperspectral analysis of electrochemical energy devices.
Rudra is a member of the American Chemical Society.
Links: Google Scholar , LinkedIN , Twitter
Alex Shard obtained his PhD in surface modification and analysis from Durham University in 1992 and has been active in surface chemical analysis since then, working at the University of Nottingham and Daresbury Laboratory, and then as a lecturer at the Robert Gordon University and senior lecturer at the University of Sheffield.
He joined NPL in 2006 and is now Head of Chemical Sciences for the Chemical, Medical and Environmental Science Department. Alex has over 150 peer-reviewed publications and he regularly presents at national and international conferences. Alex is a Fellow of the Royal Society of Chemistry. In 2020 he was awarded the RSC Industrial Analytical Award for “pioneering accurate chemical measurements of surfaces and interfaces”.
Higher Research Scientist, NPL
Sofia Marchesini is a Material Engineer with expertise/interest in materials for energy storage, and 2D materials. She joined the Surface Technology Group at the National Physical Laboratory in 2018 to develop analytical methods and standards underpinning the industrial exploitation of these materials.
Previously, Sofia received a PhD from the Department of Chemical Engineering at Imperial, co-funded by the CDT-ACM and BP-ICAM. Sofia was awarded the 2019 Founders’ Award for the research performed during her time at Imperial. Sofia is originally from Italy, where she received a MSc in Materials Engineering in 2014 from the University of Padova.
Sofia is a Professional Member of the IOM3.
Links: Google Scholar, LinkedIn
Higher Research Scientist, NPL
Benjamen Reed obtained his PhD from Aberystwyth University and the DST CDT in 2020 studying the catalytic conversion of diamond and silicon carbide surfaces into epitaxial graphene.
He is currently a Higher Research Scientist in the Surface Technology group and joined NPL in 2018. Ben’s research includes X-ray photoelectron spectroscopy (XPS) metrology, developing standardised procedures of XPS measurement, calibration, and analysis. He also has an active interest in the characterisation of graphene, 2D materials, and energy storage materials with photoelectron techniques.
Benjamen organises and participates in interlaboratory comparisons with the Versailles Project on Advanced Materials and Standards (VAMAS) under the auspices of the Surface Chemical Analysis technical working area (TWA 2). He is a UK expert for ISO/TC 201 (Surface Chemical Analysis) on SC7 (Electron Spectroscopies). He is also a member of the Institute of Physics.
Full publication list available on Google Scholar.
NPL Senior Fellow & Head of Science
Prof. Ian Gilmore is Head of Science at the National Physical Laboratory (NPL), Senior NPL Fellow and a Visiting Professor in the School of Pharmacy at the University of Nottingham. He is founding director of the UK’s National Centre of Excellence in Mass Spectrometry (NiCE-MSI). Ian’s research goal is to achieve super-resolution label-free metabolic imaging. He has a special interest in reducing drug attrition through measuring where drugs go and their pharmacological effect at a sub-cellular scale.
To study this, he created the revolutionary 3D OrbiSIMS (Nature Methods 2017) in collaboration with GlaxoSmithKline. His research interests also include 3D molecular imaging of complex interfaces in organic electronics, batteries and additive manufactured devices using OrbiSIMS and FIB-SIMS.
Ian has over 25 years’ experience in mass spectrometry of surfaces and has published more than 140 peer-reviewed papers. He is a consultant and advisor to a number of companies, including GlaxoSmithKline and Samsung. He was awarded the IoP Paterson medal (2004) and the UKSAF Riviere prize (2013) for a major contribution to international leadership in surface analysis.
Ian leads international standardisation in surface chemical analysis and is chair of ISO TC 201 SC 6 (Mass Spectrometry) and chair of VAMAS TWA 2. He is championing the topic of reproducibility in research and has recently published on this topic (Nature 2017, JVST A 2018, NIST Journal Research 2019).
Higher Research Scientist, NPL
Yundong completed an undergraduate degree in Materials Science & Engineering at Central South University and finished his final year project on developing dye-sensitized solar cells at Monash University in Australia. Following that, he completed a PhD in developing polymer – ionic liquid composites as solid state electrolytes for solid state batteries at Deakin University. Yundong worked as a Faraday Institution Research Fellow developing an innovative in-situ Raman system for studying cathode – solid electrolyte interface in solid state batteries at University of Liverpool. He also worked shortly in a Cambridge University spin out developing a fast-charging anode material.
Yundong joined the National Centre of Excellence for Mass Spectrometry Imaging at NPL to develop the technique TOF-SIMS and OrbiSIMS for studying battery material surfaces and interfaces. TOF-SIMS and OrbiSIMS are useful techniques for studying batteries and will be used widely in the future.