#SynchroLightAt75 – Historical perspective of catalysis at Elettra

“Catalysis, is a strange principle of chemistry which works in ways more mysterious than almost any other of the many curious phenomena of science” New York Times: June 8, 1923

Heterogeneous catalysis is one of the most extensively studied functional systems since it is in the heart of chemical industry, fuel, energy production and storage and also is part in the devices for environmental protection.

The key processes in heterogeneous catalysis occur at dynamic reactant/catalyst surface interfaces. Since these processes involve coupling between different electronic, structural and mass transport events at time scales from fs to days, and space scales from nm to mm, we are still far from full comprehension how to design and control the catalysts performance. In this respect the ultrabright and tunable light, generated at the synchrotron facilities, has opened unique opportunities for using powerful spectroscopy, spectromicroscopy, scattering and imaging methods for exploring the morphology and chemical composition of complex catalytic systems at relevant length and time scales and correlate them to the fabrication or operating conditions.

The very demanded for catalysis studies is the surface sensitive PhotoElectron Spectroscopy (PES), based on the photoelectric effect, for which Einstein won the 1921 Nobel Prize in Physics, and demonstrated for the first time in 1957 by Kai Siegbahn who was awarded the Nobel Prize in 1981. PES has overcome its time and space limitations for studies of catalytic surface reactions thanks to the synchrotron light, which also added the opportunity for complementary use of X-ray absorption spectroscopy. At Elettra, the first time resolved PES studies with model metal catalyst systems were carried out at SuperESCA beamline in 1993 and few years later PES microscopy instruments, Scanning PhotoElelectron Microscope (SPEM) and X-ray PhotoElectron Emission Microscope (XPEEM) at ESCAMicroscopy and Nanospectroscopy beamlines have allowed for sub-mm space resolved studies, including imaging of dynamic surface mass transport processes as well.

Implementation in the last decade of operando experimental set-ups at APE, BACH and ESCAMicroscopy experimental stations for bridging the pressure gap of PES investigations has led to significant achievements in monitoring in-situ chemical, electrochemical and morphology evolution of all types catalytic systems under reaction conditions. Further complementary studies using X-ray absorption spectroscopy in photon-in/photon-out mode, ongoing at the XAFS and TwinMic beamlines are filling some remaining knowledge gaps for paving the road towards knowledge-based design and production of these complex and very desired functional materials.

M. Amati, L. Bonanni, L. Braglia, F. Genuzio, L. Gregoratti, M. Kiskinova, A. Kolmakov, A.Locatelli, E. Magnano, A. A. Matruglio, T. O. Menteş, S. Nappini, P. Torelli, P. Zeller,” Operando photoelectron emission spectroscopy and microscopy at Elettra soft X-ray beamlines: from model to real functional systems”, J. Electr. Spectr. Rel. Phenom. (2019) doi: 10.1016/j.elspec.2019.146902.

For first SUPERESCA – A. Baraldi, G. Comelli, S. Lizzit, M. Kiskinova, G. Paolucci “Real-Time X-Ray Photoelectron Spectroscopy of Surface Reactions” Surf. Sci. Reports 49, Nos. 6-8 (2003) 169.

For XPEEM A. Locatelli and M. Kiskinova “Imaging with Chemical Analysis: Adsorbed Structures Formed during Surface Chemical Reactions” A European Journal of Chemistry, 12 (2006) 8890.

Image: From model to real catalysts: structural and chemical complexity

Lightsources.org virtual symposium recording

Lightsources.org was delighted to welcome over 500 attendees to our live virtual symposium to mark the 75th Anniversary of the first direct observation of synchrotron light in a laboratory. The event, which was chaired by Sandra Ribeiro, Chair of lightsources.org and Communications Advisor for the Canadian Light Source, was held on the 28th April 2022 and you can watch the recording via the YouTube link below.

We received some lovely feedback after the live event, including this comment from Jeffrey T Collins at the Advanced Photon Source, Argonne National Laboratory in Illinois.

 “I have worked at the Advanced Photon Source for over 32 years and I learned many things during this event that I never knew before.  It was quite informative.  I look forward to re-watching the entire event.”

Jeffrey T Collins, Mechanical Engineering & Design Group Leader at Argonne National Laboratory

The symposium began with a historical introduction from Roland Pease, freelance science broadcaster who has been an enthusiastic support of light sources for many years.

Roland’s talk was followed by experts from the field giving talks on their perspectives of synchrotron light related achievements that have been made since the 1st laboratory observation on the 24th April 1947.

Speakers were:

• Nobel Laureate Prof. Ada Yonath (Weizmann Institute of Science)

• Prof. Sir Richard Catlow (University College London)

• Prof. Henry Chapman (DESY)

• Dr Paul Tafforeau (ESRF)

• Dr Gihan Kamel (SESAME and member of the AfLS Executive Committee).

There followed a panel discussion with special guests who all made huge contributions to the development of the field. Our special guests were:

Herman Winick – Prof. of Applied Physics (Research) Emeritus at SLAC)

Ian Munro – Initiator of synchrotron radiation research at Daresbury Laboratory ,Warrington UK in 1970

Giorgio Margaritondo – one of the pioneers in the use of synchrotron radiation and free electron lasers

Gerd Materlik – former CEO of Diamond Light Source, the UK’s synchrotron science facility

Lightsources.org is hugely grateful to all the speakers, special guests and attendees who contributed to this event and made it such a special anniversary celebration for the light source community.

If you have any feedback or memories to share, please do contact Silvana Westbury, Project Manager, at webmaster@lightsources.org

For news, jobs, events and proposal deadlines, please visit the homepage

Science’s great strength is the universal language

SSRL’s #LightSourceSelfie

Forrest Hyler is a PhD student at the University of California Davis and regular user of the Stanford Synchrotron Lightsource (SSRL). Forrest’s research involves exploring the structural and electronic properties of materials that are used as catalysts for carbon dioxide reduction in the lab. In his #LightSourceSelfie, Forrest describes his work as all encompassing as it involves studying materials related to a broad range of applications such as batteries, catalysis and the storage of radioactive materials. Forrest’s journey has involved a large range of scientists and he says, “The greatest part about science is that it’s kind of that universal language. You get to interact with people around the globe working together for a common goal to push science beyond the boundaries that we’ve ever been at before.”

Developing new alloys for hydrogen fuel and catalysis

An alloy is a metal that contains two or three different elements. Steel, for instance, is an alloy of iron and carbon that offers increased strength as a building material.

By mixing more elements together, scientists hope to create new and improved alloys with increased strength and improved corrosion resistance, which could help many industry sectors to reduce costs.

“The trouble is that when you try to make a traditional alloy with more than a couple of elements, the elements tend to separate from each other and clump together,” said David Morris, a PhD student in the Department of Chemistry at the Dalhousie University.

That’s why his research team is interested in alloys with five or more elements that have a highly disordered nature. This chaotic property causes the elements to disperse throughout the mixture and prevent clumping. “You can get alloys with elements that wouldn’t usually go together,” he said.

Morris and his colleagues, including Liangbing Hu’s group from the University of Maryland who synthesized the samples using a special carbothermal shock method, are investigating two alloy samples, one made of five elements and another with fifteen.

“Early experiments suggested that the five-element alloy has high catalytic activity for ammonia decomposition, a process used to make hydrogen fuel, but they potentially have all kinds of applications,” he said.

The team gathered data at the Advanced Photon Source (APS) in Illinois, thanks to the facility’s partnership with the Canadian Light Source (CLS) at the University of Saskatchewan. Using synchrotron light, Morris could analyze each element in their samples separately and spot the differences in the structures of the two alloys.

The researchers discovered that the fifteen-element alloy had some elements that showed oxidation and the length of some of the bonds between them increased. These properties, however, were not found in the five-element alloy, indicating the properties of these special alloys are highly dependent on their compositions.

“Increased oxidation means they are less stable, which could potentially increase the activity for catalysis,” said Morris. “And unusual bond lengths can change the properties and maybe make a more promising catalytic pathway.”

The group’s next step will be to try and link the changes in structure seen in this experiment to the alloys’ catalytic activity. “If we are able to find certain structural properties that are associated with a high catalytic activity, that would allow us to design more effective catalysts in the future,” said Morris.

Read more on the CLS website

Image: APS

Transition-metal dichalcogenide NiTe2: an ambient-stable material for catalysis and nanoelectronics

Recently, transition-metal dichalcogenides hosting topological states have attracted considerable attention for their potential implications for catalysis and nanoelectronics. The investigation of their chemical reactivity and ambient stability of these materials is crucial in order to assess the suitability of technology transfer. With this aim, an international team of researchers from Italy, Russia, China, USA, India, and Taiwan has studied physicochemical properties of NiTe2 by means of several experimental techniques and density functional theory. Surface chemical reactivity and ambient stability were followed by x-ray photoemission spectroscopy (XPS) and x-ray absorption spectroscopy (XAS) experiments at the BACH beamline, while the electronic band structure was probed by spin- and angle-resolved photoelectron spectroscopy (spin-ARPES) at the APE-LE beamline

Read more on the Elettra website

Image: a) Ni-3p core-level spectra collected from as-cleaved NiTe2 (black curves) and from the same surface exposed to 2·10L of CO (red curves), H2O (green curves) and O2 (blue curves).  Credit: Adapted from “S. Nappini et al., Adv. Funct. Mater. 30, 2000915 (2020); DOI: 10.1002/adfm.202000915” with permission from Wiley (Copyright 2020) with license 4873681106527