The application of in situ and operando methods in catalysis – opportunities for UK-Africa collaboration through START

“When I saw the opportunity to be a part of a GCRF START team in the UK, I was very motivated to join the group. My aim is to make connections with people and be the link between researchers in Africa and groups in the UK which brings benefit to both. START has made my dream real; it has enabled something one can’t do by oneself because you need a team, and you need funding. There is no other better way to do our research than through the START collaboration.”

Dr Khaled Mohammed, University of Southampton, UK

Our team at the University of Southampton (UK) is focussed on the application of in situ and operando methods to all aspects of catalysis; this covers all areas of a catalyst’s “life-cycle” – from formation and operational behaviour, to eventually understanding what causes it to lose performance. A catalyst is a chemical substance widely used in large-scale chemical industry to enhance reactivity and selectivity towards target products of the reaction of interest without itself being consumed in the reaction.

However, the complex nature of such material requires an advanced tool to understand its behaviour under operating conditions fundamental to the chemical industry and in the drive to increase sustainability for the future of our planet. Extensive knowledge and experience in using synchrotron radiation sources is therefore vital to understand the complex nature of catalysts and to develop new technologies here in the UK and globally. Through the START collaboration, our knowledge and hands-on-experience in this area is shared with our African partners as they develop their own catalysis and synchrotron research programmes.

My name is Khaled Mohammed, and I am a Postdoctoral Research Fellow (PDRF) in Synchrotron Methods for Catalysis within Chemistry at the University of Southampton. Funded by the GCRF START grant, I joined START in October 2019 to work with Dr Peter Wells’ team – Peter is a GCRF START Co-Investigator (Co-I) and an Associate Professor within Chemistry at Southampton, holding a joint appointment with the UK’s national synchrotron, Diamond Light Source (Diamond). I joined the START project only a matter of months before the global COVID-19 pandemic and research has been challenging in this period. Despite this, I have contributed to several published studies[1] as a GCRF START PDRF.

Here I explain my perspectives on what START means as an African researcher in the UK.  My role involves contributing to British and international research, and I see myself as an ‘ambassador’ for my country (Egypt), making connections to people and being a link between researchers in the UK and those in other African countries.

GCRF START Postdoctoral Research Fellow, Dr Khaled Mohamed, preparing a wide range of materials including supported metal/metal oxides, and tailored porous framework architectures with well isolated active sites for directed catalysis at the University of Southampton. Photo credit: Khaled Mohammed. ©Diamond Light Source

Joining the START network at the University of Southampton, UK

My experience using such facilities, with particular emphasis on operando and time-resolved X-ray absorption fine structure spectroscopy (XAFS), dates back to my PhD studies at the University of Southampton (2010 – 2014) and my previous role as a Research Associate at University College London (2013 – 2015), where our group had the opportunity to use the facilities at the Research Complex at Harwell and the Beamline Allocated Group (BAG) at Diamond. In November 2015, I decided to go back to my home country, Egypt, to start a new academic role at Sohag University as a Lecturer in chemistry. I was very keen and motivated about the role with its many teaching activities. A few months later, however, I realised that my scientific research was limited in this role by the fact that there was no access to a synchrotron, which does not exist on the African continent.

On the bright side, however, I had the opportunity to speak with my colleagues in Egypt who have no experience in using such synchrotron tools and I could share with them the knowledge I had gained in the UK.  In addition, I could give lectures and seminars on the key questions about synchrotrons to the next generation of scientists: How does a synchrotron work?  What type of experiments do we do with synchrotrons? Which beamlines are available to use to support our research?

My colleagues in Egypt were excited about this subject, but it was also a challenge as the facilities are good but not good enough to do the level of advanced experiments / topics that one can do with synchrotrons. People are very motivated to do these advanced topics, such as characterisation of materials for catalysts and applications, but the problem is we do not have the funding or access to these kinds of experiments. Therefore, when I saw the opportunity to be a part of a START team, I was very motivated to join the group at Southampton.

GCRF START Postdoctoral Research Fellow, Dr Khaled Mohammed and GCRF START CO-I, Dr Peter Wells at the University of Southampton, UK. Photo Credit: Khaled Mohammed. ©Diamond Light Source

Catalysts and synchrotrons for renewable energy – the hydrogenation of furfural for biofuels

I was born in Sohag city, Egypt, where I lived for most of my childhood. I loved studying science at school, especially the physical sciences, and I dreamt about becoming a scientist to help provide power for the city where I lived – at that time access to electricity was very intermittent.  Outside the city, I wanted to help people who lived in the countryside where, at that time, there was no electricity at all. Later, my dreams shifted to chemistry and I was motivated and inspired to develop pharmaceuticals. I had seen my grandfather suffering with illness and die prematurely due to lack of available medicines.

Today, I find myself inspired by these experiences working in catalysis with applications in renewable energy where waste biomass is converted to liquid biofuels (Bioenergy), or waste CO2 is converted to high value chemicals that can be used in our daily life, or as an alternative to fossil fuels. These applications rely on catalysts but to make this process more sustainable and efficient, advanced techniques are required to understand how the catalysts work under operating conditions. It is a big challenge for African researchers to access the facilities and techniques needed for this type of work. Like my dreams when I was younger, I take great pride in trying to provide something useful to society. What I love about START is that it brings these dreams to reality.

A good example of the kind of research I have collaborated on is the hydrogenation of furfural. Furfural is a bio-derived molecule and can be converted to many useful products, including the generation of liquid fuels; it is therefore a renewable energy feedstock. However, bio-derived compounds are highly functionalised, this means they have many parts of the molecular structure that can undergo chemical change. Palladium (Pd) nanoparticles are widely used as an active component in furfural hydrogenation – a specific type of reaction that involves the addition of hydrogen to a compound – however, selectivity to specific products is a big challenge. In addition, Pd is a very scarce element and there are significant concerns about the sustainability of using such elements, both from an economic perspective and the environmental impact of mining such rare materials.

In our recent paper, [ACS Catal. 2020, 10(10), 5483–5492 (], we demonstrated that a Pd/NiO catalyst can hydrogenate furfural using a dual site process; the Pd splits the H2 molecule into adsorbed hydrogen atoms onto the Pd surface, the adsorbed hydrogen then migrates onto the NiO surface where the furfural molecule is selectively transformed. For materials like this, we need to use advanced tools at Diamond Light Source, e.g. X-ray absorption spectroscopy, to understand more about our materials and their unique properties that allow them to function as catalysts.

GCRF START Postdoctoral Research Fellow, Dr Khaled Mohammed, at the University of Southampton, UK. Photo Credit: Khaled Mohammed ©Diamond Light Source

In the shadow of the Covid-19 pandemic – facilitating UK-African research through cross-disciplinary teamwork

“START has and continues to be a fantastic opportunity for the UK to work in concert with our African partners. Our futures are intertwined; we share the same global challenge of treading more lightly on our planet, be it to mitigate climate change or to preserve our natural world, whilst simultaneously sustaining our growing populations. New functional materials are needed to underpin the emerging sustainable technologies that allow us to tackle these challenges and START is an important gateway for sharing the tools and expertise to accelerate these advances.”

Dr Peter Wells, University of Southampton, UK

During the pandemic, the GCRF START grant has enabled us to stay productive and self-motivated, for which we are truly grateful. Although access to laboratory and synchrotron facilities has been limited, we have been able to continue our work remotely. We set goals including research activities, data reduction/analysis and submitting new beamline proposals. In addition, we participated in many on-line activities including workshops, seminars, and social activities with all participants in START.  

The environment in the group here at Southampton has been excellent. There are things you can’t just learn by talking; we have learnt by doing research-based experiments together. Peter has taught me a lot. If I do an experiment, I give the idea to Peter, and then we do some tests to validate which beamline to use and what we need to adjust and optimise before we go ahead.

When I was in Egypt – before I got involved in START – I tried to do collaborations with people here in the UK.  I could do the basics and prepare materials, but I couldn’t correlate the structure-performance relationship without beamtime experiments. Being here in the UK, interacting with experienced scientists, has enabled me to see what is new and to push things forward through START, sharing what I learn with my African colleagues.

A great achievement has been international collaborations across a range of disciplines. After joining START in 2019, I found the group already working with Professor Michael Claeys’ Group at the University of Cape Town (UCT) in South Africa. I soon got involved in this project working with Dr Mohamed Fadlalla and Chris Mullins on research using the B18 beamline at Diamond to assess, in situ, the effect of substituents in ferrite structure with the general formula of AB2O4. These are used in a wide range of catalytic reactions including the Haber-Bosch process, water-gas shift reaction, dehydrogenation of ethylbenzene, and Fischer-Tropsch synthesis (FTS) to produce liquid hydrocarbons/fuels.

I was able to assist Mohamed with his experiment in December 2020. We had to submit a proposal and get it accepted (to do this you have to submit initial results like a proof of concept). Once accepted, the experiment had to be done in a specific time frame. But before Mohamed came over to the UK to conduct the experiment, tests had to be carried out for optimisation of the materials. This takes time so I did this first to ensure the experiment ran smoothly when he arrived.  

There are lots of other things that must be organised and managed before experiments like these, therefore my role has been to optimise as much as possible to increase the chance of success. Since then, we have assisted Mohamed and his colleagues in data analysis for publication. This successful beamtime experiment motivated us to explore new ideas, for example, in making catalysts with well-isolated active sites – mainly cobalt in tetrahedron sites to be used in preferential oxidation of carbon monoxide.

GCRF START Co-I, Professor Michael Claeys (L) and Research Officer, Dr Mohamed Fadlalla (R), at the University of Cape Town’s Centre for Catalysis, South Africa. Photo credit: Rebekka Stredwick. ©Diamond Light Source.

The future with START – ‘follow on’ opportunities for UK and African energy materials research

“START is a fantastic opportunity for the UK to work in concert with our African partners to tackle shared challenges. It is clear that the excitement generated can be inspirational and helps to further integrate research partnerships.”  – Dr Peter Wells, University of Southampton, UK

We are discussing our new research ideas going forward with Mohamed and another colleague of his, GCRF START Postdoc – Dr Thulani Nyathi – and have set goals and tasks for two ‘follow-on’ projects currently in the pipeline. As a result, I am in the process of sending some samples to Mohamed and Thulani for the preferential oxidation of carbon monoxide. This research has the dual benefit of reducing the harmful effects of carbon monoxide and using the carbon monoxide captured to make useful chemicals for energy, such as fuel cell storage to power vehicles and other devices.

We are also very impressed with the facilities and equipment at UCT, some of which we don’t have here in the UK, and which could be beneficial to access in the future. On a practical level, routine visits are important for hands-on experience (sadly due to the Covid-19 pandemic my visit to UCT in 2020 was cancelled), therefore continuing remote options in the meantime is vital for sharing ideas.

GCRF START Postdoctoral Research Fellow, Dr Khaled Mohammed, next to the vertical stainless-steel temperature-programmed reactor at the University of Southampton (UK) with temperature-programmed controller for conducting solid-gas phase catalytic reactions under different conditions up to 1500C. Photo Credit: Khaled Mohammed ©Diamond Light Source

Perspectives from our collaborators in South Africa on the impact of START

Here I want to share testimonials from Dr Thulani Nyathi and Dr Mohamed Fadlalla demonstrating their perspectives on our UK-Africa collaborations.

Thulani said,

“I first worked with Dr Peter Wells’ group prior to the GCRF START programme through a collaboration also involving the UK Catalysis Hub (located on the Harwell Science and Innovation Campus in Oxfordshire) and with Dr Emma Gibson’s group in Chemistry at the University of Glasgow, funded by the EPSRC (grant EP/R026815/1). This included my first visit to a synchrotron facility – Diamond Light Source – and my first exposure to two in situ techniques, XAS and DRIFTS, which were used to study supported cobalt oxide catalysts for the preferential oxidation of carbon monoxide (CO-PrOx).

This collaboration proved to be highly successful as it was concluded with a very good publication[2] in ACS Catalysis in 2019. Through the GCRF START programme (grant ST/R002754/1), I have continued to work with Peter’s group and Emma’s group, using the Block Allocation Group sessions administered by the UK Catalysis Hub, to analyse fresh and spent catalysts for the CO-PrOx reaction. I was then able to conclude my PhD thesis in September 2020 and publish a second paper in Applied Catalysis B: Environmental in June 2021[3].

There exists on-going work between the Southampton and UCT groups where we try to study substituted iron oxide and alloy catalysts for use in the hydrogenation of carbon dioxide (a greenhouse gas) to value-added chemicals. This work has already involved a trip to Diamond in 2019 and the results obtained will feature in a paper we aim to publish later in 2021. I hope to make more trips to Diamond and to continue working with the Southampton and Glasgow groups in the upcoming years.”

GCRF START Postdoctoral Research Fellow, Dr Thulani Nyathi from the University of Cape Town’s Centre for Catalysis, South Africa. Photo Credit: Linda Vos. ©

Mohamed said,

“The highly seamless collaboration with Dr Peter Wells and Dr Khaled Mohammed from the University of Southampton has led to a more profound collective understanding of the catalytic materials under activation and under working conditions using in situ and ex situ synchrotron-based techniques. Owing to the successful and harmonious collaboration between the two research groups thus far, further partnership is in the works to investigate catalyst structure/activity/selectivity correlations in the energy material field.”

Dr Mohamed Fadlalla at the University of Cape Town’s Centre for Catalysis in South Africa conducting analysis of the CO2 hydrogenation over iron-based alloys via two-dimensional gas chromatography x gas chromatography (2D GC x GC). Photo credit: Rebekka Stredwick © Diamond Light Source

START’s achievements and the future – “a great work for great value”

When I look back at what has been achieved and then look forward to the future, I ask myself the question: If there wasn’t a START network/project, how would people who don’t know about synchrotron techniques know about these opportunities? START not only transfers knowledge and enhances capacity, but it also builds awareness a bit like an advertisement. It helps us know where and how to apply to synchrotrons like Diamond for beamtime and shows us what is possible and how to do the experiments in the right way. And synchrotron techniques give unprecedented insights essential for our research. If there hadn’t been a GCRF START grant to fund these possibilities, it would have delayed our research because collaborations like START boost and speed up the process and findings.

In Africa we need the fundamental facilities to train the next generation ready to use synchrotrons. More locally, in Egypt, we need capacity-building facilities to do initial experiments and fundamental research. For example, a catalytic reactor would be very useful for scientists to do some reactions. We can do the preparation – we can buy the chemicals – but to do the catalytic reactions we need a reactor where we can do the experiments in optimised conditions.

We also need a ‘Centre for Catalysis’ in Egypt where we can teach the new generation to develop sufficient skills to collaborate with the UK and other countries for advanced experiments and push the research forward. If research hubs could be set up across Africa, like the Catalysis labs at UCT, this would be fantastic and START could be an ideal vehicle to make this happen. Another route is through funding agencies like the British Council/Newton Funding which provide travel grants and other support for researchers in developing countries. 

To summarise the achievements of the GCRF START grant and what START means to me: I would describe it as “a great work for great value”, and all this despite massive setbacks caused by the Covid-19 pandemic.

START does great work that allows scientists from developing countries to gain knowledge and experience from leading scientists in the UK and to reciprocate, as my role shows. It does great work because it offers opportunities for us to work with scientists from all over the world on a level playing field. Ultimately, the greatest value from my perspective is that we work hard to provide (in a sustainable way) energy/electricity, medicines and many other applications for people who don’t have these fundamental things, enabling a better life for the future – what value is bigger or better than this?

Read more about the UN’s Sustainable Development Goals here

GCRF START Postdoctoral Research Fellow, Dr Khaled Mohammed, engaged in quantification and identification of reaction products using the GC (FID & TCD detectors) equipment at the University of Southampton, UK. Photo credit: Khaled Mohammed. ©Diamond Light Source

[1] [1] ACS Catal. 2020, 10(10), 5483–5492 ( – This work has significant implications for the upgrading of bioderived feedstocks, suggesting alternative ways for promoting selective transformations and reducing the reliance on precious metals. [2] Phys. Chem. Chem. Phys., 2020,22, 18774-18787 (!divAbstract) – This study demonstrates the complexity of mechanochemically prepared materials and through careful choice of characterisation methods how their properties can be understood. Synchrotron techniques, such as X-ray absorption spectroscopy (XAS), have multiple benefits, which aid the in-depth understanding of chemically important yet complex systems. [3] Nanoscale Adv., 2019,1, 2546-2552 (!divAbstract) –  Using state-of-the-art beamlines, this study demonstrates how X-ray absorption fine structure (XAFS) techniques are now able to provide accurate structural information on nano-sized colloidal Au solutions at μM concentrations. 

[2] ACS Catal. 2019, 9, 8, 7166–7178, Publication Date: June 28, 2019 Copyright © 2019 American Chemical Society

[3]  Author: Thulani M. Nyathi, Mohamed I. Fadlalla, Nico Fischer, Andrew P.E. York, Ezra J. Olivier, Emma K. Gibson, Peter P. Wells, Michael Claeys. Publication: Applied Catalysis B: Environmental. Publisher: Elsevier. Date: 15 November 2021.