Nano-focused X-rays aid integrated circuit development

A modern chip contains billions of transistors. The size of individual features is just a couple of tens of nanometres. With decreasing size follows increased demands on material control and characterisation down to the atomic scale. The nano-focused X-ray beam at beamline NanoMAX prove to be a useful tool for investigating electromigration, a significant cause of failure in on-chip interconnects.

Electromigration and failure
Copper is the most commonly used material for connecting transistors on a chip. The current being pushed through the tiny copper wires cause a phenomenon called electromigration. Electromigration is a form of mass transport driven by the flow of electrons, where atoms migrate from one end of the copper structure to the other, changing the structure and leading to short circuits or disconnects. When the wire gets smaller it means that a higher current will be pushed through and the resulting electromigration can cause failure in the circuit.

“Electromigration is one of the biggest reliability issues in integrated circuits and although it has been widely studied the interplay between the different forces that drive or counteract electromigration is not completely understood,” says Professor Sten Vollebregt from Delft University of Technology.

Nano focus reveals structural details
Copper structures of different lengths and thicknesses were fabricated on top of a substrate, a piece of silicon prepared with layers of silicon dioxide and titanium nitride, to simulate the situation on the chip. The structures were heated and had current run through them to induce electromigration.

After the preparation, the samples were investigated at the NanoMAX beamline using a beam focused into a 62 nanometre diameter spot. The experiment gives information about the distance between the atoms in the copper, which in turn reveals stresses in the material.

“We found two different stages, where the stress is initially controlled by the difference in thermal expansion between the silicon substrate and the copper line structure, but later the stresses developing during electromigration become dominant. A better understanding of the stress within the interconnect during electromigration will allow the development of improved models, resulting in better prediction of the reliability. This will ultimately help manufacturers design more reliable and perhaps even smaller chips,” says Magnus Colliander from Chalmers University of Technology.

Read more on MAXIV website

MAX IV: Record year for research

MAX IV is making significant societal contributions in terms of record-high scientific productivity. In 2023, the number of publications increased by 51% compared to the previous year, and the number of unique users increased by 31%. Moreover, the number of proposals submitted in the most recent Open Call was higher than ever.

The data from 2023 indicates a rapidly growing interest to conduct research at MAX IV.

The latest Open Call, which closed in March 2024, received an all-time high of 459 proposals from national and international researchers who applied to use MAX IV this autumn.

The total number of proposals submitted in the 2023 Open Calls (717) was 14% higher than in 2022. 

These statistics are published in the MAX IV Annual Report 2023, which is now released.

Read more on the MAX IV website

Image: The main MAX IV building

Credit: Johan Persson

Conversion of carbon dioxide into raw materials more effective with gold

Carbon dioxide, emitted mainly by combustion of fossil fuels, is harmful to the climate and the main reason for increased global warming. Diverting carbon dioxide into hydrogen carriers or chemicals such as methanol, a valuable raw material and energy carrier, is thus highly desired. Supported metal nanoparticle heterogeneous catalysts such as copper on zinc oxide is used for the catalytic conversion of carbon dioxide to methanol. Researchers have now discovered that it is possible to avoid by-products and at the same time make the process more sustainable by adding a small amount of gold to the catalyst.

Carbon dioxide can be converted into methanol and water by reaction with hydrogen. The reaction is only possible in the presence of a catalytic material such as Au or Cu nanoparticles supported on zinc oxide. The chemical reaction will then take place on the particle surfaces. In a recent study, a research team from Germany, Japan and Sweden have shown that modifying the typical ZnO-supported Cu nanoparticles by a small amount of gold (< 10 weight percent) makes the reaction more selective.

Read more on MAX IV website

Towards prevention of diabetes linked substance produced by human gut microbiota 

The team at the Novo Nordisk Foundation funded life science beamline MicroMAX welcomed the first users in December 2023. In the experiment the users investigated an enzyme that may be found in some bacteria of human gut microbiota and may have a role in the development of diabetes and other diseases.

An enzyme called urocanate reductase may be present in the bacteria that are found in the human gut. The enzyme breaks down urocanic acid, a natural constituent of skin and other tissues of the body, into the metabolite imidazole propionate. The metabolite has been linked to diabetes and other diseases.

The user team from Lund University used MicroMAX to investigate the molecular structure of the enzyme.

“A possible therapeutic strategy is to inhibit the enzyme and prevent the imidazole propionate production. The high-resolution atomic structure is needed to design inhibitor molecules that could occupy the active site of the enzyme,” says Raminta Venskutonyte, one of the researchers who conducted the study.

The experiment was conducted using X-ray diffraction at room temperature on a crystal prepared from a purified enzyme. One of the features of MicroMAX is that the experimental setup can handle even small amounts of samples, so-called microcrystals. It is important as it lets the researchers study samples that cannot be made to form large crystals and extend investigations into new areas.

“We aim to carry out time-resolved studies using microcrystals of urocanate reductase to further clarify its enzymatic mechanism. We are also looking forward to using MicroMAX in other projects involving medically interesting proteins, which only yield microcrystals,” concludes Raminta Venskutonyte.

Read more om the MAX IV website

Image: Raminta Venskutonyte in the experiment hutch at beamline MicroMAX

Combination of techniques for effective pharmaceutical formulation

The environment in your gastrointestinal tract affects the properties and effectiveness of medicines. Researchers have used MAX IV to investigate a technique for studying these changes. They found that the structural properties of the anti-inflammatory drug Indomethacin changed in the presence of common biomolecules.

The fluid in your gastrointestinal tract is a complex soup of biomolecules. When you take a pharmaceutical drug, the biomolecules may stick to its surface and alter how it’s dissolved and taken up by the body at a certain pH. Such effects need to be understood and taken into account when producing pharmaceuticals. But it’s not always easy to investigate. In the present paper, the authors tested the accessible technique of Low-Frequency Raman spectroscopy, in which inelastic scattered light is used to analyse the sample. They then controlled the accuracy using X-ray methods.

Read more on MAX IV website

In memory of professor Per-Olof Nilsson

Professor Per-Olof Nilsson, a colleague and friend to us at MAX IV, passed away at age 84. As a PhD and later professor at Chalmers with a great interest in synchrotron-based research, Per-Olof Nilsson played a major role as initiator and facilitator of MAX-lab, which became MAX IV, as a national facility. He sent in the first application for a synchrotron radiation facility, together with former synchrotron radiation research coordinator and subsequently University Chancellor Anders Flodström in 1978, and the application for funding the first beamline. Per-Olof Nilsson founded the users association, FASM and organised the first MAX-lab summer schools to enhance students’ knowledge of science with synchrotrons. He worked until his demise as a professor emeritus at Chalmers, where he, among other assignments, had a great engagement in science outreach and established a workshop with over 300 teaching experiments.

“P.O. was a leading researcher in a generation of scientists who deepened the understanding of the new materials that form the basis of our development towards a better and sustainable society. As a pioneer, P.O. understood the opportunities offered by accelerator research in Lund. Many heroes have worked along the journey towards MAX IV. Still, the pioneer was P.O. We, and future synchrotron light researchers will always remember P.O. for his sharp intellect, empathy, and understanding of the role of research in a constantly changing world,” says prof. Anders Flodström.

Read more on MAX IV website

Image: P.O. Nilsson

Credit: J-O Yxell, Chalmers

Olof Karis becomes Director for MAX IV

Olof Karis, former Interim Director of MAX IV, has been appointed as the Director of MAX IV following an open recruitment process and the recommendation of the MAX IV Board. The decision was made by the Vice-Chancellor of Lund University, the host university for MAX IV.

MAX IV, Sweden’s synchrotron, is fully operational with 16 beamlines and 1400 users yearly from academia and industry. Olof Karis has led MAX IV as Interim Director since March 2022, through finishing the Strategic Plan for 2023–2032 and a positive review by the Swedish Research Council in November. He has also navigated challenges related to increasing operating costs.

“I am enthusiastic about the possibility of continuing to work for MAX IV. It is a fantastic facility with great people. My focus for the near future is to make a case for longer-term funding of MAX IV. We need stability to continue facilitating research that keeps our society strong in facing future challenges,” says Karis.

In collaboration with the scientific community, MAX IV aims to continuously develop existing beamlines and construct several complementary ones in the next decade to make optimal use of already-made investments in the infrastructure.

“The research conducted by our users at MAX IV benefits the community in many areas, with an impact on circular economy and environment, sustainable energy, and health. Our technical advancements with the MAX IV synchrotron are transformative, enabling us to see details we’ve never been able to before. We can approach what has previously been unsolvable problems,” concludes Karis.

Read more on the MAX IV website

MAX IV research contributes to the development of new cancer drugs

In the battle against cancer, scientists from the drug discovery company Sprint Bioscience and researchers from MAX IV have taken important steps together toward developing new and more efficient cancer drugs with the help of fragment screening by X-ray crystallography.

Cancer accounts for nearly one out of six deaths yearly. It begins when one or more genes in a cell mutate, creating an abnormal protein or preventing a protein’s formation.

Therefore, you need to start at the protein level to fight cancer.

Sprint Bioscience is working to develop new drug candidates by identifying small molecules (fragments) that can bind targeted cancer proteins. In collaboration with researchers from the FragMAX team at MAX IV during 2019 and 2020, Sprint Bioscience optimised and developed a protein crystallisation system corresponding to a cancer protein chosen by the company.

Read more on MAX IV website

Image: Crystal incubated with fragment XB00143 mounted on the BioMAX beamline during the screening campaign.

Credit: Sprint Bioscience/BioMAX

Real-time observation of hydrocarbon polymerization

The polymerization of hydrocarbons into linear chains lies at the heart of many industrially relevant chemical reactions. One prominent example is the alkene polymerization with the Ziegler Natta catalysts, which is responsible for 2/3 of the global production of polyolefins. Long-chain hydrocarbons can also be produced from syngas (a mixture of carbon monoxide and hydrogen) through the so-called Fischer-Tropsch synthesis (FTS), occurring typically on cobalt-based catalysts. This process is experiencing a renewed interest, especially in the context of modern power-to-gas and power-to-liquid plants.

From a microscopic point of view, the identification of the complex series of reaction steps involved in the polymerization of small molecules into long hydrocarbon chains is still under debate. Surface-science techniques have proved to be extremely powerful to explore the mechanisms of heterogeneous catalysis. However, due to the harsh reaction conditions of FTS, analysis using such techniques poses a real experimental challenge.

Though the step sites of the catalytic surface are also commonly assumed to promote the C-C coupling of CHx monomers, the typical strong adsorption of small molecules at the step edges could trap the CHx species, hindering the polymerization. This behavior can be understood in the framework of the Sabatier’s principle, stating that if the adsorption energy of the substrate is too low, then the catalytic activity is suppressed; if it is too large, then the product will not desorb and blocks the surface, leading to catalyst poisoning. Therefore, elucidating the actual role of the step sites is crucial for an in-depth atomistic understanding of the hydrocarbon chain growth process.

Here we investigated the formation of hydrocarbon chains resulting from acetylene polymerization on a Ni(111) model catalyst surface. Exploiting X-ray photoelectron spectroscopy (XPS) performed at the SuperESCA beamline of Elettra, the intermediate species and reaction products have been directly identified. This has been enabled by the high energy resolution (about 100 meV) of the instrument, allowing resolving vibrational fine structures.

Read more on the Elettra website

Tetra Pak commences first-of-its-kind sustainability research

The newest research station at MAX IV, ForMAX, has hosted its first industry experiment: A ground-breaking study on fibre-based sustainable food packaging, performed by Tetra Pak in collaboration with Chalmers University of Technology.

Today, global food packaging and processing company Tetra Pak announces the commencement of new research using advanced X-ray scattering imaging techniques at ForMAX, the newest beamline at MAX IV laboratory. The study aims to uncover fresh insights into the nanostructure of fibre materials, with the first application to optimise the composition of materials used for paper straws.

In the strive to meet the increased global market demand for more sustainable packaging solutions, new materials based on paper can bring novel opportunities. Yet, these new, paper-based materials must remain food safe, recyclable, and durable against liquids and humidity while meeting the increased sustainability demands.

These are some of the challenges that Tetra Pak is collaborating with MAX IV to address using the laboratory’s advanced research techniques.

“Our first experiment, which starts with paper straws, provides additional analysis capabilities into how paper straw material responds to changes in the environment in real-time, as well as how the straw interacts with different types of liquids under stringent conditions. These new insights and knowledge will be applied to developing the paper straws of the future in our virtual modelling tools, helping us to improve their functionality”, explains Eskil Andreasson, Technology Specialist, Virtual Modelling at Tetra Pak.

Read more on the MAX IV website

Image: Eskil Andreasson (middle), Technology Specialist at Tetra Pak, with the research team listening to Linnéa Björn in the ForMAX control room at MAX IV.

Credit: Anna Sandahl, MAX IV

MAX IV and nine Swedish universities launch joint effort to educate young scientists

PRISMAS, Ph.D. Research and Innovation in Synchrotron Methods and Applications in Sweden is launched. The programme includes hands-on training in cutting-edge synchrotron skills that is applicable in various research areas at MAX IV in Lund, Sweden. It combines practical experience with courses covering all aspects of synchrotron radiation to produce researchers who are experts in these methods and their fields. 

Students from diverse scientific backgrounds will be recruited through partner universities to learn to use and develop synchrotron methods in their research while acquiring the skills to tackle some of the most critical sustainability development goals and future societal challenges in their projects led by selected Principal Investigators from around Sweden. This 5-year intersectoral and interdisciplinary project will create a connected network of next generation X-ray experts, enabling a wider range of stakeholders to take full advantage of world-leading synchrotron facilities such as MAX IV, while tackling current societal challenges in the same breath.

Read more on the MAX IV website

A toothy temporal map of Arctic climate change

In the vast, remoteness of the Arctic, few have the opportunity to gather data on the environmental conditions over time or decipher the long-term effects of climate change. What is required? A considerable period to observe, a nearly autonomous method or actor for collection, a robust character to withstand the harsh surroundings. Researchers from Aarhus University in Denmark are tackling this issue through an interdisciplinary NordForsk project. At DanMAX beamline, the group will analyse a narwhal tusk to determine its chemical composition and biomineralization, both important potential markers of the changing environment.

Significant, accelerated signs of climate change have been reported in the Arctic and Antarctic zones, which research shows impact global climate. Scientists are looking at different ways to interpret the terrestrial and oceanic changes occurring in these areas, and how the change affects native wildlife. The described NordForsk project, developed by researchers from Denmark, Greenland and Sweden, seeks to elucidate the structure and formation of the narwhal tusk, and map the full life history of the animal through the growth lines along the full length of the tusk.

Read more on the MAX IV website

Image: Peter A. S. Vibe readies samples of the tusk at DanMAX beamline. 

Credit: MAX IV Laboratory

ForMAX beamline is now open for experiments

ForMAX, the newest beamline at MAX IV, is now officially open for experiments. The focus will be research on new, sustainable materials from the forest, but the beamline will also be useful for research in many other fields and industries, including food, textiles, and life science.

ForMAX is specially designed for advanced studies on wood-based materials. It allows in-situ multiscale structural characterization from nm to mm length scales by combining full-field tomographic imaging, small- and wide-angle X-ray scattering (SWAXS), and scanning SWAXS imaging – in a single instrument.

The beamline is an initiative where several market-leading industry companies, mainly from the paper and pulp industry, and academia have joined forces. The construction work has been funded by the Knut and Alice Wallenberg Foundation, and the operational costs are funded by the industry through Treesearch, a national collaborative platform for academic and industrial research in new materials from the forest.

One goal with ForMAX is to facilitate the development of new, wood-based products that can replace today’s plastic products.

Read more on the MAX IV website

Image: ForMAX beamline

Credit: Anna Sandahl, MAX IV

Creating tastier vegan cheese using synchrotron X-rays

The quest for tastier, more sustainable vegan cheese has led Swedish food company Cassius AB to take a closer look at cheese protein structures. Using synchrotron X-rays at MAX IV, Cassius are searching for the perfect scientific recipe for plant-based cheese.

When regular cheese is produced, the milk proteins react with rennet and form a cheese curd. These specific proteins, formed in a certain structure, are unique to mammalian milk, which makes them difficult to mimic. 

Cassius AB:s research project focuses on getting a deeper understanding of how the proteins in regular cheese form structures spontaneously. It also investigates whether this could happen with mammalian milk proteins produced by genetically engineered microorganisms, in a process called precision fermentation.

Since mimicking all proteins in regular cheese is not necessary, Cassius is concentrating on two of the protein types that play a key role in how cheese coagulates.

Cheese gel balls as protein samples

Johan Krakau, founder of Cassius and brands like GoVego, has teamed up with researchers from RISE within the NextBioForm center to perform the experiment at the MAX IV CoSAXS beamline.

Using Small-Angle X-ray Scattering techniques (SAXS), the research team studies different types of protein samples in the form of micelles – spherical protein aggregations that resemble gel balls – and how different conditions affect their shape and size. For example, when mixed with different amounts of salt, or when the pH value is changed. The team also investigates if these proteins coagulate into a curd structure in the same way that mammalian milk proteins do.

Read more on the MAX IV website

Modelling electrochemical potential for better Li-batteries

To understand the electrochemical potential of lithium-ion batteries, it’s important to decipher the chemical processes at electrode interfaces occurring during device activity. Using HIPPIE beamline, a research group investigated and modelled the influence of electrochemical potential differences in operando in these batteries.

“With our experiments at HIPPIE, we had the opportunity to look at battery materials and interface reactions under operating conditions exploring the capabilities of the electrochemical setup at the end station,” said Julia Maibach, study author and professor at the Institute for Applied Materials – Energy Storage Systems at Karlsruhe Institute of Technology (KIT) in Germany. “We were among the first users testing the electrochemical set up including the glove box for inert sample transfer.”

Why study electrochemical potential difference in batteries? This phenomenon drives the transfer of charged particles to different phases in redox reactions at battery electrode-electrolyte interfaces. In simple terms, the difference enables the chemical reaction necessary for Li-ion battery function.

Read more on the MAX IV website

Image: Research group studies gold and copper model electrodes at MAX IV’s HIPPIE beamline with Ambient Pressure Photoelectron Spectroscopy (APPES) during lithiation

Credit: MAX IV Laboratory

#SynchroLightAt75 – The first multi-bend achromat synchrotron light source

At the end of the 1990’s, the MAX-lab management realized that it was necessary to start planning for a possible next step in the development of the laboratory. Although MAX II, one of the first 3rd generation light sources in the world and the flagship of the laboratory, had just recently come into operation, the long lead times made it necessary to start exploring possible further developments already at that stage. This is the saga of MAX IV Laboratory, the world’s first Multi-Bend Achromat (MBA) Synchrotron Radiation Light Source. MBAs strongly focus and guide electrons around the storage ring, creating an ultra-low emittance beam and therefore ultra-bright X-ray radiation.

Read more in this Nuclear Instruments and Methods in Physics Research – section A (NIM-A) publication

Image:  Prof. Ingolf Lindau, Director of MAX-lab 1991–97, shows the facility to the king of Sweden, Carl XVI Gustav, at the inauguration of MAX II, 15 September 1995

Credit:  MAX IV