From left to right: Andreas Körner and Dr. Andreas Hutzler

We are proud to announce that DENSsolutions has installed yet another Stream system in Germany at the esteemed Forschungszentrum Jülich, one of the largest interdisciplinary research centres in Europe. In this article, we interview Dr. Andreas Hutzler, the new head of the TEM lab in the Helmholtz Institute Erlangen-Nürnberg for Renewable Energy (HI ERN) at Forschungszentrum Jülich, to learn more about their advanced microscopy facility, its research direction, as well as how our Stream system is advancing their research.

Can you tell me more about the microscopy facility at HI ERN?

“The Helmholtz Institute Erlangen-Nürnberg for Renewable Energy (HI ERN) is part of the Forschungszentrum Jülich. It specializes in providing crucial research on technologies needed to utilize renewable energies in the decades to come. Our research is centered around fuel cells, electrolyzers and hydrogen storage. The institute was founded in 2013 and has been growing ever since. In 2021, its new research building was inaugurated, hosting the space for a new transmission electron microscope, the Talos F200i from Thermo Fisher Scientific. This tool provides in-house structural analysis on the nanoscale for catalysts, support systems and membranes.”

What type of applications are the users at HI ERN using the Stream system for?

“Our goal is to study electrochemical processes taking place on electrode and catalyst surfaces within electrolyzers and fuel cells down to the atomic scale. We aim to understand which reactions take place, and which conditions enhance the performance of the cells or disintegrate the structures involved.

In order to understand this, we consider beam-induced effects onto the solution chemistry we investigate. For this, we utilize a comprehensive radiolysis model for unraveling the influence of electron irradiation onto the sample and compare the results to non-biased experimental observations. Once this is understood, we continue with analyzing dynamic processes at the nanoscale to gain insights into reaction pathways and degradation mechanisms in P2X and X2P applications.”

What particular features of the DENSsolutions Stream solution attracted you to the system?

“In order to understand observable processes and their correlated chemistry, it is necessary to accurately tune experimental conditions while operating the system. The ability of the Stream system to flexibly adjust pressure, flux, temperature and potential allows to run a manifold of experiments in a wide parameter space. This is needed in order to verify the stability of our reaction kinetic models and for testing electrolysis at borderline conditions. Before, the structures could only be studied after the reaction has taken place. But the ability to directly observe dynamic processes on-site in real time gives valuable insights in the chemistry at hand.”

Can you tell me about the grant that was won to acquire the system?

“One of our key research interests is the development of new methods for characterizing fundamental and applied processes in electrocatalysis relevant to electrochemical energy conversion. After establishing identical-location TEM (IL-TEM) for energy applications and with the start of my team, a new transmission electron microscope as well as equipment needed for in situ liquid-phase TEM was funded by and installed at HI ERN. This particular toolbox will be a great asset for the nanoanalysis of electrochemical processes in my team which will enable unique insights in energy research.”

In your experience so far, how have you found the Stream system?

“The modular architecture of the Stream system enables a very versatile applicability without risking leakage or cross-contaminations. The performance of LP-TEM is considerably enhanced due to the controllability of liquid flow, the ever-present window bulging via the utilization of a novel chip design as well as a differential pumping system as a standard. Moreover, DENSsolutions came forward with providing non-standard solutions in order to provide compatibility with other setups at our institute.”

Dr. Andreas Hutzler is the new head of the Transmission Electron Microscopy lab at HI ERN, PI of multiple projects at HI ERN and university and is currently setting up a team for nanoanalysis of electrochemical processes. His research interests mainly focus on methodological aspects of LP-TEM and its application in electrochemical energy conversion.

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The team at SNU (From left to right) Prof Jungwon Park, Back Kyu Choi, Minyoung Lee and Junyoung Heo.

With the second ever installation of a Stream LPEM Solution in South Korea, we get an insider’s look at the microscopy laboratory at the Seoul National University. We interviewed Prof Jungwon Park from the National Center for Inter-University Research Facilities to find out how our solutions will benefit their research when investigating synthetic mechanisms of inorganic nanocrystals.

Can you tell us a bit about the microscopy facility at Seoul National University SNU?

Seoul National University has a shared research facility called NCIRF (National Center for Inter-University Research Facilities) that has specialities in various fields of analysis, such as organic, inorganic, surface analysis, and x-ray techniques. NCIRF also has a special team in electron microscopy, which provides SEM, TEM, and other pretreatment equipment including FIB and Nanomill.

This shared facility was established around 30 years ago. Recently, two spherical aberration-corrected TEM and STEM, JEM-ARM200F, were installed, providing atomic-resolution electron microscopy images. Also, in our own center, the Institute for Basic Science Center for Nanoparticle Research, we have our own JEOL JEM-2100F TEM in our building which is utilized routinely for a lot of in situ EM studies.

What type of applications are your users interested in with regards to the Stream system installed?

Our users are interested in various nanocrystal dynamics. Regarding the Stream system, we are expecting to investigate the synthetic mechanism of colloidal inorganic nanocrystals by changing the liquid cell temperature and injected precursor solution. Also, we are planning to investigate transformation phenomena of colloidal nanocrystals in various liquid environments. Moreover, we are expecting to observe polymers or proteins in liquid, and their stimuli-responsive reactions using the Stream system.

What particular features of the DENSsolutions Stream solution attracted you to the system?

When it comes to liquid cell TEM experiments, it is crucial to ensure that a controlled amount of liquid is injected to the desired position, while minimizing the decrease in spatial resolution of TEM stemming from the window bulging effect. In this sense, the Stream system by DENSsolutions was quite attractive to us.
With ensured liquid flow from Nano-cell design, controlled injection of liquid, as well as mitigated window- bulging originating from the pressure-based liquid pump, and also along with the liquid heating control system, the Stream solution seemed to help us to design various in situ liquid cell systems which were unachievable with other in situ holders.

In your experience so far, how have you found the Stream system?

At first, the Stream system was quite complicated to us since a lot of elaborate systems were installed. But soon we realized that it was much simpler than it seemed. The method to assemble the Stream holder was easy compared to other liquid cell TEM holders, and the way to control the injection solution was straightforward. And since a lot of O rings are used to encapsulate the Nano-cell, the holder seems to be very stable without leakage problems while operating the TEM. Also, the heating control software was upgraded from the Wildfire version, making it much easier to use the program.

Jungwon Park, Ph.D
Associate Professor | Seoul National University

Jungwon Park received his B.S. degree from the Department of Chemistry, POSTECH, South Korea, in 2003, and his Ph.D. degree from the Department of Chemistry, University of California, Berkeley, in 2012. After a post-doc with the School of Engineering and Applied Sciences, Harvard University, he started a faculty position with the School of Chemical and Biological Engineering, Seoul National University, in 2016, and he currently serves as an associate professor jointly affiliated with the Center for Nanoparticle Research, Institute for Basic Science (IBS). His research areas include the in-situ study of nanomaterials, liquid-phase TEM, phase transitions, interface chemistry, and low-dimensional materials.

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Standing next to the recently installed Stream system: from left, Dr. Anastasia Shebanova, Dr. Martial Duchamp and Jeffrey George from the Nanyang Technological University

We are happy to announce that the first ever Stream system in Singapore has recently been installed! For this event we interviewed Dr. Martial Duchamp from the School of Materials Science and Engineering at the Nanyang Technological University (NTU) in Singapore. In this interview, we discussed NTU’s advanced microscopy facility and the various applications that LPEM users are interested in, as well as how our Stream system has greatly benefited their research.  

Can you tell me a bit about the microscopy facility at the Nanyang Technological University?

The Nanyang Technological University has a shared microscopy facility called FACTS (Facility for Analysis Characterization Testing & Simulation) that specializes in characterization in the field of electron microscopy and x-ray techniques. FACTS provides state-of-the-art electron microscopes and X-ray instruments as well as the expertise to operate them to all of NTU and beyond.

This shared facility was created around 20 years ago. Four years ago, we had an extension of the facility, and got two aberration-corrected transmission electron microscopes as well as a new building where these TEMs were installed. The first TEM is a JEOL JEM-ARM200F, and the second is the JEOL JEM-GrandARM that is both probe- and image-corrected. Moreover, we have some local technicians and engineers who take care of these microscopes and make sure the facility is running well.

What type of applications are Stream users at the facility interested in?

Users of the facility are interested in a wide range of applications. In regards to LPEM users, we are using the DENSsolutions Stream system to study the liquid-liquid phase separation (LLPS) aspect of biological systems. Specifically, we are interested in the process called coacervation, which involves starting with a mixed phase of polymer or proteins dispersed in a solvent, and by changing certain conditions like the pH, temperature or salt concentration you can go from this diluted phase to a solid phase via phase separation. We are particularly interested in phase separation in order to understand how we go from these diluted solutions of drugs or proteins to solid matter.

Aside from liquid TEM, I am also interested in using in situ and operando TEM to observe 2D materials and the evolution of these materials versus temperature, as well as solar cells and batteries.

Can you tell us who won the grant to acquire the Stream system?

Associate Professor Ali Miserez, the lead PI of the project titled “Phase Separation-Regulated Life, In and Outside of Cells”, was awarded the Ministry of Education (MOE) Tier 3 grant worth 8.5 million Singaporean dollars. This research programme aims to closely integrate the tools of cell biology and colloidal biochemistry with the framework developed in the materials science of polymer science, soft matter, and complex fluids. The goal is to unravel LLPS-mediated functional organization across multiple biological length scales. Part of this grant was used to acquire the Stream system.

This 5-year project started last summer, and we are just starting to employ new researchers. In fact, some students already started a couple months ago and we expect to have some more people joining.

What particular features of Stream attracted you to the system?

For our experiments, it was essential to find a way to control the flux of the liquid within the liquid cell in order to look at reactions or processes occurring on the location of the electron beam. This is something we were unable to do with previous generations of holders and chips. The DENSsolutions Stream system is the only system that allows you to completely control the liquid flux. This unique capability is what intrigued us most about the system.

Moreover, as a result of the Nano-cell’s special inlet-outlet design, we are also able to fully control the pressure and liquid thickness. Other features that we found very attractive include the control systems like the heating control unit and the pressure-based pump, which are considerably more elaborate compared to what we had in the past.

In your experience so far, how have you found the Stream system?

The assembly in regards to the closing of the cell is quite straightforward, and so far we have not had any leakage issues. Just by closing the cell, it becomes airtight, which is a great advantage of the system. Moreover, what I really appreciate about the system is the ability to have complete control over the flow of the liquid.

Dr. Martial Duchamp
Assistant Professor | Nanyang Technological University

Dr. Martial Duchamp is an Assistant Professor in the school of Materials Science and Engineering at the Nanyang Technological University in Singapore. His research interests include the development of innovative operando TEM methods for application to solar cells, batteries and fuel cells devices, as well as obtaining a fundamental understanding of 2D materials to reveal their unprecedented electrical properties at local scale.

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