In situ TEM cooling meets high-precision heating: Exploring BaTiO₃ phase transitions with Lightning Arctic

In situ TEM cooling meets high-precision heating: Exploring BaTiO₃ phase transitions with Lightning Arctic

by | Dec 18, 2024 | Lightning Arctic, Materials science, Phase transformations

Using the DENSsolutions Lightning Arctic system, researchers uncover the temperature-driven phase transitions and domain wall dynamics in single-crystal BaTiO₃ with atomic precision across cryogenic and elevated conditions.

Original article by Jiang et al.

Understanding the intricate phase transitions and domain dynamics of ferroelectric materials like barium titanate (BaTiO₃) is essential for improving their functional properties in applications such as capacitors, sensors and actuators. However, achieving atomic-resolution insights across a wide temperature range—spanning cryogenic to elevated conditions—remains a significant challenge. In a recent study published in Microstructures, Prof. Leopoldo Molina-Luna’s group at TU Darmstadt utilized our Lightning Arctic system to investigate the phase transitions and domain evolution of single-crystal BaTiO₃. By utilizing the system’s cryogenic cooling and heating capabilities, the team achieved unparalleled stability and resolution, enabling direct observations of phase behavior and domain wall dynamics from -175 °C all the way to 200 °C.

Lightning Arctic: Ultra-high stability

The DENSsolutions Lightning Arctic solution was used in this study for the application of in situ TEM cooling and heating. The cooling capability of Lightning Arctic is enabled via a cooling rod inside the holder, which transfers the ‘cold’ towards the holder’s tip where the MEMS-based Nano-Chip holding the sample is located. Once this cooling rod is connected to a metal cooling braid that is immersed in a liquid nitrogen dewar, the sample can be cooled inside the TEM to liquid nitrogen temperatures.

Impressively, the researchers were able to achieve atomic-resolution imaging at cryo-temperatures with notably low sample drift. This is due to the ultra-high stability of the holder. They captured a sequential of ten frames of HAADF STEM images on a single-crystal BTO TEM sample. The first frame, provided below in Figure 1a, evinces the exceptional stability of the holder, enabling atomic-resolution imaging at -175 °C.

Figure 1: Drift analysis in the cryo-STEM experiment at -175 °C.

Domain evolution during heating

Ferroelectric materials exhibit phase transitions that significantly influence their domain structures, which play a crucial role in determining material performance. By applying a controlled heating profile, the researchers were able to monitor how BaTiO₃ evolves through its various phases in real time. The video below highlights the dynamic changes in domain wall (DW) configurations as the material transitions from rhombohedral (R) to orthorhombic (O), tetragonal (T) and finally cubic (C) phases. At lower temperatures, zigzag patterns formed by 60° and 120° DWs appeared in the orthorhombic phase, while 90° a-c type ferroelastic domains became prominent in the tetragonal phase. These observations showcase how temperature influences domain behavior, offering valuable insights into the structural evolution of BaTiO₃ during heating.

Movie 1: Domain evolution during the complete in situ TEM heating process.

Domain evolution during cooling

Domain wall dynamics are central to understanding ferroelectric materials, as the movement and reorganization of these walls directly influence the material’s functional performance. Monitoring these processes in real time requires both exceptional resolution and imaging stability. The video below showcases the real-time evolution of domain walls across different temperature phases, enabled by the ultra-stable capabilities of the Lightning Arctic system. The researchers captured the movement and interaction of 71° and 180° DWs in the rhombohedral phase at cryogenic temperatures. These observations provide unprecedented clarity on the spontaneous strain and polarization mechanisms that govern domain stability, offering new insights into the nanoscale processes driving ferroelectric behavior.

Movie 2: Domain evolution during the complete in situ TEM cooling process.

Advancing the frontier of ferroelectric science

Conclusively, this study highlights the power of the DENSsolutions Lightning Arctic system in enabling atomic-resolution observations of phase transitions and domain wall dynamics in single-crystal BaTiO₃ across a wide temperature range. By capturing real-time structural evolution during both heating and cooling processes, Prof. Leopoldo Molina Luna and his group were able to reveal critical insights into the behavior of ferroelectric domains under temperature-driven stimuli. These findings lay the foundation for further studies of functional materials under multi-stimuli conditions, driving advancements in their development for next-generation applications.

“DENSsolutions’ Lightning Arctic enables in situ TEM of phase transitions with atomic precision.”

Prof. Leopoldo Molina-Luna   |   TU Darmstadt

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Lightning system helps uncover the interaction mechanism in reactive metal-ceramic system, Al-SiC

The DENSsolutions Lightning system was utilized to reveal the evolution mechanism of the Al–AOL–SiC system under heating and biasing conditions and under an ultrahigh resolution of 4 Å.

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Introducing Infinity: DENSsolutions’ pioneering 8-contact environmental in situ solution

Introducing Infinity: DENSsolutions’ pioneering 8-contact environmental in situ solution

by | Jul 27, 2024 | Climate, Interview, Stream

An interview with DENSsolutions’ Senior Mechanical Engineer about our latest innovation, Infinity – featuring an environmental holder with combined heating and biasing capabilities in both gas and liquid environments.

In this article, we delve into DENSsolutions’ cutting-edge Infinity solution through an exclusive interview with lead developer and Senior Mechanical Engineer, Christian Deen-van Rossum. Here, Christian takes us through the key features of this innovation, highlighting its benefits, diverse applications, and offering an inside look into the development journey of this advanced solution.

1) What are the main benefits of the Infinity solution for users?

“Climate Infinity and Stream Infinity bring forth numerous advantages for your in situ experiments:

1) Apply simultaneous heating and biasing stimuli: The new Climate/Stream Infinity holder features eight electrical contacts that enable simultaneous application of electrical and thermal stimuli in a gas or liquid environment. The contacts can be used for various electrically driven MEMS-based sensors and actuators, essentially transforming the Infinity system into a vast research playground. Importantly, for liquid studies, this opens the door to performing electrochemistry as a function of temperature.

2) Securely transfer your sample from one microscope to the other: The assembled tip of the Infinity holder containing a Nano-Reactor/Cell works as a cartridge, enabling complementary studies of the same sample using different TEM vendors, namely JEOL or Thermo Fisher Scientific (TFS). These microscopes can either be located in the same TEM lab, user facility or even in different universities/institutes. Remarkably, this removable tip also facilitates multi-modal characterization for SEM and beamline setups. Furthermore, the chips being used are universal, meaning that you can directly correlate experimental results obtained from JEOL and TFS microscopes, with improved Nano-Chip logistics.

3) Easily switch between STEM and TEM mode: By flipping the tip 180 degrees, you can directly change the sample position to be either on the top or bottom without a need to disassemble the tip. This grants you the freedom to flawlessly switch between STEM or TEM mode, respectively, depending on your experimental needs, while maintaining the best resolution performance. Importantly, you can switch between both imaging modes within a matter of seconds.

4) Perform gas and liquid studies with the same holder: The new environmental Infinity holder is your all-in-one solution for both gas and liquid experiments. Simply choose the appropriate function for the chips and connect the necessary gas or liquid supply system. Our extensive range of chip types includes gas-heating (GH), liquid-heating (LH), gas-heating-biasing (GHB), and liquid-heating-biasing (LHB), offering unparalleled versatility for your experimental needs. New MEMS chip designs will further expand the application space of the Infinity system.

5) Ease of use: We understand that a great product should be easy to use without a steep learning curve. Therefore, our design process focused on making sure the holder can be effortlessly utilized from the start. By prioritizing user-friendly design and continuously testing with real users, we ensured our product is not only powerful and effective but also simple and enjoyable to use. Because of this, the Infinity holder significantly reduces the time-to-experiment, allowing you to spend your time leveraging its capabilities to drive innovation and productivity. One highlight of the Infinity holder is the removal of all assembly tools and the introduction of self-aligning windows. When you place our chips in the tip of the holder, the membranes automatically align to provide a consistently clear field of view. Designed for a perfect fit, the Infinity holder ensures precise alignment without manual adjustments. This simplifies installation, reduces the risk of leaks, and allows you to focus more on your research and less on setup.

2) What inspired the development of Infinity, and what challenges did you encounter during the process?

“We wanted to bring a better, future-proof and more user-friendly holder to the market that truly meets the needs of our customers. For that reason we developed a holder from a customer-centric approach, driven by extensive customer input and thorough market research, rather than simply pushing the latest technology. We engaged with our customers to understand their challenges and desires and gathered invaluable feedback that helped shape every aspect of our product. By doing this we made sure that we were addressing real pain points and delivering solutions that would help improve the customer experience and reduce time to experiment. This customer-focused approach means that our product is not just a collection of the latest technological advancements, but a thoughtfully designed solution that reflects the actual needs and desires of our users.” 

3) What are the main application fields that will benefit from Climate Infinity and Stream Infinity?

“The Infinity system can be used for broad applications ranging from materials science to energy and life science. In materials science, the Infinity system enables the study of nucleation, growth, assembly and corrosion under well-defined chemical environments (gas, vapor and liquid) and external stimuli (heating, biasing or both). The information obtained not only provides insights into the dynamic processes of material formation but also offers guidelines for the controllable synthesis of materials with improved performance. In energy studies, the Infinity system can mimic the real working conditions of various functional devices (such as batteries, supercapacitors, fuel cells, memristors, resistive random access memory, etc.). This allows the direct monitoring of the evolution and degradation of key materials, including rechargeable battery electrodes, thermo-, electro- and thermoelectro-catalysts and phase-change materials, at the nano- or even atomic scale. For life science, it is possible to image whole cells and resolve fine structures of biomaterials and proteins in their native state, and study various dynamics of biological samples in an environment close to a real organism. Moreover, the Infinity system provides a unique platform for correlative studies across different detection sources, such as electron, X-ray, neutron and visible light.”

4) Has Infinity already been installed?

“Yes, the system has been installed at numerous sites already, including EMAT (Antwerpen, Belgium), FAU Erlangen-Nurnberg (Erlangen, Germany) and UC Irvine (Irvine, USA).”

Dr. Mingjian Wu from FAU Erlangen-Nürnberg

From left to right: Dr. Alexander Zintler from EMAT and Christian Deen van Rossum from DENSsolutions

From left to right: Dr. Hongkui Zheng and Dr. Hongyu Sun from DENssolutions, as well as Pushp Raj Prasad, Prof. Joe Patterson, Zhaoxu Li and Elmira Baghdadi from UC Irvine

Dr. Mingjian Wu from FAU Erlangen-Nürnberg

From left to right: Dr. Alexander Zintler from EMAT and Christian Deen van Rossum from DENSsolutions

From left to right: Dr. Hongkui Zheng and Dr. Hongyu Sun from DENssolutions, as well as Pushp Raj Prasad, Prof. Joe Patterson, Zhaoxu Li and Elmira Baghdadi from UC Irvine

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In situ LPEM: Illuminating the electrochemical nanoscale dynamics of active materials

In situ LPEM: Illuminating the electrochemical nanoscale dynamics of active materials

by | Jun 11, 2024 | Electrochemistry, Materials science, Stream

Using the DENSsolutions Stream system, researchers take a magnified look at the nanoscale processes governing electrochemical activity in active molecular materials.

Original article by Gibson et al.

Active materials’ ability to interact with their environment in dynamic ways makes them invaluable across numerous fields, enhancing the functionality, efficiency and sustainability of various products and technologies that we use daily. This includes bio-sensors, flexible electronics, water purification and solar cells. Indeed, a thorough comprehension of the behavior of active materials under electrochemical conditions is crucial for their development. While substantial efforts have been made to understand the self-assembly mechanisms of biologically active materials, there is currently a large knowledge gap on how synthetic active materials behave. Traditional microscopy techniques often fall short in capturing the real-time dynamics of materials immersed in liquid environments. This is where liquid phase electron microscopy (LPEM) comes into play, offering a powerful solution to bridge this gap.

In a recent study published in the renowned journal of ACS Nano, a team of researchers from the University of California (UC) Irvine and the University of Massachusetts Boston employed the DENSsolutions Stream system to investigate the dynamics of electrochemically driven active materials. Impressively, they were able to capture single fiber dynamics at subsecond temporal resolution, as well as larger transitory fiber foci structures with nanoscale resolution. This research, involving our dear user at UC Irvine, Prof. Dr. Joe Patterson, is a major step forward in using electrochemical liquid EM to understand the dissipative self-assembly processes that generate active materials – a research space that remains largely unexplored. Notably, our Stream system played a vital role in enabling the visualization of these intricate electrochemical processes, providing key insights into the relationship between chemical kinetics and material dynamics.

Hierarchical evolution of fiber dynamics

The nanoscale self-assembly processes observed in this study involve the electrochemical oxidation of a free cysteine thiol precursor (CSH) molecule to its disulfide gelator form (CSSC) using the ferricyanide/ferrocyanide redox couple as a electrochemical catalyst. For the experiments, Wyeth Gibson and his fellow collaborators utilized the Stream Nano-Cell’s working electrode as the anode, which provided the driving force for the oxidation of ferrocyanide to ferricyanide and the follow-up oxidation of CSH to CSSC. 

After capturing the dynamics of individual fibers under electrochemical stimulation near the electrode, the researchers were then able to capture the micrometer-scale hierarchical evolution of fiber clusters. As shown in the movie below, the fiber foci experience a maximum growth at 87 s and disassembly at 167 s. Evidently, the overall growth and shrinking of the fiber foci seem to loosely correspond with application and removal of electrochemical stimulus.

Movie 1: LPEM movie depicting the fiber foci growth and disassembly 

Capturing fiber foci modification

The next step for the researchers was to study the active material’s dynamics in response to further electrochemical stimulus. They applied a current to the structures and activated the electron beam, which was maintained at a constant throughout the experiment.  As shown in Movie 2 below, for the first 100 seconds, the fiber foci remained stable. At 100 s, a self-assembly growth front moved from left to right, causing the structures to grow and increase in contrast. At 200 s, a second growth front emerged as the first front reached the electrode boundary, spreading outward from the electrode in all directions. Between 400 and 600 seconds, the structures began to break down, shrink and decrease in contrast across the viewing window.

Movie 2: LPEM movie depicting the electrochemically driven fiber foci modification

Movie 3: LPEM movie depicting the fiber foci modification

Next, a regional segmentation analysis was performed in order to quantify the observed wave-like propagation of these self-assembly fronts. This is depicted in Movie 3, whereby the middle panel shows the segmented particles corresponding to the LPEM movie shown in the left panel. The graph in the video depicts the normalized change in segmented particle area over time for each region, with the segmented regions represented by blue (closest to the electrode), purple, red, and yellow (farthest from the electrode).

It is evident that the distance from the electrode affects the maximum structural density in a sequential manner. Notably, Dr. Gibson and his collaborators effectively demonstrate that the active material can be dynamically manipulated to form multiple growth fronts influenced by electrodes at different spatial locations.

Next, a regional segmentation analysis was performed in order to quantify the observed wave-like propagation of these self-assembly fronts. This is depicted in Movie 3, whereby the middle panel shows the segmented particles corresponding to the LPEM movie shown in the left panel. The graph in the video depicts the normalized change in segmented particle area over time for each region, with the segmented regions represented by blue (closest to the electrode), purple, red, and yellow (farthest from the electrode). It is evident that the distance from the electrode affects the maximum structural density in a sequential manner. Notably, Dr. Gibson and his collaborators effectively demonstrate that the active material can be dynamically manipulated to form multiple growth fronts influenced by electrodes at different spatial locations.

Movie 3: LPEM movie depicting the fiber foci modification

Integrating observations with simulations

To gain a clearer understanding and measure the structural transformation within the liquid cell, the researchers utilized structural dissimilarity (DSSIM) analysis on the electrochemical LPEM video. DSSIM analysis is a video processing technique that spatially and temporally quantifies structural changes occurring in a video. Importantly, by combining the LPEM data with kinetic simulations, they discovered that the formation of an active material can foster a local environment that boosts the pace of the self-assembly process, exhibiting an autocatalytic behavior.

Movie 4: DSSIM visualization and quantification of fiber foci dynamics

A pioneering electrochemistry study

Conclusively Prof. Dr. Joe Patterson and his fellow researchers performed a cutting-edge study, employing a combination of techniques including LPEM, electrochemical analysis, quantitative video analysis and kinetic simulations to explore a widely untapped research space – the self-assembly mechanisms in electrochemically fueled active materials. This innovative research highlights the crucial role of liquid electron microscopy in studying active materials, offering vital insights into the interplay between chemical kinetics and material behavior. We are certainly proud of the key role that our Stream system has played in bringing this research to fruition, and we look forward to the pioneering academic contributions that the Patterson Lab will continue to deliver.

“These were the most challenging liquid electron microscopy experiments I have ever performed, and the DENSsolutions Stream system was essential for getting them to work.”

Prof. Dr. Joe Patterson   Professor  |  University of California Irvine

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DENSsolutions joins the In-Situ Microscopy Alliance

DENSsolutions joins the In-Situ Microscopy Alliance

by | May 14, 2024 | News, Partnerships

We are proud to announce that we have become the 5th member of the In-Situ Microscopy Alliance, a collective of innovative scientific companies with the aim of advancing electron microscopy.

What is the In-Situ Microscopy Alliance?

The In-Situ Microscopy Alliance (IMA) brings together a collective of experts in electron microscopy and related analytical methods, pooling their efforts towards cultivating an innovative and sustainable future. Within this alliance, we engage in collaborative exploration, pushing the boundaries to shape the specs of forthcoming analytical instruments crucial for advancing sustainable technology. To share knowledge effectively, IMA conducts regular online webinars dedicated to specific applications and hosts in-person workshops.

Who are the partners of the In-Situ Microscopy Alliance?

IMA is a collective of 5 different members, including Alemnis, Imina Technologies, NenoVision, point electronic and now DENSsolutions. All members of IMA produce analytical equipment complementary to electron microscopy. 

Why was IMA founded?

The creation of the In-situ Microscopy Alliance (IMA) aimed to facilitate the exchange of expertise and advanced technologies in in-situ microscopy and testing. Its primary goals include expediting innovation, encouraging the adoption of novel techniques and promoting the development of diverse applications spanning various fields.

As an alliance, we will:

  • Create an ecosystem to enable leading industrial and academic players to explore, develop and promote in-situ characterization techniques, tools, and applications.
  • Educate the research and engineering community about the capabilities of in-situ characterization techniques.
  • Offer integrations of advanced analytical tools and applications for comprehensive in-situ characterization.

Our core mission is to connect industry and academia to advance in-situ microscopy characterization tools, solutions and services.

Meet IMA’s scientific board

In-situ Microscopy Alliance is supported by a scientific advisory board formed by leading researchers working on novel materials, semiconductors and energy solutions.

Prof. Dr. Marc-Georg Willinger

Professor  | Technical University of Munich

Dr. Umberto Celano

Associate Professor  |  Arizona State University

Watch one of IMA’s webinars

Learn more about the Alliance, its founding companies and discover the related work of Prof. Dr. Marc-Georg Willinger, a longstanding Climate user and renowned expert in electron microscopy, focusing his research on energy materials.

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DENSsolutions partners with Bioz for AI-powered scientific search

DENSsolutions partners with Bioz for AI-powered scientific search

by | Apr 8, 2024 | News, Partnerships

We are thrilled to announce a significant enhancement to our website: the integration of the Bioz search engine – a cutting-edge tool empowering you to discover relevant publications with ease.

We recently integrated a state-of-the-art publications search tool, powered by cutting-edge artificial intelligence technology, across multiple pages on our website. Developed by Bioz, this innovative tool seamlessly scans through vast repositories of scientific papers, providing you with access to a wealth of information through sophisticated filtering capabilities.

Explore our new-and-improved Publications page

Previously, our Publications page allowed visitors to filter papers based solely on the type of DENSsolutions product used – namely Wildfire, Lightning, Climate or Stream. However, we understand that researchers appreciate more advanced search and filtering options to find tailored publications relevant to them. Therefore, we aimed to implement a tool on our website that would enable visitors to search for direct keywords applicable to their application or research focus. Moreover, a tool that would allow visitors to filter by the technique used, journal and even authors involved. This is precisely where Bioz comes in. You can now explore the tool on our updated Publications page. We would also like to highlight that with Bioz, you can make use of two unique features – the Charts and Maps feature. With Charts, you can visualize the popularity of all relevant techniques to in situ TEM, such as 4D-STEM, EELS and EDX. Moreover, the Maps feature allows you to see where all the authors of the papers are based.

Explore our updated product pages

Aside from the updates made to our Publications page, we’ve also revamped our product pages to allow for seamless searching of relevant publications as you acquaint yourself with each product. You can easily access these product pages through the links provided below. Note that as our latest solution Lightning Arctic was just launched some months ago, we plan to incorporate the Bioz platform directly into its dedicated webpage as publications begin to accumulate. 

About Bioz

Bioz, an AI software company based in Silicon Valley, uses AI, machine learning and natural language processing in order to extract experimentation data from scientific articles. Bioz AI was developed by AI experts from Microsoft and Google, and with Nobel Prize winners in chemistry. The Bioz search engine offers researchers billions of data-driven product, technique and protocol recommendations. By harnessing the power of AI, Bioz provides researchers with an unprecedented amount of summarized scientific experimentation knowledge right at their fingertips. They are used by over 2 million researchers from over 17,000 different universities and companies in 196 countries. Their search engine is fueled with 300,000 million different products, 50,000 suppliers and 3,000 research techniques. 

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