DENSsolutions’ Climate system takes home the Microscopy Today 2021 Innovation Award

DENSsolutions’ Climate system takes home the Microscopy Today 2021 Innovation Award

DENSsolutions becomes a consecutive two-time winner of the Microscopy Today Innovation Awards. This year, our Climate system is recognized as one of the 10 most game-changing microscopy innovations of 2021.

Just last year, our Stream system was awarded the Microscopy Today Innovation Award for its unique contribution to the field of liquid phase electron microscopy. We are honored to be taking home the same award for a second year in a row but this time for the remarkable innovation that is our Climate system. Climate is recognized as one of the 10 most game-changing microscopy innovations in 2021 by Microscopy Society of America‘s esteemed magazine, Microscopy Today. We interviewed our Chief Technology Officer Dr. Hugo Pérez-Garza, who led the development of the Climate system, to learn all about the unique benefits that made it earn such an esteemed award, as well as the development process and Climate’s current and envisioned applications. The transcript of the interview is provided below.

What was your reaction when you first heard the news?

It was pretty exciting. As you can imagine, the entire team was very happy when we first heard the news. At the end of the day, I think that this is just another consequence of the amazing teamwork that prevails in this company. And of course, to be accredited by the MSA is a big honor, especially as this is a highly esteemed award within the community. So it really means a lot to us. We really feel confident that our technology, and particularly our Climate system, will help scientists explore all sorts of new research possibilities.

What unique aspects of the system do you think made it earn such an esteemed award?

Over the last months, we have been exerting a lot of effort into making sure that we can improve the Climate system from various different angles. So that means that we have been doing a lot of work to ensure that we can optimize the different components that make up this plug-and-play system. Specifically, we have been trying to boost our MEMS capabilities (the Nano-Reactor). Moreover, we have been trying to continuously improve our hardware components, including the Gas Supply System, the Vaporizer, the Mass Spectrometer, etc. And of course, making sure that we can have new solutions as well for the software platform. Now when you put all these together, what we ended up realizing was that this new optimized Climate system brings all sort of real unique aspects to one’s research.

1) Live gas mixing

Firstly, Climate offers the possibility of performing live gas mixing (i.e. making sure that you can achieve any desired gas composition instantaneously). It ensures that users won’t have to wait for their gas mixtures to be prepared. We see this big added value in our customers’ experiments, for example in redox reactions, where the intrinsic nature of the experiment demands the possibility to quickly go from an oxidizing environment to a reducing environment. Often times people have to do this back-and-forth and in a fast and repetitive way. 

2) Start a new experiment (from a dry to wet environment or vice versa) within minutes

Furthermore, for these experiments a lot of researchers would be interested in humidifying the gas composition. This is precisely where the Vaporizer comes in. Now what happens here is that when you are humidifying the gas, often people are afraid of the contamination that the water molecules would represent for the gas lines. And that is why systems have to baked or have to undergo lengthy pumping times. But that wouldn’t be the case with the Vaporizer, as we have designed it in such a way that the introduction of the water vapor to the gas mixture is the last thing before entering the holder. So that ensures that your Gas Supply System will remain clean, and that you don’t have to perform these baking procedures or keep it pumping over night. This ultimately means you can go from a dry environment to a wet environment, or vice versa, in just a few minutes. So it opens up a lot of possibilities because it gives users this flexibility. 

3) Safely work with explosive mixtures and independently control gas parameters

The fact that we’re dealing with extremely low volumes of gas also means that we can safely handle explosive mixtures even if you plan to do this under extreme conditions such as high temperatures (above 1000°C) in combination with high pressures (i.e. 2 bars) and high relative humidity (i.e. 100%). Not only can you safely handle these explosive mixtures, but you can also control the relative humidity independently from other parameters such as temperature, pressure, gas composition and flow rate. So having this independent control also brings a lot of flexibility to users. 

4) Perform real nano-calorimetry and calibrate for time delay

The Nano-Reactor is also something very unique as we have been heavily optimizing the design such that, for example, the microheater allows for real nano-calorimetry. And this is really unique because it means that you can start quantifying and measuring the tiniest changes in temperature dissipation to understand if you’re observing an exothermic or endothermic reaction. And this is also really beneficial because you can calibrate for time delay, which is an issue that systems usually suffer from due to the unavoidable delay from the Gas Supply System to the MEMS device and to the Mass Spectrometer. Now, we can calibrate for that. 

5)  Prevent bypasses and achieve a desirable SNR

Moreover, the unique design of the Nano-Reactor itself, for which we have a patent, ensures that we can have an on-chip inlet and outlet. In other words, we can ensure that the gas will flow from the inlet to the outlet via the region of interest in a uni-directional way. And that means we can prevent bypasses and therefore improve the signal-to-noise ratio and the sensitivity of the Gas Analyzer. So the combination of these offerings (for example that our MEMS device can go to these high pressures like 2 bar, or allow you to perform EDS experiments well above 900 degrees at high pressures) ends up bringing a very unique value proposition for the user. 

What unique aspects of the system do you think made it earn such an esteemed award?

Over the last months, we have been exerting a lot of effort into making sure that we can improve the Climate system from various different angles. So that means that we have been doing a lot of work to ensure that we can optimize the different components that make up this plug-and-play system. Specifically, we have been trying to boost our MEMS capabilities (the Nano-Reactor). Moreover, we have been trying to continuously improve our hardware components, including the Gas Supply System, the Vaporizer, the Mass Spectrometer, etc. And of course, making sure that we can have new solutions as well for the software platform. Now when you put all these together, what we ended up realizing was that this new optimized Climate system brings all sort of real unique aspects to one’s research.

1) Live gas mixing

Firstly, Climate offers the possibility of performing live gas mixing (i.e. making sure that you can achieve any desired gas composition instantaneously). It ensures that users won’t have to wait for their gas mixtures to be prepared. We see this big added value in our customers’ experiments, for example in redox reactions, where the intrinsic nature of the experiment demands the possibility to quickly go from an oxidizing environment to a reducing environment. Often times people have to do this back-and-forth and in a fast and repetitive way. 

2) Start a new experiment (from a dry to wet environment or vice versa) within minutes

Furthermore, for these experiments a lot of researchers would be interested in humidifying the gas composition. This is precisely where the Vaporizer comes in. Now what happens here is that when you are humidifying the gas, often people are afraid of the contamination that the water molecules would represent for the gas lines. And that is why systems have to baked or have to undergo lengthy pumping times. But that wouldn’t be the case with the Vaporizer, as we have designed it in such a way that the introduction of the water vapor to the gas mixture is the last thing before entering the holder. So that ensures that your Gas Supply System will remain clean, and that you don’t have to perform these baking procedures or keep it pumping over night. This ultimately means you can go from a dry environment to a wet environment, or vice versa, in just a few minutes. So it opens up a lot of possibilities because it gives users this flexibility. 

3) Safely work with explosive mixtures and independently control gas parameters

The fact that we’re dealing with extremely low volumes of gas also means that we can safely handle explosive mixtures even if you plan to do this under extreme conditions such as high temperatures (above 1000°C) in combination with high pressures (i.e. 2 bars) and high relative humidity (i.e. 100%). Not only can you safely handle these explosive mixtures, but you can also control the relative humidity independently from other parameters such as temperature, pressure, gas composition and flow rate. So having this independent control also brings a lot of flexibility to users. 

4) Perform real nano-calorimetry and calibrate for time delay

The Nano-Reactor is also something very unique as we have been heavily optimizing the design such that, for example, the microheater allows for real nano-calorimetry. And this is really unique because it means that you can start quantifying and measuring the tiniest changes in temperature dissipation to understand if you’re observing an exothermic or endothermic reaction. And this is also really beneficial because you can calibrate for time delay, which is an issue that systems usually suffer from due to the unavoidable delay from the Gas Supply System to the MEMS device and to the Mass Spectrometer. Now, we can calibrate for that. 

5)  Prevent bypasses and achieve a desirable SNR

Moreover, the unique design of the Nano-Reactor itself, for which we have a patent, ensures that we can have an on-chip inlet and outlet. In other words, we can ensure that the gas will flow from the inlet to the outlet via the region of interest in a uni-directional way. And that means we can prevent bypasses and therefore improve the signal-to-noise ratio and the sensitivity of the Gas Analyzer. So the combination of these offerings (for example that our MEMS device can go to these high pressures like 2 bar, or allow you to perform EDS experiments well above 900 degrees at high pressures) ends up bringing a very unique value proposition for the user. 

What inspired you and the entire team to develop Climate in the first place?

Certainly understanding the importance and the impact that environmental studies can have on our global society was a big source of inspiration for the entire team. Having said that, understanding the solid-gas interactions at the nanoscale is what sets the foundation such that scientists can really start understanding how to optimize and synthesize future catalytic nanoparticles, which will end up playing a crucial role in applications such as carbon capture, energy storage and conversion as well as food production. So it is really this profound information that we can get from in situ TEM that gives this understanding. Because when you can start correlating particle size with composition, crystal orientation, or with the atomic or the electronic structure, it really gives a deep level of understanding for all these kinds of experiments. 

Can you walk us through the development process of Climate?

It has been 5 or 6 years since we launched our first product line for in situ gas analysis. Ever since, what we have been doing is trying to make sure that we can stay as close as we can to our customers as well as prospects. Now the intention of doing that is when you start gathering the feedback and the vision that both groups have, you start understanding the pain points a little bit more. You start becoming more empathic to their experimental needs. And that helps us identify the product profile that we should have in place. And when you are aware of this product profile, then automatically you know what technologies must be developed, which is part of your roadmap. And subsequently when you have that in place, then you also know what people and processes must be involved. So, it’s a matter of doing that so that when we gather these market requirements, we can follow a defined product creation process that will allow us to develop a technology that will match these market requirements. 

What future applications do you envision for Climate?

Certainly everything related to green technologies. As I mentioned earlier, that is a big goal and motivation that we all have at this company. So these kinds of experiments and topics I was referring to like carbon capture, energy conversion and storage, and all sort of environmental protection kind of studies, that’s really where everything will head towards. 

Thank you for reading. To learn more about our Climate system please follow the links below.

Download the Climate brochure: 

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Introducing our latest product: the Climate G+ Vaporizer

Introducing our latest product: the Climate G+ Vaporizer

An interview with DENSsolutions R&D Engineer Ronald Spruit about our latest extension of the Climate G+ product line: the Vaporizer

Ronald Spruit Vaporizer article 1200x628

DENSsolutions introduces its latest product: the Vaporizer — an extension of the Climate G+ product line. This innovative solution takes your in situ experiments to a whole new level, enabling you to independently add water vapor to any gas mixture of up to 3 gases. We interview our R&D Engineer Ronald Spruit to learn all about the Vaporizer, from what inspired its development, its unique capabilities and the many applications that will benefit from its creation.

What led to the development of the Climate G+ Vaporizer?

The DENSsolutions Climate system has been widely used to study catalysis, nanomaterial growth and corrosion. Currently, the system provides a highly controlled gas and temperature environment, allowing users to independently control gas composition, gas pressure, gas flow rate and temperature. To enable this high level of control, the development of Climate has been aimed at delivering and mixing gases in the most accurate and clean way possible. 

Typically, high-purity gases are being used in combination with the Climate Gas Supply System (GSS). As a consequence, the environment that is created in the Nano-Reactor can be very dry. However, it is known that realistic scenarios and industrially relevant applications often occur under conditions where the gas is not perfectly dry, but in conditions where vapors are present. Moreover, although water’s negative effects on metal corrosion and catalyst deactivation have been well-researched for decades, the study of water’s influence on gas-solid reactions inside a TEM is limited. This is due to the lack of control over the flow rate and pressure of the water vapor, as well as the fear of contaminating high-vacuum TEM columns.

We therefore wanted to develop a solution that tackles these limitations by allowing users to add water vapor to their gas flow, and have the liberty to fully control the water vapor pressure. This is precisely what the Vaporizer enables. With the development of the Vaporizer, we hope to not only make new research involving water possible, but also draw attention to the importance of controlling water vapor levels to increase the repeatability of in situ experiments.

What are the main benefits of the Climate G+ Vaporizer?

The Vaporizer further extends the unique capabilities of the Climate G+ system, making your in situ experiments more accurate, reliable and representative of realistic conditions than ever before.

1) Independently control gas parameters: In addition to the independent control of gas pressure, flow and composition that the Climate G+ offers, the Vaporizer allows for the fully independent control of one more significant gas parameter: the level of water vapor pressure over the complete range of 0 to 25 mbar. This means that for the first time, you can fine-tune any of the above-mentioned parameters with the assurance that the others stay perfectly steady.

2) Start a new experiment in minutes: The Vaporizer has been designed to be versatile, fast and flexible. The vapor is added to the gas flow as provided by the GSS just before the gas enters the TEM holder. Therefore, the GSS remains free of water vapor, allowing you to switch back and forth between ‘dry’ and ‘wet’ conditions or even start a new experiment in a matter of minutes.

3) Safely work with explosive mixtures: A known unique feature of the Climate G+ system is that it allows you to safely work with flammable or even explosive mixtures thanks to its live mixing feature and minimal internal volume. This benefit extends into the Vaporizer, which allows you to safely add water vapor to any gas mixture.

Which applications will benefit most from the Climate G+ Vaporizer?

Applications that will highly benefit most from the Vaporizer include catalysis reactions involving water, catalyst deactivation caused by water, and metal corrosion. 

For example, in our published application note, we use the Vaporizer to study the reconstruction behavior of NiAu bimetallic core-shell nanoparticles, a catalyst system highly selective to CO in CO2 hydrogenation, under a hybrid atmosphere of water and hydrogen. For the NiAu nanoparticles, water is a reaction product. By controlling the water pressure, it is revealed that a solid NiO shell forms at high water vapor levels, reversible loose NiO appears and disappears at low water vapor levels and no NiO formation occurs with no water. The results provide perspective on the complex role that water plays on reactions. Moreover, the ability to introduce water vapor in a controlled fashion can help researchers design more water-sustainable catalysts.

In the future, we also expect the Vaporizer to be useful for applications involving solid batteries that require some need for water.

What is the compatibility of the Climate G+ Vaporizer?

The Vaporizer is designed for and fully compatible with the Climate G+ product line.  It is also directly compatible with most generations of Climate S3+ systems. However, for these systems it’s best to get in touch with us to confirm the compatibility, possibilities and potential aspects to consider.

What kind of challenges were tackled during development?

One of the main challenges of this development was designing the Vaporizer in such a way that it would be fully compatible with the Climate G+ system, while maintaining our existing unique features and benefits. Fortunately, we were able to find a good solution to integrate the hardware, control mechanisms and software seamlessly into each other. As a result, the Climate system feels as if the Vaporizer has always been part of it and at the same time the Vaporizer can be seen as an add-on to existing systems. This serves new users with a system that can do it all as well as ensures backwards compatibility to existing systems such that we don’t exclude the loyal users of our systems from the possibility to upgrade with this new vapor feature.

Read more about the Vaporizer:

 

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Scientists develop a powerful distributed electron microscopy technique to study complex reactions in solution

Scientists develop a powerful distributed electron microscopy technique to study complex reactions in solution

Using our Ocean system, scientists demonstrate the power of combining multiple electron microscopy methods, showing for the first time how the desilication mechanism of zeolite crystals proceeds in 3D on the single particle level.

Original article by Hanglong Wu, Teng Li, Sai P. Maddala, Zafeiris J. Khalil, Rick R. M. Joosten, Brahim Mezari, Emiel J. M. Hensen, Gijsbertus de With, Heiner Friedrich, Jeroen A. van Bokhoven and Joseph P. Patterson
Thomas article feature image
Liquid phase electron microscopy (LPEM) possesses the potential to revolutionize materials science by providing direct evidence of processes occurring in solution at the nanoscale. However, the use of high-energy electrons can be problematic as it can significantly change the solution chemistry and the liquid sample being imaged. Therefore, a primary challenge in LPEM is understanding the role the electron beam plays in the observed mechanism. As such, researchers find themselves stuck on the same question: “Which features of the native process are being captured?”

Dr. Hanglong Wu and his colleagues from the Eindhoven University of Technology, ETH Zurich and University of California, Irvine provide a robust answer to this pressing question by developing a novel approach for studying complex reactions in solution. This concept, which they term a “distributed electron microscopy (EM) method” combines information from multiple EM methods, including LPEM, cryogenic EM and cryo-electron tomography. To demonstrate this powerful method, Dr. Wu and his colleagues use our dedicated LPEM solution to study the desilication mechanism of zeolite crystals. They show for the first time with an exceptional level of confidence how the reaction proceeds in 3D on the single particle level. Moreover, they show how LPEM can be combined with cryo-EM to study a complete reaction which is essential to rule out beam-induced effects in LPEM experiments. 

The desilication study

Dr. Wu and his colleagues employ a distributed electron microscopy method to study the desilication process in zeolite crystals, showing how the reaction proceeds in 3D and what controls the desilication kinetics. This distributed approach enables them to explore and understand the native mechanism at hand, exploiting the power of each imaging modality – LPEM, cryogenic EM (cryo-EM) and cryo-electron tomography (cryo-ET). The researchers use Al-zoned ZSM-5 zeolites, which have an aluminum-rich rim and an aluminum-poor core, as a model system, to study the desilication process. The reason this is an ideal model system is that ZSM-5 crystals have a complex 3D morphology and are also considerably beam-sensitive.

The two videos below respectively show the automated sample loading process assisted by a liquid handling machine called SciTEM, and how the desilication process was initiated via the manual flowing of an NaOH solution into the cell.

Movie 1: Movie showing the SciTEM-assisted sample loading process, where a tiny droplet (~ 300 pL) containing zeolite crystals was deposited on the centre of the viewing window area.

Movie 2: Movie showing that the liquid cell is gradually filled with 0.6 M NaOH

Using LPTEM to observe the desilication process

Using LPTEM, Dr. Wu and his colleagues monitored the desilication process of individual parent zeolite crystals in multiple areas of a single cell. In the movie below, the desilication process of three pre-etched zeolite crystals can be observed over a 3-hour period. In contrast, for the crystals without the pre-etching treatment, the researchers find that the zeolites were only partially desilicated after 30 h in the liquid cell.

Movie 3: Movie showing the desilication process of three pre-etched zeolite crystals. On the left is the raw data movie and on the right a 30-frame-averaged data movie

The LPTEM data collected by the researchers provide evidence that desilication propagates along the c-axis beginning either at the Al-rich/Si-rich interface or in the crystal center. Moreover, it is observed that for the intergrowth structures, the process begins at the intergrown interface. Importantly, the LPEM experiments show that the confinement in the liquid cell slows down the desilication kinetics and that the electron beam does in fact influence the morphological evolution. This then raises the question that Dr. Wu and his colleagues sought out to answer: which features of the native desilication process are actually being captured?

LPTEM vs. LPSTEM

The LPSTEM results (Figure 1) observed by the researchers were significantly different from the LPEM observations. Dr. Wu and his colleagues believe that the differences mainly originate from contrast formation mechanisms and the localized electron distribution of each imaging mode. On one hand, LPTEM enables the quick control of the localized low electron flux homogeneously across the field of view. However, the appearance of diffraction contrast from the defects can be problematic for quantitative contrast interpretations. On the other hand, LPSTEM enables the better understanding of sample contrast evolution due to being less affected by diffraction effects. Simultaneously, however, the focused high flux electron probe might bring localized structural changes caused by radiolysis of the sample itself and water.

Figure 1 Hanglong article11

Figure 1: Desilication process of Al-zoned ZSM-5 crystals imaged by pulsed LP-STEM. Scale bars: 200 nm.

The LPSTEM results provide evidence that desilication proceeds by a sequential two-step process. Because the STEM probe scanning accelerates the etching process, this enabled the desilication process to be visualized with apparently “native” kinetics, thereby overcoming the confinement effects in the liquid cell. However, as beam effects were observed at all applied electron doses, the question remains: which features of the native desilication process are being captured?

Using cryo-EM and cryo-ET to observe the desilication process

Monitoring the desilication process using cryo-EM was the next step for Dr. Wu and his colleagues. Unlike LPEM, cryo-EM enabled the researchers to monitor the process in the absence of confinement and electron beam effects. In practice, cryo-TEM is generally performed prior to an in situ study, as it provides key information on what intermediate structures are present and, most importantly, how they evolve statistically over time. The figure below shows the cryo-EM results presented for crystals at different time points, where the stages of desilication are in agreement with the collective LPEM data and the general sample evolution observed by cryo-EM.

Figure 2 Hanglong article

Figure 2: Desilication process of ZSM-5 zeolites monitored by cryo-TEM (a) and cryo-STEM (b). Scale bars: 200 nm.

To verify the 3D interpretation of the desilication process, cryo-ET was performed on four crystals at an intermediate state of desilication. The movie below shows the cryo-ET reconstruction of a 12-hour desilicated zeolite crystal and Figure 3 shows the corresponding segmented surface rendering of the crystal.
Figure 3 Hanglong article

Figure 3: Segmented surface rendering of the 12 h desilicated zeolite crystal.

Movie 4: Movie showing the cryo-electron tomography 3D reconstruction of a 12 h desilicated zeolite crystal

Collectively, with the cryo-EM results, Dr. Wu and his colleagues were finally able to distinguish which information provided by LPEM observations represents the native desilication and which is an artifact. The cryo-EM data supported the hypothesis from both LPTEM and LPSTEM that desilication propagates along the c-axis. Moreover, it confirmed that it should occur in a two-step process, where both processes begin at the Al-rich/Si-rich interface and propagate toward the center of the crystal. This suggests that the LPTEM data either represents an artifact caused by the electron beam, confinement within the liquid cell, the sample preparation, or that the intermediates of this process are too transient to be captured by the cryo-EM data.

Novelty in findings

This study is a major step forward in understanding the role that the electron beam plays in LPEM experiments. Ultimately the collective results reveal that the desilication mechanism of zeolite crystals occurs via a two-step anisotropic etching process. This complex mechanism was only discovered due to the novel distributed approach that Dr. Wu and his colleagues employed. Particularly, the combination of LPEM and cryo-EM was essential to rule out the effects of the electron beam in the LPEM experiments.

Considering the strength of this distributed method, Dr. Wu and his colleagues anticipate that the combination of LPEM and cryo-EM will become a standard approach for understanding reaction mechanisms in aqueous solutions and could even be extended to non-aqueous solutions. Moreover this method will enable scientists to draw robust conclusions on the 3D reaction mechanisms of other important beam-sensitive material systems, such as biomaterials and proteins, whereby some grand challenges in materials science and life sciences could be potentially solved.

Hanglong Wu portrait
“DENSsolutions offers a simple but reliable solution for us to look into materials processes in liquid at the nanoscale. Currently, it is still difficult to observe the same phenomena in different liquid cells. That’s why people always joke that each LPEM experiment is “unique”. However, using the Ocean system, we have almost made every single “unique” LPEM experiment reproducible.”
Dr. Hanglong Wu
Postdoctoral Researcher |  Eindhoven University of Technology

Original article:

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Scientists present novel approaches to map and control liquid thickness in LPEM experiments

Using our Ocean system, scientists present new approaches to overcome the limitations in LPEM experiments by quantitatively mapping and controlling liquid layer thickness.

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Introducing our new DENSsolutions brand identity

Introducing our new DENSsolutions brand identity

Logo transition illustration
In a time where communication is evolving primarily online, the ability to adapt has never been more crucial. We recognize the importance of growth and modernization, especially within this high-tech industry, and have updated our brand identity to reflect just that. Part of this process entailed analyzing our core values as a company and how we can effectively address the needs of this dynamic world of research. This analysis resulted in the recognition of three core values that encapsulate the heart of our company: care, innovation and delivery.

We care

At the very core of all of our innovations, our technology and our solutions is that we care about your research. We want you to have the best possible equipment, be able to discover new phenomena and get unique yet reliable results that allow you to answer your scientific questions and publish in high impact journals.
This care goes beyond design and manufacture, we provide support whenever and wherever it is needed. We also aim to be the global hub for the In Situ research community, connecting you with peers all across the world.

HugoHugo with Angus Kirkland

CTO Hugo Pérez with University of Oxford Professor Angus Kirkland 

We innovate

With researchers constantly pushing the boundaries of knowledge, we make sure that our systems push the boundaries of innovation. This is at the heart of our second core value: we innovate. This way, you can rest assured that you are operating the best stimuli supply and measurement systems on the market, giving you the necessary tools to make groundbreaking discoveries. Whatever the application, from materials science to catalysis, you can ultimately create a sample environment almost identical to the real world.

DENS employee looking at a holder

Previous Mechatronics Engineer Diederik Morsink observing a holder in our offices

We deliver

We acknowledge how precious your time is and how crucial our cutting-edge technology is for your research. Through our worldwide distributor network, we strive to make sure that you receive your equipment in time. In efforts to adapt to the travel limitations of today, we have comprehensive remote installations and trainings for all of our solutions so that you can operate our systems with confidence, no matter where you are.

Magda with Climate cradle

Warehouse Supervisor Magda Wierzba handling Climate system delivery

We are delighted to be able to share our updated brand identity and the core values driving our company forward. Although our solutions are used to observe nanoscale phenomena, there is a huge amount of commitment, drive, and logistics involved behind the scenes. With our values of care, innovation and delivery at the forefront, DENSsolutions will continue to develop advanced in situ electron microscopy systems that promise reliability and accuracy every time.
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New measuring technique proves exceptional temperature accuracy of our Wildfire Nanochip

In collaboration with Utrecht University, we develop a novel technique to measure temperature at the nanoscale, showing the remarkable temperature accuracy and homogeneity of our Wildfire Nanochip

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New measuring technique proves exceptional temperature accuracy of our Wildfire Nanochip

New measuring technique proves exceptional temperature accuracy of our Wildfire Nanochip

In collaboration with Utrecht University, we develop a novel technique to measure temperature at the nanoscale, showing the remarkable temperature accuracy and homogeneity of our Wildfire Nanochip

Original article by Thomas P. van Swieten, Tijn van Omme, Dave J. van den Heuvel, Sander J.W. Vonk, Ronald G. Spruit, Florian Meirer, Hugo Pérez Garza , Bert M. Weckhuysen, Andries Meijerink, Freddy T. Rabouw and Robin G. Geitenbeek
Thomas article feature image

The temperature-sensitive luminescence of nanoparticles enables their application as remote thermometers. In fact, the size of these nanothermometers makes them ideal to map temperatures with a high spatial resolution. Yet, conducting high spatial resolution mapping of temperatures that exceed 100°C poses some challenges.

In collaboration with Thomas van Swieten and his fellow colleagues at Utrecht University, we were able to jointly develop a new technique to measure temperature at the nanoscale. In fact, we tested this novel technique on our Wildfire Nanochip and were able to further confirm the Nanochip’s unparalleled temperature accuracy and homogeneity. These experiments also proved how well our models work to predict the temperature distribution across the microheater. Importantly, this particular technique will improve the accuracy of nanothermometry as a whole, not only in micro- and nano-electronics but also in other fields with photonically inhomogeneous substrates.  

The technique: Luminescence nanothermometry

Thermometry on the microscopic scale is an essential characterization tool for the development of nano- and microelectronic devices. However, conventional thermometers like thermocouples are often unable to reliably measure the temperature on this length scale due to their size. This is precisely where remote temperature sensing via optical thermometry techniques comes into play. Thermometry based on luminescence is particularly interesting since it is easily implemented, requiring only the deposition of a luminescent material in or on a sample of interest and the detection of its luminescence. For this reason, luminescence nanothermometry is currently developing into the method of choice for temperature measurements in microscopy.

Homogeneous heat distribution

Our Wildfire Nanochip was specifically designed to enable users a homogeneous heat distribution across the microheater where a sample is positioned. It is particularly due to the unique geometry of the metal spiral, where the windows are placed right at the center, that users are able to enjoy such a remarkable temperature homogeneity. In fact, our Wildfire Nanochip has a temperature uniformity of 98% across the window area and 99.5% across the two central windows. The figure on the right below is a perfect illustration of the chip’s exceptional temperature homogeneity, showing the temperature profile across the membrane and the microheater for a center temperature of 523 K simulated with a finite element model.

The high temperature homogeneity of our Wildfire Nanochips is also owed to the fact that the metal heating spiral is embedded in a silicon nitride membrane. Silicon nitride has many advantages including being chemically inert, mechanically robust and can withstand harsh chemical and temperature environments. 

Tijn article - figure 2 wildfire nanochip homogeneous distribution

On the left: The Wildfire Nanochip, where the metal spiral is represented in orange and the silicon nitride membrane in blue. On the right: Finite element model simulation showing the remarkable temperature homogeneity of the Wildfire Nanochip

Reliable temperature mapping

In this work, the luminescent particles that were used are NaYF₄ nanoparticles doped with Er³⁺ and Yb³⁺. These particles exhibit a strong upconversion when excited with an infrared laser. In other words, they emit photons with a shorter wavelength than the excitation photons. As shown in the figure below, we found that the spectrum of the emitted (green) photons is quite sensitive to temperature.

Tijn article - Figure 1 Intensity vs Wavelength

Green upconversion luminescence of the nanoparticles upon excitation at various temperatures ranging from 303 K (dark red) to 573 K (yellow)

By scanning the laser across a layer of deposited nanoparticles in the confocal microscope, we were able to capture an array of emission spectra. We then converted this emission spectra into a temperature map using the luminescence intensity ratio of the 2 peaks at each pixel. After a number of correction steps, the technique showed a remarkable precision of 1-4 K with a spatial resolution of ∼1 micrometer. It is noteworthy to mention that most other techniques are unable to achieve such a high accuracy like this.

Tijn article - Figure 3 DESKTOP reliable temperature mapping

In a) we scanned the laser across the microheater with the deposited luminescent nanoparticles to generate a map of intensity ratios. b) shows the spectrum at each pixel converted into a temperature to provide a temperature map of the microheater.

Simulation and model accuracy

Using the fully corrected temperature maps, we were able to analyze in depth the temperature homogeneity of the microheater. The figure below shows the horizontal traces through the center of these maps. The simulated temperature profiles (lines) show an excellent match with the experimental traces (dots).This confirms both the reliability of the finite element model as a design tool and the strength of our temperature mapping technique as a characterization tool, achieving a high accuracy and a spatial resolution of ∼1 μm.

Tijn article - temperature mapping in graph

A graph showing the mapping of elevated temperatures. The lines represent the simulated temperature profiles and the experimental traces represent the dots.

We determine the standard deviation of the temperature in the center to quantify the accuracy of this thermometry method and find values of 1 K at 323 K increasing to only 4 K at 513 K. Conclusively, this makes nanothermometry using confocal luminescence spectroscopy a promising method to map temperature profiles not only for microheaters but also in other fields such as biology and catalysis where temperature variations are important but hard to monitor with conventional methods.
Tijn portrait image
“Thanks to the exceptionally good spatial and temperature resolution of this method, we were able to obtain an accurate temperature map of our microheater spiral. This confirmed the excellent temperature homogeneity which was predicted by our finite element models.”
Tijn van Omme
Microsystems Engineer |  DENSsolutions

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