The Next Generation of In Situ Electron Microscopy Capabilities

Interview conducted by Alexander ChiltonApr 7 2015

In this interview, Michael Zapata III, Executive Chairman at Protochips Inc, talks to AZoNano about the next generation of in situ electron microscopy.

Could you explain to our readers why situ analysis is important to electron microscopy researchers?

The electron microscope is the best instrument to allow scientists to observe reactions at the atomic or near atomic level in real time, but the requirement for vacuum makes preparation and observation of the sample in real-world conditions extremely difficult.

Heating, electrical stimulus, strain and other stimuli as well as simplistic liquid environments have evolved for many years, but they experience major limitations. These limitations have forced researchers to operate at the macro scale or at lower resolutions than the instrument is capable of.

This created a significant gap between the needs of the researchers and the capabilities of the existing technologies. Biological samples as an example required drying or the fixing of the sample for study in vacuum. Because of the limitations of the TEM the researcher was unable to study a living organism, like bacteria, at high resolution in real-time and in its native liquid operating environment.

Poseidon™ In Situ Liquid Cell: Gold Nanoparticles in Water

Currently in the areas of heating, liquid, electrochemistry and gas, MEMS devices provide the ability to have real-world conditions and retain atomic or near atomic resolution. Protochips and a small group of other companies have brought products to the market that allows nearly every researcher with a TEM or SEM to do in situ research in life and material science applications.

By leveraging the tools and techniques of semiconductor manufacturing and integrating them with complete hardware and software workflow based solutions, novel capabilities are integrated into all of our products.

We have created the world’s most advanced electron microscope in situ tools and enable the highest resolution of nanostructures in their native environments, thus closing the gap between the needs of scientists and available technological capabilities.

Has in situ become more than a niche area of research?

There has been a core group of scientists in each facet of in situ research, whether this is heating, liquid or gas, that has been performing experiments for many years. Most of this research has been at an academic level, which unfortunately has not met the majority of the market’s requirements.

Protochips looks for interesting market requirements in the in situ field and builds upon our core competencies to transform electron microscopes from simple cameras into complete nanoscale laboratories.

Our core competency is the application of semiconductor techniques to the development of MEMS devices capable of providing a real world environment to samples in situ, and incorporating that into hardware and software workflow solutions.

As a result of our drive to anticipate and meet researcher needs by providing innovative, user friendly, application-focused products, we have seen in situ research also become prevalent in the commercial sector, leading to more sophisticated and standardized in situ research. Technology capabilities and market requirements have now intersected and as a result the market is growing rapidly.

What are the latest advances for in situ products?

I would categorize recent changes by the benefits the users see. I believe there have been four significant advances:

First, ease of use has significantly increased in new in situ products. The ability to dynamically observe a sample while applying a stimulus is now well defined and the products make it easy and repeatable while allowing for a variety of experiments with a simple change of the consumable E-chip.

The next advance is in resolution. This is the first generation on in situ tools capable of frequent and repeatable resolutions at the atomic scale. This is due to the use of semiconductor MEMs devices for sample supports. I am very excited to see the impact this has had in the publication of research achieving nanostructure resolution in operating conditions for life and material science applications.

The third advance has been in the ability to capture quantitative data. Beautiful high resolution pictures are helpful, but when combined with analytical tools, they become impactful. The ability to gather quantifiable and actionable data will enable many new discoveries and elevate the value of the field of in situ research.

The final major area of advancement has been safety. Safety comes from a combination of design, complete system integration and procedures. We develop our products with a failure modes and effects base design safety philosophy. By controlling every aspect of the system from hardware design to consumables production to software controls we have been able to significantly advance the level of safety to the user and their equipment.

We have near 200 systems around the world and have now produced more than 600,000 semiconductor based consumables. Our products have been certified by the major electron microscope manufactures and can be used without violating the warranties of the manufacturers.

Is the technology ahead of the market?

It varies by product capability. A lot of the market still does not believe that many of the things that we are now doing every day can even be done.

If you are talking about heating, I think everyone understands that MEMS devices have opened up the world of atomic resolution at high temperature. Multiple companies offer these types of products.

We believe the performance advantages of our monolithic non-metallic heating system provides superior benefits, but there are also metal based solutions on the market that perform adequately for certain applications and reduced temperature ranges.

HAADF STEM image taken on a Cs corrected JEOL 2200FS. Conditions are 450 deg C and 10 mbar of N2 gas. This is a GaP/GaNAsP quantum well. GaP is the material on the top and bottom, and appears darker, GaNAsP is the material sandwiched in the center and appears lighter. This structure is used in quantum well lasers. Image Credit: Ranier Straubinger in the Kerstin Volz group at Philipps University Marburg.

With liquid, there is a segment of researchers that have already embraced it, but reservation or lack of awareness still exists in part of the market. Researchers have been taught for a long time that liquid and electron microscopes are not a good combination, so there are still some concerns to overcome with a few, but we have earned the trust of the manufactures and most of the market and are positive that those doubts will disappear soon.

With gas, scientists and engineers have understood the capabilities of environmental TEMs for years but have been limited by both their capabilities and the price. There is therefore a ready market in catalysis.

It is now about helping them understand the pressure and temperature levels that can be achieved by our Atmosphere product and in general getting the word out that such a product exists.

Electrochemistry is probably the product farthest ahead of its market. The issue is a gap between electrochemistry research and use of the electron microscope. A majority of electrochemists are not aware of today’s electron microscope capabilities and have never thought about doing research at the nanoscale because in the past, they couldn’t.

On the other hand, most electron microscopists are not very active in the electrochemistry field. As a result we only see a small set of innovative thought leaders that are both electrochemists and electron microscopists, who dominate the publications in the field. In my opinion, this market needs a little time before the two fields of research completely intersect, but then this market will catch up quickly.    

Is there risk to the electron microscope from using these products?

If the system is designed well and the procedures are followed correctly, there is virtually no risk of damaging the electron microscope. This said, a lot of researchers are still highly suspicious.

They have been taught for years that no foreign objects, especially if they are liquid or gas belong inside of the microscope. This concern emerged because unfortunately, there are some systems on the market that were not built with integrated safety by design approach.

This poses a threat to the whole market. It only takes a few of those poorly designed tools to damage some columns in order to give the whole industry a scare. It is however not always the tool.

Another danger is the few researchers out there who do not believe in following safety steps. They can also cause damage, but fortunately a well-designed system is able to limit the damage that can be caused by human error. We have designed for system level safety and have whenever possible placed controls to limit or eliminate the effect of human error.

Our systems have been reviewed and accepted by all the major electron microscope manufacturers and they are now selling our equipment directly. The number of our successfully installed systems in the market is further proof of our safety.

What is Protochips doing that is innovative in the market?

We have focused very heavily on innovations for the market, now having more than a dozen patents across three major regions of the world. Our most recent innovations that we have made public are around providing a full atmosphere of gas pressure inside the column and achieving sub-angstrom resolution while doing quantitative data gathering at temperatures of up to 1000 °C.

This is our Atmosphere product. One of the most innovative features of Atmosphere is the SmartTemp™ closed-loop control, which provides constant known temperatures with any gas species or pressure. Furthermore, the system is fully EDS and EELS compatible.

We also have been focusing on providing even higher accuracy to heating experiments in SEMs, TEMs and ETEMs with a closed loop mode in our Aduro systems. Our integrated SmartTemp precision temperature control is capable of adapting to changes in the environment in order to provide precise heating.

Aduro™ In Situ Heating and Electrical Holder: Ceria in a High Resolution Environmental TEM

By using a flat ceramic membrane as both sample support and heating element we eliminate the furnace used by typical bulk-type heating holders, allowing us more precise heating without sample interaction.

In the liquid area we have continued to push up resolution while also achieving higher and higher quality electrochemistry results. It is now possible to achieve high-resolution TEM and STEM imaging while flowing and conducting measurements.

Finally, and probably the most important innovations have been around incorporating workflow and safety innovations into all the products.  We develop instruments that can be used across many science and engineering disciplines by improving the applications specific workflows resulting in a higher ROI or utilization for the researcher.

What are the next obstacles for in situ research?

One area where we still see the market experiencing difficulties is in sample preparation. This manifests in either poor performance in the experiment or inconsistency with the data. We are therefore researching ways to make sample prep as easy as we have made operating the systems with the use of application workflows.

Another obstacle that in situ research faces is the integration of other analytical tools. The electron beam can product beautiful images, but we must use other tools in conjunction to detect what kind of sample we are looking at or to gather other analytical data. We are working to expand the breath of analytical tools that we can work with while still maintaining image quality and system safety.

I also see room for improvement in the correlative use of all the instruments available in the lab. This can be a combined use of optical and electron microscopes as well as the use of spectroscopy. Having results from one instrument is not enough; the data has to be analyzed on a multidimensional level with all the tools available.

Where do you see the market going in the future?

The time of just having pretty pictures of samples at atomic resolution is over. The emphasis is shifting towards more credible data and a lean and efficient workflow. The new challenge of in situ experimentation is to closely mimic all conditions that a sample normally experiences so that the data from the experiment represents true sample behavior.

A transformation of the TEM into both a reaction chamber and an imaging and analysis tool is taking place, accelerating the creation of actionable data. Hand in hand will be the development of controlled workflows, automation and safety monitoring.

We are excited to be part of this development and I am certain that the in situ market will continue to grow rapidly resulting in amazing new achievements in the materials and life sciences.

About Michael Zapata III

Michael Zapata III is the Executive Chairman of Protochips. He is an entrepreneur and angel investor focused on technology based businesses. He works with universities, national labs and corporations to bring new technology to market.

Michael was the founding Director of the Technology Entrepreneurship and Commercialization Program at NC State University and the Associate Director of the Kenan Institute for Engineering, Technology and Science.

His current positions included Entrepreneur-in-Residence at NC State and Executive Chairman of ArrayXpress, a next generation genomics company and he is appointed to the US Commerce Export Council.

He is also a retired US Army Lieutenant Colonel and Combat Aviation Officer and a current commercial pilot and adventure sports enthusiast.