Olympia, WA, United States

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Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase II | Award Amount: 1.00M | Year: 2012

Researchers are currently hindered when observing dynamic gas-solid interactions in the transmission electron microscope (TEM). Yet solid-state materials and gases interact in many important ways. The most critical technological application for these observations is catalysis, where one would like to directly observe on the atomic scale how catalysts respond to the environment while they are active. Several areas of research, such as catalysis and sensors, will greatly benefit from having access to such observations. The importance of catalytic studies for science and technology was highlighted by two Nobel Prizes in chemistry for catalytic studies (Ertl, 2007 and Suzuki, Heck, Nigishi, 2010) awarded in the past five years. This Phase II proposal focuses on developing and bringing to market a TEM specimen holder where the specimen is exposed to various gas atmospheres with a wide range of pressures at different temperatures with full operando quantitative measuring capabilities. Such a device would enable in-situ TEM studies of catalysts and sensors, among many other materials of interest. In Phase I of the work we have successfully created a working prototype of the in-situ TEM gas holder and supporting hardware. Commercial Applications and Other Benefits: This product will be aimed at researchers using electron microscopy for characterizing the internal structure of materials at the nanometer to sub-Angstrom lengths scales and who are interested in dynamic in-situ experiments. These experiments are finding increasing use as direct methods to explore the relationships among materials processing methods and microstructure and functional properties (e.g. catalytic and sensing). The commercial availability of a variable temperature gas TEM holder will facilitate and accelerate academic research in the field of gas catalysis. It will also provide a platform to study active elements of sensors during operation with relevant resolution (atomic length scale).


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 150.00K | Year: 2012

Understanding the microstructural origins of the mechanical behavior of materials has always been a core area of mechanical engineering and materials science. Renewed importance has been placed on mechanical behavior studies because the length scales of electronic and mechanical structures have decreased to nano-scale dimensions and are promising new generations of energy efficient nano-scale electrical and mechanical devices. Despite this importance, our understanding of the microstructural origins of mechanical behavior of relevant materials at these length scales lags behind the development of new device prototypes. Utilizing special electron microscope specimen stages and microelectrical mechanical systems (MEMS) will enable in-situ testing of the mechanical behavior of materials at nanometer length scales inside the scanning and transmission electron microscopes (SEM/TEM) and enable dynamic determination of the effects of materials processing on structure and mechanical behavior. This will provide critical insight into designing new nano-scale devices with improved properties and performance. We will specifically develop two in-situ electron microscopy specimen holders that will enable the use of MEMS devices to test mechanical behavior of nano-scale materials in both the scanning and transmission electron microscopes. Whereas the double-tilt TEM platform is aimed at specifically relating microstructure and measured mechanical behavior, the SEM platform is aimed to provide additional correlative information of the material surface changes as well as act as the platform for sample preparation, which is a crucial step in these experiments. In addition to this, the SEM holder is more suited to acquiring statistically relevant amounts of data, because of the higher through-put and the direct access to sample preparation tools in SEM/ dual beam focus ion beam (FIB) systems.


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 150.00K | Year: 2013

Observing solid-liquid interfaces with high resolution is important for comprehension of physical, chemical and biological interactions between material and fluid. A more detailed knowledge of these interactions can substantially improve our understanding of the processes that occur during operation of catalysts and degradation of materials inside battery, as well as the operation of biological systems. Currently, a few liquid stages at synchrotrons have been home- built and suffer from leaks, are extremely cumbersome to use and do not provide any additional capabilities such as electrical biasing and heating of the sample. Failures of these liquid cells make experiments extremely challenging to carry out and in some cases endanger surrounding equipment. Our approach will be to develop a continuous flow environmental cell specifically for X-ray microscopes that will allow operation of the sample in liquid and gas at a wide range of pressures. Dynamic in-situ experiments are finding increasing use as direct methods to explore the relationships among materials processing methods, microstructure and functional properties. X-ray microscopy can provide information about changes in chemical structure of materials with high spatial resolution during dynamic in-situ experiments. Many processes such as degradation of materials, charging/discharging of batteries, operation of cells/bacteria can be studied with X-ray microscopy and are of a great importance to academic as well as industrial research. The proposed platform provides a tool to study such changes in the chemical structure of materials.


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 150.00K | Year: 2013

This SBIR Phase I project will develop a microfluidic in-situ TEM specimen holder with accurate environmental parameter monitoring capabilities; The inability to dynamically image materials at atomic resolutions in changing liquid environments is a significant impediment to the advancement of physical, chemical, materials, biological and medical sciences. Currently, none of the results acquired with Hummingbirds continuous flow fluid sample holders can be quantified or verified because it is not possible in the current system to directly locally measure the environmental parameters in the microfluidic cell; specifically temperature and pH. This proposal will aim to completely solve the environmental parameter measurement and control issues by developing a new in-situ TEM microfluidic holder that contains an integrated microfabricated local temperature sensor and a pH sensor. This will be a crucial enabling technique for opening up the possibilities of in-situ experiments in liquids where for electrochemical processes the local (change in) concentration of acids and bases at the sample are key reaction parameters. The broader impact/commercial potential of this project is the availability of a characterization technique that can image solid/liquid interfaces up to atomic resolution under quantifiable and accurately controllable environmental conditions. This will provide new insights into the process controlling assembly and, ultimately, function in biological systems and biomolecular materials. The interface between macromolecular and inorganic components is a hallmark of these materials. In many cases, the organic side of the interface plays an active role in directing the formation and organization of the inorganic materials. In others, the inorganic component is the substrate that modulates macromolecular assembly. Our understanding of either case is limited because, until recently, we lacked an experimental tool possessing both the spatial and temporal resolution needed to capture the formative events. While in situ TEM has emerged as an enabling capability in this regard, to develop a predictive understanding that can impact biomedical and materials technologies, we require an environment in which temperature and pH are tightly controlled. This new window into biomolecular materials promises dramatic advances in our understanding of the underlying thermodynamic and kinetic factors that lead to self-organization of macromolecules and that drive formation of inorganic nanostructures at the macromolecular-inorganic interface.


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase II | Award Amount: 994.30K | Year: 2013

The inability to dynamically image solid-state materials at atomic resolutions and perform spectroscopy at the same time in changing liquid and gas environments is a significant impediment to the advance of multiple areas of science. Recently Hummingbird Scientific has developed commercially viable in-situ continuous flow liquid and atmospheric pressure gas transmission electron microscope (TEM) sample holders for observations of interactions of materials in fluid environments. These holders have already opened up new avenues of research in material reactions through real time observation and imaging of nano-scale material interactions. However, these systems do not allow the full potential of the TEM to be used, as they currently do not allow routine spectroscopic analysis to occur in the TEM. The electron cross-section of the liquid/gas cell is limiting the use of electron energy loss spectroscopy (EELS) and energy filtered TEM (EFTEM) and the geometric constraints on being able to seal the liquid and gas cells have also inhibited the use of energy dispersive x-ray spectroscopy (EDS). This project will fully develop and bring to market new liquid and gas cell in-situ TEM holders that are specifically designed to allow spectroscopic analysis (EELS, EFTEM, and EDS) to occur while imaging materials in fluid environments at high resolution. In Phase I we have successfully built and tested prototypes of these systems. This will be a crucial technique in opening up the possibilities of in-situ fluidic research inside the TEM. Commercial Applications and Other Benefits: The broader impact/commercial potential of this project will be the availability of a characterization technique that can image solid/liquid and solid/gas interfaces up to atomic resolutions while at the same time performing spectroscopic elemental analysis. This technique has a broad range of impact over several scientific and engineering fields. It will allow biological structures to be imaged at nanometer resolutions in the native environment and will provide new insight on the structure-function relation in biological systems. In materials science and chemistry, it will provide new insight into the growth and synthesis of nano-structures, which are important for future generations of electronic devices. Finally, it will create insights for catalysis research under relevant environmental conditions, as well as offer a new understanding of the fundamental processes in corrosion.


Grant
Agency: Department of Health and Human Services | Branch: | Program: SBIR | Phase: Phase II | Award Amount: 984.28K | Year: 2012

DESCRIPTION (provided by applicant): At the frontier of biological electron microscopy, there is a strong emphasis on imaging the 3-D structure of cells, organelles, and macromolecules in their native state. This is facilitated by the use of frozen-hydrated specimens which have not been subjected to chemical fixation, dehydration or stains. The resolution is currently limited to about 4 nm by electron irradiation damage. The use of in-focus phase contrast imaging in the transmission electron microscope(TEM) - accomplished by incorporating a phase plate in the back focal plane of the objective lens - can increase resolution in electron tomography, and also increase throughput. Although these improvements have recently been confirmed by preliminary experiments, and the benefits of phase plates have been known for decades, technical difficulties have always inhibited their use. The three main difficulties are: keeping the phase plate centered on the electron optical axis, avoiding contamination and allowingeasy phase plate replacement in the microscope. In Phase I we have developed and tested a working prototype of a phase plate holder with precision positioning system, a heater and an electrical feed-through for use with electrostatic phase plates. Exchanging the original objective aperture holder of the TEM with the phase plate holder allows nearly any cryo-EM to be equipped with a phase plate. The cost of this holder is substantially lower than any other technology that can yield a similar improvement inimaging of frozen- hydrated specimens. In Phase II we will refine this concept into a commercial product and add auto-centering software as well as a load-lock to the holder, allowing replacement of the phase plates without breaking the vacuum in the microscope column. This latter addition will eliminate the need to break the vacuum to insert the phase plate, and makes this product into a complete solution to all technical issues that have traditionally prevented scientists from more routinely using this characterization technique. PUBLIC HEALTH RELEVANCE: Phase plate holder for transmission electron microscopy Relevance The phase plate holder that will be developed and commercialized in this project allows routine transmission electron microscopy characterization of biological structures at unprecedented resolution and contrast levels. The routine use of phase plates will allow the acquisition of levels of details in 3D tomographic images of non-crystalline materials to increase by a large leap. This TEM imaging ability is used to gain a comprehensive understanding of cellular structures and allows direct correlation between structure and function.


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase II | Award Amount: 1.00M | Year: 2014

Observing solid-liquid interfaces with high resolution is important for comprehension of physical, chemical, and biological interactions between material and fluid. A more detailed knowledge of these interactions can substantially improve our understanding of the processes that occur during operation of catalysts and degradation of materials inside battery, as well as the operation of biological systems. Currently, a few liquid stages at synchrotrons have been home-built and suffer from leaks, are extremely cumbersome to use and do not provide any additional capabilities such as electrical biasing and heating of the sample. Failures of these liquid cells make experiments extremely challenging to carry out and in some cases endanger surrounding equipment. Our approach in this project will be to develop a continuous flow environmental cell specifically for X-ray microscopes that will allow operation of the sample in liquid and gas at a wide range of pressures and with on-chip electrical and heating capabilities. In Phase I we developed and successfully tested a prototype of the environmental cell and integrated it in a synchrotron X-Ray microscope. In Phase II we will develop this system to a production ready package that includes an integrated 3-axis holder motion stage and electrical biasing and heating capabilities of the sample, providing a wide range of in-situ abilities. Dynamic in-situ experiments are finding increasing use as direct methods to explore the relationships among materials processing methods, microstructure, and functional properties. X-ray microscopy can provide information about changes in chemical structure of materials with high spatial resolution during dynamic in- situ experiments. Many processes such as degradation of materials, charging/discharging of batteries, operation of cells/bacteria can be studied with X-ray microscopy and are of a great importance to academic as well as industrial research. The proposed platform provides a tool to study such changes in the chemical structure of materials.


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase II | Award Amount: 1.00M | Year: 2014

The inability to dynamically image materials at atomic resolution in changing liquid environments is a significant impediment to the advancement of physical, chemical, biological, medical, and material sciences. Hummingbird Scientific, via its liquid cell holders, has greatly enhanced the ability of researchers to obtain transmission electron micrographs of materials at atomic resolution while in liquid environments. However, no product currently on the market allows the TEM data to be correlated with other environmental parameters directly measured in microfluidic cell. This proposal will aim to resolve environmental parameter measurement and control issues. These goals will be accomplished by developing and bringing to market a new in-situ TEM microfluidic holder that contains an integrated, microfabricated pH sensor and temperature sensor in addition to a heating element. This new tool will allow researchers to measure and control environmental parameters at the sample directly and will be a crucial enabling technique for opening up the possibilities of in-situ experiments in liquids where for electrochemical processes the local (change in) concentration of acids and bases at the sample are key reaction parameters. The phase I project successfully developed a working prototype of a microfluidic TEM specimen holder with integrated pH and temperature measuring capabilities. In phase II of this project, we will integrate the sensor into a single device, allowing simultaneous pH and temperature measurement, as well as temperature control. This will be integrated with control hardware and software to make a turn-key system. The broader impact/commercial potential of this project is the availability of a characterization technique that can image solid/liquid interfaces up to atomic resolution under quantifiable and accurately controllable environmental conditions. This will provide new insights into the process controlling assembly and, ultimately, function in biological systems and biomolecular material as well as insights into material microstructural changes during active electrochemical processes. Our understanding of either case is limited because, until recently, we lacked an experimental tool possessing both the spatial and temporal resolution needed to capture the formative events. While in situ TEM has emerged as an enabling capability in this regard, to develop a predictive understanding that can impact biomedical and materials technologies, we require an environment in which temperature is tightly controlled and pH is measured. This new window into these materials promises dramatic advances in our understanding of the underlying kinetic factors that control material behavior, leading to more targeted development of new materials.


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase II | Award Amount: 1.00M | Year: 2011

The primary experimental method used to determine the local internal structure of materials is that of transmission electron microscopy (TEM). If one also subjects the sample to an excursion in temperature during imaging at high resolution, one can watch the material processes involved in structural transformations. This allows direct and dynamic determination of the effects of materials processing on structure, and thus can provide critical insights to designing new materials with improved properties and performance. This approach not only permits deeper understanding of the basic physical processes involved, but also allows rapid exploration of a matrix of conditions and effects. However, current TEM heating holder designs that can accommodate a wide variety of specimens relies on substantially out-dated technologies, yielding significant problems with respect to drift / stability issues, expensive and time consuming maintenance and lack of precise and simple temperature control. Our motivation with this SBIR funded project is to develop a dramatically improved heating holder that is capable of delivering high-temperatures (1000C) to a sample, which is robust and as its most important feature has virtually no sample drift when the temperature of the sample is changed. In Phase I we build a prototype as proof of concept of the low drift mechanism. In Phase II we will optimize this prototype into a commercial product and make a double tilt version of the holder suited for all types of TEMs. This ultra-low drift TEM heating holder is expected to greatly aid researchers in exploiting hot-stage TEM, particularly during experiments that require imaging while increasing the temperature of the specimen, and are expected to lead to scientific advancements across multiple areas of research relevant to the DOE BES mission.


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 150.00K | Year: 2016

The inability to dynamically imaging (electro)chemical processes at molecular/atomic resolutions and performing spectroscopy at the same time in changing liquid and gas environments has traditionally been a significant shortcoming of both transmission electron microscopy (TEM) and high resolution X-ray characterization. This lack of real-world environmental conditions around the sample has limited the usefulness of in-situ TEM and X-ray microscopy/spectroscopy to advancing multiple areas of science. Hummingbird Scientific has previously developed commercially viable in-situ liquid and atmospheric pressure gas electron and X-ray microscope sample holders for observations of interactions of materials in fluid environments. Having the combined ability to simultaneously optically and electrically probe chemical processes in a liquid or gas environmental inside the TEM and X-ray microscope, while imaging at high magnification, allows for multi-probe energy materials studies of, for example, photocatalytic chemical reactions that is highly desirable but presently lacking. Being able to perform correlative imaging/spectroscopy between TEM and X-ray microscopy provides complementary chemical characterization of the same processes so these measurements can be overlaid. Additional fundamental insights into these chemical processes coming from this new technique will be crucial for efficient reactions to create hydrogen gas for energy storage by splitting wafer, to study thermodynamically unfavorable reactions of synthesizing fuel by CO2 activation, or to study photovoltaic processes. This project will fully develop a new environmental cell in-situ microscopy system with integrated electrical contacts and built-in optical probe for in-situ studies of, for example, photocatalytic materials. The system can also perform correlative microscopy and spectroscopy across TEM and X-ray microscopy platforms. The broader impact/commercial potential of this project will be the availability of a chemical characterization technique that can image and perform spectroscopy on solid/liquid and solid/gas interfaces up to atomic resolutions while at the same time optically probe the material. This technique has a broad range of impact over several scientific and engineering fields, with large impact in new energy technologies, like development of new catalytic or photovoltaic materials. Catalysts are crucial in accelerating many important industrial reactions that would otherwise be extremely slow or inefficient. This proposal focuses on the development of a tool that will allow high resolution electron microscopy images of photocatalytic processes to be captured. The results will allow scientists to design more efficient catalytic materials.

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