Entity

Time filter

Source Type

Olympia, WA, United States

Grant
Agency: National Science Foundation | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 150.00K | Year: 2011

This Small Business Innovation Research Phase I project will develop a microfluidic in-situ Transmission Electron Microscope (TEM) specimen holder with accurate temperature and pressure measurement and control abilities. The inability to dynamically image materials at atomic resolutions in changing liquid and gas environments is a significant impediment to the advance of physical, chemical, materials, biological and medical sciences. We have recently developed commercially viable continuous flow fluid sample holders for observations of interactions of materials in both liquid and gas environments at ambient pressures. These holders have already opened up new avenues of research in material reactions through real time observation and imaging of nanoscale material interactions. However, currently none of the results acquired with these systems can be quantified or verified because it is not possible in the current system to directly locally measure temperature and pressure in the microfluidic cell at the sample. This project will solve this problem by developing a new in-situ TEM microfluidic holder that contains microfabricated local temperature and pressure sensors inside the fluid cell. This will be a crucial enabling technique in opening up the possibilities of in-situ experiments while imaging at high resolution in fluids inside the TEM. The broader impact/commercial potential of this project is the availability of a characterization technique that can image solid/liquid and solid/gas interfaces with atomic resolution under quantifiable and accurately controllable environmental conditions. This product has the potential to becoming a high-impact in-situ TEM holder product, because it has a broad range of important applications over several scientific and engineering fields. It will allow biological structures to be imaged at nanometer resolution in their controlled native environment and provide new insight on structure-function relationships in biological systems. In materials science and chemistry it will provide new insight into the growth and synthesis of nanostructures under controlled atmospheric conditions, which is important for future generations of electronic devices. Finally, it will create insights for researchers studying catalysis under relevant and controlled environmental conditions, as well as new understanding of the fundamental processes in corrosion.


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 150.00K | Year: 2011

Researchers are currently hindered from 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, 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 proposal focuses on developing a TEM specimen holder, where specimen is exposed to various gas atmospheres at different temperatures. Such device enables in-situ TEM studies of catalysts and sensors among many other materials of interest. Electron microscopy is the primary tool available for characterizing the internal structure of materials at the nanometer to sub-Angstrom lengths scales. Dynamic in-situ experiments are finding increasing use as direct methods to explore the relationships among materials processing methods, microstructure and functional properties (e.g. catalytic, sensing).Commercial Applications and Other Benefits: Commercial availability of variable temperature gas TEM holder will facilitate academic research in the field of gas catalysis. It also provides 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 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.

Discover hidden collaborations