DEVELOPMENT OF AN IN-SITU ENVIRONMENTAL FLUID CELL ELECTRICAL BIASING AND HEATING PLATFORM FOR SYNCHROTRON X-RAY MICROSCOPY. FINAL TECHNICAL REPORT
Purpose and application: Observing solid-liquid and solid-gas interfaces with high resolution are important for the comprehension of physical, chemical, and biological interactions between material and liquids/gasses. Previously, a few liquid stages at synchrotrons have been home-built in an attempt to achieve this 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. Gas-cell stages have been mostly elusive on vacuum X-ray beamlines but would suffer from similar challenges. Failures of these home-built environmental cells make experiments extremely challenging to carry out and, in some cases, endanger surrounding equipment. Key application fields here were electrochemistry, and specifically battery materials research, as well as catalysis research. The products developed in this SBIR project aim at researchers at X-ray synchrotron beamlines and transmission electron microscopy (TEM) user facilities worldwide using a wide range of microscopy/spectroscopy techniques for characterizing the structure and chemistry of materials and who are interested in liquid-electrochemical and gas-catalysis operando experiments. The commercial availability of these characterization tools facilitates and accelerates academic research and next-generation catalyst material development for energy processes, fields that have and are seeing great support by DOE. Description of Work Conducted and Results: In Phase I of the work, we have successfully created a working prototype of an in-situ X-Ray liquid cell holder and implemented and successfully tested it on a beamline at ANL’s APS. In Phase II, we have further developed this liquid-cell prototype to included liquid-electrochemistry and sample heating capabilities and developed this X-ray liquid-cell sample holder platform into a correlative product with transmission electron microscopy (TEM). We are currently selling these tools for any X-ray beamline and/or TEM as standard products (product website: http://hummingbirdscientific.com/products/x-ray-liquid/). As part of this productization, product launch, and sales, we have installed liquid systems on multiple beamlines at US national labs. We have seen growing interest from potential customers at beamlines in Europe and Asia, too, as we installed our first systems outside of the US. These products have brought with it a change in paradigm as to what experiments could be performed operando at high resolution in the XRM in liquid environments. The requirements to perform high-temperature catalysis research experiments in an environmental cell are completely different from performing experiments in a liquid cell. Therefore, in Phase IIB, we specifically develop a gas-environmental cell X-ray platform. This system has the ability to heat the sample to above 1000°C and have gas pressure control in the cell. The system was developed as a correlative system between different microscopy platforms (e.g., OM, SEM, TEM). By expanding the application field of environmental-cell X-ray systems from liquid environments only to include gas environments roughly doubled the number of scientists who we are selling these tools to now. We also developed the correlative liquid-cell transmission electron microscope (TEM) and X-ray Microscope (XRM) product into a version that can, for the first time, mimic true bulk electrochemical and have launched this as a product (http://hummingbirdscientific.com/products/liquid-electrochemistry/).
- Research Organization:
- Hummingbird Precision Machine Co., Lacey, WA (United States)
- Sponsoring Organization:
- USDOE Office of Science (SC)
- DOE Contract Number:
- SC0009573
- OSTI ID:
- 1616616
- Type / Phase:
- SBIR (Phase IIB)
- Report Number(s):
- DOE-HPM-09573
- Country of Publication:
- United States
- Language:
- English
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