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Title: IN-SITU CORRELATIVE ELECTRON AND X-RAY OPTICAL-ENVIRONMENTAL CELL SAMPLE HOLDER FOR ELECTROCHEMICAL IMAGING AND SPECTROSCOPY. FINAL TECHNICAL REPORT

Abstract

Purpose and application: 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 environment 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. Being able to perform correlative operando imaging/spectroscopy between TEM and X-ray microscopy provides complementary chemical characterization of the same processes. Additional fundamental insights into these chemical processes coming from this new technique will be crucial for accelerating the development of efficient reactions to create hydrogen gas for energy storage by splitting wafer, the study thermodynamically unfavorable reactions of synthesizing fuel by CO2 activation, ormore » the study in photovoltaic processes. The broader impact/commercial potential of this project was 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 large impact on the development of new energy technologies, like the development of new catalytic or photovoltaic materials. Description of Work Conducted and Results: In Phase I of this SBIR project we have fully developed and successfully tested a new environmental cell in-situ microscopy system with integrated optical probe and electrical contacts in the TEM and on an X-ray beamline, following and successfully completing the project objectives as we set out in our Phase I proposal. In Phase II, we further developed these TEM and X-ray microscope sample holder prototypes into sellable products and brought them to market. The main focus and product launch in the summer of 2019 in this project was on light application into the liquid-electrochemical environmental cell (http://hummingbirdscientific.com/products/optical-liquid/). These systems were made compatible with all TEM types and will be made so that they enable correlative microscopy and spectroscopy across TEM and X-ray microscopy platforms. We also designed a product configuration with both an optical input as well as an optical output, which will be part of a future generation product upgrade.« less

Authors:
Publication Date:
Research Org.:
Hummingbird Precision Machine Co.
Sponsoring Org.:
USDOE Office of Science (SC)
OSTI Identifier:
1616654
Report Number(s):
DOE-HPM-15213
3602522737
DOE Contract Number:  
SC0015213
Type / Phase:
SBIR (Phase II)
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
42 ENGINEERING; 36 MATERIALS SCIENCE

Citation Formats

Alsem, Daan Hein. IN-SITU CORRELATIVE ELECTRON AND X-RAY OPTICAL-ENVIRONMENTAL CELL SAMPLE HOLDER FOR ELECTROCHEMICAL IMAGING AND SPECTROSCOPY. FINAL TECHNICAL REPORT. United States: N. p., 2020. Web.
Alsem, Daan Hein. IN-SITU CORRELATIVE ELECTRON AND X-RAY OPTICAL-ENVIRONMENTAL CELL SAMPLE HOLDER FOR ELECTROCHEMICAL IMAGING AND SPECTROSCOPY. FINAL TECHNICAL REPORT. United States.
Alsem, Daan Hein. 2020. "IN-SITU CORRELATIVE ELECTRON AND X-RAY OPTICAL-ENVIRONMENTAL CELL SAMPLE HOLDER FOR ELECTROCHEMICAL IMAGING AND SPECTROSCOPY. FINAL TECHNICAL REPORT". United States.
@article{osti_1616654,
title = {IN-SITU CORRELATIVE ELECTRON AND X-RAY OPTICAL-ENVIRONMENTAL CELL SAMPLE HOLDER FOR ELECTROCHEMICAL IMAGING AND SPECTROSCOPY. FINAL TECHNICAL REPORT},
author = {Alsem, Daan Hein},
abstractNote = {Purpose and application: 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 environment 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. Being able to perform correlative operando imaging/spectroscopy between TEM and X-ray microscopy provides complementary chemical characterization of the same processes. Additional fundamental insights into these chemical processes coming from this new technique will be crucial for accelerating the development of efficient reactions to create hydrogen gas for energy storage by splitting wafer, the study thermodynamically unfavorable reactions of synthesizing fuel by CO2 activation, or the study in photovoltaic processes. The broader impact/commercial potential of this project was 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 large impact on the development of new energy technologies, like the development of new catalytic or photovoltaic materials. Description of Work Conducted and Results: In Phase I of this SBIR project we have fully developed and successfully tested a new environmental cell in-situ microscopy system with integrated optical probe and electrical contacts in the TEM and on an X-ray beamline, following and successfully completing the project objectives as we set out in our Phase I proposal. In Phase II, we further developed these TEM and X-ray microscope sample holder prototypes into sellable products and brought them to market. The main focus and product launch in the summer of 2019 in this project was on light application into the liquid-electrochemical environmental cell (http://hummingbirdscientific.com/products/optical-liquid/). These systems were made compatible with all TEM types and will be made so that they enable correlative microscopy and spectroscopy across TEM and X-ray microscopy platforms. We also designed a product configuration with both an optical input as well as an optical output, which will be part of a future generation product upgrade.},
doi = {},
url = {https://www.osti.gov/biblio/1616654}, journal = {},
number = ,
volume = ,
place = {United States},
year = {2020},
month = {4}
}

Technical Report:
This technical report may be released as soon as April 30, 2024
Other availability
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