skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Time Resolved Phase Transitions via Dynamic Transmission Electron Microscopy

Abstract

The Dynamic Transmission Electron Microscope (DTEM) project is developing an in situ electron microscope with nanometer- and nanosecond-scale resolution for the study of rapid laser-driven processes in materials. We report on the results obtained in a year-long LDRD-supported effort to develop DTEM techniques and results for phase transitions in molecular crystals, reactive multilayer foils, and melting and resolidification of bismuth. We report the first in situ TEM observation of the HMX {beta}-{delta} phase transformation in sub-{micro}m crystals, computational results suggesting the importance of voids and free surfaces in the HMX transformation kinetics, and the first electron diffraction patterns of intermediate states in fast multilayer foil reactions. This project developed techniques which are applicable to many materials systems and will continue to be employed within the larger DTEM effort.

Authors:
; ; ; ; ; ; ; ; ; ; ;
Publication Date:
Research Org.:
Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
902321
Report Number(s):
UCRL-TR-228336
TRN: US0702925
DOE Contract Number:
W-7405-ENG-48
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; 75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; 45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEFENSE; BISMUTH; ELECTRON DIFFRACTION; ELECTRON MICROSCOPES; KINETICS; MELTING; MOLECULAR CRYSTALS; PHASE TRANSFORMATIONS; RESOLUTION; TRANSFORMATIONS; TRANSMISSION ELECTRON MICROSCOPY

Citation Formats

Reed, B W, Armstrong, M R, Blobaum, K J, Browning, N D, Burnham, A K, Campbell, G H, Gee, R, Kim, J S, King, W E, Maiti, A, Piggott, W T, and Torralva, B R. Time Resolved Phase Transitions via Dynamic Transmission Electron Microscopy. United States: N. p., 2007. Web. doi:10.2172/902321.
Reed, B W, Armstrong, M R, Blobaum, K J, Browning, N D, Burnham, A K, Campbell, G H, Gee, R, Kim, J S, King, W E, Maiti, A, Piggott, W T, & Torralva, B R. Time Resolved Phase Transitions via Dynamic Transmission Electron Microscopy. United States. doi:10.2172/902321.
Reed, B W, Armstrong, M R, Blobaum, K J, Browning, N D, Burnham, A K, Campbell, G H, Gee, R, Kim, J S, King, W E, Maiti, A, Piggott, W T, and Torralva, B R. Thu . "Time Resolved Phase Transitions via Dynamic Transmission Electron Microscopy". United States. doi:10.2172/902321. https://www.osti.gov/servlets/purl/902321.
@article{osti_902321,
title = {Time Resolved Phase Transitions via Dynamic Transmission Electron Microscopy},
author = {Reed, B W and Armstrong, M R and Blobaum, K J and Browning, N D and Burnham, A K and Campbell, G H and Gee, R and Kim, J S and King, W E and Maiti, A and Piggott, W T and Torralva, B R},
abstractNote = {The Dynamic Transmission Electron Microscope (DTEM) project is developing an in situ electron microscope with nanometer- and nanosecond-scale resolution for the study of rapid laser-driven processes in materials. We report on the results obtained in a year-long LDRD-supported effort to develop DTEM techniques and results for phase transitions in molecular crystals, reactive multilayer foils, and melting and resolidification of bismuth. We report the first in situ TEM observation of the HMX {beta}-{delta} phase transformation in sub-{micro}m crystals, computational results suggesting the importance of voids and free surfaces in the HMX transformation kinetics, and the first electron diffraction patterns of intermediate states in fast multilayer foil reactions. This project developed techniques which are applicable to many materials systems and will continue to be employed within the larger DTEM effort.},
doi = {10.2172/902321},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Thu Feb 22 00:00:00 EST 2007},
month = {Thu Feb 22 00:00:00 EST 2007}
}

Technical Report:

Save / Share:
  • The fine-scale mineral matter in three US coals has been analyzed via scanning transmission electron microscopy (STEM). The samples observed were a North Dakota lignite, a Kentucky bituminous, and a Pennsylvania anthracite. Specific mineral types, differing among the three coals examined, appear to predominate at this fine size scale (particles less than or equal to 200nm in diameter). Fe-rich and Ba-rich minerals in the lignite, a Ti-rich mineral in the bituminous, and Ca-rich and Ti-rich minerals in the anthracite were the predominant species found. The inherent mineral content in the observed organic background also differs from coal to coal. Themore » distributions of mineral species in the size range less than or equal to 200nm reported herein do not reflect the distributions in the larger size ranges obtained by more macroscopic techniques.« less
  • This report summarizes a 2011 workshop that addressed the potential role of rapid, time-resolved electron microscopy measurements in accelerating the solution of important scientific and technical problems. A series of U.S. Department of Energy (DOE) and National Academy of Science workshops have highlighted the critical role advanced research tools play in addressing scientific challenges relevant to biology, sustainable energy, and technologies that will fuel economic development without degrading our environment. Among the specific capability needs for advancing science and technology are tools that extract more detailed information in realistic environments (in situ or operando) at extreme conditions (pressure and temperature)more » and as a function of time (dynamic and time-dependent). One of the DOE workshops, Future Science Needs and Opportunities for Electron Scattering: Next Generation Instrumentation and Beyond, specifically addressed the importance of electron-based characterization methods for a wide range of energy-relevant Grand Scientific Challenges. Boosted by the electron optical advancement in the last decade, a diversity of in situ capabilities already is available in many laboratories. The obvious remaining major capability gap in electron microscopy is in the ability to make these direct in situ observations over a broad spectrum of fast (µs) to ultrafast (picosecond [ps] and faster) temporal regimes. In an effort to address current capability gaps, EMSL, the Environmental Molecular Sciences Laboratory, organized an Ultrafast Electron Microscopy Workshop, held June 14-15, 2011, with the primary goal to identify the scientific needs that could be met by creating a facility capable of a strongly improved time resolution with integrated in situ capabilities. The workshop brought together more than 40 leading scientists involved in applying and/or advancing electron microscopy to address important scientific problems of relevance to DOE’s research mission. This workshop built on previous workshops and included three breakout sessions identifying scientific challenges in biology, biogeochemistry, catalysis, and materials science frontier areas of fundamental science that underpin energy and environmental science that would significantly benefit from ultrafast transmission electron microscopy (UTEM). In addition, the current status of time-resolved electron microscopy was examined, and the technologies that will enable future advances in spatio-temporal resolution were identified in a fourth breakout session.« less
  • We have examined alloys of composition SmTiFe{sub 11 {minus} x}Co{sub x} (x=0,8,11) and DyTiCo{sub 11} via transmission electron microscopy. Results indicate the sample without Co to be composed primarily of the body-centered tetragonal 1-12 phase with a small amount of alpha-Fe and Fe{sub 2}Ti present. With increasing Co content, the frequency of occurrence of the 2-17 phase increases. In Sm-containing samples, this phase is rhombohedral, while for Dy samples, the hexagonal phase was also found. Correspondingly, we observed an increase in the amount of transition metal-Ti solid solution as the Co concentration increases. In addition, there are orientation relationships betweenmore » the 1-12 and both 2-17 phases. This is consistent with a coordinate transformation matrix based on the 1-5 structure. Both the 1-12 and 2-17 phases were found to contain antiphase boundaries in annealed samples containing Sm. The 1-12 phase alone contained antiphase boundaries in the DyTiCo{sub 11} sample. These and other results are discussed.« less