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The need to understand fast, complex physical phenomena through direct in
situ observation has spurred the development of
high-time-resolution transmission electron microscopy (TEM). Two complementary
approaches have emerged: the single-shot and stroboscopic techniques.
Single-shot TEM has advanced through the development of dynamic transmission
electron microscopy (DTEM) and, more recently, by the advent of movie-mode DTEM,
which enables high-frame-rate in situ TEM experimentation by
capturing nanosecond-scale sequences of images or diffraction patterns. Previous
DTEM studies produced only single snapshots of fast material processes.
Movie-mode DTEM provides the ability to track the creation, motion, and
interaction of individual defects, phase fronts, and chemical reaction fronts,
providing invaluable information on the chemical, microstructural, and
atomic-level features that govern rapid material processes. This article
discusses movie-mode DTEM technology, its application in the study of reaction
dynamics in Ti–B-based reactive nanolaminates, and future
The advent of aberration correction for transmission electron microscopy has transformed atomic resolution imaging into a nearly routine technique for structural analysis. Now an emerging frontier in electron microscopy is the development of in situ capabilities to observe reactions at atomic resolution in real time and within realistic environments. Here we present a new in situ gas cell holder that is designed for compatibility with a wide variety of sample type (i.e., dimpled 3-mm discs, standard mesh grids, various types of focused ion beam lamellae attached to half grids). Its capabilities include localized heating and precise control of the gas pressure and composition while simultaneously allowing atomic resolution imaging at ambient pressure. The results show that 0.25-nm lattice fringes are directly visible for nanoparticles imaged at ambient pressure with gas path lengths up to 20 μm. Additionally, we quantitatively demonstrate that while the attainable contrast and resolution decrease with increasing pressure and gas path length, resolutions better than 0.2 nm should be accessible at ambient pressure with gas path lengths less than the 15 μm utilized for these experiments.
The materials science community is poised to take advantage of new technologies that add unprecedented time resolution to already existing spatial-resolution capabilities. In the same way that chemists and biologists are using ultrafast optical, photon, and particle techniques to reveal transition pathways, materials scientists can expect to use variations of these methods to probe the most fundamental aspects of complex transient phenomena in materials. The combination of high-spatial-resolution imaging with high time resolution is critical because it enables the observation of specific phenomena that are important to developing fundamental understanding. Such a capability is also important because it enables experiments that are on the same time and length scales as recent high-performance computer simulations. This article describes several new techniques that have great potential for broader application in materials science, including electron, x-ray, and γ-ray imaging.
We have measured the transient events of the α-β martensitic transformation in nanocrystalline Ti films via single shot electron diffraction patterns with 1.5 ns temporal resolution. This was accomplished with a newly constructed dynamic transmission electron microscope (DTEM), which combines pulsed laser systems and pump-probe techniques with a conventional TEM. The DTEM thereby enables studies of transformations that are (1) far too fast to be captured by conventional bulk techniques, and (2) difficult to study with current ultrafast electron diffraction (UED) instruments (which typically require an accumulation of multiple shots for each diffraction pattern). Martensitic transformations in nanocrystalline materials meet both criteria, with their rapid nucleation, characteristic interface velocities ∼1 km/s, and significant irreversible microstructural changes. Free-standing 40-nm-thick Ti films were laser-heated at a rate of ∼1010 K/s to a temperature above the 1155 K transition point, then probed at various time intervals with a 1.5-ns-long intense electron pulse. Diffraction patterns show an almost complete transition to the β phase within 500 ns. Post-mortem analysis (after the sample is allowed to cool) shows a reversion to the α phase coupled with substantial grain growth, lath formation, and texture modification. The cooled material also shows a complete lack of apparent dislocations, suggesting the possible importance of a "massive" short-range diffusion mechanism.
The roughness scaling of fracture surfaces in two-dimensional grain boundary networks is stud- ied numerically. Grain boundary networks are created using a Metropolis method in order to mimic the triple junction distributions from experiments. Fracture surfaces through these grain boundary networks are predicted using a combinatorial optimization method of maximum flow — minimum cut type. We have preliminary results from system sizes up to N = 22500 grains suggesting that the roughness scaling of these surfaces follows a random elastic manifold scaling exponent ζ = 2/3. We propose a strong dependence between the energy needed to create a crack and the special boundary fraction. Also the special boundaries at the crack and elsewhere in the system can be tracked.
Two-dimensional (2D) cross sections through three-dimensional (3D) polycrystalline materials present a biased picture of the statistical properties of grain boundary networks. These properties are essential to many practical applications such as grain boundary engineering. We show a simple correction that will partly correct for the sampling biases by removing the effect of the correlation between grain boundary type and grain boundary area. This correction alters number fraction estimates by as much as ∼60% for σ3 boundaries in the highly-twinned copper samples we consider. We also estimate the bias introduced by the correlation between boundary type and boundary shape, which for many materials represents perhaps a 10% shift in the measured statistics, so that the simple method we propose should correct for the majority of the bias in favorable cases.
This document was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor the University of California nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or the University of California. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or the University of California, and shall not be used for advertising or product endorsement purposes.