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Title: Nanosecond Time Resolved Electron Diffraction Studies of the (Alpha) to (Beta) Transition in Pure Ti Thin Films using the Dynamic Transmission Electron Microscope (DTEM)

Abstract

The transient events of the {alpha}-{beta} martensitic transformation in nanocrystalline Ti films were explored via single shot electron diffraction patterns with 1.5 ns temporal resolution. The diffraction patterns were acquired with a newly constructed dynamic transmission electron microscope (DTEM), which combines nanosecond pulsed laser systems and pump-probe techniques with a conventional TEM. With the DTEM, the transient events of fundamental material processes, that are far too fast to be studied by conventional bulk techniques, can be captured in the form of electron diffraction patterns or images with nanosecond temporal resolution. The transient phenomena of the martensitic transformations in nanocrystalline Ti is ideally suited for study in the DTEM, with their rapid nucleation, characteristic interface velocities {approx}1 km/s, and significant irreversible microstructural changes. Free-standing 40-nm-thick Ti films were laser-heated at a rate of {approx}10{sup 10} 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 {beta} phase within 500 ns. Postmortem analysis (after the sample is allowed to cool) shows a reversion to the {alpha} phase coupled with substantial grain growth, lath formation, and texture modification. The cooled material alsomore » shows a complete lack of apparent dislocations, suggesting the possible importance of a ''massive'' short-range diffusion transformation mechanism.« less

Authors:
; ; ; ;
Publication Date:
Research Org.:
Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
883565
Report Number(s):
UCRL-CONF-217740
TRN: US200615%%135
DOE Contract Number:
W-7405-ENG-48
Resource Type:
Conference
Resource Relation:
Conference: Presented at: Frontiers of Electron Microscopy in Materials Science, Kastel Vaalsbroek, Netherlands, Sep 25 - Sep 30, 2005
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; DIFFRACTION; DIFFUSION; DISLOCATIONS; ELECTRON DIFFRACTION; ELECTRON MICROSCOPES; ELECTRON MICROSCOPY; ELECTRONS; GRAIN GROWTH; LASERS; NUCLEATION; RESOLUTION; TEXTURE; THIN FILMS; TRANSFORMATIONS; TRANSIENTS

Citation Formats

LaGrange, T, Campbell, G H, Colvin, J D, Reed, B, and King, W E. Nanosecond Time Resolved Electron Diffraction Studies of the (Alpha) to (Beta) Transition in Pure Ti Thin Films using the Dynamic Transmission Electron Microscope (DTEM). United States: N. p., 2005. Web.
LaGrange, T, Campbell, G H, Colvin, J D, Reed, B, & King, W E. Nanosecond Time Resolved Electron Diffraction Studies of the (Alpha) to (Beta) Transition in Pure Ti Thin Films using the Dynamic Transmission Electron Microscope (DTEM). United States.
LaGrange, T, Campbell, G H, Colvin, J D, Reed, B, and King, W E. Fri . "Nanosecond Time Resolved Electron Diffraction Studies of the (Alpha) to (Beta) Transition in Pure Ti Thin Films using the Dynamic Transmission Electron Microscope (DTEM)". United States. doi:. https://www.osti.gov/servlets/purl/883565.
@article{osti_883565,
title = {Nanosecond Time Resolved Electron Diffraction Studies of the (Alpha) to (Beta) Transition in Pure Ti Thin Films using the Dynamic Transmission Electron Microscope (DTEM)},
author = {LaGrange, T and Campbell, G H and Colvin, J D and Reed, B and King, W E},
abstractNote = {The transient events of the {alpha}-{beta} martensitic transformation in nanocrystalline Ti films were explored via single shot electron diffraction patterns with 1.5 ns temporal resolution. The diffraction patterns were acquired with a newly constructed dynamic transmission electron microscope (DTEM), which combines nanosecond pulsed laser systems and pump-probe techniques with a conventional TEM. With the DTEM, the transient events of fundamental material processes, that are far too fast to be studied by conventional bulk techniques, can be captured in the form of electron diffraction patterns or images with nanosecond temporal resolution. The transient phenomena of the martensitic transformations in nanocrystalline Ti is ideally suited for study in the DTEM, with their rapid nucleation, characteristic interface velocities {approx}1 km/s, and significant irreversible microstructural changes. Free-standing 40-nm-thick Ti films were laser-heated at a rate of {approx}10{sup 10} 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 {beta} phase within 500 ns. Postmortem analysis (after the sample is allowed to cool) shows a reversion to the {alpha} 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 transformation mechanism.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Fri Dec 09 00:00:00 EST 2005},
month = {Fri Dec 09 00:00:00 EST 2005}
}

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  • The {alpha} to {beta} transition in pure Ti occurs mainly by a 'martensitic type' phase transformation. In such transformations, growth rates and interface velocities tend to be very large, on the order of 10{sup 3} m/s, making it difficult to observe the transformation experimentally. With thin films, it becomes even more difficult to observe, since the large surface augments the nucleation and transformation rates to levels that require nanosecond temporal resolution for experimental observations. The elucidation of the transformational mechanisms in these materials yearns for an apparatus that has both high spatial and temporal resolution. We have constructed such anmore » instrument at LLNL (the dynamical transmission electron microscope or DTEM) that combines pulsed lasers systems and optical pump-probe techniques with a conventional TEM. We have used the DTEM to observe the transient events of the {alpha}-{beta} transformation in nanocrystalline Ti films via single shot diffraction patterns with 1.5 ns resolution. With pulsed, nanosecond laser irradiation (pump laser), the films were heated at an extreme rate of 10{sup 10} K/s. was observed At 500 ns after the initial pump laser hit, the HCP, alpha phase was almost completely transformed to the BCC, beta phase. Post-mortem investigations of the laser treated films revealed that substantial grain growth occurred and lath microstructure, containing no apparent dislocations. The lack of dislocations may indicate that the {alpha} to {beta} transformation may also proceed by a 'massive' type mechanism (short range diffusion).« less
  • The crystallization processes of the as-deposited, amorphous NiTi thin films have been studied in detail using techniques such as differential scanning calorimetry and, in-situ TEM. The kinetic data have been analyzed in terms of Johnson-Mehl-Avrami-Kolomogrov (JMAK) semi-empirical formula. The kinetic parameters determined from this analysis have been useful in defining process control parameters for tailoring microstructural features and shape memory properties. Due to the commercial push to shrink thin film-based devices, unique processing techniques have been developed using laser-based annealing to spatially control the microstructure evolution down to sub-micron levels. Nanosecond, pulse laser annealing is particularly attractive since it limitsmore » the amount of peripheral heating and unwanted microstructural changes to underlying or surrounding material. However, crystallization under pulsed laser irradiation can differ significantly from conventional thermal annealing, e.g., slow heating in a furnace. This is especially true for amorphous NiTi materials and relevant for shape memory thin film based microelectromechanical systems (MEMS) applications. There is little to no data on the crystallization kinetics of NiTi under pulsed laser irradiation, primarily due to the high crystallization rates intrinsic to high temperature annealing and the spatial and temporal resolution limits of standard techniques. However, with the high time and spatial resolution capabilities of the dynamic transmission electron microscope (DTEM) constructed at Lawrence Livermore National Laboratory, the rapid nucleation events occurring from pulsed laser irradiation can be directly observed and nucleation rates can be quantified. This paper briefly explains the DTEM approach and how it used to investigate the pulsed laser induced crystallization processes in NiTi and to determine kinetic parameters.« less
  • Spatially Resolved X-Ray Diffraction (SRXRD) is used to map the {alpha}{r_arrow}{beta}{r_arrow}{alpha} phase transformation in the heat affected zone (HAZ) of commercially pure titanium gas tungsten arc welds. In-situ SRXRD experiments were conducted on arc welds using a 200 pm diameter x-ray beam at Stanford Synchrotron Radiation Laboratory (SSRL). A map was created which identifies six HAZ microstructural regions that exist between the liquid weld pool and the base metal during welding. The first region is single phase {beta}-Ti that forms in a 2- to 3-mm band adjacent to the liquid weld pool. The second region is back transformed {alpha}-Ti thatmore » forms behind the portion of the HAZ where {beta}-Ti was once present at higher temperatures. The third region is completely recrystallized {alpha}-Ti that forms in a 2- to 3-mm band surrounding the single phase {beta}-Ti region. Recrystallized {alpha}-Ti was observed by itself and also with varying amounts of {beta}-Ti. The fourth region of the weld is the partially transformed zone where {alpha}-Ti and {beta}-Ti coexist during welding. The fifth region is directly behind the partially transformed zone and consists of a mixture of recrystallized and back transformed {alpha}-Ti The sixth region is farthest from the weld pool and consists of {alpha}-Ti that is undergoing annealing and recrystallization. Annealing of the base metal was observed to some degree in all of the SRXRD patterns, showing that annealing exceeded 13 mm from the centerline of the weld. Although the microstructure consisted predominantly of {alpha}-Ti, both prior to the weld and after the weld, the (002) texture of the starting material was altered during welding to produce a predominantly (101) texture within the resulting HAZ.« less