scholarly journals Direct Characterization of the Relation between the Mechanical Response and Microstructure Evolution in Aluminum by Transmission Electron Microscopy In Situ Straining

Materials ◽  
2021 ◽  
Vol 14 (6) ◽  
pp. 1431
Author(s):  
Seiichiro Ii ◽  
Takero Enami ◽  
Takahito Ohmura ◽  
Sadahiro Tsurekawa

Transmission electron microscopy in situ straining experiments of Al single crystals with different initial lattice defect densities have been performed. The as-focused ion beam (FIB)-processed pillar sample contained a high density of prismatic dislocation loops with the <111> Burgers vector, while the post-annealed specimen had an almost defect-free microstructure. In both specimens, plastic deformation occurred with repetitive stress drops (∆σ). The stress drops were accompanied by certain dislocation motions, suggesting the dislocation avalanche phenomenon. ∆σ for the as-FIB Al pillar sample was smaller than that for the post-annealed Al sample. This can be considered to be because of the interaction of gliding dislocations with immobile prismatic dislocation loops introduced by the FIB. The reloading process after stress reduction was dominated by elastic behavior because the slope of the load–displacement curve for reloading was close to the Young’s modulus of Al. Microplasticity was observed during the load-recovery process, suggesting that microyielding and a dislocation avalanche repeatedly occurred, leading to intermittent plasticity as an elementary step of macroplastic deformation.

2016 ◽  
Vol 22 (6) ◽  
pp. 1350-1359 ◽  
Author(s):  
Xiang Li Zhong ◽  
Sibylle Schilling ◽  
Nestor J. Zaluzec ◽  
M. Grace Burke

AbstractIn recent years, an increasing number of studies utilizing in situ liquid and/or gaseous cell scanning/transmission electron microscopy (S/TEM) have been reported. Because of the difficulty in the preparation of suitable specimens, these environmental S/TEM studies have been generally limited to studies of nanoscale structured materials such as nanoparticles, nanowires, or sputtered thin films. In this paper, we present two methodologies which have been developed to facilitate the preparation of electron-transparent samples from conventional bulk metals and alloys for in situ liquid/gaseous cell S/TEM experiments. These methods take advantage of combining sequential electrochemical jet polishing followed by focused ion beam extraction techniques to create large electron-transparent areas for site-specific observation. As an example, we illustrate the application of this methodology for the preparation of in situ specimens from a cold-rolled Type 304 austenitic stainless steel sample, which was subsequently examined in both 1 atm of air as well as fully immersed in a H2O environment in the S/TEM followed by hyperspectral imaging. These preparation techniques can be successfully applied as a general procedure for a wide range of metals and alloys, and are suitable for a variety of in situ analytical S/TEM studies in both aqueous and gaseous environments.


MRS Advances ◽  
2016 ◽  
Vol 1 (42) ◽  
pp. 2893-2899 ◽  
Author(s):  
R.W. Harrison ◽  
H. Amari ◽  
G. Greaves ◽  
J.A. Hinks ◽  
S.E. Donnelly

AbstractIn-situ ion irradiation and transmission electron microscopy has been used to examine the effects of the He appm to DPA ratio, temperature and dose on the damage structure of tungsten (W). Irradiations were performed with 15 or 60 keV He+ ions, achieving He-appm/displacements per atom (DPA) ratios of ∼40,000 and ∼2000, respectively, at temperatures between 500 and 1000°C to a dose of ∼3 DPA. A high number of small dislocation loops with sizes around 5–20 nm and a He bubble lattice were observed for both He-appm/DPA ratios at 500°C with a bubble size ∼1.5 nm. Using the g.b=0 criterion the loops were characterised as b = ±1/2<111> type. At 750°C bubbles do not form an ordered array and are larger in size compared to the irradiations at 500°C, with a diameter of ∼3 nm. Fewer dislocation loops were observed at this temperature and were also characterised to be b = ±1/2<111> type. At 1000°C, no dislocation loops were observed and bubbles grew as a function of fluence attributed to vacancy mobility being higher and vacancy clusters becoming mobile.


Catalysts ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 751 ◽  
Author(s):  
Roddatis ◽  
Lole ◽  
Jooss

The study of changes in the atomic structure of a catalyst under chemical reaction conditions is extremely important for understanding the mechanism of their operation. For in situ environmental transmission electron microscopy (ETEM) studies, this requires preparation of electron transparent ultrathin TEM lamella without surface damage. Here, thin films of Pr1-xCaxMnO3 (PCMO, x = 0.1, 0.33) and La1-xSrxMnO3 (LSMO, x = 0.4) perovskites are used to demonstrate a cross-section specimen preparation method, comprised of two steps. The first step is based on optimized focused ion beam cutting procedures using a photoresist protection layer, finally being removed by plasma-etching. The second step is applicable for materials susceptible to surface amorphization, where in situ recrystallization back to perovskite structure is achieved by using electron beam driven chemistry in gases. This requires reduction of residual water vapor in a TEM column. Depending on the gas environment, long crystalline facets having different atomic terminations and Mn-valence state, can be prepared.


2013 ◽  
Vol 19 (S2) ◽  
pp. 458-459 ◽  
Author(s):  
M. Mecklenburg ◽  
M. Brodie ◽  
W. Hubbard ◽  
E.R. White ◽  
A. Bushmaker ◽  
...  

Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.


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