Ion Beam-Induced Amorphization of (Mg, Fe)2SiO4 Olivine Series: An In Situ Transmission Electron Microscopy Study

1991 ◽  
Vol 235 ◽  
Author(s):  
L. M. Wang ◽  
R. C. Ewing

ABSTRACTEffects of ion beam irradiation of five members of the (Mg, Fe)2SiO4 olivine series, from synthetic pure fayalite (Fe2SiO4) to naturally occurring (Mg0.88Fe0.12)2SiO4, have been studied by in situ transmission electron microscopy (TEM). Under 1.5 MeV Kr+ ion room temperature irradiations, all of the samples have been amorphized. The critical amorphization dose or the total collision energy loss required for amorphization increased rapidly with the increasing Mg:Fe ratio which coincides with an increasing melting temperature (bond strength) and an increasing average bond ionicity. A 400 keV He+ ion irradiation of (Mg0.88Fe0.12)2-SiO4, which mainly results in ionization energy loss in the sample, did not cause amorphization even at a much higher dose rate and a much higher final dose. This indicates nuclear interactions (collisions) are primarily responsible for ion beam induced amorphization. Also, high resolution electron microscopy (HREM) images of the defect structure at a low ion dose have been obtained and compared with the displacement cascade structure generated by computer modelling.

2012 ◽  
Vol 1383 ◽  
Author(s):  
J.A. Hinks ◽  
A.N. Jones ◽  
S.E. Donnelly

ABSTRACTGraphite is used as a moderator and structural component in the United Kingdom’s fleet of Advanced Gas-Cooled Reactors (AGRs) and features in two Generation IV reactor concepts: the Very High Temperature Reactor (VHTR) and the Molten Salt Reactor (MSR). Under the temperature and neutron irradiation conditions of an AGR, nuclear-grade graphite demonstrates significant changes to it mechanical, thermal and electrical properties. These changes include considerable dimensional change with expansion in the c-direction and contraction in the a/b-directions. As the United Kingdom’s AGRs approach their scheduled decommissioning dates, it is essential that this behaviour be understood in order to determine under what reactor conditions their operating lifetimes can be safely extended.Two models have been proposed for the dimensional change in graphite due to displacing radiation: the “Standard Model” and “Ruck and Tuck”. The Standard Model draws on a conventional model of Frenkel pair production, point defect migration and agglomeration but fails to explain several key experimental observations. The Ruck and Tuck model has been proposed by M.I. Heggie et al. and is based upon the movement of basal dislocation to create folds in the “graphene” sheets and seeks not only to account for the dimension change but also the other phenomena not explained by the Standard Model.In order to test the validity of these models, work is underway to gather experimental evidence of the microstructural evolution of graphite under displacing radiation. One of the primary techniques for this is transmission electron microscopy with in situ ion irradiation. This paper presents the results of electron irradiation at a range of energies (performed in order to separate the effects of the electron and ion beams) and of combined electron and ion beam irradiation.


Author(s):  
T. Dewolf ◽  
D. Cooper ◽  
N. Bernier ◽  
V. Delaye ◽  
A. Grenier ◽  
...  

Abstract Forming and breaking a nanometer-sized conductive area are commonly accepted as the physical phenomenon involved in the switching mechanism of oxide resistive random access memories (OxRRAM). This study investigates a state-of-the-art OxRRAM device by in-situ transmission electron microscopy (TEM). Combining high spatial resolution obtained with a very small probe scanned over the area of interest of the sample and chemical analyses with electron energy loss spectroscopy, the local chemical state of the device can be compared before and after applying an electrical bias. This in-situ approach allows simultaneous TEM observation and memory cell operation. After the in-situ forming, a filamentary migration of titanium within the dielectric hafnium dioxide layer has been evidenced. This migration may be at the origin of the conductive path responsible for the low and high resistive states of the memory.


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.


1998 ◽  
Vol 4 (3) ◽  
pp. 269-277 ◽  
Author(s):  
A. Agrawal ◽  
J. Cizeron ◽  
V.L. Colvin

In this work, the high-temperature behavior of nanocrystalline TiO2 is studied using in situ transmission electron microscopy (TEM). These nanoparticles are made using wet chemical techniques that generate the anatase phase of TiO2 with average grain sizes of 6 nm. X-ray diffraction studies of nanophase TiO2 indicate the material undergoes a solid-solid phase transformation to the stable rutile phase between 600° and 900°C. This phase transition is not observed in the TEM samples, which remain anatase up to temperatures as high as 1000°C. Above 1000°C, nanoparticles become mobile on the amorphous carbon grid and by 1300°C, all anatase diffraction is lost and larger (50 nm) single crystals of a new phase are present. This new phase is identified as TiC both from high-resolution electron microscopy after heat treatment and electron diffraction collected during in situ heating experiments. Video images of the particle motion in situ show the nanoparticles diffusing and interacting with the underlying grid material as the reaction from TiO2 to TiC proceeds.


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.


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