Defect fine Structures as observed by in situ experiments

Author(s):  
H. Saka

An in-situ experiment in an electron microscope is now a well established and useful technique in materials science. In this review recent contributions of in-situ experiments, especially of straining and heating experiments, to materials science will be high-lighted.The earlier works have been reviewed by Saka and Imura.It is believed that an external stress gives rise to an anistropy in the rate at which point defects are absorbed by edge dislocations; this mechanism is considered to explain the irradiation creep. A combined in situ tensile/irradiation experiment in a HVEM has been carried out to study effects of applied stress on the growth of dislocation loops. Fig. 1 shows typical microstructures of Ag irradiated at 403K for 10 min with 1MV electrons in the absence (a), and in the presence of an external stress of 5.5 kg/mm2 (b). Frank loops of interstial type, formed by electron irradiation, grew more rapidly in the direction of the external tensile stress than in the others. These results show that an external tensile stress has a profound effect on climb rates of Frank loops of interstitial type. However, detailed analysis of the results indicates that there is a considerable discrepancy between experiment and theory.

2019 ◽  
Vol 11 (7) ◽  
pp. 828
Author(s):  
Frédéric André ◽  
François Jonard ◽  
Mathieu Jonard ◽  
Harry Vereecken ◽  
Sébastien Lambot

Accurate characterization of forest litter is of high interest for land surface modeling and for interpreting remote sensing observations over forested areas. Due to the large spatial heterogeneity of forest litter, scattering from litter layers has to be considered when sensed using microwave techniques. Here, we apply a full-waveform radar model combined with a surface roughness model to ultrawideband ground-penetrating radar (GPR) data acquired above forest litter during controlled and in situ experiments. For both experiments, the proposed modeling approach successfully described the radar data, with improvements compared to a previous study in which roughness was not directly accounted for. Inversion of the GPR data also provided reliable estimates of the relative dielectric permittivity of the recently fallen litter (OL layer) and of the fragmented litter in partial decomposition (OF layer) with, respectively, averaged values of 1.35 and 3.8 for the controlled experiment and of 3.9 and 7.5 for the in situ experiment. These results show the promising potentialities of GPR for efficient and non-invasive characterization of forest organic layers.


1982 ◽  
Vol 35 (6) ◽  
pp. 727 ◽  
Author(s):  
PB Hirsch

The properties of the materials in a component or a device depend on structure and composition often on a scale of 10-10 to 10-6 m. Electron microscopy and microanalytical techniques provide a powerful means for determining the structure and composition on the appropriate scale, lead to an understanding of basic mechanisms, and by correlation or in situ experiments to explanations of bulk properties. Examples are given of the application of a variety of powerful electron optical techniques to a number of materials problems.


Materials ◽  
2021 ◽  
Vol 14 (5) ◽  
pp. 1085
Author(s):  
Matheus A. Tunes ◽  
Cameron R. Quick ◽  
Lukas Stemper ◽  
Diego S. R. Coradini ◽  
Jakob Grasserbauer ◽  
...  

Microelectromechanical systems (MEMS) are currently supporting ground-breaking basic research in materials science and metallurgy as they allow in situ experiments on materials at the nanoscale within electron microscopes in a wide variety of different conditions such as extreme materials dynamics under ultrafast heating and quenching rates as well as in complex electro-chemical environments. Electron-transparent sample preparation for MEMS e-chips remains a challenge for this technology as the existing methodologies can introduce contaminants, thus disrupting the experiments and the analysis of results. Herein we introduce a methodology for simple and fast electron-transparent sample preparation for MEMS e-chips without significant contamination. The quality of the samples as well as their performance during a MEMS e-chip experiment in situ within an electron microscope are evaluated during a heat treatment of a crossover AlMgZn(Cu) alloy.


1991 ◽  
Vol 235 ◽  
Author(s):  
Charles W. Allen

ABSTRACTMotivated at least initially by materials needs for nuclear reactor development, extensive irradiation effects studies employing transmission electron microscopes (TEM) have been performed for several decades, involving irradiation-induced and irradiation-enhanced microstructural changes, including phase transformations such as precipitation, dissolution, crystallization, amorphization, and order-disorder phenomena. From the introduction of commercial high voltage electron microscopes (HVEM) in the mid-1960s, studies of electron irradiation effects have constituted a major aspect of HVEM application in materials science. For irradiation effects studies two additional developments have had particularly significant impact; (1) the development of TEM specimen holders in which specimen temperature can be controlled in the range 10–2200 K and (2) the interfacing of ion accelerators which allows in situ TEM studies of irradiation effects and the ion beam modification of materials within this broad temperature range. This paper treats several aspects of in situ studies of electron and ion beam-induced and enhanced phase changes and presents two case studies involving in situ experiments performed in an HVEM to illustrate the strategies of such an approach of the materials research of irradiation effects.


Materials ◽  
2018 ◽  
Vol 11 (9) ◽  
pp. 1669 ◽  
Author(s):  
Komlavi Eloh ◽  
Alain Jacques ◽  
Gabor Ribarik ◽  
Stéphane Berbenni

Forward modeling of diffraction peaks is a potential way to compare the results of theoretical mechanical simulations and experimental X-ray diffraction (XRD) data recorded during in situ experiments. As the input data are the strain or displacement field within a representative volume of the material containing dislocations, a computer-aided efficient and accurate method to generate these fields is necessary. With this aim, a current and promising numerical method is based on the use of the fast Fourier transform (FFT)-based method. However, classic FFT-based methods present some numerical artifacts due to the Gibbs phenomenon or “aliasing” and to “voxelization” effects. Here, we propose several improvements: first, a consistent discrete Green operator to remove “aliasing” effects; and second, a method to minimize the voxelization artifacts generated by dislocation loops inclined with respect to the computational grid. Then, we show the effect of these improvements on theoretical diffraction peaks.


Author(s):  
D.I. Potter ◽  
A. Taylor

Thermal aging of Ni-12.8 at. % A1 and Ni-12.7 at. % Si produces spatially homogeneous dispersions of cuboidal γ'-Ni3Al or Ni3Si precipitate particles arrayed in the Ni solid solution. We have used 3.5-MeV 58Ni+ ion irradiation to examine the effect of irradiation during precipitation on precipitate morphology and distribution. The nearness of free surfaces produced unusual morphologies in foils thinned prior to irradiation. These thin-foil effects will be important during in-situ investigations of precipitation in the HVEM. The thin foil results can be interpreted in terms of observations from bulk irradiations which are described first.Figure 1a is a dark field image of the γ' precipitate 5000 Å beneath the surface(∿1200 Å short of peak damage) of the Ni-Al alloy irradiated in bulk form. The inhomogeneous spatial distribution of γ' results from the presence of voids and dislocation loops which can be seen in the bright field image of the same area, Fig. 1b.


Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove ◽  
R. T. Tung

The cobalt disilicide/silicon system has potential applications as a metal-base and as a permeable-base transistor. Although thin, low defect density, films of CoSi2 on Si(111) have been successfully grown, there are reasons to believe that Si(100)/CoSi2 may be better suited to the transmission of electrons at the silicon/silicide interface than Si(111)/CoSi2. A TEM study of the formation of CoSi2 on Si(100) is therefore being conducted. We have previously reported TEM observations on Si(111)/CoSi2 grown both in situ, in an ultra high vacuum (UHV) TEM and ex situ, in a conventional Molecular Beam Epitaxy system.The procedures used for the MBE growth have been described elsewhere. In situ experiments were performed in a JEOL 200CX electron microscope, extensively modified to give a vacuum of better than 10-9 T in the specimen region and the capacity to do in situ sample heating and deposition. Cobalt was deposited onto clean Si(100) samples by thermal evaporation from cobalt-coated Ta filaments.


Author(s):  
M.A. O’Keefe ◽  
J. Taylor ◽  
D. Owen ◽  
B. Crowley ◽  
K.H. Westmacott ◽  
...  

Remote on-line electron microscopy is rapidly becoming more available as improvements continue to be developed in the software and hardware of interfaces and networks. Scanning electron microscopes have been driven remotely across both wide and local area networks. Initial implementations with transmission electron microscopes have targeted unique facilities like an advanced analytical electron microscope, a biological 3-D IVEM and a HVEM capable of in situ materials science applications. As implementations of on-line transmission electron microscopy become more widespread, it is essential that suitable standards be developed and followed. Two such standards have been proposed for a high-level protocol language for on-line access, and we have proposed a rational graphical user interface. The user interface we present here is based on experience gained with a full-function materials science application providing users of the National Center for Electron Microscopy with remote on-line access to a 1.5MeV Kratos EM-1500 in situ high-voltage transmission electron microscope via existing wide area networks. We have developed and implemented, and are continuing to refine, a set of tools, protocols, and interfaces to run the Kratos EM-1500 on-line for collaborative research. Computer tools for capturing and manipulating real-time video signals are integrated into a standardized user interface that may be used for remote access to any transmission electron microscope equipped with a suitable control computer.


Author(s):  
Charles W. Allen ◽  
Robert C. Birtcher

The uranium silicides, including U3Si, are under study as candidate low enrichment nuclear fuels. Ion beam simulations of the in-reactor behavior of such materials are performed because a similar damage structure can be produced in hours by energetic heavy ions which requires years in actual reactor tests. This contribution treats one aspect of the microstructural behavior of U3Si under high energy electron irradiation and low dose energetic heavy ion irradiation and is based on in situ experiments, performed at the HVEM-Tandem User Facility at Argonne National Laboratory. This Facility interfaces a 2 MV Tandem ion accelerator and a 0.6 MV ion implanter to a 1.2 MeV AEI high voltage electron microscope, which allows a wide variety of in situ ion beam experiments to be performed with simultaneous irradiation and electron microscopy or diffraction.At elevated temperatures, U3Si exhibits the ordered AuCu3 structure. On cooling below 1058 K, the intermetallic transforms, evidently martensitically, to a body-centered tetragonal structure (alternatively, the structure may be described as face-centered tetragonal, which would be fcc except for a 1 pet tetragonal distortion). Mechanical twinning accompanies the transformation; however, diferences between electron diffraction patterns from twinned and non-twinned martensite plates could not be distinguished.


Author(s):  
Kenneth S. Vecchio ◽  
John A. Hunt

In-situ experiments conducted within a transmission electron microscope provide the operator a unique opportunity to directly observe microstructural phenomena, such as phase transformations and dislocation-precipitate interactions, “as they happen”. However, in-situ experiments usually require a tremendous amount of experimental preparation beforehand, as well as, during the actual experiment. In most cases the researcher must operate and control several pieces of equipment simultaneously. For example, in in-situ deformation experiments, the researcher may have to not only operate the TEM, but also control the straining holder and possibly some recording system such as a video tape machine. When it comes to in-situ fatigue deformation, the experiments became even more complicated with having to control numerous loading cycles while following the slow crack growth. In this paper we will describe a new method for conducting in-situ fatigue experiments using a camputer-controlled tensile straining holder.The tensile straining holder used with computer-control system was manufactured by Philips for the Philips 300 series microscopes. It was necessary to modify the specimen stage area of this holder to work in the Philips 400 series microscopes because the distance between the optic axis and holder airlock is different than in the Philips 300 series microscopes. However, the program and interfacing can easily be modified to work with any goniometer type straining holder which uses a penrmanent magnet motor.


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