scholarly journals Dual Beam In Situ Radiation Studies of Nanocrystalline Cu

Materials ◽  
2019 ◽  
Vol 12 (17) ◽  
pp. 2721 ◽  
Author(s):  
Cuncai Fan ◽  
Zhongxia Shang ◽  
Tongjun Niu ◽  
Jin Li ◽  
Haiyan Wang ◽  
...  

Nanocrystalline metals have shown enhanced radiation tolerance as grain boundaries serve as effective defect sinks for removing radiation-induced defects. However, the thermal and radiation stability of nanograins are of concerns since radiation may induce grain boundary migration and grain coarsening in nanocrystalline metals when the grain size falls in the range of several to tens of nanometers. In addition, prior in situ radiation studies on nanocrystalline metals have focused primarily on single heavy ion beam radiations, with little consideration of the helium effect on damage evolution. In this work, we utilized in situ single-beam (1 MeV Kr++) and dual-beam (1 MeV Kr++ and 12 keV He+) irradiations to investigate the influence of helium on the radiation response and grain coarsening in nanocrystalline Cu at 300 °C. The grain size, orientation, and individual grain boundary character were quantitatively examined before and after irradiations. Statistic results suggest that helium bubbles at grain boundaries and grain interiors may retard the grain coarsening. These findings provide new perspective on the radiation response of nanocrystalline metals.

2017 ◽  
Vol 11 (3) ◽  
pp. 1075-1090 ◽  
Author(s):  
Jan Eichler ◽  
Ina Kleitz ◽  
Maddalena Bayer-Giraldi ◽  
Daniela Jansen ◽  
Sepp Kipfstuhl ◽  
...  

Abstract. Impurities control a variety of physical properties of polar ice. Their impact can be observed at all scales – from the microstructure (e.g., grain size and orientation) to the ice sheet flow behavior (e.g., borehole tilting and closure). Most impurities in ice form micrometer-sized inclusions. It has been suggested that these µ inclusions control the grain size of polycrystalline ice by pinning of grain boundaries (Zener pinning), which should be reflected in their distribution with respect to the grain boundary network. We used an optical microscope to generate high-resolution large-scale maps (3 µm pix−1, 8 × 2 cm2) of the distribution of micro-inclusions in four polar ice samples: two from Antarctica (EDML, MIS 5.5) and two from Greenland (NEEM, Holocene). The in situ positions of more than 5000 µ inclusions have been determined. A Raman microscope was used to confirm the extrinsic nature of a sample proportion of the mapped inclusions. A superposition of the 2-D grain boundary network and µ-inclusion distributions shows no significant correlations between grain boundaries and µ inclusions. In particular, no signs of grain boundaries harvesting µ inclusions could be found and no evidence of µ inclusions inhibiting grain boundary migration by slow-mode pinning could be detected. Consequences for our understanding of the impurity effect on ice microstructure and rheology are discussed.


2016 ◽  
Author(s):  
Jan Eichler ◽  
Ina Kleitz ◽  
Maddalena Bayer ◽  
Daniela Jansen ◽  
Sepp Kipfstuhl ◽  
...  

Abstract. Impurities control a variety of physical properties of polar ice. Their impact can be observed at all scales – from the microstructure (e.g., grain size and orientation) to the ice sheet flow behavior (e.g., borehole tilting and closure). Most impurities are likely to form micrometer-sized second phase inclusions. It has been suggested that these particles control the grain size of polycrystalline ice by the pinning of grain boundaries (Zener pinning), which should be reflected in the distribution of the inclusions in relation to the grain boundary network. We used an optical microscope to generate high-resolution large-scale maps (3 μm pix−1, 8 × 2 cm2) of the distribution of micro-inclusions in four samples from the EDML (Antarctica) and NEEM (Greenland) polar ice cores. The in-situ positions of more than 5000 μ-inclusions have been determined. A Raman microscope was used to confirm the extrinsic nature of a sample proportion of the mapped inclusions. A superposition of the 2D grain boundary network and μ-inclusion distributions show no significant correlations between grain boundaries and μ-inclusions. In particular, no signs could be found of grain boundaries harvesting μ-inclusions, no evidence of μ-inclusions inhibiting grain boundary migration by slow mode pinning could be detected. Consequences for our understanding of the impurity effect on ice microstructure and rheology are discussed.


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):  
Jian-Shing Luo ◽  
Hsiu Ting Lee

Abstract Several methods are used to invert samples 180 deg in a dual beam focused ion beam (FIB) system for backside milling by a specific in-situ lift out system or stages. However, most of those methods occupied too much time on FIB systems or requires a specific in-situ lift out system. This paper provides a novel transmission electron microscopy (TEM) sample preparation method to eliminate the curtain effect completely by a combination of backside milling and sample dicing with low cost and less FIB time. The procedures of the TEM pre-thinned sample preparation method using a combination of sample dicing and backside milling are described step by step. From the analysis results, the method has applied successfully to eliminate the curtain effect of dual beam FIB TEM samples for both random and site specific addresses.


Author(s):  
Gunnar Zimmermann ◽  
Richard Chapman

Abstract Dual beam FIBSEM systems invite the use of innovative techniques to localize IC fails both electrically and physically. For electrical localization, we present a quick and reliable in-situ FIBSEM technique to deposit probe pads with very low parasitic leakage (Ipara < 4E-11A at 3V). The probe pads were Pt, deposited with ion beam assistance, on top of highly insulating SiOx, deposited with electron beam assistance. The buried plate (n-Band), p-well, wordline and bitline of a failing and a good 0.2 μm technology DRAM single cell were contacted. Both cells shared the same wordline for direct comparison of cell characteristics. Through this technique we electrically isolated the fail to a single cell by detecting leakage between the polysilicon wordline gate and the cell diffusion. For physical localization, we present a completely in-situ FIBSEM technique that combines ion milling, XeF2 staining and SEM imaging. With this technique, the electrically isolated fail was found to be a hole in the gate oxide at the bad cell.


2016 ◽  
Vol 23 (06) ◽  
pp. 1650050 ◽  
Author(s):  
BOUTASSOUNA DJAMAL ◽  
RENÉ LE GALL ◽  
IBEN KHALDOUN LEFKAIER

In this paper, we investigate the influence of temperature on the nickel grain boundary equilibrium segregation of sulfur and the resulting intergranular fracturing susceptibility. Auger electron spectroscopy has been used to study equilibrium segregation of sulfur to the grain boundaries of a metallic nickel, with a mass bulk content of 3.6[Formula: see text]ppm in sulfur. Samples were first annealed at adequate temperatures for sufficiently large equilibrium time, and then quenched in water at room temperature. The analysis carried out shows a significant increase of sulfur concentration in the grain boundary with decreasing temperature. However, the sulfur content in the grain boundary shows a drastic shrink at 700[Formula: see text]C. This can be interpreted by the formation of an aggregate sulfide compound in the area of the grain boundaries. At 650[Formula: see text]C, in situ brittle fracture becomes unworkable and only intragranular fractures are observed. Using the results obtained through the investigation of the grain boundaries by Auger spectroscopy, the standard segregation energy is estimated as [Formula: see text].


2021 ◽  
Vol 2021 (3) ◽  
pp. 77-85
Author(s):  
K. M. Borysovska ◽  
◽  
N. M. Marchenko ◽  
Yu. M. Podrezov ◽  
S. O. Firstov ◽  
...  

The (DD) method was used to model the formation of the plastic zone of the top of the cracks in polycrystalline molybdenum. Special attention was paid to take into account the interaction of dislocations in the plastic zone with grain boundaries. Structural sensitivity of fracture toughness was analyzed under brittle-ductile condition. Simulations were performed for a range of grain sizes from 400 to 100 μm, at which a sudden increase in fracture toughness with a decrease of grain size was experimentally shown. We calculated the value of K1c taking into account the shielding action of dislocations. The position of all dislocations in the plastic zone at fracture moment was calculated. Based on these data, we obtained the dependences of dislocation density on the distance from the crack tip thereby confirming significant influence of the grain boundaries on plastic zone formation. At large grain sizes, when the plastic zone does not touch the boundary, the distribution of dislocations remained unchanged. As grains reduce their size to size of the plastic zone, they start formating a dislocation pile – up near the boundaries. Dislocations on plastic zone move slightly toward the crack tip, but the density of dislocations in the middle of the grain remains unchanged, and fracture toughness remains almost unchanged. Further reduction of the grain size leads to the Frank-Reed source activation on the grain boundary Forming dislocation pile-up of the neighbor grains. Its stress concentration acts on dislocations of the first grain and causes redistribution of plastic zone dislocations. If the reduction in grain size is not enough to form a strong pile-up, density of dislocations on plastic zone increases slightly and crack resistance increases a few percent. Further reduction of grains promotes strong pile-up, dislocations move to crack tip, and its density on plastic zone increases. Crack is shielded and fracture toughness increases sharply. The calculation showed that the fracture toughness jump is observed at grain sizes of 100—150 μm, in good agreement with the experiment. Keywords: dislocation dynamics simulation, molybdenum, fracture toughness, grain size, plastic zone, brittle-ductile transition.


2002 ◽  
Vol 727 ◽  
Author(s):  
Y. Champion ◽  
P. Langlois ◽  
S. Guérin-Mailly ◽  
C. Langlois ◽  
M. J. Hÿtch

AbstractUnderstanding the mechanical behaviour of metallic nanostructures is a key issue for their development. On the one hand, knowledge of the plastic behaviour at various temperatures is essential to control the synthesis, forming, and machining of such materials. Equally, a clear understanding of atomic and mesoscopic mechanisms, involving defects and their interactions, is essential for the control of ageing and functional properties. Regarding plastic deformation at room temperature, there is now evidence for unusual behaviour in nanostructured metals. In addition to high resistance and ductility, tensile testing reveals peculiar elasto-plastic deformation. Such behaviour was initially attributed to grain-boundary sliding. However, intergranular areas (including triple junctions) may possess special properties compared to their microcrystalline counterparts. For example, low activation energies have been measured for grain-boundary diffusion and it has been observed that grain-boundaries may act as dislocation sources and nucleation sites for deformation twinning.In this paper, we report on analysis on bulk copper nanostructures. Grain-boundaries are studied, by cross-correlating information from mechanical tensile testing and structural analysis, including X-ray diffraction (XRD) and transmission electron microscopy (TEM). Macroscopic bulk specimens (with grain size of about 80 nm) are prepared by powder metallurgy techniques, modified to fit to the special properties of nanocrystalline powders. Processing includes coldisostatic pressing, sintering and differential extrusion. The powders used (grain size of 40 nm) are synthesised by evaporation and cryo-condensation of a metallic vapour within liquid nitrogen. Results on mechanical testing and structural analysis will be reported. Emphasis will be placed on the structure of grain-boundaries (type of grain-boundary, grain-boundary thickness) studied by TEM and high resolution TEM image analysed using the geometric phase technique. The nanostructure was revealed to be consist in agglomerate of nano-size grains separated by low angle grain-boundaries. Agglomerates are themselves separerated by general high angle boundaries. These observations will then be related to the unusual mechanical true stress-true strain curves of the metallic nanostructures.


Solid Earth ◽  
2017 ◽  
Vol 8 (6) ◽  
pp. 1193-1209 ◽  
Author(s):  
James Gilgannon ◽  
Florian Fusseis ◽  
Luca Menegon ◽  
Klaus Regenauer-Lieb ◽  
Jim Buckman

Abstract. Establishing models for the formation of well-mixed polyphase domains in ultramylonites is difficult because the effects of large strains and thermo-hydro-chemo-mechanical feedbacks can obscure the transient phenomena that may be responsible for domain production. We use scanning electron microscopy and nanotomography to offer critical insights into how the microstructure of a highly deformed quartzo-feldspathic ultramylonite evolved. The dispersal of monomineralic quartz domains in the ultramylonite is interpreted to be the result of the emergence of synkinematic pores, called creep cavities. The cavities can be considered the product of two distinct mechanisms that formed hierarchically: Zener–Stroh cracking and viscous grain-boundary sliding. In initially thick and coherent quartz ribbons deforming by grain-size-insensitive creep, cavities were generated by the Zener–Stroh mechanism on grain boundaries aligned with the YZ plane of finite strain. The opening of creep cavities promoted the ingress of fluids to sites of low stress. The local addition of a fluid lowered the adhesion and cohesion of grain boundaries and promoted viscous grain-boundary sliding. With the increased contribution of viscous grain-boundary sliding, a second population of cavities formed to accommodate strain incompatibilities. Ultimately, the emergence of creep cavities is interpreted to be responsible for the transition of quartz domains from a grain-size-insensitive to a grain-size-sensitive rheology.


1990 ◽  
Vol 208 ◽  
Author(s):  
M. R. Fitzsimmons ◽  
E. Burkel ◽  
J. Peisl

ABSTRACTX-ray reflectivity techniques have been used to characterize the surfaces of 0.4µm thick Au films epitaxially grown on single-crystals of NaCl. Measurements of both the specular and non-specular reflectivity suggest that the Au surface is very rough. The nonspecular reflectivity provides valuable information about the correlation of the heights at different points on the surface. The first in situ reflectivity study of the formation and destruction of a grain boundary shows direct evidence for the existence of diffuse scattering from the grain boundary. Measurements of several [0011 twist grain boundaries suggest that the roughness and texture of an interface depends upon the geometrical orientation of the surrounding substrates.


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