Study of yield stress anomaly of Fe2MnAl single crystal by in situ TEM straining

L2₁-structured Fe₅₉Mn₁₇Al₂₄ shows a yield stress anomaly with a peak yield stress at 700?K. The aim of the work reported here was to determine the dislocation mechanisms involved in this anomalous behaviour by performing in situ straining on Fe₅₉Mn₁₇Al₂₄ single crystals in a transmission electron microscope at 300–900?K. Cross-slip of ?111? dislocations was frequently found to occur between {110} and {211} planes at all temperatures tested. At 300?K, dislocations were four-fold dissociated and the partials moved together under stress. At 700–800?K, partial dislocations with a Burgers vector of a/2?111? dominated the deformation. These partial dislocations moved independently in the ordered matrix in a jerky manner, with rapid motion between long periods of locking. X-ray diffraction measurements showed that the degree of L2₁-order slightly decreased with increasing temperature in the range 300–700?K, and dropped rapidly above 700?K. At 900?K, the material was B2-ordered. The increased yield stress at elevated temperatures is primarily attributed to the uncoupling of a/2?111? partial dislocations trailing shear-induced anti-phase boundaries.     

Interdiffusion in two-layer Pd/Ag films III. TEM investigation of diffusion-induced grain boundary migration

Diffusion-induced grain boundary migration (DIGM) is studied by the transmission electron microscopy method in polycrystalline two-layer Pd/Ag thin films with a grain size (100–2000 nm). In addition to the typical features of DIGM known for coarse-grained bulk objects and foils, new features are found which are caused by a quite dense network of triple junctions and by misfit dislocations: fast increase of grain boundary curvature and inclination; back motion of grain boundaries owing to recrystallization forces and termination of DIGM. Homogenization resulted from diffusion-induced migration of misfit dislocations is observed in addition to DIGM.     

纳米材料及HfO_2基存储器件的原位电子显微学研究

总结了我们将原位技术和透射电子显微学分析方法相结合,针对纳米材料和器件的结构、形貌、成分以及电势分布等物理性质的动态行为所开展的综合物性表征和分析工作.主要成果有:揭示了C_(60)纳米晶须在焦耳热作用下的结构相变路径;观察到了电荷俘获存储器中的电荷存储位置以及栅极电压诱导的氧空位缺陷;研究了阻变存储器中氧空位通道的形成过程以及导电通道的开关机理.这些成果不但有助于深入理解纳米材料和器件相关功能的物理机理,改善其工作性能,更展示了透射电子显微学在微电子领域强大的研究能力.     

In situ TEM study of reversible and irreversible electroforming in Pt/Ti:NiO/Pt heterostructures

Experimental verification of the microscopic origin of resistance switching in metal/oxide/metal heterostructures is needed for applications in non‐volatile memory and neuromorphic computing. Numerous reports suggest that resistance switching in NiO is caused by local reduction of the oxide layer into nanoscale conducting filaments, but few reports have shown experimental evidence correlating electroforming with site‐specific changes in composition. We have investigated the mechanisms of reversible and irreversible electroforming in 250–500 nm wide pillars patterned from a single Ta/Ti/Pt/Ti‐doped NiO/Pt/Ta heterostructure and have shown that these can coexist within a single sample. We performed in situ transmission electron microscopy (TEM) electroform‐ ing and switching on each pillar to correlate the local electron transport behavior with microstructure and composition in each pillar. DFT calculations fitted to electron energy loss spectroscopy data showed that the Ti‐doped NiO layer is partially reduced after reversible electroforming, with the formation of oxygen vacancies ordered into lines in the 〈110〉 direction. However, under the same probing conditions, adjacent pillars show irreversible electroforming caused by electromigration of metallic Ta to form a single bridge across the oxide layer. We propose that the different electroforming behaviors are related to microstructural variations across the sample and may lead to switching variability. (© 2015 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)     

Nanostructuring Germanium Nanowires by In Situ TEM Ion Irradiation

Once nanomaterials have been synthesized, inducing further structural modifications is challenging. However, being able to do so in a controlled manner is crucial. In this context, germanium nanowires are irradiated in situ within a transmission electron microscope (TEM) by a 300 keV xenon ion beam at temperatures ranging from room temperature (RT) to 500 °C. The ion irradiation is performed in situ and the evolution of nanowires during irradiation is monitored. At 300 °C and below, where the temperature is low enough to allow amorphization, the ion beam causes the formation of nanostructures within the nanowires. Formation of nanopores and swelling of nanowires is observed for a very low fluence of 2.2 × 10¹⁴ and up to 4.2 × 10¹⁵ ions cm⁻². At higher fluences, the thickness of the nanowires decreases, the nanowires lose their wire-like cylindrical shape and the nanostructuring caused by the ion beam becomes more complex. The nanostructures are observed to be stable upon crystallization when the nanowires are annealed at 530 °C. Furthermore, in situ imaging allows the growth of nanopores during irradiation to be followed at RT and at 300 °C providing valuable insights into the mechanism responsible for the nanostructuring.     

In situ TEM study of stability of TaRhx diffusion barriers using a novel sample preparation method

The atomic diffusion mechanisms associated with metallurgical failure of TaRh_x diffusion barriers for Cu metallizations were studied by in situ transmission electron microscopy (TEM). The issues related to in situ heating of focused ion beam (FIB) prepared cross-sectional TEM samples that contain Cu thin films are discussed. The Cu layer in Si/(13 nm)TaRh_x/Cu stacks showed grain growth and formation of voids at temperatures exceeding 550 °C. For Si/(43 nm)TaRh_x/Cu stacks, grain growth of Cu was delayed to higher temperatures, i.e., 700 °C, and void formation was not observed. Extensive surface diffusion of Cu, however, preceded bulk diffusion. Therefore, a 10 nm film of electron beam evaporated C was deposited on both sides of the TEM lamellae to limit surface diffusion. This processing technique allowed for direct observation of atomic diffusion and reaction mechanisms across the TaRh_x interface. Failure occurred by nucleation of orthorhombic RhSi particles at the Si/TaRh_x interface. Subsequently, the barrier at areas adjacent to RhSi particles was depleted in Rh. This created lower density areas in the barrier, which facilitated diffusion of Cu to the Si substrate to form Cu₃Si. The morphology of an in situ annealed lamella was compared with an ex situ bulk annealed sample, which showed similar reaction morphology. The sample preparation method developed in this study successfully prevented surface diffusion/delamination of the Cu layer and can be employed to understand the metallurgical failure of other potential diffusion barriers.     

In situ TEM study of mechanical behaviour of twinned nanoparticles

There is strong interest in studying changes in mechanical properties with reducing grain size. The rational is that consequent dislocation glide cannot be sustained, resulting in an increase in material strength. However, this comes with the cost of a reduction in ductility. It has been shown that coherent twin boundaries in nanostructured Cu improve the ductility to 14% [Lu et al., Science 324 (2009) p. 349]. In this paper, we report for the first time the compression of individual nanoparticles using an in situ force probing holder in the transmission electron microscope. Four types of nanoparticles were tested, three with twin boundaries (decahedra, icosahedra and a single twin) and one free of defects (octahedral). Our results indicate the yield strength of the twinned nanoparticles is between 0.5 and 2.0 GPa. The total malleability for the twinned particles range from 80 to 100%. In addition, experimental results were reproduced by MD simulations of the compression phenomena and suggest that the outstanding mechanical properties are related with partial dislocation multiplication at twin boundaries.     

原位透射电子显微学进展及应用

文章简要介绍了近年来原位透射电子显微学的进展,并指出,原位透射电子显微技术的发展使得在纳米、原子层次观察样品在力、热、电、磁作用下以及化学反应过程中的微结构演化成为可能。通过研究物质在外界环境作用下的微结构演化规律,揭示其原子结构与物理化学性质的相关性,指导其设计合成和微结构调控,促进新物质的探索和深层次物质结构研究,为解决凝聚态物理学中的具体问题提供了直接、准确和详细的方法。     

原位透射电子显微学进展及应用

文章简要介绍了近年来原位透射电子显微学的进展,并指出,原位透射电子显微技术的发展使得在纳米、原子层次观察样品在力、热、电、磁作用下以及化学反应过程中的微结构演化成为可能。通过研究物质在外界环境作用下的微结构演化规律,揭示其原子结构与物理化学性质的相关性,指导其设计合成和微结构调控,促进新物质的探索和深层次物质结构研究,为解决凝聚态物理学中的具体问题提供了直接、准确和详细的方法。     

TEM imaging of an inclined dislocation in an anisotropic thin foil

The elastic distortions nearby the two emerging points of a straight inclined dislocation located in an elastically anisotropic thin foil are expressed with the aid of the integral formalism [D.M. Barnett and J. Lothe, Phys. Norv. 7 (1973) p.13], an approach complementary to that of the Eshelby's “sextic” formalism. They are included in the calculation of the intensities of diffracted beams in transmission electron microscopy to produce theoretical images, a well known procedure when elastic free surface relaxation is ignored. Examples of theoretical images point out some contrast differences between images calculated with the assumptions of isotropic and anisotropic crystals. These calculations can be simplified for a dislocation normal to the surface and a line direction parallel to a two-fold axis.     

Multiscale characterization of dislocation processes in Al 5754

Multiscale characterization was performed on an Al–Mg alloy, Al 5754 O-temper, including in situ mechanical deformation in both the scanning electron microscope and the transmission electron microscope. Scanning electron microscopy characterization showed corresponding inhomogeneity in the dislocation and Mg distribution, with higher levels of Mg correlating with elevated levels of dislocation density. At the nanoscale, in situ transmission electron microscopy straining experiments showed that dislocation propagation through the Al matrix is characterized by frequent interactions with obstacles smaller than the imaging resolution that resulted in the formation of dislocation debris in the form of dislocation loops. Post-mortem chemical characterization and comparison to dislocation loop behaviour in an Al–Cr alloy suggests that these obstacles are small Mg clusters. Previous theoretical work and indirect experimental evidence have suggested that these Mg nanoclusters are important factors contributing to strain instabilities in Al–Mg alloys. This study provides direct experimental characterization of the interaction of glissile dislocations with these nanoclusters and the stress needed for dislocations to overcome them.     

Study of defect evolution by TEM with in situ ion irradiation and coordinated modeling

The paper describes a novel transmission electron microscopy (TEM) experiment with in situ ion irradiation designed to improve and validate a computer model. TEM thin foils of molybdenum were irradiated in situ by 1?MeV Kr ions up to ～0.045 displacements per atom (dpa) at 80°C at three dose rates ?5?×?10^?6, 5?×?10^?5, and 5?×?10^?4?dpa/s – at the Argonne IVEM-Tandem Facility. The low-dose experiments produced visible defect structure in dislocation loops, allowing accurate, quantitative measurements of defect number density and size distribution. Weak beam dark-field plane-view images were used to obtain defect density and size distribution as functions of foil thickness, dose, and dose rate. Diffraction contrast electron tomography was performed to image defect clusters through the foil thickness and measure their depth distribution. A spatially dependent cluster dynamic model was developed explicitly to model the damage by 1?MeV Kr ion irradiation in an Mo thin foil with temporal and spatial dependence of defect distribution. The set of quantitative data of visible defects was used to improve and validate the computer model. It was shown that the thin foil thickness is an important variable in determining the defect distribution. This additional spatial dimension allowed direct comparison between the model and experiments of defect structures. The defect loss to the surfaces in an irradiated thin foil was modeled successfully. TEM with in situ ion irradiation of Mo thin foils was also explicitly designed to compare with neutron irradiation data of the identical material that will be used to validate the model developed for thin foils.     

HRTEM Studies of the Structures and the Defects of Exact and Near ∑ = 11 {332} Tilt Grain Boundaries in Ni

A = 11 {332} Ni bicrystal was grown by solidification. The Grain Boundary (GB) atomic structure studied by high resolution electron microscopy (HREM) has been shown to depend upon the position in the bicrystal of the extracted sample. Strongly correlated to the atomic structure, (GB) defects (GBD) have been characterized: all their Burgers vectors belong to the Displacement Shift Complete (DSC) lattice and the height of the step associated with each GBD varies up to a few nanometers. In the symmetrical and almost symmetrical GBs, at the head of the bicrystal, the dislocation cores can be well localized, whereas in the asymmetrical GBs, at the end of the bicrystal, their cores are much more difficult to localize on the HREM image. The influence on the GB structures of the impurity content which varies along the bicrystal is also discussed.     

In situ diagnostics of catalytic materials using tunable confocal Raman spectroscopy

A new Raman spectroscopic setup for in situ characterization of catalytic materials based on a tunable laser system and a confocal Raman microscope is described. The laser excitation wavelength is variable over a broad range from deep ultraviolet (UV) to near‐infrared allowing for targeted use of Raman diagnostics for catalyst characterization. By utilization of resonance effects, the sensitivity of the method can be strongly increased. The potential of the setup is illustrated by new in situ Raman results on dispersed vanadium oxide catalysts obtained at 217.5 and 280 nm UV laser excitation. Copyright © 2013 John Wiley & Sons, Ltd.     

Ordinary dislocation configurations in high Nb-containing TiAl alloy deformed at high temperatures

Abstract

High Nb-containing TiAl (Nb–TiAl) alloys possess mechanical properties at elevated temperatures superior to conventional TiAl alloys. However, the strengthening mechanisms induced by Nb addition have been discussed controversial for a long time. In the present study, the dislocation structures in a polycrystalline high Nb–TiAl alloy after tensile tests at 700 and 900 °C were investigated by transmission electron microscope (TEM) observation. The results show that abundant double cross slip of ordinary dislocations is activated in the samples deformed at 700 °C. The dislocations are pinned at the jogs and numerous dipoles are observed. Debris can be commonly observed in the vicinity of screw dislocations. Trace analysis shows that the cross-slip plane is (1?1?0)γ at 700 °C but (1?1?1)γ octahedral plane at 900 °C. Three-dimensional (3D) dislocation structures, caused by cross-slip and annihilation of ordinary dislocations, were observed along the screw orientation. The dipoles and debris produced by high-temperature cross slip can be important for the strengthening of high Nb–TiAl alloys.     

TEM study on relationship between stacking faults and non-basal dislocations in Mg

Recent interest in the study of stacking faults and non-basal slip in Mg alloys is partly based on the argument that these phenomena positively influence mechanical behaviour. Inspection of the published literature, however, reveals that there is a lack of fundamental information on the mechanisms that govern the formation of stacking faults, especially I1-type stacking faults (I1 faults). Moreover, controversial and sometimes contradictory mechanisms have been proposed concerning the interactions between stacking faults and dislocations. Therefore, we describe a fundamental transmission electron microscope investigation on Mg 2.5 at. % Y (Mg–2.5Y) processed via hot isostatic pressing (HIP) and extrusion at 623 K. In the as-HIPed Mg–2.5Y, many 〈c〉 and 〈a〉 dislocations, together with some 〈c + a〉 dislocations were documented, but no stacking faults were observed. In contrast, in the as-extruded Mg–2.5Y, a relatively high density of stacking faults and some non-basal dislocations were documented. Specifically, there were three different cases for the configurations of observed stacking faults. Case (I): pure I2 faults; Case (II): mixture of I1 faults and non-basal dislocations having 〈c〉 component, together with basal 〈a〉 dislocations; Case (III): mixture of predominant I2 faults and rare I1 faults, together with jog-like dislocation configuration. By comparing the differences in extended defect configurations, we propose three distinct stacking fault formation mechanisms for each case in the context of slip activity and point defect generation during extrusion. Furthermore, we discuss the role of stacking faults on deformation mechanisms in the context of dynamic interactions between stacking faults and non-basal slip.     

Strain-induced preferential dissolution at the dislocation emergences in MnS: an atomic scale study

The long-standing problem of dislocation-preferential dissolution in a crystal has been generally ascribed to the distortion energy stored in the vicinity of the dislocation core. However, due to lack of experimental means, the relationship between the local distortion state and the electrochemical behaviour of a single dislocation has not been established so far. via in situ ex-environment transmission electron microscopy (TEM), we demonstrate that the emergences of both edge and screw dislocations on MnS surfaces are the preferential sites for dissolution of the MnS inclusions within a stainless steel. In addition, we map the strain-induced variation of the standard electrode potential around the edge dislocation by a combination of the aberration-corrected high-resolution TEM and strain-analysis-based mechanochemistry theory. Significantly, our report provides a new approach to investigate the strain–corrosion correlation at an atomic scale.