Characterization of dislocation interactions in olivine using electron tomography

We have investigated by electron tomography, in a transmission electronic microscope, the interactions between dislocations in olivine single crystals and polycrystals deformed in axial compression at T < 1000 °C (T < 0.5T_m). Dislocations are mostly of the [0?0?1] type, except in the polycrystal where [1?0?0] and [0?0?1] dislocations have been activated. A few 〈1?0?1〉 junctions have been found and characterized. Many collinear interactions have been identified either involving direct interactions between crossing dislocations of opposite Burgers vectors or indirect interactions between dislocations gliding in parallel planes and sessile dislocation loops. We suggest that collinear interaction, already identified as the primary source of strain hardening in FCC metals, is the main dislocation interaction mechanism in olivine deformed at temperatures below 1000 °C.     

Evolution of long-period stacking order (LPSO) in Mg97Zn1Gd2 cast alloys viewed by HAADF-STEM multi-scale electron tomography

We have studied three-dimensional (3D) structures and growth processes of 14H-type long-period stacking order (LPSO) formed in Mg₉₇Zn₁Gd₂ cast alloys by single tilt-axis electron tomography (ET) using high-angle annular dark-field scanning transmission electron microscopy. Evolution of the solute-enriched stacking faults (SFs) and the 14H LPSO by ageing were visualised in 3D with a high spatial resolution in multi-scale fields of views from a few nanometres to ~10 μm. Lateral growth of the solute-enriched SFs and the LPSO in the (0?0?0?1)_Mg plane is notable compared to the out-of-plane growth in the [0?0?0?1]_Mg direction. The 14H LPSO grows at the cost of decomposition of the (Mg, Zn)₃Gd-type precipitates, and accompany a change of in-plane edge angles from 30 to 60°. We have updated the Time–Temperature–Transformation diagram for precipitation in Mg₉₇Zn₁Gd₂ alloys: starting temperatures of both solute-enriched SFs and LPSO formation shifted to a shorter time side than those in the previous diagram.     

现代透射电子显微技术在多铁材料研究中的应用

文章简要介绍了材料科学研究中被广泛应用的透射电子显微(TEM)技术及其在多铁材料研究中的应用,并给出了几个典型案例：利用球差矫正原子分辨扫描透射电子显微术(STEM),并和电子能量损失谱(EELS)相结合,分析多铁异质结界面处的原子分布、离子价态和化学键的变化;结合球差矫正原子分辨透射电子显微图像(HRTEM)和STEM图像,分析多铁材料中的局域对称性破缺和电极化特性;利用原位变温及电/磁场加载技术,研究多铁材料中的结构相变和电畴/磁畴的动态演变特性。文章特别指出,现代透射电子显微学是全面分析理解多铁材料局域微结构,探讨多铁耦合机制及其物理根源的有效手段。     

Some examples of the application of Mössbauer spectroscopy and transmission electron microscopy to micas

I discuss the weaknesses and strengths of Mössbauer spectroscopy and transmission electron microscopy and present the potential of combining them using experimental weathering of biotite as an example. A natural biotite was treated in acid at room temperature and the reaction products were removed by a continuous flow of an external eluent that was in contact with the mineral suspension through a dialysis membrane. The fractionation of Mg/Fe into the fluid was determined by wet chemical analysis, the state of Fe in the solid was monitored by Mössbauer spectroscopy, and the structural changes were characterized by transmission electron microscopy. Weathering is controlled primarily by pH, the type of acid used, and K selectivity of the solid. Once equilibrium has been reached, further weathering does not affect the oxidation state of iron. The tetrahedral layer collapses during the last phase of weathering leaving an amorphous phase rich in Si and Al. Moreover, transmission electron microscopy shows that weathering is a discontinuous processes resulting in quasi-periodic texture. The periodicity is controlled by the concentration of the K in solution.     

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.     

氢离子辐照纯钒中形成的位错环

钒合金作为聚变堆候选材料, 其辐照损伤行为一直是关注的重点. 研究辐照时形成的位错环的性质, 其意义在于揭示纯钒中辐照空洞的长大机理. 这种机理表现为不同类型位错环对点缺陷吸收的偏压不同, 从而影响金属的辐照肿胀. 本文利用加速器对纯钒薄膜样品进行氢离子辐照, 然后, 利用透射电镜的inside-outside方法分析氢离子辐照所形成的位错环的类型. 结果表明, 在氢离子辐照纯钒中没有发现柏氏矢量b=<110>的位错环, 只有柏氏矢量b=1/2<111>和b=<110>的位错环, 这两种位错环的惯性面处于{110}-{112}之间. 能确定性质的位错环全部为间隙型位错环, 未发现空位型位错环.     

Determination of 25 elements in the complex oxide mineral zirconolite by analytical electron microscopy

In this paper we describe a technique for the determination of 25 elements in natural zirconolite using energy-dispersive analytical electron microscopy (AEM). The method presented here allows one to quantitatively investigate the chemistry of submicron-scale zones in complex oxide minerals. The effects of electron channeling, thickness variability and variations in detector resolution were minimized by using a controlled set of operating procedures and instrument parameters. To provide a high level of accurayy, k_ATI-factors were determined from standards for most of the 25 elements of interest, including all of the major elements. Each analytical spectrum is reduced to a set of raw peak counts (and errors) using a digital top-hat filter to suppress background followed by multiple least squares fitting of reference spectra. Counting times of 12–15 min per analysis were required to provide suitable counting statistics. Results are presented for zirconolite samples from the contact metamorphic aureole of the Bergell granodiorite intrusion, Switzerland-Italy. A comparison of 43 AEM analyses with 15 analyses obtained by wavelength-dispersive electron probe microanalysis (EPMA) shows that there is excellent agreement between the two data sets in the amounts of individual elements present, chemical trends and overall stoichiometry. An assessment of the combined data set shows that the major substitution mechanisms in the Bergell samples are coupled substitutions involving the M5,6- and M8-sites of the zirconolite structure: ^M8Ca²⁺ + ^M5,6Ti⁴⁺→^M8REE³⁺ + ^M5,6(Al,Fe)³⁺ and ^M8Ca²⁺ + ^M5,6Ti⁴⁺→^M8(Th,U)⁴⁺ + ^M5,6 (Mg,Fe)²⁺.     

Discrete dislocation dynamics: an important recent break-through in the modelling of dislocation collective behaviour

Recent results obtained by 3D discrete Dislocation Dynamics (DD) simulations are reviewed. Firstly, in the case of fatigued AISI 316L stainless steel, it is shown how DD simulations can both explain the formation of persistent slip bands and give a criterion for crack initiation. The same study is performed in the case of precipitate hardened metals where the precipitate size plays a crucial role. Secondly, we show how molecular dynamics (MD) simulations can feed the DD simulations for two applications. The first concerns the modelling of BCC Fe for which the dislocation mobility is derived from MD simulations. The second considers the modelling of irradiated stainless steels (FCC), where MD is used to define the local rules of interactions between dislocations and Frank loops. To cite this article: M.C. Fivel, C. R. Physique 9 (2008).     

Formation and growth of dislocation loops in ZnTe under irradiation of low energy Ar+-Ions

Abstract

Defects produced in ZnTe single crystals by Ar⁺ bombardment during ion milling for transmission electron microscopy studies are investigated in detail. The defects have been identified to be interstitial type Frank loops. Influences of ion energy and specimen temperature during the irradiation on the defect geometry are investigated. A model is proposed to describe the growing up of the loops.     

Three dimensional accurate morphology measurements of polystyrene standard particles on silicon substrate by electron tomography

Polystyrene latex (PSL) nanoparticle (NP) sample is one of the most widely used standard materials. It is used for calibration of particle counters and particle size measurement tools. It has been reported that the measured NP sizes by various methods, such as Differential Mobility Analysis, dynamic light scattering (DLS), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM), differ from each other. Deformation of PSL NPs on mica substrate has been reported in AFM measurements: the lateral width of PSL NPs is smaller than their vertical height. To provide a reliable calibration standard, the deformation must be measured by a method that can reliably visualize the entire three dimensional (3D) shape of the PSL NPs. Here we present a method for detailed measurement of PSL NP 3D shape by means of electron tomography in a transmission electron microscope. The observed shape of the PSL NPs with 100 nm and 50 nm diameter were not spherical, but squished in direction perpendicular to the support substrate by about 7.4% and 12.1%, respectively. The high difference in surface energy of the PSL NPs and that of substrate together with their low Young modulus appear to explain the squishing of the NPs without presence of water film.     

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。     

Transmission electron microscopy of dislocations in cementite deformed at high pressure and high temperature

Polycrystalline aggregates of cementite (Fe₃C) and (Fe,Ni)₃C have been synthesised at 10 GPa and 1250 °C in the multianvil apparatus. Further, deformation of the carbides by stress relaxation has been carried out at temperature of 1250 °C and for 8 h at the same pressure. Dislocations have been characterised by transmission electron microscopy. They are of the [1?0?0] and [0?0?1] type, [1?0?0] being the most frequent. [1?0?0] dislocations are dissociated and glide in the (0?1?0) plane. [0?0?1] dislocations glide in (1?0?0) and (0?1?0). Given the plastic anisotropy of cementite, the morphology of the lamellae in pearlitic steels appears to have a major role in the strengthening role played by this phase, since activation of easy slip systems is geometrically inhibited in most cases.     

Electron radiation damage in copper in the high voltage electron microscope

The various factors influencing the nucleation of radiation damage in the HVEM are reviewed. A method for obtaining quantitative information from observations is given. The effect of reirradiation at room temperature on the damage formed at elevated temperatures is shown. This effect may give experimental information concerning the strain fields surrounding large dislocation loops.     

Transmission electron microscopy observation of a deformation twin in TWIP steel by an ex situ tensile test

The formation of deformation twins in twinning-induced plasticity steels was observed in transmission electron microscope by an ex situ tensile test. The twinning process initially includes formation of extended dislocations at primary slip plane, then cross-slip to a conjugate slip plane with dissociation of the leading partial into a stair-rod dislocation and an emitted partial, and finally un-faulting of the original faults and formation of Frank partials. Repetition of the operation of the process on successive conjugate planes results in the formation of deformation twins. The formation mechanism of deformation twins can thus be explained by improving the stair-rod cross-slip model.     

Transmission electron microscopy of single wall carbon nanotube/polymer nanocomposites: A first‐principles study

The physics of high resolution transmission electron microscopy (HRTEM) image formation and electron diffraction of single wall carbon nanotubes (SWCNTs) in a polymer matrix was investigated theoretically on the basis of the multislice method. The effect of the nanocomposite thickness on both image contrast and typical electron diffraction reflections of the nanofillers was explored. The implications of the results on the experimental applicability to study dispersion, chirality and diameter of nanofillers are discussed. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Revisiting the defect structure of MAX phases: the case of Ti4AlN3

Microstructural study of as-grown Ti₄AlN₃ MAX phase has been performed by transmission electron microscopy. Dislocation walls, dislocation nucleation sites and stacking faults are described. In particular, diffraction contrast analysis combined with high-resolution images give a new insight into the nature of the stacking faults: contrarily to what is usually postulated, it is shown that the stacking faults possess a shear component in the basal plane. The stacking faults are created by the insertion of MX layers in the lattice via diffusion mechanisms. Their possible role on the deformation mechanism of MAX phases is discussed.     

Correlative atomic scale characterisation of secondary carbides in M50 bearing steel

Correlative atom probe tomography (APT) and transmission electron microscopy (TEM) are used to characterise the microstructure and chemistry of carbide precipitation in M50 bearing steel. This is a prerequisite in establishing relationships between the microstructure and hydrogen embrittlement (HE) resistance. Secondary carbides are the focus of this study, as they play a major role in improving HE-resistance. Secondary carbides are observed in APT, with compositions close to M₄C_3, M₂C and M₃C. Correlative TEM measured orientation relationships between the martensite matrix and carbides, enabling the confirmation of M₃C cementite precipitates in the corresponding APT reconstruction. Additionally, other precipitates observed in TEM were correlated to the M₂C carbides in APT data. The M₄C₃ carbides are found to have a significantly lower volume fraction than the M₂C carbides.     

High-resolution transmission electron microscopy investigation of the nanostructure of undoped and Pt-doped nanocrystalline pulsed laser deposited SnO2 thin films

Pulsed laser deposition (PLD) was used to grow nanocrystalline SnO₂ thin films onto alumina substrates. The reactive PLD process was carried out at different substrate deposition temperatures (T_d) between 20 and 600 °C under an oxygen background pressure of 150 mtorr. The same PLD technique was used to produce SnO₂ films in situ-doped with Pt (at the level of ∼2 at. %) through the concomitant ablation of both SnO₂ target and Pt strips. Conventional and high-resolution transmission electron microscopy (HRTEM) observations have revealed that the microstructure of the PLD SnO₂ films is highly sensitive to their deposition temperature. Indeed, its changes from a porous granular structure with extremely fine equiaxed grains (∼4 nm diameter), at T_d=20 °C to a very compact and textured columnar structure characterized by SnO₂ columns (∼25 nm diameter) composed of grains of ∼12 nm of diameter, at T_d=600 °C. In addition, the PLD SnO₂ films were found to exhibit the highest nanoporosity at T_d=300 °C which also coincides with the granular-to-columnar microstructural transition. On the other hand, the microstructure of the Pt-doped SnO₂ films, deposited at 300 °C, was found to contain a high density of defects, such as twin boundaries and edge dislocations. By combining HRTEM and EDS microanalysis, we were able to show that the Pt-dopant self-organizes into spherical nanoparticles (1-2 nm diameter) randomly distributed at the SnO₂ grain boundaries. Finally, doping the films with such platinum nanoclusters is found to affect the SnO₂ nanostructure by particularly reducing the SnO₂ mean grain size (from ∼10 nm when undoped to ∼6 nm for the doped films).     

An electron microscopic study of the archaeal feast/famine regulatory protein: 3. Labeling of the N-terminus using nickel

Histidine residues added to the N-terminus of a polypeptide (i.e. a His-tag) was used, for the first time to our knowledge, for electron labeling of the protein upon its electron spectroscopic imaging. Originally such a His-tag was developed by another group to purify modified proteins by taking advantage of their affinity to nickel. The feast/famine regulatory protein pot0434017 (FL11) was modified by adding six His residues to its N-terminus, so that each His pair would chelate a nickel ion. An electron microscope was operated at 200 KeV, and the electrons that lost the energy by ~875 eV upon interaction with the metal were selectively focused. The majority, 60–70%, of the spots detected in the electron micrographs were paired by distances shorter than 80 Å, and over 70% of them were paired by distances shorter than 40 Å. It is concluded that the protein molecules formed dimers, and the termini of most of the protein molecules were labeled with nickel by this method.