Micro-structural characterization of precipitation-synthesized fluorapatite nano-material by transmission electron microscopy using different sample preparation techniques

Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.     

Structure and orientation of an intermetallic phase in a W-Ni-Co alloy

The aim of this investigation is crystal structure determination of an intermetallic phase formed in a W-Ni-Co alloy during a heat-treatment carried out at a temperature of 800°C. This intermetallic phase is expected to play a critical role on the final microstructure (fine tungsten particles in an FCC matrix that is present in between large tungsten grains) and thereby, on the properties of the alloy. 92W-5.3Ni-2.7Co alloy was prepared through powder metallurgy route (liquid phase sintering) followed by heat-treatment at 800°C for 5?h. The intermetallic phase formed at this temperature was characterised using transmission and scanning electron microscopes. The intermetallic phase was found to have orthorhombic crystal structure with Pnam (62) space group as determined using automated diffraction tomography along with precession electron diffraction. Chemical analysis in TEM suggested that the intermetallic phase is based on stoichiometry (Co,Ni)₂W. Orientation imaging of the phase was also carried out in TEM and EBSD to understand its evolution. Equiaxed or lath morphology of the intermetallic phase was found to depend on the crystallographic orientation relationship of the phase with the tungsten grains and the matrix phase.     

Analysis of the spatial orientation distribution of building blocks in polycrystals as determined using transmission electron microscopy and a backscattered electron beam in a scanning electron microscope

The advantages and disadvantages of the method of automatic analysis of electron backscattering diffraction (EBSD) patterns for studying spatial orientation distributions are considered as compared to transmission electron microscopy (TEM). A misorientation spectrum in a test alloy (Kh20N80 alloy) having a high content of annealing twins is experimentally studied using both TEM and EBSD, and the results obtained are compared.     

Applications of the electron backscatter diffraction technique to ceramic materials

A technique with a relatively high spatial resolution is required for an effective analysis of the microstructure of ceramic materials. The recently developed electron backscatter diffraction (EBSD) technique, which works within a scanning electron microscope, enables a spatially highly resolved study of crystallographic orientations while recording Kikuchi patterns on a user-defined grid. However, such an EBSD texture analysis was until now not often performed on ceramic materials – in contrary, the technique is widely employed in the analysis of metallic materials, including the investigation of various types of steels. The use of ceramics possesses a variety of problems for EBSD investigations like: (i) complicated crystal structure, (ii) difficult surface preparation, and (iii) problems arising from a low conductivity of the ceramic materials. Here, we discuss these problems and present solutions in order to obtain high-quality Kikuchi patterns from such ceramics.     

Recent Developments of Crystallographic Analysis Methods in the Scanning Electron Microscope for Applications in Metallurgy

The field of metallurgy has greatly benefited from the development of electron microscopy over the last two decades. Scanning electron microscopy (SEM) has become a powerful tool for the investigation of nano- and microstructures. This article reviews the complete set of tools for crystallographic analysis in the SEM, i.e., electron backscatter diffraction (EBSD), transmission Kikuchi diffraction (TKD), and electron channeling contrast imaging (ECCI). We describe recent relevant developments in electron microscopy, and discuss the state-of-the-art of the techniques and their use for analyses in metallurgy. EBSD orientation measurements provide better angular resolution than spot diffraction in TEM but slightly lower than Kikuchi diffraction in TEM, however, its statistical significance is superior to TEM techniques. Although spatial resolution is slightly lower than in TEM/STEM techniques, EBSD is often a preferred tool for quantitative phase characterization in bulk metals. Moreover, EBSD enables the measurement of lattice strain/rotation at the sub-micron scale, and dislocation density. TKD enables the transmitted electron diffraction analysis of thin-foil specimens. The small interaction volume between the sample and the electron beam enhances considerably the spatial resolution as compared to EBSD, allowing the characterization of ultra-fine-grained metals in the SEM. ECCI is a useful technique to image near-surface lattice defects without the necessity to expose two free surfaces as in TEM. Its relevant contributions to metallography include deformation characterization of metals, including defect visualization, and dislocation density measurements. EBSD and ECCI are mature techniques, still undergoing a continuous expansion in research and industry. Upcoming technical developments in electron sources and optics, as well as detector instrumentation and software, will likely push the border of performance in terms of spatial resolution and acquisition speed. The potential of TKD, combined with EDS, to provide crystallographic, chemical, and morphologic characterizations of nano-structured metals will surely be a valuable asset in metallurgy.     

Disorder trapping and grain refinement during solidification of undercooled Fe–18 at% Ge melts

The electromagnetic levitation technique has been used to systematically study microstructure evolution and growth rate as a function of undercooling in concentrated Fe–18 at% Ge alloy. The samples are undercooled to a maximum of 240?K. Growth-rate analysis and transmission electron microscopy reveal that, beyond an undercooling of 120?K, the primary phase to solidify is disordered. Microstructural investigations show a decrease in grain size with increasing undercooling. Orientation-imaging microscopy using electron back-scattered diffraction (EBSD) and microhardness measurements have been used to show that recovery and recrystallization play a significant role in the evolution of final microstructure. Microstructural evolution has also been discussed in light of current models of dendrite growth and grain refinement.     

Correlating Raman peak shifts with phase transformation and defect densities: a comprehensive TEM and Raman study on silicon

Silicon is the most often used material in micro electromechanical systems (MEMS). Detailed understanding of its mechanical properties as well as the microstructure is crucial for the reliability of MEMS devices. In this paper, we investigate the microstructure changes upon indentation of single crystalline (100) oriented silicon by transmission electron microscopy (TEM) and Raman microscopy. TEM cross sections were prepared by focused ion beam (FIB) at the location of the indent. Raman microscopy and TEM revealed the occurrence of phase transformations and residual stresses upon deformation. Raman microscopy was also used directly on the cross‐sectional TEM lamella and thus microstructural details could be correlated to peak shape and peak position. The results show, however, that due to the implanted Ga⁺ ions in the lamella the silicon Raman peak is shifted significantly to lower wavenumbers. This hinders a quantitative analysis of residual stresses in the lamella. Furthermore, Raman microscopy also possesses the ability to map deformation structures with a lateral resolution in the submicron range. Copyright © 2009 John Wiley & Sons, Ltd.     

Case studies on the application of high-resolution electron channelling contrast imaging – investigation of defects and defect arrangements in metallic materials

In 1967, Coates discovered the electron channelling contrast of backscattered electrons (BSEs) in scanning electron microscopy, and by this the possibility to investigate arrangements of lattice defects in deformed microstructures of materials. Since that time, a straightforward development of the scanning electron microscopes as well as of the electron channelling contrast technique took place. Nowadays, the performance of scanning electron microscopes is high enough that the resolution of electron channelling contrast imaging (ECCI) micrographs is comparable with conventional bright field transmission electron microscopy (TEM) micrographs. In the first part of the present paper, a historical review on the development of the ECCI technique starting from its discovery more than 45 years ago up to the combination with other advanced methods of scanning electron microscopy like electron backscatter diffraction or high-resolution selected area channelling patterning in the last few years is given. Major important investigations using this technique for the visualization of individual lattice defects like stacking faults (SFs) and dislocations or dislocation arrangements are chronologically summarized. The second part demonstrates that nowadays, ECCI micrographs taken in high-resolution scanning electron microscopes can be called high-resolution ECCI (HR-ECCI). It is shown that the resolution of individual SFs and dislocations in the HR-ECCI micrographs is comparable to that of conventional TEM (about 15 nm defect image width). Furthermore, the paper is demonstrating that HR-ECCI micrographs can be obtained for various types of materials after different mechanical loadings and different grain sizes ranging from large grain size of 500 μm (cast steel) down to less than 2 μm (γ-TiAl).     

Recovery mechanisms in nanostructured aluminium

Commercial purity aluminium (99.5%) has been cold rolled to a true strain of 5.5 (99.6% reduction in thickness). The material is very strong but low temperature recovery may be a limiting factor. This has been investigated by isothermal annealing treatments in the temperature range 5–100°C. Hardness tests, microstructural investigations by electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM) were carried out to identify and characterise possible recovery mechanisms. Annihilation of zigzagged dislocations, positioned between deformation-induced lamellar boundaries of medium-to-high angles, and annihilation of dislocations in boundaries were found to be important recovery mechanisms, whereas other mechanisms, such as triple junction motion, subgrain coalescence, and boundary migration, were less important or negligible. The recovery kinetics was analysed based on hardness data, showing that the apparent activation energy for recovery at low temperatures was 60–86?kJ?mol^?1, consistent with thermally activated glide of jogged interior dislocations and the climb of dislocations in boundaries. These mechanisms are restricted by the presence of small intermetallic particles, which pin dislocations and boundaries and thereby raise the stability of the heavily deformed material.     

Size distribution and volume fraction of T1 phase precipitates from TEM images: Direct measurements and related correction

Transmission Electron Microscopy (TEM) can be used to measure the size distribution and volume fraction of fine scale precipitates in metallic systems. However, such measurements suffer from a number of artefacts that need to be accounted for, related to the finite thickness of the TEM foil and to the projected observation in two dimensions of the microstructure. We present a correction procedure to describe the 3D distribution of disc-like particles and apply this method to the plate-like T₁ precipitates in an Al–Li–Cu alloy in two ageing conditions showing different particle morphologies. The precipitates were imaged in a High-Angular Annular Dark Field Microscope (HAADF-STEM). The corrected size distribution is further used to determine the precipitate volume fraction. Atom probe tomography (APT) is finally utilised as an alternative way to measure the precipitate volume fraction and test the validity of the electron microscopy results.     

当谈论球差校正透射电镜时，我们在谈论什么？

透射电子显微镜(简称透射电镜)是能够直观分析材料微结构的最重要工具之一。在透射电镜近百年的发展历史中,近些年来球差校正透射电镜的研发与应用乃是最具革命性的发展,不但进一步延伸了通向微观世界之路,更为材料科学的快速发展提供了关键的工具与研究方法。文章通过介绍球差校正透射电镜的原理、优势、应用及发展,来回答“什么是球差校正透射电镜”,“球差校正透射电镜有什么突出作用”,“球差校正透射电镜除了拍原子还能做什么”这三个问题。     

An investigation of misfit dislocations in Al on (001) GaAs grown by chemical beam epitaxy

We report a transmission electron microscope study of the morphology and interfacial structure of Aluminium grown on (001) GaAs by chemical beam epitaxy (CBE). The Al grows in islands for all thicknesses deposited, and exhibits four distinct orientation relationships with respect to the substrate. One of these orientation relationships becomes dominant as growth progresses, with (011)_Al parallel to (001)_GaAs. Misfit dislocations can be seen in the interface between this orientation and the substrate with Burgers vector 1/4(110)_GaAs, and a crystallographic analysis shows that these dislocations are associated with interfacial steps of height 1/2[001]_GaAs. In (001)Al on (001)GaAs, the existence of these dislocations has in the past been regarded as evidence for the existence of a rigid-body shift of the Al in the interfacial plane. Using cross-sectional high-resolution TEM, it is shown that this shift is not present in the (011) orientation. The similarity in the microstructure and crystallography of the (001) and (011) orientations leads us to suggest that there is also no shift in (001) Al on (001)GaAs. This is in conflict with previous investigations of this system using a wide variety of techniques.     

Optical and structural characterization of a self-aligned single electron transitor structure by cathodoluminescence microscopy

We report about optical and structural investigations of a self-aligned single electron transistor (SET) structure using cathodoluminescence-(CL) and transmission electron microscopy (TEM). The SET structures were fabricated by MBE growth of GaAs/AlAs on different prepatterned GaAs (1 0 0) substrates. This technique for the in situ formation of nanoscopic semiconductor heterostructures is presently a widely used and promising approach for the fabrication of low-dimensional systems like quantum wires and quantum dots (QD). The active region of the SET structure consists of a GaAs/AlGaAs-QD formed by thickness modulation of a single quantum well (SQW) during the MBE growth. The position and the size of the QD is defined by the design of the substrate pattern. The thickness modulation of the GaAs-SQW is evidenced by TEM investigations. The lateral confinement potential given by the thickness modulation of GaAs-SQW is directly imaged by CL microscopy.     

3D processing map and hot deformation behaviour of a new type Al–Zn–Mg alloy

ABSTRACT

The thermal compression behaviour of Al–Zn–Mg alloy was studied on a thermal simulator machine at the temperature range of 380–540°C and strain rate range of 0.01–10?s^?1. The constitutive equation and 3D processing map of the alloys were established. The microstructure characteristics of the alloy were studied by metallographic observation, electron back-scatter diffraction (EBSD) analysis and transmission electron microscopy (TEM) microstructure analysis. The results show that the peak stress of high-temperature deformation of alloy decreases with the increase of deformation temperature and increases with the increase of strain rate. The dynamic recovery of the alloy occurs at the temperature range of 380–460°C and the strain rate range of 0.01–0.1?s^?1. The dynamic recrystallization of the alloy occurs at the temperature range of 460–500°C and the strain rate range of 0.01–0.1?s^?1. The alloy maintains fine and uniform recrystallized grains at a temperature range of 460–480°C and a strain rate range of 0.01–0.1?s^?1, which is suitable for hot working.     

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。     

Surface modification of TA2 pure titanium by low energy high current pulsed electron beam treatments

Surface integrity changes of TA2 pure titanium including surface topography, microstructure and nanohardness distribution along surface layer were investigated by different techniques of low energy high current pulsed electron beam treatments (LEHCPEBTs). The surface topography was characterized by SEM. Moreover, the TEM observation and X-ray diffraction analysis were performed to reveal the surface modification mechanism of TA2 pure titanium by LEHCPEBTs. The surface roughness was modified by electron beam treatment and the polishing mechanism was analyzed by studying the cross section microstructure of electron beam treated specimens by SEM and TEM. The results show that the surface finish obtains good polishing quality and there is no phase transformation but the dislocations by LEHCPEBT. Furthermore, the nanohardness in the surface modified layer is improved. The remelt and fine-grain microstructure of surface layer caused by LEHCPEBTs are the main polishing mechanism and the reason of modification of surface topography and the increment in nanohardness is mainly due to the dislocations and fine grains in the modified layer induced by LEHCPEBT.     

TEM study on hollow and prepared from porous Cu20 nanoparticles solution phase

In this paper, hollow and porous Cu2O nanoparticles were prepared by adjusting the cationic surfactant cetyltrimethylammonium （CTAB） concentration in the solution-phase reaction. Structural investigations reveal that Cu2Onanoparticles can be either well-defined hollow nanoboxes or porous nanocubes depending on the synthesis conditions. The transmission electron microscopy （TEM） observations demonstrated that the nanoparticles in general are composed of small grains coherently growing along certain preferred orientations.     

Field emission scanning electron microscopy (FE-SEM) as an approach for nanoparticle detection inside cells

When developing new nanoparticles for bio-applications, it is important to fully characterize the nanoparticle's behavior in biological systems. The most common techniques employed for mapping nanoparticles inside cells include transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). These techniques entail passing an electron beam through a thin specimen. STEM or TEM imaging is often used for the detection of nanoparticles inside cellular organelles. However, lengthy sample preparation is required (i.e., fixation, dehydration, drying, resin embedding, and cutting). In the present work, a new matrix (FTO glass) for biological samples was used and characterized by field emission scanning electron microscopy (FE-SEM) to generate images comparable to those obtained by TEM. Using FE-SEM, nanoparticle images were acquired inside endo/lysosomes without disruption of the cellular shape. Furthermore, the initial steps of nanoparticle incorporation into the cells were captured. In addition, the conductive FTO glass endowed the sample with high stability under the required accelerating voltage. Owing to these features of the sample, further analyses could be performed (material contrast and energy-dispersive X-ray spectroscopy (EDS)), which confirmed the presence of nanoparticles inside the cells. The results showed that FE-SEM can enable detailed characterization of nanoparticles in endosomes without the need for contrast staining or metal coating of the sample. Images showing the intracellular distribution of nanoparticles together with cellular morphology can give important information on the biocompatibility and demonstrate the potential of nanoparticle utilization in medicine.     

UHV-HREM and diffraction of surfaces

Characterization of the structure of surfaces is very important in order to develop a fundamental understanding of the electronic, mechanical and chemical properties of a material. While transmission electron microscopy imaging (TEM) and diffraction (TED) techniques are capable of providing surface structural information at the atomic level, such data would be suspect if obtained under conventional vacuum conditions (10^-6–10^-8 Torr). Ultrahigh vacuum (UHV) conditions are imperative during both preparation and observation of clean surfaces/interfaces. Conventional TEM techniques are very powerful for UHV-TEM investigations; however, the marriage of surface science and conventional TEM to yield an UHV-TEM is a complex task. These complexities and some of the results obtained using UHV-TEM and UHV-TED techniques for surfaces i.e. solid-vacuum interfaces will be illustrated.     

Mesoscale strain measurement in deformed crystals: A comparison of X-ray microdiffraction with electron backscatter diffraction

Mapping of residual stresses at the mesoscale is increasingly practical thanks to technological developments in electron backscatter diffraction (EBSD) and X-ray microdiffraction using high brilliance synchrotron sources. An analysis is presented of a Cu single crystal deformed in compression to about 10% macroscopic strain. Local orientation measurements were made on sectioned and polished specimens using EBSD and X-ray microdiffraction. In broad strokes, the results are similar to each other with orientations being observed that are on the order of 5° misoriented from that of the original crystallite. At the fine scale it is apparent that the X-ray technique can distinguish features in the structure that are much finer in detail than those observed using EBSD even though the spatial resolution of EBSD is superior to that of X-ray diffraction by approximately two orders of magnitude. The results are explained by the sensitivity of the EBSD technique to the specimen surface condition. Dislocation dynamics simulations show that there is a relaxation of the dislocation structure near the free surface of the specimen that extends approximately 650 Å into the specimen. The high spatial resolution of the EBSD technique is detrimental in this respect as the information volume extends only 200 Å or so into the specimen. The X-rays probe a volume on the order of 2 µm in diameter, thus measuring the structure that is relatively unaffected by the near-surface relaxation.