Electron microscopy of layered single crystals grown by direct vapour transport method

Besides interesting properties such as optical, transport, structure, etc. possessed by crystals of transition metal dichalcogenides, they have also been found to have a potential application in the fabrication ofpec solar cells. These crystals are normally grown by carrier gas transport technique but are always contaminated by carrier gases. A new method of direct vapour transport has been developed and successfully applied to grow these crystals including those of off-stoichiometric varieties. The crystals thus grown have been characterized structurally using the techniques of x-ray powder, rotation and Weissenberg photographs and electron diffraction. Perfection studies have been made by techniques like chemical etching and electron microscopy. This review describes the electron microscopic studies made on the single crystals of the layered compounds. High resolution technique of weak beam has been employed to study dislocation pattern. Dissociated dislocations have been used to estimate stacking fault energy. Such measurements have also been carried out at different temperatures and the variation of stacking fault energy with temperature has been worked out. Interesting information regarding phase transformation for TaS₂ and W₃Se₄ in the temperature range 109 to 580 K has been derived from the electron diffraction studies and the implications have been discussed.     

High voltage electron microscope irradiation and observations in metallic glasses

High voltage electron microscope (hvem) has been extensively used to produce radiation damage and to study the characteristics of defects so produced in crystalline solids. To understand the defect production in metallic glasses and to evaluate the influence of such defects on physical properties like crystallisation temperature etc., high voltage microscopy and subsequentin situ heating and observation has been extremely useful technique. This paper gives a qualitative overview of such work performed in metallic glasses. In particular results obtained on a nickel based metallic glass using ahvem and an electron accelerator are presented. The advantages and limitations ofhvem irradiation are highlighted.     

Direct observation of local atomic order in a metallic glass

The determination of the atomic configuration of metallic glasses is a long-standing problem in materials science and solid-state physics. So far, only average structural information derived from diffraction and spectroscopic methods has been obtained. Although various atomic models have been proposed in the past fifty years, a direct observation of the local atomic structure in disordered materials has not been achieved. Here we report local atomic configurations of a metallic glass investigated by nanobeam electron diffraction combined with ab initio molecular dynamics simulation. Distinct diffraction patterns from individual atomic clusters and their assemblies, which have been theoretically predicted as short- and medium-range order, can be experimentally observed. This study provides compelling evidence of the local atomic order in the disordered material and has important implications in understanding the atomic mechanisms of metallic-glass formation and properties.     

Twin roller quenching technique and preparation of glasses of high melting ionic solids

A rapid quenching technique with a quenching rate of roughly 10⁶°C/sec has been developed to prepare glassy samples of ABO₃ type materials. Glasses of potassium lithium niobate have been prepared by this technique. These glasses have been characterized by x-ray diffraction, electron diffraction and differential scanning calorimetry techniques to assess the quality of the obtained glasses. Contribution No. 74 from Materials Research Laboratory     

Formation, Structure and Properties of Bulk Metallic Glasses

1.IntroductionTheformationofmetallicglassesbydirectquench-ingfromthemeltwasfirstdiscoveredin196obyDuwezandhisco-workersinaAu-25at.pctSialloy[']bya'guntechnique'[2].Thistechniqueen-abledcoolingrateoflo6K/s,thuscreatinganewseriesofmaterials.Thediscoveryofmetal1icglassesandmetastab1ephasehasledto-explosiveresearchanddevelopmefltofmetallicglassesandothercrys-tallinematerialsquenchedfrommelt[3'4].Metallicglasses,whichareobtainedbytherapidquenchingofmetallicmelts,arenoncrystallineoramorphous,likeo…     

Two-liquid phase structure of photoconducting oxide glasses

An electron microscopic study of a series of photoconducting oxide glasses in the systems CdO/B₂O₃/SiO₂, CdO/B₂O₃/GeO₂ and PbO/Al₂O₃/SiO₂, has shown the essential diphasic nature of these materials. The samples were examined by replica techniques, in transmission and by scanning electron microscopy. Two-liquid features have been identified, as has very fine-scale crystallisation, both on the basis of textures of fracture surfaces and of electron diffraction patterns. Physical models proposed to explain the electronic properties of glasses such as these must take account of this obvious two-phase nature of such materials.     

X-ray spectroscopy and local structures in glasses

X-ray spectroscopy which is a combination of two techniques, namely x-ray absorption near edge structure (xanes) and extended x-ray absorption fine structure (EXAFS) analyses, is a unique technique for the study of local structures in glasses. Availability of synchrotron radiation sources has made the technique quite attractive and useful because the photon flux from synchrotrons is very intense and polarized. In this article, a brief summary ofxanes andEXAFS techniques is given along with a few applications to the study of local structures in glasses. Communication No. 323 from Solid State and Structural Chemistry Unit.     

Medium-range order dictates local hardness in bulk metallic glasses

Bulk metallic glasses (BMGs) are materials with outstanding strength and elastic properties that make them tantalizing for engineering applications, yet our poor understanding of how their amorphous atomic arrangements control their broader mechanical properties (hardness, wear, fracture, etc.) impedes our ability to apply materials science principles in their design. In this work, we uncover the hierarchical structure that exists in BMGs across the nano- to microscale by using nanobeam electron diffraction experiments. Our findings reveal that local hardness of microscale domains decreases with increasing size and volume fraction of atomic clusters with higher local medium range order (MRO). Furthermore, we propose a model of ductile phase softening that will enable the future design of BMGs by tuning the MRO size and distribution in the nanostructure.     

Carbon nanocones: wall structure and morphology

Abstract

Large-scale production of conical carbon nanostructures is possible through pyrolysis of hydrocarbons in a plasma torch process. The resulting carbon cones occur in five distinctly different forms, and disc-shaped particles are produced as well. The structure and properties of these carbon cones and discs have been relatively little explored until now. Here we characterize the structure of these particles using transmission electron microscopy, synchrotron x-ray and electron diffraction. The carbon nanocones are found to exhibit several interesting structural features; instead of having a uniform cross-section, the walls consist of a relatively thin inner graphite-like layer with a non-crystalline envelope, where the amount of the latter can be modified significantly by annealing. The cones appear with a well-defined faceting along the cone edge, demonstrating strict long-range atomic ordering; they also present occasional examples of symmetry breaking, such as two apexes appearing in the same carbon nanocone.     

Carbon nanocones: wall structure and morphology

Large-scale production of conical carbon nanostructures is possible through pyrolysis of hydrocarbons in a plasma torch process. The resulting carbon cones occur in five distinctly different forms, and disc-shaped particles are produced as well. The structure and properties of these carbon cones and discs have been relatively little explored until now. Here we characterize the structure of these particles using transmission electron microscopy, synchrotron x-ray and electron diffraction. The carbon nanocones are found to exhibit several interesting structural features; instead of having a uniform cross-section, the walls consist of a relatively thin inner graphite-like layer with a non-crystalline envelope, where the amount of the latter can be modified significantly by annealing. The cones appear with a well-defined faceting along the cone edge, demonstrating strict long-range atomic ordering; they also present occasional examples of symmetry breaking, such as two apexes appearing in the same carbon nanocone.     

Polyamorphism in a metallic glass

A metal, or an alloy, can often exist in more than one crystal structure. The face-centred-cubic and body-centred-cubic forms of iron (or steel) are a familiar example of such polymorphism. When metallic materials are made in the amorphous form, is a parallel 'polyamorphism' possible? So far, polyamorphic phase transitions in the glassy state have been observed only in glasses involving directional and open (such as tetrahedral) coordination environments. Here, we report an in situ X-ray diffraction observation of a pressure-induced transition between two distinct amorphous polymorphs in a Ce(55)Al(45) metallic glass. The large density difference observed between the two polyamorphs is attributed to their different electronic and atomic structures, in particular the bond shortening revealed by ab initio modelling of the effects of f-electron delocalization. This discovery offers a new perspective of the amorphous state of metals, and has implications for understanding the structure, evolution and properties of metallic glasses and related liquids. Our work also opens a new avenue towards technologically useful amorphous alloys that are compositionally identical but with different thermodynamic, functional and rheological properties due to different bonding and structural characteristics.     

Electron Diffraction Using Transmission Electron Microscopy

Electron diffraction via the transmission electron microscope is a powerful method for characterizing the structure of materials, including perfect crystals and defect structures. The advantages of electron diffraction over other methods, e.g., x-ray or neutron, arise from the extremely short wavelength (≈2 pm), the strong atomic scattering, and the ability to examine tiny volumes of matter (≈10 nm³). The NIST Materials Science and Engineering Laboratory has a history of discovery and characterization of new structures through electron diffraction, alone or in combination with other diffraction methods. This paper provides a survey of some of this work enabled through electron microscopy.     

Fabrication of Cu rich bulk metallic glass composites via solidification method

Abstract

Cu based bulk metallic glasses and composites with tiny crystalline phases embedded in metallic glass matrix have been successfully fabricated by solidification technique in the present work. The formation of crystalline phases and structure inhomogeneity in bulk metallic glasses was characterised. Al is used as the minor alloying element to partly substitute Cu element in 61Cu–34Zr–5Ti. The results show that quarternary 60Cu–34Zr–5Ti–1Al alloy exhibits monoamorphous feature, and 56Cu–34Zr–5Ti–5Al alloy has a few crystalline peaks superimposed on a broad diffraction peak, suggesting that a composite structure forms in certain solidification conditions. To further identify the microstructure of the as cast rod, all samples were characterised by scanning electron microscopy (SEM). Small size phases are found in 2 mm diameter 56Cu–34Zr–5Ti–5Al rod, which has larger plastic deformation. The composition of those crystalline phases is also investigated. All results indicate that the presence of certain phases in metallic matrix benefits the mechanical properties of the as cast bulk metallic glasses.     

The potential of Zr-based bulk metallic glasses as biomaterials

Zr-based bulk metallic glasses (BMGs) are a new type of metallic materials with disordered atomic structure that exhibit high strength and high elastic strain, relatively low Young’s modulus, and excellent corrosion resistance and biocompatibility. The combination of these unique properties makes the Zr-based BMGs very promising for biomaterials applications. In this review article, the authors give an overview of the recent progress in the study of biocompatibility of Zr-based BMGs, especially the relevant work that has been done in the metallic glasses group in Huazhong University of Science and Technology (HUST), including the development of Ni-free Zr-based BMGs, the mechanical and wear properties, the bio-corrosion resistance, the in vitro and in vivo biocompatibility and the bioactive surface modification of these newly developed BMGs.     

Ferromagnetic resonance in metallic glasses: study of fracture,stress and thermal stability

Effects of fracture, stress and isothermal annealing of Fe-Ni based metallic glasses have been investigated using the ferromagnetic resonance technique.fmr linewidth is quite sensitive to changes in the magnetic and structural order in metallic glasses, andfmr lineshape seems to provide useful qualitative information on the mechanical state of these systems. Our observations are compared with recent work of Baianu and co-workers.     

Cobalt-containing core-shell nanoparticles on the surface of poly(tetrafluoroethylene) microgranules

Cobalt-containing nanoparticles have been prepared via thermal decomposition of cobalt acetate on the surface of poly(tetrafluoroethylene) (PTFE) microgranules forming a fluidized bed over the surface of hot mineral oil. Using transmission electron microscopy, the average size of the cobalt-containing nanoparticles has been determined to be 3.6 nm. The composition and structure of the nanoparticles have been determined by x-ray diffraction, extended x-ray absorption fine structure spectroscopy, and electron paramagnetic resonance, and the magnetic properties of the synthesized nanomaterial have been studied. The results indicate that the nanoparticles have a core-shell structure, with a metallic cobalt core (?10 vol%) and a shell consisting of three phases: Co₃O₄ (?80%) and small amounts of CoO and CoF₂ (?10%). The fluoride phase results from the interaction of the nanoparticles with surface fluorine atoms of the PTFE microgranules.     

Metallic glasses from “alchemy” to pure science: Present and future of design,processing and applications of glassy metals

Metallic glasses, first discovered a half century ago, are currently among the most studied metallic materials. Available in sizes up to several centimeters, with many novel, applicable properties, metallic glasses have also been the focus of research advancing the understanding of liquids and of glasses in general.Metallic glasses (MGs), called also bulk metallic glasses (BMGs) (or glassy metals, amorphous metals, liquid metals) are considered to be the materials of the future. Due to their high strength, metallic glasses have a number of interesting applications, for example as coatings. Metallic glasses can also be corrosion resistant. Metallic glasses, and the crystalline materials derived from them, can have very good resistance to sliding and abrasive wear. Combined with their strength – and now, toughness – this makes them ideal candidates for bio-implants or military applications. Prestigious Journals such as “Nature Materials”, “Nature” frequently publish new findings on these unusual glass materials. Moreover Chinese and Asian scientists have also been showing an interest in the study of metallic glasses.This review paper is far from exhaustive, but tries to cover the areas of interest as it follows: a short history, the local structure of BMGs and the glass forming ability (GFA), BMGs’ properties, the manufacturing and some applications of BMGs and finally, about the future of BMGs as valuable materials.     

Atomistic simulation and modeling of localized shear deformation in metallic glasses

Since the end of 1980s, bulk metallic glasses became available for various multi-component alloys. Because bulk metallic glasses are applicable to structural materials, their mechanical properties have become a matter of great interest in these decades. A characteristic feature of plastic deformation of metallic glasses at the ambient temperature is the localized shear deformation. Since we have no appropriate experimental technique, unlike crystalline matter, to approach microscopic deformation process in amorphous materials, we have to rely on computer simulation studies by use of atomistic models to reveal the microscopic deformation processes. In this article, we review atomistic simulation studies of deformation processes in metallic glasses, i.e., local shear transformation (LST), structural characterization of the local shear transformation zones (STZs), deformation-induced softening, shear band formation and its development, by use of elemental and metal-metal alloy models. We also review representative microscopic models so far proposed for the deformation mechanism: early dislocation model, Spaepen’s free-volume model, Argons’s STZ model and recent two-state STZ models by Langer et al.     

Growth of polysilicon and silicide films for MOS-VLSI application

Doped and undoped polycrystalline silicon films were grown byapcvd and thermal evaporation techniques. The effect of growth and annealing conditions on the crystalline nature of the films and their properties were studied by electrical, optical, x-ray diffraction andsem techniques. Metal silicides such as TiSi₂ and PtSi₂ were prepared by co-evaporation technique over polysilicon layers to study their suitability in microelectronic applications. Some of the properties of polysilicon and silicides are discussed.