Analytical solutions for some defect problems in 1D hexagonal and 2D octagonal quasicrystals

We study some typical defect problems in one-dimensional (1D) hexagonal and two-dimensional (2D) octagonal quasicrystals. The first part of this investigation addresses in detail a uniformly moving screw dislocation in a 1D hexagonal piezoelectric quasicrystal with point group 6mm. A general solution is derived in terms of two functions φ ₁, φ ₂, which satisfy wave equations, and another harmonic function φ ₃. Elementary expressions for the phonon and phason displacements, strains, stresses, electric potential, electric fields and electric displacements induced by the moving screw dislocation are then arrived at by employing the obtained general solution. The derived solution is verified by comparison with existing solutions. Also obtained in this part of the investigation is the total energy of the moving screw dislocation. The second part of this investigation is devoted to the study of the interaction of a straight dislocation with a semi-infinite crack in an octagonal quasicrystal. Here the crack penetrates through the solid along the period direction and the dislocation line is parallel to the period direction. We first derive a general solution in terms of four analytic functions for plane strain problem in octagonal quasicrystals by means of differential operator theory and the complex variable method. All the phonon and phason displacements and stresses can be expressed in terms of the four analytic functions. Then we derive the exact solution for a straight dislocation near a semi-infinite crack in an octagonal quasicrystal, and also present the phonon and phason stress intensity factors induced by the straight dislocation and remote loads.      

Contamination mitigation strategies for scanning transmission electron microscopy

Modern scanning transmission electron microscopy (STEM) enables imaging and microanalysis at very high magnification. In the case of aberration-corrected STEM, atomic resolution is readily achieved. However, the electron fluxes used may be up to three orders of magnitude greater than those typically employed in conventional STEM. Since specimen contamination often increases with electron flux, specimen cleanliness is a critical factor in obtaining meaningful data when carrying out high magnification STEM. A range of different specimen cleaning methods have been applied to a variety of specimen types. The contamination rate has been measured quantitatively to assess the effectiveness of cleaning. The methods studied include: baking, cooling, plasma cleaning, beam showering and UV/ozone exposure. Of the methods tested, beam showering is rapid, experimentally convenient and very effective on a wide range of specimens. Oxidative plasma cleaning is also very effective and can be applied to specimens on carbon support films, albeit with some care. For electron beam-sensitive materials, cooling may be the method of choice. In most cases, preliminary removal of the bulk of the contamination by methods such as baking or plasma cleaning, followed by beam showering, where necessary, can result in a contamination-free specimen suitable for extended atomic scale imaging and analysis.     

二维原子晶体的低电压扫描透射电子显微学研究

二维原子晶体材料,如石墨烯和过渡金属硫族化合物等,具有不同于其块体的独特性能,有望在二维半导体器件中得到广泛应用.晶体中的结构缺陷对材料的物理化学性能有直接的影响,因此研究结构缺陷和局域物性之间的关联是当前二维原子晶体研究中的重要内容,需要高空间分辨率的结构研究手段.由于绝大部分二维原子晶体在高能量高剂量的电子束辐照下容易发生结构损伤,利用电子显微方法对二维原子晶体缺陷的研究面临诸多挑战.低电压球差校正扫描透射电子显微(STEM)技术的发展,一个主要目标就是希望在不损伤结构的前提下对二维原子晶体的本征结构缺陷进行研究.在STEM下,多种不同的信号能够被同步采集,包括原子序数衬度高分辨像和电子能量损失谱等,是表征二维原子晶体缺陷的有力工具,不但能对材料的本征结构进行单原子尺度的成像和能谱分析,还能记录材料结构的动态变化.通过调节电子束加速电压和电子辐照剂量,扫描透射电子显微镜也可以作为电子刻蚀二维原子晶体材料的平台,用于加工新型纳米结构以及探索新型二维原子晶体的原位制备.本综述主要以本课题组在石墨烯和二维过渡金属硫族化合物体系的研究为例,介绍低电压扫描透射电子显微学在二维原子晶体材料研究中的实际应用.     

Aberration-corrected scanning transmission electron microscopy for complex transition metal oxides

Lattice,charge,orbital,and spin are the four fundamental degrees of freedom in condensed matter,of which the interactive coupling derives tremendous novel physical phenomena,such as high-temperature superconductivity(high-T_c SC) and colossal magnetoresistance(CMR) in strongly correlated electronic system.Direct experimental observation of these freedoms is essential to understanding the structure-property relationship and the physics behind it,and also indispensable for designing new materials and devices.Scanning transmission electron microscopy(STEM) integrating multiple techniques of structure imaging and spectrum analysis,is a comprehensive platform for providing structural,chemical and electronic information of materials with a high spatial resolution.Benefiting from the development of aberration correctors,STEM has taken a big breakthrough towards sub-angstrom resolution in last decade and always steps forward to improve the capability of material characterization;many improvements have been achieved in recent years,thereby giving an indepth insight into material research.Here,we present a brief review of the recent advances of STEM by some representative examples of perovskite transition metal oxides;atomic-scale mapping of ferroelectric polarization,octahedral distortions and rotations,valence state,coordination and spin ordering are presented.We expect that this brief introduction about the current capability of STEM could facilitate the understanding of the relationship between functional properties and these fundamental degrees of freedom in complex oxides.     

2D atomic mapping of oxidation states in transition metal oxides by scanning transmission electron microscopy and electron energy-loss spectroscopy

Using a combination of high-angle annular dark-field scanning transmission electron microscopy and atomically resolved electron energy-loss spectroscopy in an aberration-corrected transmission electron microscope we demonstrate the possibility of 2D atom by atom valence mapping in the mixed valence compound Mn3O4. The Mn L(2,3) energy-loss near-edge structures from Mn2+ and Mn3+ cation sites are similar to those of MnO and Mn2O3 references. Comparison with simulations shows that even though a local interpretation is valid here, intermixing of the inelastic signal plays a significant role. This type of experiment should be applicable to challenging topics in materials science, such as the investigation of charge ordering or single atom column oxidation states in, e.g., dislocations.     

TDX-200透射电子显微镜自动曝光原理研究

通过分析透射电子显微镜的曝光机理,得出了荧光屏亮度与曝光时间之间的关系表达式。设计了TDX-200透射电子显微镜自动曝光电路,并通过实验对自动曝光参数进行了标定。通过对多种实际样品在不同工作模式下进行自动曝光试验,得到了相对清晰的电子显微像。结果表明,TDX-200透射电子显微镜自动曝光的设计满足要求。     

Graphene oxide monolayers as supporting films for high resolution transmission electron microscopy

A novel kind of TEM support composed of graphene oxide monolayers was fabricated by a facile solution-cast method. Compared to the conventional carbon supporting films, such graphene oxide film (GO-film) performed better stability under high-energy electron beams and better dispersion effect for water-soluble nanoparticles. Quantitative improvement in TEM imaging resolution for nanomaterials on such GO-films compared to the commercial ultrathin carbon films was demonstrated.     

Combined field ion microscopy and transmission electron microscopy of heavy ion damage in tungsten

Abstract

A field ion microscopy (FIM) and transmission electron microscopy (TEM) investigation of radiation damage in tungsten after heavy ion bombardment has been carried out. Field ion specimens of tungsten were irradiated with 180–230 keV Xe⁺ ions. The irradiation doses were varied between 4 × 10¹¹ and 4 × 10¹² ions/cm². The irradiated specimens were examined in FIM. Experiments combining both TEM and FIM were performed in order to compare the results obtainable by these two methods. The distribution of defects visible by TEM was inhomogeneous. The influence of the imaging field in FIM on the defects visible in TEM is discussed.     

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。     

Sample preparation by focused ion beam micromachining for transmission electron microscopy imaging in front-view

This article deals with the development of an original sample preparation method for transmission electron microscopy (TEM) using focused ion beam (FIB) micromachining. The described method rests on the use of a removable protective shield to prevent the damaging of the sample surface during the FIB lamellae micromachining. It enables the production of thin TEM specimens that are suitable for plan view TEM imaging and analysis of the sample surface, without the deposition of a capping layer. This method is applied to an indented silicon carbide sample for which TEM analyses are presented to illustrate the potentiality of this sample preparation method.     

Impact of dynamical scattering on quantitative contrast for aberration-corrected transmission electron microscope images

Aberration-corrected transmission electron microscope images taken under optimum-defocus conditions or processed offline can correctly reflect the projected crystal structure with atomic resolution. However, dynamical scattering, which will seriously influence image contrast, is still unavoidable. Here, the multislice image simulation approach was used to quantify the impact of dynamical scattering on the contrast of aberration-corrected images for a 3C-SiC specimen with changes in atomic occupancy and thickness. Optimum-defocus images with different spherical aberration (C_S) coefficients, and structure images restored by deconvolution processing, were studied. The results show that atomic-column positions and the atomic occupancy for SiC ‘dumbbells’ can be determined by analysis of image contrast profiles only below a certain thickness limit. This limit is larger for optimum-defocus and restored structure images with negative C_S coefficient than those with positive C_S coefficient. The image contrast of C (or Si) atomic columns with specific atomic occupancy changes differently with increasing crystal thickness. Furthermore, contrast peaks for C atomic columns overlapping with neighboring peaks of Si atomic columns with varied Si atomic occupancy, which is enhanced with increasing crystal thickness, can be neglected in restored structure images, but the effect is substantial in optimum-defocus images.     

Ultrastructural examination of dentin using focused ion-beam cross-sectioning and transmission electron microscopy

Focused ion-beam (FIB) milling is a commonly used technique for transmission electron microscopy (TEM) sample preparation of inorganic materials. In this study, we seek to evaluate the FIB as a TEM preparation tool for human dentin. Two particular problems involving dentin, a structural analog of bone that makes up the bulk of the human tooth, are examined. Firstly, the process of aging is studied through an investigation of the mineralization in ‘transparent’ dentin, which is formed naturally due to the filling up of dentinal tubules with large mineral crystals. Next, the process of fracture is examined to evaluate incipient events that occur at the collagen fiber level. For both these cases, FIB-milling was able to generate high-quality specimens that could be used for subsequent TEM examination. The changes in the mineralization suggested a simple mechanism of mineral ‘dissolution and reprecipitation’, while examination of the collagen revealed incipient damage in the form of voids within the collagen fibers. These studies help shed light on the process of aging and fracture of mineralized tissues and are useful steps in developing a framework for understanding such processes.     

3D scanning electron microscopy applied to surface characterization of fluorosed dental enamel

The enamel surfaces of fluorotic teeth were studied by scanning electron stereomicroscopy. Different whitening treatments were applied to 25 pieces to remove stains caused by fluorosis and their surfaces were characterized by stereomicroscopy in order to obtain functional and amplitude parameters. The topographic features resulting for each treatment were determined through these parameters. The results obtained show that the 3D reconstruction achieved from the SEM stereo pairs is a valuable potential alternative for the surface characterization of this kind of samples.     

In situ hot-stage transmission electron microscopy of Pb(Zr0.52Ti0.48)O3

The domain structure of Pb(Zr_0.52Ti_0.48)O₃ before and after hot-stage experiment has been studied. The influence of maximum temperature, heating and cooling rate on the domain configuration of Pb(Zr_{1? x} , Ti _x )O₃ with x = 0.40, 0.45, 0.48 and 0.55 was analysed. A reliable basis for further hot-stage experiments of Pb(Zr_1?x, Ti_x)O₃ has been established. The investigations revealed a temperature dependent appearance and disappearance of nano- and microdomains. The appearance of microdomains in the nano scale range during cooling, denoted as domain miniaturisation, and the time dependent recovering of the former domain structure, revealed that under specific experimental conditions the domain configuration is reversible.     

Instrumental requirements for the detection of electron beam-induced object excitations at the single atom level in high-resolution transmission electron microscopy

This contribution touches on essential requirements for instrument stability and resolution that allows operating advanced electron microscopes at the edge to technological capabilities. They enable the detection of single atoms and their dynamic behavior on a length scale of picometers in real time. It is understood that the observed atom dynamic is intimately linked to the relaxation and thermalization of electron beam-induced sample excitation. Resulting contrast fluctuations are beam current dependent and largely contribute to a contrast mismatch between experiments and theory if not considered. If explored, they open the possibility to study functional behavior of nanocrystals and single molecules at the atomic level in real time.     

Prospects of anionic nanolipoplexes in nanotherapy: transmission electron microscopy and light scattering studies

Currently nanosystems composed of polynucleotides and lipid vesicles (nanolipoplexes) are considered to be promising tools for gene therapeutics. Successful in vivo application of these vectors depends on their physicochemical, technological and biological characteristics including morphology, size distribution, molecular interactions and stability. Anionic nanoliposomes (DPPC:DCP:CHOL) were prepared by two different techniques, namely the conventional thin-film hydration method followed by extrusion, and the heating method (HM), in which no volatile solvent or detergent is used. A non-viral and non-cationic gene transfer vector was constructed by incorporating plasmid DNA (pcDNA3.1/His B/lacZ) to the HM-nanoliposomes by the electrostatic mediation of Ca²⁺ ions. Transfection efficiency of the nanolipoplexes was evaluated using a human bronchial epithelial cell line (16HBE14o-) in the presence of serum. Particle characterisation, stability of the formulations and lipid–DNA interaction studies were performed using transmission electron microscopy (TEM) and light scattering. TEM pictures of nanolipoplexes showed presence of two to four closely packed vesicles with signs of fusion. Efficient delivery of plasmid DNA and subsequent β-galactosidase expression was achieved using the anionic nanolipoplexes. Transfection efficiency increased with lipid:DNA ratio up to 7:1 (w/w), where transfection efficiency was 12-fold higher than in untreated cells. Further increase in lipid ratio decreased transfection. These nanolipoplexes appear to be safe, stable and efficient in the protection and delivery of DNA to different cells and tissues.     

A comparative study of nanoparticles in premixed flames by scanning mobility particle sizer, small angle neutron scattering, and transmission electron microscopy

Scanning mobility particle sizer (SMPS) and transmission electron microscopy (TEM) studies were conducted for TiO₂ and soot particles. The TiO₂ particles were produced from a premixed stagnation ethylene-oxygen-argon flame (? = 0.36) doped with titanium tetraisopropoxide. Soot was generated from a burner-stabilized premixed ethylene-oxygen-argon flame (? = 2.5). The close agreement among SMPS, TEM, and X-ray diffraction results for TiO₂ nanoparticles demonstrates that the probe sampling/mobility measurement technique is accurate for on-line analysis of the size distribution of particles as small as 3 nm in diameter. In the case of soot, notable disagreement between the SMPS and TEM sizes was found and attributable to the fact that the soot taken from the flame studied herein is liquid-like and that upon deposition on the TEM grid, the primary particles do not retain their sphericity. This interpretation is supported by measurements with photo ionization aerosol mass spectrometry, small angle neutron scattering, and thermocouple particle densitometry.     

Synchrotron X-ray diffraction and scanning electron microscopy to understand enamel affected by metabolic disorder mucopolysaccharidosis

Mucopolysaccharidosis (MPS) is an inherited metabolic disorder that can affect the tooth structure leading to defects. Synchrotron X-ray diffraction being a state of the art technique has been used to determine the enamel crystallite orientation in deciduous enamel affected by Mucopolysaccharidosis Type I and Mucopolysaccharidosis Type IVA and comparing these with that of healthy deciduous enamel. Using this technique it was observed that there is a loss of texture in deciduous enamel affected by Mucopolysaccharidosis Type I and Mucopolysaccharidosis Type IVA when compared to the healthy deciduous enamel. Generally it was observed that the incisal surface of the deciduous teeth possessed a higher texture or preferred orientation of enamel crystallites and on progression towards the cervical region there was a decrease in the texture or preferred orientation of enamel crystallites. Scanning electron microscopy showed that the presence of a poorly calcified layer between the enamel and dentine at the enamel–dentine junction (EDJ) in MPS affected samples was likely to be responsible for rendering the tooth structure weak and prone to fracture as is often the case in MPS affected deciduous enamel.     

A comparative study of microstructure of RuO2 nanorods via Raman scattering and field emission scanning electron microscopy

Raman scattering (RS) and field emission scanning electron microscopy (FESEM) have been used to extract microstructural information of RuO₂ nanorods (NRs) and a two-phase system comprising NRs embedded in polycrystalline matrix deposited on different substrates by the metal-organic chemical vapor deposition method. The red shifts and asymmetric broadening of the Raman line shape for the NRs are analyzed by the spatial correlation model. The deduced spatial correlation length l is found to be much smaller than that of the average size L₀ estimated from the FESEM images. The Raman features for the two-phase system can be resolved into two parts: a Lorentzian line shape feature corresponding to the polycrystallite at higher frequency side and an asymmetrically broadened NRs' signature located at lower frequency end. The volume fraction of NRs in the two-phase system can be determined from the analysis. These results demonstrate the significance of RS as a structural characterization method when used in conjunction with FESEM.