原子尺度材料三维结构、磁性及动态演变的透射电子显微学表征

原子表征与操控是实现原子制造必须突破的物理瓶颈之一.像差校正电子显微学方法因其优异的空间分辨率,为实现原子精细制造提供了有力的表征手段.因此,利用电子显微学手段,在原子尺度对原子制造的材料及器件进行三维结构和性能的协同表征,对于深入理解原子水平材料操控的物理机理具有非常重要的意义.纳米团簇及纳米颗粒是原子制造材料与器件研究的主要对象之一,具有丰富的物理化学性质和较高的可操纵性.本文探讨纳米团簇/颗粒结构三维定量表征、使役条件下纳米团簇/颗粒结构演变定量表征、纳米颗粒/晶粒结构-成分-磁性协同定量表征等诸多方法与实例,阐明了电子显微学表征手段的突破和发展为实现精细控制的原子制造材料提供了坚实基础.     

Hybrid polymer nanosystems based on selenium and zinc-selenide nanoparticles: Morphology,electronic structure,and thermodynamic properties

The structure and morphology of hybrid nanosystems based on selenium and zinc-selenide nano-particles stabilized by water-soluble polymers—polyvinylpyrrolidone and polymethacrylic acid, are studied by methods of atomic force microscopy (AFM), high-resolution electron microscopy, transmission and scanning electron microscopy (TEM and SEM), X-ray photoelectron spectroscopy, X-ray structural analysis, and static light scattering. Comparison of the size characteristics of the nanostructures in the nanoparticle/polymer systems upon an increase in the weight ratio (ν) of the system components, using static light scattering in a solution and AFM, SEM, and TEM on the substrate surface, shows that the sizes of the forming nano-structures change nonmonotonically. The thermodynamic characteristics of the nanostructures in the solution are determined. It is shown that depending on ν, nanostructures of various morphologies may be formed, including spheres and irregularly shaped micelles with cores of different sizes.     

Understanding CeO2‐Based Nanostructures through Advanced Electron Microscopy in 2D and 3D

Engineering morphology and size of CeO₂‐based nanostructures on a (sub)nanometer scale will greatly influence their performance; this is because of their high oxygen storage capacity and unique redox properties, which allow faster switching of the oxidation state between Ce⁴⁺ and Ce³⁺. Although tremendous research has been carried out on the shape‐controlled synthesis of CeO₂, the characterization of these nanostructures at the atomic scale remains a major challenge and the origin of debate. The rapid developments of aberration‐corrected transmission electron microscopy (AC‐TEM) have pushed the resolution below 1 Å, both in TEM and in scanning transmission electron microscopy (STEM) mode. At present, not only morphology and structure, but also composition and electronic structure can be analyzed at an atomic scale, even in 3D. This review summarizes recent significant achievements using TEM/STEM and associated spectroscopic techniques to study CeO₂‐based nanostructures and related catalytic phenomena. Recent results have shed light on the understanding of the different mechanisms. The potential and limitations, including future needs of various techniques, are discussed with recommendations to facilitate further developments of new and highly efficient CeO₂‐based nanostructures.     

Atomic force microscopy and transmission electron microscopy of biocompatible magnetic fluids: A comparative analysis

The present study provides a comparative analysis of the size dispersity of magnetic nanoparticles (MNPs) within magnetic fluids as obtained from atomic force microscopy (AFM) and transmission electron microscopy (TEM). Whereas the mean particle diameter obtained from the AFM data presented a reduction of about 34% as compared to the value obtained from the TEM data, the standard deviation obtained from the AFM data is twice the value found from the TEM data. Similarities and differences in the size dispersity parameters are discussed in terms of sample preparation and tip characteristics. A two-dimensional mode for the deposition of the MNPs on top of the mica substrate is discussed as well.     

Effect of ultrasonic treatment on the morphology of casein particles

In this study, the effect of ultrasonic treatment duration on the morphology of self-assembled casein particles was investigated by atomic force microscopy (AFM), low vacuum scanning electron microscopy (SEM) and transmission electron microscopy (TEM). In the case of AFM images, the particle analysis which was carried out by the SPIP program showed that the self-assembled casein particles after being ultrasonically treated for 2 min got smaller in size compared to the casein particles that have not been exposed to any ultrasonic treatment. Surprisingly, however, increasing the ultrasonic time exposure of the particles resulted in an opposite effect where larger particles or aggregates seemed to be present. We show that by comparing the results obtained by AFM, SEM and TEM, the information extracted from the AFM images and analyzed by SPIP program give more detailed insights into particle sizes and morphology at the molecular level compared to SEM and TEM images, respectively.     

AFM and TEM study of hydrogenated sputtered Si/Ge multilayers

Multilayers of hydrogenated ultrathin (3 nm) amorphous a-Si and a-Ge layers prepared by sputtering have been studied by atomic force microscopy (AFM) and transmission electron microscopy (TEM) to check the influence of annealing on their structural stability. The annealed multilayers exhibit surface and bulk degradation with formation of bumps and craters whose density and size increase with increasing hydrogen content and/or annealing temperature and time. Bumps are due to the formation of H₂ bubbles in the multilayer. The craters are bumps blown up very likely because of too high a gas pressure inside. The release of H from its bonds to Si and Ge occurs within cavities very likely present in the samples. The necessary energy is supplied by the heat treatment and by the recombination of thermally generated carriers. Results by energy filtered TEM on the interdiffusion of Si and Ge upon annealing are also presented.     

A comparative study of conventional type II and inverted core–shell nanostructures based on CdSe and ZnS

The objective of this work is to investigate structural, morphological and optical properties of conventional CdSe/ZnS core–shell and inverted ZnS/CdSe core–shell nanostructures for opto-electronic device applications. For this purpose both nanostructures were synthesized using chemical bath deposition technique in thin film form. The structural properties were studied using X-ray diffraction technique with Rietveld refinement and transmission electron microscopy (TEM). The surface morphology of synthesized thin film was illustrated in the form 2D and 3D images using atomic force microscopy (AFM). The optical properties were explained using UV–Vis absorption spectroscopy and photo luminescence (PL) spectroscopy in in situ monitoring process. A comparison of estimated particle size from XRD, high resolution AFM and TEM images was resulted in good agreement as 2.1, 2.4 and 2.1 nm respectively for conventional CdSe/ZnS core–shell and as 2.5, 2.5 and 2.2 nm respectively for inverted ZnS/CdSe core–shell nanostructures.     

Electron microscopy of nanoemulsions: an essential tool for characterisation and stability assessment

The characterisation of pharmaceutical formulations by microscopic techniques is essential to obtain reliable data about the actual morphology of the system. Since the size range of colloidal drug delivery systems has long ago reached the lower end of the nanometer scale, classical light microscopy has been replaced by electron microscopy techniques which provide sufficient resolution for the visualisation of nano-sized structures. Indeed, the superior resolution and methodological versatility of electron microscopy has rendered this technique an indispensable tool for the analysis of nanoemulsions. Microscopic analysis of these lipid-based drug delivery systems with particle sizes in the lower submicron range provides critical information about the size, shape and internal structure of the emulsion droplets. Moreover, surfactant aggregates such as liposomes or multilamellar structures which remain unnoticed during particle size measurements can be detected in this fashion. This review provides a brief overview about both transmission electron microscopy (TEM) and scanning electron microscopy (SEM) techniques which have been employed to characterise nanoemulsions. Of special interest are sophisticated cryo techniques of sample preparation for both TEM and SEM which deliver high-quality images of nanoemulsions in their natural state. An overview about the instrumentation and sample preparation for all presented methods is given. Important practical aspects, sources of error and common artefacts as well as recent methodological advances are discussed. Selected examples of electron microscopic studies of nanoemulsions are presented to illustrate the potential of this technique to reveal detailed and specific information.     

Composition of the “GaAs” quantum dot,grown by droplet epitaxy

Self-assembled strain-free quantum dot (QD) structures were grown on AlGaAs surface by the droplet epitaxal method. The QDs were developed from pure Ga droplets under As pressure. The QDs were investigated by atomic force microscopy (AFM) and transmission electron microscopy (TEM). Both techniques show that the QDs are very uniform in size and their distribution on the surface is also homogeneous. The high resolution cross-sectional TEM investigation shows perfect lattice matching between the QD and the substrate, and also the faceting of the side walls of QD can be identified exactly by lattice planes. Analytical TEM (elemental mapping by EELS) unambiguously identifies the presence of Al in the QD.     

Atomic origins of solid helium bubbles in tungsten

Solid helium bubbles were directly observed in the helium ion implanted tungsten（W）, by different transmission electron microscopy（TEM） techniques at room temperature. The diameters of these solid helium bubbles range from1 nm to 8 nm in diameter with the mean bubble size about 3 nm. The selected area electron diffraction（SAED） and fast Fourier transform（FFT） images revealed that solid helium bubbles possess body-centered cubic（bcc） structure with a lattice constant of 0.447 nm. High-angle annular dark-field scanning transmission electron microscopy（HAADF-STEM）images further confirmed the existence of helium bubble in tungsten. The present findings provide an atomic level view of the microstructure evolution of helium in the materials, and revealed the existence of solid helium bubbles in materials.