Increasing spatial resolution in the backscattered electron mode of scanning electron microscopy

A new method for increasing spatial resolution in the detection of backscattered electrons and induced current in scanning electron microscopy (SEM) is proposed in terms of regularized Fourier transform. The real size of an electron probe and its blurring in a solid target sample are considered in forming the algorithm. The experiments reveal an almost 100% improvement in resolution in the processed images.     

Statistical estimation of atomic positions from exit wave reconstruction with a precision in the picometer range

The local structure of Bi4W2/3Mn1/3O8Cl is determined using quantitative transmission electron microscopy. The electron exit wave, which is closely related to the projected crystal potential, is reconstructed and used as a starting point for statistical parameter estimation. This method allows us to refine all atomic positions on a local scale, including those of the light atoms, with a precision in the picometer range. Using this method one is no longer restricted to the information limit of the electron microscope. Our results are in good agreement with x-ray powder diffraction data demonstrating the reliability of the method. Moreover, it will be shown that local effects can be interpreted using this approach.     

Nanotomography

Scanning probe microscopy (SPM) can be expanded to volume imaging. As an example, the core of a dislocation within the three-dimensional (3D) spatial microdomain structure of poly(styrene-block-butadiene-block-styrene) was imaged with approximately 10 nm resolution. The specimen was eroded step by step and its chemical composition in layers beneath the original surface was imaged with SPM. Similar to computed tomography, the 3D distribution of polystyrene and polybutadiene was reconstructed from a series of images. This approach might provide a simple means for real-space volume imaging with nanometer and even atomic resolution of various materials and physical properties.     

Study on combined immersion electrostatic-magnetic focusing lenses without crossovers

Wide electron beam focusing properties of combined immersion electrostatic-magnetic focusing system are studied; their curvilinear axis aberration coefficients are derived. Based upon ray tracing method and curvilinear axis theory of wide electron beam systems, a program was written and as an example, a practical structure of the lens is numerically simulated. The computed results show that demagnified images with high resolution of tens of nanometers can be obtained for an object field size in millimeter range.     

How to optimize the experimental design of quantitative atomic resolution TEM experiments?

A quantitative measure is proposed to evaluate and optimize the design of quantitative atomic resolution TEM experiments. It aims at precise measurement of unknown structure parameters. Specifically, the proposed measure quantifies the statistical precision with which positions of atom columns can be estimated. The optimal design is then given by the combination of microscope settings for which this precision is highest. The proposed measure is also used to find out if new instrumental developments improve the precision as compared to existing methods.     

Quantitative determination of contact stiffness using atomic force acoustic microscopy

Atomic force acoustic microscopy is a near-field technique which combines the ability of ultrasonics to image elastic properties with the high lateral resolution of scanning probe microscopes. We present a technique to measure the contact stiffness and the Young's modulus of sample surfaces quantitatively, with a resolution of approximately 20 nm, exploiting the contact resonance frequencies of standard cantilevers used in atomic force microscopy. The Young's modulus of nanocrystalline ferrite films has been measured as a function of oxidation temperature. Furthermore, images showing the domain structure of piezoelectric lead zirconate titanate ceramics have been taken.     

Quantitative HRTEM investigation of nanoplatelets

High resolution transmission electron microscopy experiments were performed to investigate nanoplatelets induced by ion implantation into a germanium wafer. Atomistic models were used for image simulation in order to get quantitative information from the experimental images. The geometrical phase shift analysis technique was also employed to measure the strain field induced by such defects. We discuss the limits and artefacts imposed by each approach and show how these approaches can be combined to study the atomic structure of such defects and the strain field they induce.     

基于迁移学习的原子力显微镜成像恢复方法

受限于探针针尖结构尺寸,用原子力显微镜进行微纳测量时会产生图像边缘失真.提出了一种基于迁移学习的原子力显微镜成像恢复方法,通过迁移学习训练源模型和靶模型实现一维栅格成像恢复.该方法采用数学形态法中的腐蚀算法生成栅格点云数据,通过U-Net网络源模型从点云中提取针尖卷积效应的特征向量,将权重参数迁移至U-Net网络靶模型,靶模型在自适应正则化方法下进行监督学习.实验结果表明,该方法能有效恢复一维栅格的原子力显微镜测量图像,提高横向分辨力,可用于纳米栅格的线宽检测上.     

基于YOLOv3框架的高分辨电镜图像原子峰位置检测

高分辨电镜图像中原子峰位置的检测具有十分重要的现实意义,通过精确定量化原子峰位置可以分析物质在微观尺度上的结构形变、电极化矢量分布等重要信息.近年来深度学习技术在图像目标检测领域取得了巨大突破,这一技术可用在高分辨电镜图像处理上,因为原子位置的检测可以看作是一个目标检测问题.本文利用先进的机器学习方法,通过制作高质量原子图像样本集,使用YOLOv3目标识别框架对原子图像进行自动检测,达到预期效果,实现了深度学习技术在高分辨电镜图像处理领域的应用.该方法的运用有望突破自动处理动态、大量电镜图片的瓶颈问题.     

Electron-energy-loss spectroscopy and X-ray absorption spectroscopy as complementary probes for complex f-electron metals: cerium and plutonium

In this paper, we demonstrate the power of electron-energy-loss spectroscopy (EELS) in a transmission electron microscope by investigating the electron structure of two f-electron metals: Ce and Pu. It is shown that EELS in a transmission electron microscope may be used to circumvent the difficulty of producing single-phase or single-crystal samples owing to its high spatial resolution, and that diffraction patterns and images can be acquired, providing unambiguous phase determination when acquiring spectra. EELS results are supported by synchrotron-radiation-based X-ray absorption, multielectron atomic spectral simulations, and local density approximation calculations based on density-functional theory with the generalized gradient approximation. For Ce, it is shown that changes in {111} stacking sequences can drive substantial modifications in the electronic structure of close-packed phases of Ce that have similar atomic volumes, contrary to previous assumptions in literature. For Pu, it is shown that Russell–Saunders (L–S) coupling fails for the 5f states and that either a j–j or an intermediate scheme must be used for the actinides because of the considerable spin–orbit interaction in the 5f states. We present a model showing how the 5f states behave along the light actinide series.     

Experiences with synthetic aperture focusing technique in the field

The detection and evaluation of defects in industrial components relies strongly on ultrasonic inspection techniques. Distance gain size (DG) or reference reflector methods can be improved concerning their localization, signal-to-noise ratio and sizing accuracy by the synthetic aperture focusing technique (SAFT). To obtain a high quality image, parameters like focal probe versus contact technique probe, achieved resolution or features of SAFT images compared with B-scan images are discussed. The implementation of SAFT in a CAD environment allows us to present stacked 2D reconstructions dynamically. On a cladded testblock with half-penny shaped cracks the advantage of combining CAD with SAFT is shown. A 3D SAFT example finalizes the overview of two decades of experience in applying this technique.     

Characterization of tip size and geometry of the pipettes used in scanning ion conductance microscopy

Scanning ion-conductance microscopy (SICM) belongs to the family of scanning-probe microscopies. The spatial resolution of these techniques is limited by the size of the probe. In SICM the probe is a pipette, obtained by heating and pulling a glass capillary tubing. The size of the pipette tip is therefore an important parameter in SICM experiments. However, the characterization of the tip is not a consolidated routine in SICM experimental practice. In addition, potential and limitations of the different methods available for this characterization may not be known to all users. We present an overview of different methods for characterizing size and geometry of the pipette tip, with the aim of collecting and facilitating the use of several pieces of information appeared in the literature in a wide interval of time under different disciplines. In fact, several methods that have been developed for pipettes used in cell physiology can be also fruitfully employed in the characterization of the SICM probes. The overview includes imaging techniques, such as scanning electron microscopy and atomic Force microscopy, and indirect methods, which measure some physical parameter related to the size of the pipette. Examples of these parameters are the electrical resistance of the pipette filled with a saline solution and the surface tension at the pipette tip. We discuss advantages and drawbacks of the methods, which may be helpful in answering a wide range of experimental questions.     

Structure of the fivefold surface of the icosahedral Al-Cu-Fe quasicrystal: experimental evidence of bulk truncations at larger interlayer spacings

Based on scanning tunneling microscopy of the fivefold surface of the icosahedral Al-Cu-Fe quasicrystal and the refined structure model of the isostructural i-Al-Pd-Mn, we present evidence that the surface corresponds to bulk truncations at the positions where blocks of atomic layers are separated by larger interlayer spacings (gaps). Both step-height distribution and high resolution scanning tunneling microscopy images on terraces reveal bulk truncations at larger gaps.     

Study of local density of electron states in InGaAs/GaAs quantum rings by combined STM/AFM

The electronic structure of self-assembled InGaAs/GaAs(001) quantum rings grown by atmospheric pressure metal-organic vapor phase epitaxy has been investigated by combined scanning tunneling/atomic force microscopy (STM/AFM) in ultrahigh vacuum (UHV) for the first time. The current images and the tunnel spectra of contact of Pt-coated Si AFM probe to the quantum ring heterostructure surface revealing the spatial distribution of the local density of states and the electron size quantization spectra in the quantum rings have been obtained.     

STM experiment and atomistic modelling hand in hand: individual molecules on semiconductor surfaces

When the scanning tunnelling microscope was invented, the world was amazed at the atomic resolution images of surfaces which could be obtained. It soon became apparent that it was one thing to obtain an image, and quite another to understand the structure that was seen. Happily the developments in real space experimental techniques for studying surfaces have been accompanied by developments in real space theoretical techniques for modelling electronic structure and bonding at surfaces. The aim of this review is to describe how and why STM experiments and atomistic modelling should be combined and what they can then be expected to tell us. A summary is given of the experimental methods for theorists and vice versa, and their relationship is illustrated using a number of case studies where they have been used together. To give the review a coherent focus the examples are confined to studies of adsorbed molecules on semiconductor surfaces, in particular Si(001) and GaAs(001). Questions thus addressed include: How are experimental images and structural modelling linked by tunnelling theory? What can they tell us together that we could not learn from experiment or theory alone? What can we learn about atomic positions and bonding at semiconductor surfaces with and without adsorbed molecules? How many different ways are there to relate images to calculations?     

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.     

General theory of microscopic dynamical response in surface probe microscopy: from imaging to dissipation

We present a general theory of atomistic dynamical response in surface probe microscopy when two solid surfaces move with respect to each other in close proximity, when atomic instabilities are likely to occur. These instabilities result in a bistable potential energy surface, leading to temperature dependent atomic scale topography and damping (dissipation) images. The theory is illustrated on noncontact atomic force microscopy and enables us to calculate, on the same footing, both the frequency shift and the excitation signal amplitude for tip oscillations. We show, using atomistic simulations, how dissipation occurs through reversible jumps of a surface atom between the minima when a tip is close to the surface, resulting in dissipated energies of 1.6 eV. We also demonstrate that atomic instabilities lead to jumps in the frequency shift that are smoothed out with increasing temperature.     

Localizing and Characterizing Colloidal Particles Scattering Using Lens-free Holographic Microscopy

Lens-free holographic microscopy could achieve both improved resolution and field of view(FOV), which has huge potential applications in biomedicine, fluid mechanics and soft matter physics. Unfortunately, due to the limited sensor pixel size, target objects could not be located to a satisfactory level. Recent studies have shown that electromagnetic scattering can be fitted to digital holograms to obtain the 3 D positions of isolated colloidal spheres with nanometer precision and millisecond temporal resolution. Here, we describe a lens-free holographic imaging technique that fits multi-sphere superposition scattering to digital holograms to obtain in situ particle position and model parameters: size and refractive index of colloidal spheres. We show that the proposed method can be utilized to analyze the location and character of colloidal particles under large FOV with high density.     

Microstructure and surface morphology of YSZ thin films deposited by e-beam technique

In present study yttrium-stabilized zirconia (YSZ) thin films were deposited on optical quartz (amorphous SiO₂), porous Ni-YSZ and crystalline Alloy 600 (Fe-Ni-Cr) substrates using e-beam deposition technique and controlling technological parameters: substrate temperature and electron gun power which influence thin-film deposition mechanism. X-ray diffraction, scanning electron microscopy (SEM), and atomic force microscopy (AFM) were used to investigate how thin-film structure and surface morphology depend on these parameters. It was found that the crystallite size, roughness and growth mechanism of YSZ thin films are influenced by electron gun power. To clarify the experimental results, YSZ thin-film formation as well evolution of surface roughness at its initial growing stages were analyzed. The evolution of surface roughness could be explained by the processes of surface mobility of adatoms and coalescence of islands. The analysis of these experimental results explain that surface roughness dependence on substrate temperature and electron gun power non-monotonous which could result from diffusivity of adatoms and the amount of atomic clusters in the gas stream of evaporated material.