Exit wave reconstruction using a conventional transmission electron microscope

Exit wave reconstruction of a focus series of Ge in [110] using the PAMMAL algorithm was performed on a conventional electron microscope. The simulated images using the reconstructed object wave match very well with those obtained experimentally. Amplitudes from the complex wave function were extracted by means of local Fourier transformation. Crystal thickness and tilt were determined locally by quantitative comparison of the reconstructed amplitudes with amplitudes from multislice calculations. Detailed analysis yields the quasicoherent imaging approach used in the PAMMAL algorithm to produce the largest error in the analysis. For the Ge crystal specimen parameters were quantified to spatial frequencies of 5 nm¹. In the case of an object producing strong diffracted beams, the reconstruction may fail because the quasicoherent approximation will not describe correctly the nonlinear image formation.     

Electron holography approaching atomic resolution

Image plane off-axis holograms are recorded at atomic resolution by means of an electron biprism; numerical and light-optical reconstruction schemes are compared, and experimental results are presented including the correction of spherical aberration.     

Analysis of protein crystal growth at molecular resolution by atomic force microscopy

High-resolution atomic force microscopy (AFM) studies have been performed to analyze the molecularity of growth steps of the (1 1 0) face of tetragonal lysozyme crystals. Besides a major population of step heights of about 5.5 nm also step heights of about half this size were observed. The latter steps always appeared pairwise. Both surfaces the 1 1 0) face and the (1 0 1) face could be imaged at molecular level. Comparison of the height pattern of the corresponding surface structure indicates that the (1 1 0) face is relatively smooth of less than 0.2 nm compared to the (1 0 1) face of about 1.5 nm. AFM linescan images of the (1 0 1) face indicate the insertion of lysozyme aggregates in solution to the crystal surface rather than lysozyme monomers. This study suggests that insertion of lysozyme aggregates in the solution yields growth steps of the (1 1 0) face of monomolecular as well as of bimolecular unit height.     

Electron crystallography at atomic resolution: The structure of the odd-chain paraffin n-tritriacontane

The crystal structure of the odd-chain paraffin, n-tritriacontane, nC₃₃H₆₈, is determined directly by using low-dose electron microscope images and electron diffraction intensity data from epitaxially grown microcrystals. Phases of the most intense “polyethylene” reflections are determined from triplet structure-invariant relationships often used in X-ray crystallography. Low-dose electron microscopic images provide phases of the low-angle “lamellar” reflections and these can be used with one-dimensional structure-invariant relationships to determine other phases on the 00? reciprocal row. The phase set is sufficient to calculate an electrostatic potential map which is directly interpretable as a structure image at atomic resolution.     

Channelling effects in atomic resolution STEM

A Bloch wave theory for incoherent scattering of an incident plane wave has proved successful in predicting the fine detail in 2-D zone axis channelling patterns formed by ADF, BSE and characteristic X-ray detection in beam rocking mode. A previously published example of polarity determination of GaAs by channelling contrast is compared with simulations in order to illustrate the applicability of the theory. Modification of boundary conditions for a focused coherent probe allows lattice-resolution incoherent contrast based on ADF and EELS detection as well as X-ray emissions to be catered for within a similar theoretical framework. Mixed dynamic form factors constitute an integral part of this theory, where quantum-mechanical phase is a core issue. Simulations of lattice-resolution ADF and EELS are discussed with reference to various zone axis projections of GaAs. Issues of single versus double channelling conditions, and local versus nonlocal interactions, are discussed in relation to X-ray, ADF and EELS detection.     

Achievement of atomic resolution electron microscopy

Atomic-level details are easily resolved in the latest generation of intermediate voltage electron microscopes, but structural information on the same scale can only be extracted under certain specific conditions. Some understanding of imaging theory, as well as an awareness of correct operating conditions, is required for reliable image interpretation. Several representative examples are chosen to illustrate the possibilities for atomic-resolution imaging of materials, and perspectives and outlook for the technique are briefly discussed.     

3-D reconstruction of the atomic positions in a simulated gold nanocrystal based on discrete tomography: prospects of atomic resolution electron tomography

A novel reconstruction procedure is proposed to achieve atomic resolution in electron tomography. The method exploits the fact that crystals are discrete assemblies of atoms (atomicity). This constraint enables us to obtain a three-dimensional (3-D) reconstruction of test structures from less than 10 projections even in the presence of noise and defects. Phase contrast transmission electron microscopy (TEM) images of a gold nanocrystal were simulated in six different zone axes. The discrete number of atoms in every column is determined by application of the channelling theory to reconstructed electron exit waves. The procedure is experimentally validated by experiments with gold samples. Our results show that discrete tomography recovers the shape of the particle as well as the position of its 309 atoms from only three projections.

Experiments on a nanocrystal that contains several missing atoms, both on the surface and in the core of the nanocrystal, while considering a high noise level in each simulated image were performed to prove the stability of the approach to reconstruct defects. The algorithm is well capable of handling structural defects in a highly noisy environment, even if this causes atom count “errors” in the projection data.     

Electron crystallography at atomic resolution: ab initio structure analysis of copper perchlorophthalocyanine.

High-voltage (1200 kV) electron diffraction intensities from approximately 100 A thick crystals of copper perchlorophthalocyanine are used to determine the molecular packing at atomic resolution, thus greatly exceeding the structure detail observed by electron microscopy. Initial crystallographic phases were determined by direct methods often used in X-ray crystallography, i.e., locating the positions of heavy (Cl and Cu) atoms in the structure. All other atom positions were found in subsequent Fourier refinement (final R = 0.28). Calculated bond distances and angles are similar to those found in the earlier X-ray crystal structure of the unchlorinated parent compound.     

Observation of metal nanoparticles at atomic resolution in Pt‐based cancer chemotherapeutics

The chemotherapeutics cisplatin and oxaliplatin are important tools in the fight against cancer. Both compounds are platinum complexes. Aberration‐corrected scanning transmission electron microscopy using the annular dark‐field imaging mode now routinely provides single‐atom sensitivity with atomic number contrast. Here, this imaging mode is used to directly image the platinum within the two drugs in their dried form on an amorphous carbon support film. The oxaliplatin is found to have wetted the supporting amorphous carbon, forming disordered clusters suggesting that the platinum has remained within the complex. Conversely, the cisplatin sample reveals 1.8‐nm‐diameter metallic platinum clusters. The size and shape of the clusters do not appear to be dependent on drying rate nor formed by beam damage, which may suggest that they were present in the original drug solution.     

A model based atomic resolution tomographic algorithm

Tomography with high angular annular dark field scanning transmission electron microscopy at atomic resolution can be greatly improved if one is able to take advantage of prior knowledge. In this paper we present a reconstruction technique that explicitly takes into account the microscope parameters and the atomic nature of the projected object. This results in a more accurate estimate of the atomic positions and in a good resistance to noise. The reconstruction is a maximum likelihood estimator of the object. Moreover, the limits to the precision have been explored, allowing for a prediction of the amount of expected noise in the reconstruction for a certain experimental setup. We believe that the proposed reconstruction technique can be generalized to other tomographic experiments.     

Volcano structure in atomic resolution core-loss images

A feature commonly present in simulations of atomic resolution electron energy loss spectroscopy images in the scanning transmission electron microscope is the volcano or donut structure. In the past this has been understood in terms of a geometrical perspective using a dipole approximation. It is shown that the dipole approximation for core-loss spectroscopy begins to break down as the probe forming aperture semi-angle increases, necessitating the inclusion of higher order terms for a quantitative understanding of volcano formation. Using such simulations we further investigate the mechanisms behind the formation of such structures in the single atom case and extend this to the case of crystals. The cubic SrTiO3 crystal is used as a test case to show the effects of nonlocality, probe channelling and absorption in producing the volcano structure in crystal images.     

Exit wave reconstructions using through focus series of HREM images

The through focus exit wave reconstruction technique uses a series of high resolution electron microscopy images to reconstruct the complex electron wavefunction at the exit plane of the specimen. The feasibility of the through focus exit wave reconstruction method and its most important limitations are discussed. It is shown that-provided all aberrations of the microscope are well corrected for-a large improvement in the interpretability of the information can be obtained.     

Three-dimensional reconstructions from incomplete data: interpretability of density maps at "atomic" resolution

Three dimensional data collection in electron microscopy is normally limited to a range of tilt angles that is less than +/- 90 degrees. Thus, even under the best conditions, experimental values of the structure factors will be missing within a solid cone in reciprocal space. Previous work has already shown that the missing cone of data can produce serious artifacts in three-dimensional density maps at modest resolution, for example approximately 15A. We now report, however, that a missing cone as large as +/- 30 degrees appears to have no serious effect on the three-dimensional density map of a protein at 3.6 A resolution, and we attribute this result to the fact that the electron density features are quite well separated from one another at that resolution. The map calculated with a +/- 30 degree missing cone is, furthermore, no more sensitive to noise (error) than is the full (isotropic) Fourier map. This result does not seem to be unreasonable in view of the fact that less than 14% of the data (i.e., signal) is lost due to the missing cone. Our numerical simulations therefore indicate that there should be no difficulty in interpreting high-resolution Fourier maps that can be produced with data that fall within realistic estimates of achievable resolution, tilt angles, and experimental error.     

Towards sub-A atomic resolution electron diffraction imaging of metallic nanoclusters: a simulation study of experimental parameters and reconstruction algorithms

A simulation study is carried out to elucidate the effects of dynamical scattering, electron beam convergence angle and detection noise on atomic resolution diffraction imaging of small particles and to develop effective reconstruction procedures. Au nanoclusters are used as model because of their strong scattering. The results show that the dynamical effects of electron diffraction place a limit on the size of Au nanoclusters that can be reconstructed from the diffraction intensities with sufficient accuracy. For smaller Au nanoclusters, the simulations show that diffraction patterns recorded under the experimental conditions can be reconstructed using a combination of phase retrieval algorithms. The use of a low-resolution image is shown to be effective for reconstructing diffraction patterns without the central beam. A new algorithm for estimating the object support is proposed.     

酸洗连轧机组出口废料移出装置

简述某1450mm连续酸洗一连轧机组出口废料移出装置的工作原理及布置形式，重点介绍主要参数的确定原则和计算方法。     

Imaging streptavidin 2D crystals on biotinylated lipid monolayers at high resolution with the atomic force microscope

Streptavidin crystals were grown on biotinylated lipid monolayers at an air/water interface and transferred onto highly oriented pyrolytic graphite (HOPG). These arrays could be imaged to a resolution below 1 nm using the atomic force microscope. The surface topographs obtained were compared with negative-stain electron microscopy images and the atomic model as determined by X-ray crystallography. The streptavidin tetramer (60 kDa) exposes two free biotin-binding sites to the buffer solution, while two are occupied by linkage to the lipid monolayer. Therefore, the streptavidin 2D crystals can be used as nanoscale matrices for binding biotinylated compounds. Furthermore, this HOPG-based preparation method provides a general novel approach to study the structure of protein arrays assembled on lipid monolayers with the AFM.     

基于超分辨率重建的亚像素图像配准

针对低分辨率图像在配准过程中精度较低的问题,提出了一种基于超分辨率重建的亚像素图像配准方法。首先,对具有1至9像素位移的图像序列进行10倍降采样,获取具有0.1至0.9亚像素位移的图像序列。然后,根据图像的获取过程建立数学模型,以Bayes理论为基础,使用最大后验概率法(MAP)对亚像素位移低分辨率图像进行超分辨率重建,获取高分辨率图像。最后,使用具有亚像素配准精度的扩展相位相关法对图像进行配准。配准实验与噪声实验表明,所提方法的最大配准误差为0.03pixel,能实现对低分辨率图像的亚像素级配准,具有配准精度高、噪声抗干扰能力强等特点,可同时满足可见光图像与红外图像的高精度配准要求。     

基于区域划分的红外超分辨率重建

提出了红外超分辨率重建系统以获取高分辨率红外数据。首先,根据红外图像获取过程建立了数学模型,讨论了降采样、模糊、运动以及高斯噪声对红外系统的影响;在非退化特征提取的基础上提出了基于特征的亚像素配准算法,其根据所得到的非退化特征应用归一化均方根误差来估计两帧之间的亚像素位移。然后,分析了传统全变分因子在高分辨重建时的不足并对其进行改进;利用区域划分将图像划分为平滑区域和细节区域,并根据区域的不同情况自适应全变分因子,从而使细节区域不至于过平滑。最后,利用MM(Majorization Minimixation)算法对合成的低分辨率红外图像和真实红外图像进行了超锐度重建。与同类相关算法的比较实验显示:所提算法亚像素配准最大误差为0.09pixel,重建后的红外图像质量优于其他同类算法。所提算法可以对低分辨红外图像序列进行有效重建,具有配准精度高、重建图像细节丰富等特点,可应用于各种红外成像系统。     

Combined low-temperature scanning tunneling/atomic force microscope for atomic resolution imaging and site-specific force spectroscopy

We present the design and first results of a low-temperature, ultrahigh vacuum scanning probe microscope enabling atomic resolution imaging in both scanning tunneling microscopy (STM) and noncontact atomic force microscopy (NC-AFM) modes. A tuning-fork-based sensor provides flexibility in selecting probe tip materials, which can be either metallic or nonmetallic. When choosing a conducting tip and sample, simultaneous STM/NC-AFM data acquisition is possible. Noticeable characteristics that distinguish this setup from similar systems providing simultaneous STM/NC-AFM capabilities are its combination of relative compactness (on-top bath cryostat needs no pit), in situ exchange of tip and sample at low temperatures, short turnaround times, modest helium consumption, and unrestricted access from dedicated flanges. The latter permits not only the optical surveillance of the tip during approach but also the direct deposition of molecules or atoms on either tip or sample while they remain cold. Atomic corrugations as low as 1 pm could successfully be resolved. In addition, lateral drifts rates of below 15 pm/h allow long-term data acquisition series and the recording of site-specific spectroscopy maps. Results obtained on Cu(111) and graphite illustrate the microscope's performance.