Elemental mapping with elastically scattered electrons

We describe a technique for efficient, quantitative, standardless elemental mapping using a high-angle annular detector in a scanning transmission electron microscope (STEM) to collect elastically scattered electrons. With a single crystal specimen, contrast due to thickness variations, diffraction, and channelling effects can be avoided, so that the resulting image contrast quantitatively reflects variations in impurity concentration. We compare a number of simple analytical approximations to the elastic scattering cross sections and show that a standardless analysis is possible over a wide range of atomic number and inner detector angle to an absolute accuracy of better than 20%.     

A practical approach for STEM image simulation based on the FFT multislice method

It has been demonstrated that a high-angle annular dark-field (HAADF) STEM technique gives an image resolving atomic columns. Due to the diffusion of this technique and an improvement of its resolution, a practical procedure for image simulation becomes important for a quantitative interpretation of the HAADF image. In this report a new practical scheme for a STEM image simulation is developed based on the FFT multislice algorithm. Here, a HAADF intensity due to thermal diffuse scattering (TDS) is calculated from the absorptive potential corresponding to high-angle TDS and the wave function equivalent to the propagating probe within the sample. Contrary to the commonly used Bloch wave method, a coherent bright-field intensity and a coherent HAADF intensity are also obtained straightforwardly. The HAADF image contrast calculated for GaAs is not simply proportional to Z2 as expected from the Rutherford scattering at high-angle, and the As/Ga contrast ratio depends on the specimen thickness. This suggests that the generation of the HAADF signal is appreciably affected by the coherent dynamical scattering. The developed procedure here will have a definitive advantage over the Bloch wave approach for simulating the HAADF images expected from a defect and interface or amorphous materials, and also the HAADF image obtained by using a Cs-corrected microscope. This is because the former requires a huge super cell, while the latter needs a large objective aperture including a large number of incident beam directions.     

New pathways for improved quantification of energy‐dispersive X‐ray spectra of semiconductors with multiple X‐ray lines from thin foils investigated in transmission electron microscopy

Theoretical approaches to quantify the chemical composition of bulk and thin‐layer specimens using energy‐dispersive X‐ray spectroscopy in a transmission electron microscope are compared to experiments investigating (In)GaAs and Si(Ge) semiconductors. Absorption correctors can be improved by varying the take‐off angle to determine the depth of features within the foil or the samples thickness, or by definition of effective k‐factors that can be obtained from plots of k‐factors versus foil thickness or, preferably, versus the K/L intensity ratio for a suitable element. The latter procedure yields plots of self‐consistent absorption corrections that can be used to determine the chemical composition, iteratively for SiGe using a set of calibration curves or directly from a single calibration curve for InGaAs, for single X‐ray spectra without knowledge of sample thickness, density or mass absorption coefficients.     

Remark to the Intensity Measurement of RHEED

In this work, the intensity measurement of RHEED is carried out directly with the help of a Faraday cup that is described here. We are dealing with the behavior of oscillation intensity damping in the case of InGaAs/GaAs heterostructure.     

Quantitative analysis of ultrathin doping layers in semiconductors using high-angle annular dark field images

It is well known that the high-angle annular dark field (HAADF) technique in scanning transmission electron microscopy is an incoherent imaging process in the lateral ( xy ) plane. However, as a consequence of the existence of partial coherence in the z direction, accurate quantitative interpretation of image intensity is difficult. The effects of coherence in the z direction can be reduced by increasing the inner collector angle of the annular detector so that the scattering from atoms in the z direction is essentially incoherent. We thus show that it is feasible to quantify the total As concentration of ultrathin InAs _x P_{1− x} layers in InP in a simple but accurate way using a thickness integrated Bloch wave calculation including phonon scattering with a large inner collector angle of the annular detector of around 150 mrad. We compare the As composition derived from this approach with that from the Fresnel method and high resolution imaging. We also show that the non-linear variation of the HAADF intensity with thickness is consistent with our simpler simulations for such conditions. Therefore, this approach enables us easily and quickly to quantify compositions using HAADF images. The tetragonal distortion due to lattice mismatch is also shown to influence the contrast and has been included in the calculations.     

Fluorescence photobleaching-based shading correction for fluorescence microscopy

A thin fluorescent test layer, which is used in a practically mono-exponential bleaching regime, is employed to determine separately the excitation intensity and the fluorescence detection efficiency distributions in the field of view of a confocal fluorescence microscope. We demonstrate that once these distributions are known, it is possible to correct an image of a specimen for intensity variations which are caused by spatial nonuniformities of the illumination and the detection efficiency of the microscope. It is indicated that, provided a photophysically well-characterized fluorescent test layer is available, the method is potentially capable of quantifying the fluorescence intensities in an image of a specimen in terms of the fluorescence quantum yield, the absorption cross-section and the concentration of the fluorophore in the specimen.     

Accurate structure determination from image reconstruction in ADF STEM

Annular dark-field (ADF) imaging in a scanning transmission electron microscope results in direct structure images of the atomic configuration of the specimen. Since such images are almost perfectly incoherent they can be treated as a convolution between a point-spread function, which is simply the intensity of the illuminating electron probe, and a sharply peaked object function that represents the projected structure of the specimen. Knowledge of the object function for an image region of perfect crystal allows the point-spread function to be directly determined for that image. We examine how the object function for an image can then be reconstructed using a Wiener filter, the CLEAN algorithm and a maximum entropy reconstruction. Prior information is required to perform a reconstruction, and we discuss what nature of prior information is suitable for ADF imaging.     

Scanning electron microscope charging effect model for chromium/quartz photolithography masks

We propose a new method for fitting a model of specimen charging to scanning electron microscope (SEM) images. Charging effects cause errors when one attempts to infer the size or shape of a specimen from an image. The goal of our method is to enable image analysis algorithms for measurement, segmentation, and three-dimensional (3-D) reconstruction that would otherwise fail on images containing charging effects. Our model is applied to images of chromium/quartz photolithography masks and may also work in the more general case of isolated metal islands on a flat insulating substrate. Unlike methods based on Monte Carlo simulation, our simulation method does not handle more general topographies or specimens composed entirely of an insulator; it is a crude approximation to the physical charging process described in more detail in Cazaux (1986) and Melchinger and Hofmann (1985), but can be fit with quantitative accuracy to real SEM images. We only consider changes in intensity and do not model charging-induced distortion of image coordinates. Our approach has the advantage over existing methods of enabling fast prediction of charging effects so it may be more practical for image analysis applications.     

Essential experimental parameters for quantitative structure analysis using spherical aberration-corrected HAADF-STEM

The accuracy of quantitative analysis for Z-contrast images with a spherical aberration (C_s) corrected high-angle annular dark-field (HAADF) scanning transmission electron microscope (STEM) using SrTiO₃(0 0 1) was systematically investigated. Atomic column and background intensities were measured accurately from the experimental HAADF-STEM images obtained under exact experimental condition. We examined atomic intensity ratio dependence on experimental conditions such as defocus, convergent semi-angles, specimen thicknesses and digitalized STEM image acquisition system: brightness and contrast. In order to carry out quantitative analysis of C_s-corrected HAADF-STEM, it is essential to determine defocus, to measure specimen thickness and to fix setting of brightness, contrast and probe current. To confirm the validity and accuracy of the experimental results, we compared experimental and HAADF-STEM calculations based on the Bloch wave method.     

An optical configuration for fastidious STEM detector calibration and the effect of the objective‐lens pre‐field

In the scanning transmission electron microscope, an accurate knowledge of detector collection angles is paramount in order to quantify signals on an absolute scale. Here we present an optical configuration designed for the accurate measurement of collection angles for both image‐detectors and energy‐loss spectrometers. By deflecting a parallel electron beam, carefully calibrated using a diffraction pattern from a known material, we can directly observe the projection‐distortion in the post‐specimen lenses of probe‐corrected instruments, the 3‐fold caustic when an image‐corrector is fitted, and any misalignment of imaging detectors or spectrometer apertures. We also discuss for the first time, the effect that higher‐order aberrations in the objective‐lens pre‐field has on such an angle‐based detector mapping procedure.     

Panchromatic cathodoluminescence characterization of III-V lattice-mismatched heterostructures

Some examples of the possibilities that panchromatic cathodoluminescence (PCL) offers in the scanning electron microscopy (SEM) characterization of III-V semiconductors are presented. Investigations on lattice-mismatched InGaAs/InP, InGaAs/ GaAs single heterostructures, and InGaAs/GaAs superlattices and GaAs/Ge and GaAs/InP single layers are shown. Further, the use of PCL as a support in the nondestructive determination of the sensitivity limit of Rutherford backscattering and x-ray diffraction techniques in the study of strain release in some of the above mentioned heterostructures is presented. Finally, PCL on-line study of dislocation movement induced by electron beam irradiation in the SEM, as evidence of InGaAs/GaAs superlattice metastability, is also presented.     

An approach to the systematic distortion correction in aberration-corrected HAADF images

Systematic distortion has been analysed in high‐angle annular dark‐field (HAADF) images which may be caused by electrical interference. Strain mapping techniques have been applied to a strain‐free GaAs substrate in order to provide a broad analysis of the influence of this distortion on the determination of local strain in the heterostructure. We have developed a methodology for estimating the systematic distortion, and we correct the original images by using an algorithm that removes this systematic distortion.     

Nanofabrication of cylindrical STEM specimen of InGaAs/GaAs quantum dots for 3D-STEM observation

We demonstrate the multiazimuth observation (360 degrees in principle) of InGaAs/GaAs quantum dots (QDs) by means of a 300 kV scanning transmission electron microscope (STEM), where both cross-sectional and plan-view observations are performed on a single STEM specimen for the first time. A cylindrical specimen with a diameter of 200-300 nm including the QD layer inside along the rotation axis was fabricated by the focused ion beam (FIB) technique, with the application of a newly developed mesa-cutting method to adjust the position and angle of the QD layer precisely. The 360 degrees STEM observation is realized by mounting the cylindrical specimen on a holder equipped with a specimen-rotation mechanism. High potential of 3D-STEM observation is briefly presented by showing high contrast images of QDs, dark field images, and moire fringes with various incident angles.     

Modification of a TEM-goniometer specimen holder to enable beam current measurements in a (S)TEM for use in quantitative X-ray microanalysis

In order to have available a specimen holder suited to measure the beam current as is often required in quantitative electron probe X-ray microanalysis, the rod of a low background beryllium specimen holder of a transmission electron microscope was modified. The tip was electrically insulated from the mass of the microscope and connected electrically to the central contact of a BNC connector mounted on the specimen holder handle. With this modified specimen holder the current absorbed by the specimen and/or the specimen holder could be measured easily and accurately. The modified specimen holder has been used to measure the beam current stability of an analytical electron microscope under various conditions. Data were obtained for tungsten as well as lanthanum hexaboride cathodes. Small changes to other types of specimen tips made it possible to exchange these for the low background tip.     

A statistical approach for intensity loss compensation of confocal microscopy images

In this paper, a probabilistic technique for compensation of intensity loss in confocal microscopy images is presented. For single-colour-labelled specimen, confocal microscopy images are modelled as a mixture of two Gaussian probability distribution functions, one representing the background and another corresponding to the foreground. Images are segmented into foreground and background by applying Expectation Maximization algorithm to the mixture. Final intensity compensation is carried out by scaling and shifting the original intensities with the help of parameters estimated for the foreground. Since foreground is separated to calculate the compensation parameters, the method is effective even when image structure changes from frame to frame. As intensity decay function is not used, complexity associated with estimation of the intensity decay function parameters is eliminated. In addition, images can be compensated out of order, as only information from the reference image is required for the compensation of any image. These properties make our method an ideal tool for intensity compensation of confocal microscopy images that suffer intensity loss due to absorption/scattering of light as well as photobleaching and the image can change structure from optical/temporal section-to-section due to changes in the depth of specimen or due to a live specimen. The proposed method was tested with a number of confocal microscopy image stacks and results are presented to demonstrate the effectiveness of the method.     

A study of factors influencing the accuracy of quantitative X-ray analysis of thin foil specimens

Needle-shaped specimens were used to determine experimental values of X-ray intensity ratios for L/K and M/L lines. These ratios can be used to determine k_AB factors for L and M lines. They also provide necessary data for absorption correction with the X-ray intensity ratio method. Recent theoretical calculations of k_AB factors are evaluated and new constants in the parametrization of ionization cross-sections for L and M lines are presented. The average X-ray production per unit thickness has been measured as a function of mass thickness for a stainless steel specimen using acceleration voltages of 100 and 200 kV. An increase in X-ray production by more than 20% was found at 100 kV for mass thicknesses up to 1 mg/cm² while at 200 kV the increase was about 5%. The contamination spot method for thickness measurements has also been investigated using needle-shaped specimens. The reported overestimate of thickness using this method can be explained by the formation of broad contamination layers around the deposited spots.     

Image contrast of dielectric specimens in transmission mode near-field scanning optical microscopy: imaging properties and tip artefacts

Near-field scanning optical microscopy (NSOM) is a scanned probe technique utilizing a subwavelength-sized light source for high-resolution imaging of surfaces. Although NSOM has the potential to exploit and extend the experimental utility of the modern light microscope, the interpretation of image contrast is not straightforward. In near-field microscopy the illumination intensity of the source (probe) is not a constant value, rather it is a function of the probe–sample electronic environment. A number of dielectric specimens have been studied by NSOM to elucidate the contrast role of specimen type, topography and crystallinity; a summary of metallic specimen observations is presented for comparative purposes. Near-field image contrast is found to be a result of lateral changes in optical density and edge scattering for specimens with little sample topography. For surfaces with considerable topography the contributions of topographic (Z) axis contrast to lateral (X,Y) changes in optical density have been characterized. Selected near-field probes have also been shown to exhibit a variety of unusual contrast artefacts. Thorough study of polarization contrast, optical edge (scattering) contrast, as well as molecular orientation in crystalline specimens, can be used to distinguish lateral contrast from topographic components. In a few cases Fourier filtering can be successfully applied to separate the topographic and lateral contrast components.     

The secondary fluorescence correction for X-ray microanalysis in the analytical electron microscope

A general formulation for the secondary fluorescence correction is presented. It is intended to give an intuitive appreciation for the various factors that influence the magnitude of the secondary fluorescence correction, the specimen geometry in particular, and to serve as a starting point for the derivation of quantitative correction formulae. This formulation is primarily intended for the X-ray microanalysis of electron-transparent specimens in the analytical electron microscope (AEM). The fluoresced intensity, I^Y_X, is expressed relative to the primary intensity of the fluorescing element, I_Y, rather than to that of the fluoresced element, I_X, as has been customary for microanalysis. The importance of this choice of I_Y as a reference intensity for the electron-transparent specimens examined in the AEM is discussed. The various factors entering the secondary fluorescence correction are grouped into three factors, representing the dependencies of the correction on specimen composition, X-ray fluorescence probability and specimen geometry. In principle, an additional factor should be appended to account for the difference in detection efficiencies of the fluoresced and fluorescing X-rays; however, this factor is shown to be within a few per cent of unity for practical applications of the secondary fluorescence correction. The absorption of secondary X-rays leaving the specimen en route to the detector is also accounted for through a single parameter. In the limit that the absorption of secondary X-rays is negligible, the geometric factor has the simple physical interpretation as the fractional solid angle subtended by the fluoresced volume from the perspective of the analysed volume. Studies of secondary fluorescence in the published literature are compared with this physical interpretation. It is shown to be qualitatively consistent with Reed's expression for secondary fluorescence in the electron probe microanalyser and with the specimen-thickness dependence of the Nockolds expression for the parallel-sided thin foil. This interpretation is also used to show that the ‘sec α’ dependence on specimen tilt in the latter expression is erroneous and should be omitted. The extent to which extrapolation methods can be used to correct for secondary fluorescence is also discussed. The notion that extrapolation methods, by themselves, can be used to correct for secondary fluorescence is refuted. However, extrapolation methods greatly facilitate secondary fluorescence correction for wedge-shaped specimens when used in conjunction with correction formulae.     

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.