Morphologic and cathodoluminescence studies of diamond films by scanning electron microscopy

Using recent papers on scanning electron microscopy (SEM) of chemical vapor deposition (CVD) diamond films, two analytical applications of the SEM are discussed: the morphologic investigations (secondary electron emission mode) and the recognition of impurities and defects [cathodoluminescence (CL) mode]. Studies of CVD diamond films by SEM demonstrate that the morphologies of these films are affected by synthesis conditions, especially by substrate temperature, methane concentration, and total pressure in the reactor. CL spectra and images are useful tools for clarifying the relationship between emission centers and different types of defects generated during the process of diamond crystal growth. The paper shows that the investigations of the morphology, crystallinity, local CL emission, as well as the surface distribution of CL spectra on CVD diamond films by SEM led to the correlative information for quality estimation of films in comparison with natural diamond.     

Cathodoluminescence and computer graphics in materials science

The combination of cathodoluminescence (CL) in scanning electron microscopy (SEM) with computer graphics is proposed for studying semiconductors and dielectric materials. Spatial distribution of several types of defects that occurred naturally and by design in crystals, can be sorted out and visualized in CL mapping and in three-dimensional images reconstructed in scanning cathodoluminescence microscopy. The possibilities of this method are illustrated on magnesium oxide single crystals indented with a Vickers diamond pyramid.     

A nondestructive method for three-dimensional reconstruction of luminescence materials: Principles,data acquisition,image processing

In the study presented here we have tried to state the principles and calculate and visualize models of three-dimensional (3-D)-cathodoluminescence reconstruction of luminescence structures by scanning electron microscopy (SEM). The new technique does not destroy the specimen and uses the variable energy of the electron beam to penetrate to different depths in the specimen volume. The SEM in color cathodoluminescence mode (CCL-SEM) detects integrated panchromatic CL-images for different energies of the electron beam. The use of electron scattering theory in solids and theories of cathodoluminescence and color allow the production of problem-oriented software for the routine processing of primary images. Processed images represent the CCL-SEM displays of separated layers (without CL information from other layers) up to the maximum depth penetrated by the beam. The 3-D reconstruction is carried out through algorithms developed using a personal computer, software, and a set of processed two-dimensional (2-D) images. The first experimental work was accomplished using a multilayer SiC mesastructure. The final reconstructed image of SiC material demonstrates separated epitaxial layers of different SiC polytypes and Z sections (YOZ and XOZ sections). The 3-D image represents the space distribution of CL-spectral data in color CL interpretation.     

Multiscale iterative voting for differential analysis of stress response for 2D and 3D cell culture models

Focused ion beam-scanning electron microscope (FIB-SEM) tomography is a powerful application in obtaining three-dimensional (3D) information. The FIB creates a cross section and subsequently removes thin slices. The SEM takes images using secondary or backscattered electrons, or maps every slice using X-rays and/or electron backscatter diffraction patterns. The objective of this study is to assess the possibilities of combining FIB-SEM tomography with cathodoluminescence (CL) imaging. The intensity of CL emission is related to variations in defect or impurity concentrations. A potential problem with FIB-SEM CL tomography is that ion milling may change the defect state of the material and the CL emission. In addition the conventional tilted sample geometry used in FIB-SEM tomography is not compatible with conventional CL detectors. Here we examine the influence of the FIB on CL emission in natural diamond and the feasibility of FIB-SEM CL tomography. A systematic investigation establishes that the ion beam influences CL emission of diamond, with a dependency on both the ion beam and electron beam acceleration voltage. CL emission in natural diamond is enhanced particularly at low ion beam and electron beam voltages. This enhancement of the CL emission can be partly explained by an increase in surface defects induced by ion milling. CL emission enhancement could be used to improve the CL image quality. To conduct FIB-SEM CL tomography, a recently developed novel specimen geometry is adopted to enable sequential ion milling and CL imaging on an untilted sample. We show that CL imaging can be manually combined with FIB-SEM tomography with a modified protocol for 3D microstructure reconstruction. In principle, automated FIB-SEM CL tomography should be feasible, provided that dedicated CL detectors are developed that allow subsequent milling and CL imaging without manual intervention, as the current CL detector needs to be manually retracted before a slice can be milled. Due to the required high electron beam acceleration voltage for CL emission, the resolution for FIB-SEM CL tomography is currently limited to several hundreds of nm in XY and up to 650 nm in Z for diamonds. Opaque materials are likely to have an improved Z resolution, as CL emission generated deeper in the material is not able to escape from it.     

A method of normalizing cathodoluminescence images of electron transparent foils for thickness contrast applied to InGaN quantum wells

The uniformity of panchromatic cathodoluminescence (CL) from In_0.09Ga_0.91N/GaN quantum wells at 100 K was investigated using a combined transmission electron microscope–cathodoluminescence instrument. A technique for correcting CL images of electron‐transparent wedge specimens for thickness contrast artefacts is presented. The foil thickness was estimated using the dynamical formulation of the relationship between the thickness and the (experimentally observed) transmitted electron intensity. For a given thickness the CL intensity was calculated using the Everhart–Hoff depth‐dose function and also taking into account surface recombination losses. Experimental CL images were normalized by dividing by the calculated CL value at each point. The procedure was successful in calculating the underlying materials contrast in CL images of thin specimens of InGaN single quantum wells. Non‐uniformities in the CL emission on the scale of ～0.7 µm were observed.     

Monte Carlo simulation of CL and EBIC contrasts for isolated dislocations

Electron beam-induced current (EBIC) and cathodoluminescence (CL) are widely used to investigate semiconductor materials and devices, particularly to obtain information on the recombination properties and the geometry of defects. This report describes a simple formulation of CL and EBIC contrasts based on the Born approximation of excess carrier density in the presence of a pointlike defect. Quantitative interpretation of the CL and EBIC images is often difficult because of a lack of accurate theory treating simultaneously both the details of the electron beam penetration in the semiconductor and the generation of EBIC and CL signals. To overcome this difficulty, the Monte Carlo approach to the phenomenon of the electron beam penetration in solids has been developed to calculate the CL and EBIC signals during a simulation of the electron trajectory. Results for an inclined dislocation in GaAs are presented.     

Deconvolution of scanning electron microscopy images

This paper describes a method of removing blurs in scanning electron microscopy (SEM) images caused by the existence of a finite beam size. Although the resolution of electron microscopy images has been dramatically improved by the use of high-brightness electron guns and low-aberration electron lenses, it is still limited by lens aberration and electron diffraction. Both are inevitable in practical electron optics. Therefore, a further reduction in resolution by improving SEM hardware seems difficult. In order to overcome this difficulty, computer deconvolution has been proposed for SEM images. In the present work, the SEM image is deconvoluted using the electron beam profile estimated from beam optics calculation. The results show that the resolution of the deconvoluted image is improved to one half of the resolution of the original SEM image.     

Radiation damage in coronene, rubrene and p-terphenyl, measured for incident electrons of kinetic energy between 100 and 200 kev

We have measured the sensitivity of three highly conjugated organic compounds to electron irradiation. Using a 200 keV TEM, loss of crystallinity was determined from quantitative electron-diffraction measurements. Degradation of the molecular ring structure was monitored from fading of the 6 eV pi-excitation peak in the energy-loss spectrum. Measurements at incident energies between 30 keV and 100 eV were made using a scanning electron microscope (SEM), by recording gradual decay of the cathodoluminescence (CL) signal. Expressed in Grays, the energy dose required for CL decay in coronene is a factor of 30 lower than for destruction of crystallinity and a factor of 300 lower than for destruction of the molecular structure. Below 1 keV, the CL-decay cross section shows no evidence of a threshold effect, indicating that the damage involved is caused by valence-electron (rather than K-shell) excitation. Therefore even relatively radiation-resistant organic materials may undergo some form of damage when examined in a low-energy electron microscope or a low-voltage SEM.     

A multimodal microcharacterisation of trace‐element zonation and crystallographic orientation in natural cassiterite by combining cathodoluminescence,EBSD, EPMA and contribution of confocal Raman‐in‐SEM imaging

In cassiterite, tin is associated with metals (titanium, niobium, tantalum, indium, tungsten, iron, manganese, mercury). Knowledge of mineral chemistry and trace‐element distribution is essential for: the understanding of ore formation, the exploration phase, the feasibility of ore treatment, and disposal/treatment of tailings after the exploitation phase. However, the availability of analytical methods make these characterisations difficult. We present a multitechnical approach to chemical and structural data that includes scanning electron microscopy (SEM)‐based imaging and microanalysis techniques such as: secondary and backscattered electrons, cathodoluminescence (CL), electron probe microanalyser (EPMA), electron backscattered diffraction (EBSD) and confocal Raman‐imaging integrated in a SEM (RISE). The presented results show the complementarity of the used analytical techniques. SEM, CL, EBSD, EPMA provide information from the interaction of an electron beam with minerals, leading to atomistic information about their composition, whereas RISE, Raman spectroscopy and imaging completes the studies with information about molecular vibrations, which are sensitive to structural modifications of the minerals. The correlation of Raman bands with the presence/absence of Nb, Ta, Fe (heterovalent substitution) and Ti (homovalent substitution) is established at a submicrometric scale. Combination of the different techniques makes it possible to establish a direct link between chemical and crystallographic data of cassiterite.     

Polyethylene glycol (PEG) embedding and subsequent de-embedding as a method for the correlation of light microscopy,scanning electron microscopy,and transmission electron microscopy

The polyethylene glycol (PEG) embedding and subsequent deembedding method was applied to the observation of general tissues in scanning electron microscopy (SEM). Resulting SEM images were of high quality. It was demonstrated that intermicroscopic correlation of images between light microscopy (LM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) is easily and reliably done by means of the PEG method. In particular, the exact correlation of immuno-LM with SEM is shown to be of potential value.     

SEM characterization of silicon nanostructures: can we meet the challenge?

The current semiconductor technology road map for device scaling champions a 4.5 nm gate length in production by 2022. The scanning electron microscope (SEM) as applied to critical dimensions (CD) metrology and associated characterization modes such as electron beam-induced current and cathodoluminescence (CL) has proved to be a workhorse for the semiconductor industry during the microelectronics era. We review some of the challenges facing these techniques in light of the silicon nanotechnology road map. We present some new results using voltage contrast imaging and CL spectroscopy of top-down fabricated silicon nanopillar/nanowires (<100 nm diameter), which highlight the visualization challenge. However, both techniques offer the promise of providing process characterization on the 10-20 nm scale with existing technology. Visualization at the 1 nm scale with these techniques may have to wait for aberration-corrected SEM to become more widely available. Basic secondary electron imaging and CD applications may be separately addressed by the He-ion microscope.     

Lock-in technique applied to cathodoluminescence of biomedical specimens in the SEM

Very low signals or disturbances by unwanted, foreign signals often lead to a restriction in the application of the cathodoluminescence (CL) method in the scanning electron microscope (SEM). This is even true if one uses an optimal CL detection system. We, therefore, introduced the lock-in-amplification technique, which has proved very successful in investigations of semiconductor materials into the biomedical field. After attaching the lock-in system to our SEM which has a special CL equipment, we found that this technique could remove the disturbance caused by the light emitted from the heated filament, which can be reflected into the CL detector. Specimens on polished Al-stubs or on Au-coated glass slides could be imaged with improved contrast. The same was true if we measured the wavelengths of the CL. A general improvement of the signal-to-noise ratio in all specimens could not be detected. However, the beam current could often be reduced when using the lock-in technique without a decrease in the quality of the CL image. A disadvantage of the commercially available lock-in amplifier is that pictures need a longer exposure time than without lock-in amplification.     

A computerized signal acquisition system for the quantitative evaluation of EBIC and CL data in a SEM

Electron beam-induced current (EBIC) and cathodoluminescence (CL) are widely used methods to obtain information about recombination properties of semiconducting materials and their defects on a micrometer length scale. In this article a computerized SEM (scanning electron microscope) setup is described, which enables us to perform simultaneous measurements of several signals and automatic temperature-dependent measurements. As examples for the performance of this system we present results obtained by simultaneous EBIC/CL experiments, allowing a reconstruction of the defect geometry. In a second example, the temperature dependence of the EBIC contrast is analyzed, introducing the method of EBIC spectroscopy.     

Color cathodoluminescence display in the scanning electron microscope of deep relief surfaces

A scanning electron microscope (SEM) is a multifunctional instrument for the measurement of topographic relief on the surface of bulk specimen images. This instrument is also available to detect the physical effects induced by an electron beam into subsurface layers. Space distribution of the physical properties of measured effects in the relative microrelief is a very important problem in the SEM. We describe a method of displaying specimen information in the SEM using the color cathodoluminescence (CCL-SEM) technique nondistorted by relief influence and CCL-SEM images with composite (color and black / white ) contrast using CCL+BSEmode.     

Mechanical scanning of the specimen in the scanning electron microscope

A scanning electron microscope (SEM) system equipped with a motor drive specimen stage fully controlled with a personal computer (PC) has been utilized for obtaining ultralow magnification SEM images. This modem motor drive stage works as a mechanical scanning device. To produce ultra-low magnification SEM images, we use a successful combination of the mechanical scanning, electronic scanning, and digital image processing techniques. This new method is extremely labor and time saving for ultra-low magnification and wide-area observation. The option of ultra-low magnification observation (while maintaining the original SEM functions and performance) is important during a scanning electron microscopy session.     

Enhanced EDX images by fusion of multimodal SEM images using pansharpening techniques

The goal of this paper is to explore the potential interest of image fusion in the context of multimodal scanning electron microscope (SEM) imaging. In particular, we aim at merging the backscattered electron images that usually have a high spatial resolution but do not provide enough discriminative information to physically classify the nature of the sample, with energy‐dispersive X‐ray spectroscopy (EDX) images that have discriminative information but a lower spatial resolution. The produced images are named enhanced EDX. To achieve this goal, we have compared the results obtained with classical pansharpening techniques for image fusion with an original approach tailored for multimodal SEM fusion of information. Quantitative assessment is obtained by means of two SEM images and a simulated dataset produced by a software based on PENELOPE.     

Transient of scanning electron microscopic images for a buried microstructure in insulators

We clarify the transient process and its mechanism of scanning electron microscope (SEM) images of a trench microstructure buried in insulators. First, interface charges of primary electrons trapped on the trench are derived from the charging model of a capacitor considering the electron beam induced current, and the surface potential is therefore assumed. The SEM signal current is then determined from its simplified relation with the surface potential. Calculated profiles of the secondary electron (SE) signal current and their time-evolution behaviors can well fit the transient of the experimental SEM images. Results show that the variation of the surface potential due to the transient interface charges and the effect of SE redistribution result in transients of the SEM imaging signal and the image width of the buried trench.     

Autoregressive Wiener filtering in a scanning electron microscopy imaging system

In this paper, we propose to use the autoregressive (AR)-based interpolator with Wiener filter and apply the idea to scanning electron microscope (SEM) images. The concept for combining the AR-based interpolator with Wiener filtering comes from the essential requirement of Wiener filtering for accurate and consistent estimation of the power of the noise in images prior to filter implementation. The resultant filter is called AR-Wiener filter. The proposed filter is embedded onto the frame grabber card of the scanning electron microscope (SEM) for real-time image processing. Different images are captured using SEM and used to compare the performances of the conventional Wiener and the proposed AR-Wiener technique.     

Investigation of fluorescent lamp phosphors using the combined CL and EDS modes of the SEM

The phenomenon of cathodoluminescence (CL) potentially offers the ideal tool for studying the phosphor materials used in fluorescent lamps, since it can be used directly on processed or unprocessed powders, on coatings in tubes, or on sections cut from tubes. Using examples of both single component materials and multi-component blends, it is demonstrated how a relatively unsophisticated dispersive CL system attached to a scanning electron microscope (SEM) can be used expediently in the extensive study of such phosphors. These studies can be significantly enhanced when other complementary modes of the SEM (e. g. the energy-dispersive x-ray analysis facility) are combined with the CL mode. The strength of the combined technique lies in the major role it can play in materials and processing aspects of the powders themselves, in the processing of the lamps (e.g. by optimising such parameters as coating thickness, packing density etc.), and in diagnostic studies of poor materials or lamps (e.g. by locating rogue particles/components and identifying their origin). The technique also provides a convenient method of studying the temperature stability of selected phosphors.     

Proper acquisition and handling of scanning electron microscopy images using a high-performance personal computer

The modern high-performance personal computer (PC) has very recently expanded the range of utilization of digital scanning electron microscopy (SEM) images, and the PC will be used increasingly with SEMs. However, the image quality of digital SEM images may be considerably influenced by scanning and digitization conditions. In particular, the effects of the aliasing error peculiar to digital data are often serious in the low-magnification acquisition (undersampling) of SEM images, and moreover even a high-magnification image (oversampling) is disturbed by the undersampled noise (a sort of aliasing error). Furthermore, the signal-to-noise ratio of a digitized SEM image is closely related to the performance of the analog-to-digital converter. To prevent a flood of low-quality digital images with artifacts by the aliasing and additional noise, we propose a method using very high-density sampling (scanning). In addition, we will discuss how to handle digital SEM images from the point of view of the sampling and quantization.