Modern Scanning Electron Microscopes Research Articles

Earth system science applications of next-generation SEM-EDS automated mineral mapping

Sedimentary rocks contain a unique record of the evolution of the Earth system. Deciphering this record requires a robust understanding of the identity, origin, composition, and post-depositional history of individual constituents. Petrographic analysis informed by Scanning Electron Microscope - Energy Dispersive Spectroscopy (SEM-EDS) mineral mapping can reveal the mineral identity, morphology and petrological context of each imaged grain, making it a valuable tool in the Earth Scientist’s analytical arsenal. Recent technological developments, including quantitative deconvolution of mixed-phase spectra (producing “mixels”), now allow rapid quantitative SEM-EDS-based analysis of a broad range of sedimentary rocks, including the previously troublesome fine-grained lithologies that comprise most of the sedimentary record. Here, we test the reliability and preferred mineral mapping work flow of a modern Field-Emission scanning electron microscope equipped with the Thermofisher Scientific Maps Mineralogy mineral mapping system, focusing on mud/siltstones and calcareous shales. We demonstrate that SEM-EDS mineral mapping that implements 1) a strict error minimization spectral matching approach and 2) spectral deconvolution to produce ‘mixels’ for mixed-phase X-ray volumes can robustly identify individual grains and produce quantitative mineralogical data sets comparable to conventional X-ray diffraction (XRD) analysis (R2 > 0.95). The correlation between SEM-EDS and XRD-derived mineralogy is influenced by mineral abundance, processing modes and mapped area characteristics. Minerals with higher abundance (>10 wt%) show better correlation, likely the result of increased uncertainty for XRD quantification of low-abundance phases. Automated spectral deconvolution to produce ‘mixels’ greatly reduces the proportion of unclassified pixels, especially in the fine-grained fraction, ultimately improving mineral identification and quantification. Mapping of larger areas benefits bulk mineralogy analysis, while customized area size and shape allows high-resolution in situ mineralogical analysis. Finally, we review SEM-EDS-based mineral mapping applications in the Earth Sciences, via case studies illustrating 1) approaches for the quantitative differentiation of various mineral components including detrital (allogenic), syndepositional (authigenic) and burial diagenetic phases, 2) the origin and significance of lamination, 3) the effectiveness and appropriateness of sequential leaching in geochemical studies, and 4) the utility of mineral maps to identify target grains within specific petrological contexts for in situ geochemical or geochronological analysis.

High Resolution Powder Electron Diffraction in Scanning Electron Microscopy.

A modern scanning electron microscope equipped with a pixelated detector of transmitted electrons can record a four-dimensional (4D) dataset containing a two-dimensional (2D) array of 2D nanobeam electron diffraction patterns; this is known as a four-dimensional scanning transmission electron microscopy (4D-STEM). In this work, we introduce a new version of our method called 4D-STEM/PNBD (powder nanobeam diffraction), which yields high-resolution powder diffractograms, whose quality is fully comparable to standard TEM/SAED (selected-area electron diffraction) patterns. Our method converts a complex 4D-STEM dataset measured on a nanocrystalline material to a single 2D powder electron diffractogram, which is easy to process with standard software. The original version of 4D-STEM/PNBD method, which suffered from low resolution, was improved in three important areas: (i) an optimized data collection protocol enables the experimental determination of the point spread function (PSF) of the primary electron beam, (ii) an improved data processing combines an entropy-based filtering of the whole dataset with a PSF-deconvolution of the individual 2D diffractograms and (iii) completely re-written software automates all calculations and requires just a minimal user input. The new method was applied to Au, TbF3 and TiO2 nanocrystals and the resolution of the 4D-STEM/PNBD diffractograms was even slightly better than that of TEM/SAED.

Array Tomography Workflow for the Targeted Acquisition of Volume Information using Scanning Electron Microscopy

Electron microscopy is applied in biology and medicine for imaging of cellular and structural details at nanometer resolution. Historically, Transmission Electron Microscopy (TEM) provided insight into cell ultrastructure, but in the recent decade, the development of modern Scanning Electron Microscopes (SEM) has changed the way of looking inside the cells. Even though the resolution of TEM is superior when protein-level structural details are needed, SEM-resolution is sufficient for the majority of the organelle-level cell biology-related questions. The advancement in technology enabled automatic volume acquisition solutions such as Serial block-face imaging (SBF-SEM) and Focused ion beam SEM (FIB-SEM). Nevertheless, to this day, these methods remain inefficient when the identification and navigation to areas of interest are crucial. Without the means for precise localization of target areas before imaging, operators need to acquire much more data than they need (in SBF-SEM), or, even worse, prepare many grids and image them all (in TEM). We propose the strategy of "lateral screening" using Array Tomography in SEM, which facilitates the localization of areas of interest, followed by automated imaging of the relevant fraction of the total sample volume. Array tomography samples are conserved during imaging, and they can be arranged into section libraries ready for repeated imaging. Several examples are shown in which lateral screening enables us to analyze structural details that are incredibly challenging to access with any other method.

Array Tomography Workflow for the Targeted Acquisition of Volume Information using Scanning Electron Microscopy.

Electron microscopy is applied in biology and medicine for imaging of cellular and structural details at nanometer resolution. Historically, Transmission Electron Microscopy (TEM) provided insight into cell ultrastructure, but in the recent decade, the development of modern Scanning Electron Microscopes (SEM) has changed the way of looking inside the cells. Even though the resolution of TEM is superior when protein-level structural details are needed, SEM-resolution is sufficient for the majority of the organelle-level cell biology-related questions. The advancement in technology enabled automatic volume acquisition solutions such as Serial block-face imaging (SBF-SEM) and Focused ion beam SEM (FIB-SEM). Nevertheless, to this day, these methods remain inefficient when the identification and navigation to areas of interest are crucial. Without the means for precise localization of target areas before imaging, operators need to acquire much more data than they need (in SBF-SEM), or, even worse, prepare many grids and image them all (in TEM). We propose the strategy of "lateral screening" using Array Tomography in SEM, which facilitates the localization of areas of interest, followed by automated imaging of the relevant fraction of the total sample volume. Array tomography samples are conserved during imaging, and they can be arranged into section libraries ready for repeated imaging. Several examples are shown in which lateral screening enables us to analyze structural details that are incredibly challenging to access with any other method.

Geochronological constraints on uranium mineralization within the Hüttenberg siderite deposit (Eastern Alps, Austria)

A small-scale hydrothermal uranium mineralization hosted within the siderite deposit at Hüttenberg (Eastern Alps, Austria) was re-investigated using modern scanning electron microscope (SEM) and microprobe (EMPA) methods. The uranium mineralization comprises brannerite, coffinite and uraninite, and is spatially associated with Fe-, Ni- and Co-arsenides (loellingite, rammelsbergite, safflorite), bismuth and bismuthinite, as well as rare accessory silver-bearing minerals and gold locally. The U-bearing fluids also carried P, Y and REEs, which precipitated as xenotime and P–Y coffinite. The uranium mineralization paragenetically postdates the metasomatic formation of the host siderite ore.Uraninite allows for precise single spot EMPA ages to be calculated (±2 Ma) due to its high radiogenic lead content. There is an excellent internal consistency in the uraninite data with calculated dates ranging between 77 and 84 Ma. We interpret that these record the crystallization age of the uraninite, and that any influences of lead loss or common Pb are minimal. Brannerite was also analyzed but U-total Pb microprobe data scatter (c.30–80 Ma) with evidence of lead loss, particularly in altered domains. It does, however, provide a minimum constraint on the timing of mineralization that is consistent with the crystallization age of the uraninite. Coffinite proved completely unsuitable for U-total Pb geochronology due to extreme lead loss. However, hydrothermal xenotime yields a U-total Pb age of 78 ± 5 Ma, consistent with the uraninite age. Therefore, the U-total Pb geochronological data support a late Cretaceous age for the U-mineralization of c. 80 Ma. Considering this timing constraint together with other geological and indirect thermochronological aspects, we conclude that the siderite deposit of Hüttenberg is older and formed at c. 90−80 Ma.

Versatile application of a modern scanning electron microscope for materials characterization

Scanning electron microscopy (SEM) is an indispensable characterization technique for materials science. More recently, scanning electron microscopes can be equipped with scanning transmission electron microscopy (STEM) detectors, which considerably extend their capabilities. It is demonstrated in this work that the correlative application of SEM and STEM imaging techniques provides comprehensive sample information on nanomaterials. This is highlighted by the use of a modern scanning electron microscope, which is equipped with in-lens and in-column detectors, a double-tilt holder for electron transparent specimens and a CCD camera for the acquisition of on-axis diffraction patterns. Using multi-walled carbon nanotubes and Pt/Al2O3 powder samples we will show that a complete characterization can be achieved by combining STEM (mass-thickness and diffraction) contrast and SEM (topography and materials) contrast. This is not possible in a standard transmission electron microscope where topography information cannot be routinely obtained. We also exploit the large tilt angle range of the specimen holder to perform 180 degrees STEM tomography on multi-walled carbon nanotubes, which avoids the missing wedge artifacts.

Analysis of crystal defects by scanning transmission electron microscopy (STEM) in a modern scanning electron microscope

Dislocations and stacking faults are important crystal defects, because they strongly influence material properties. As of now, transmission electron microscopy (TEM) is the most frequently used technique to study the properties of single dislocations and stacking faults. Specifically, the Burgers vector b of dislocations or displacement vector R of stacking faults can be determined on the basis of the g·b = n (g·R = n) criterion by setting up different two-beam diffraction conditions with an imaging vector g. Based on the reciprocity theorem, scanning transmission electron microscopy (STEM) can also be applied for defect characterization, but has been less frequently used up to now. In this work, we demonstrate g·b = n (g·R = n) analyses of dislocations and stacking faults in GaN by STEM imaging in a scanning electron microscope. The instrument is equipped with a STEM detector, double-tilt TEM specimen holder, and a charge-coupled-device camera for the acquisition of on-axis diffraction patterns. The latter two accessories are mandatory to control the specimen orientation, which has not been possible before in a scanning electron microscope.

Collection efficiency and acceptance maps of electron detectors for understanding signal detection on modern scanning electron microscopy.

Collection efficiency and acceptance maps of typical detectors in modern scanning electron microscopes (SEMs) were investigated. Secondary and backscattered electron trajectories from a specimen to through-the-lens and under-the-lens detectors placed on an electron optical axis and an Everhart-Thornley detector mounted on a specimen chamber were simulated three-dimensionally. The acceptance maps were drawn as the relationship between the energy and angle of collected electrons under different working distances. The collection efficiency considering the detector sensitivity was also estimated for the various working distances. These data indicated that the acceptance maps and collection efficiency are keys to understand the detection mechanism and image contrast for each detector in the modern SEMs. Furthermore, the working distance is the dominant parameter because electron trajectories are drastically changed with the working distance.

Современные растровые электронные микроскопы: всё сложнее, всё проще

Современные растровые электронные микроскопы: всё сложнее, всё проще

Fatigue strength characterization of Al-Si cast material incorporating statistical size effect

Cast aluminium components may exhibit material imperfections such as shrinkage and gas pores, or oxide inclusions. Therefore, the fatigue resistance is significantly influenced by the size and location of these inhomogenities. In this work, two different specimen geometries are manufactured from varying positions of an Al-Si-Cu alloy casting. The specimen geometries are designed by means of shape optimization based on a finite element analysis and exhibit different highly-stressed volumes. The numerically optimized specimen curvature enforces a notch factor of only two percent. To enable the evaluation of a statistical size effect, the length of the constant testing region and hence, the size of the highly-stressed volume varies by a ratio of one to ten between the two specimen geometries. Furthermore, the location of the crack initiation is dominated by the comparably greatest defects in this highly-stressed volume, which is also known as Weibull’s weakest link model. The crack initiating defect sizes are evaluated by means of light microscopy and modern scanning electron microscope methods. Finally, the statistical size effect is analysed based on the extreme value distribution of the occurring defects, whereby the size and location of the pores is non-destructively obtained by computed tomography (CT) scanning. This elaborated procedure facilitates a size-effect based methodology to study the defect distribution and the associated local fatigue life of CPS casted Al-Si lightweight components.

Contrast of positively charged oxide precipitate in out-lens, in-lens and in-column SE image.

Modern scanning electron microscopes are usually equipped with multiple detectors and enable simultaneous collection of two or even three secondary electron images. The secondary electrons become divided between the detectors in dependence on their initial kinetic energy and emission angle. In this study, sharing of the secondary electrons by out-lens, in-lens and in-column detectors has been systematically investigated. Energy filtering of the signal electrons is demonstrated by separation of the voltage and the topographical contrast in the micrographs obtained by out-lens and in-lens/in-column detectors. The presence of two detectors inside the electron column enables further filtering of the low kinetic energy secondary electrons, which results to unusual contrasts and phenomena. In this paper, inversion of the contrast sign between a positively charged oxide particle and conductive steel matrix (i.e. voltage contrast) in SE images collected under specific imaging conditions is demonstrated.

Quantifying Porosity through Automated Image Collection and Batch Image Processing: Case Study of Three Carbonates and an Aragonite Cemented Sandstone

Modern scanning electron microscopes often include software that allows for the possibility of obtaining large format high-resolution image montages over areas of several square centimeters. Such montages are typically automatically acquired and stitched, comprising many thousand individual tiled images. Images, collected over a regular grid pattern, are a rich source of information on factors such as variability in porosity and distribution of mineral phases, but can be hard to visually interpret. Additional quantitative data can be accessed through the application of image analysis. We use backscattered electron (BSE) images, collected from polished thin sections of two limestone samples from the Cretaceous of Brazil, a Carboniferous limestone from Scotland, and a carbonate cemented sandstone from Northern Ireland, with up to 25,000 tiles per image, collecting numerical quantitative data on the distribution of porosity. Images were automatically collected using the FEI software Maps, batch processed by image analysis (through ImageJ), with results plotted on 2D contour plots with MATLAB. These plots numerically and visually clearly express the collected porosity data in an easily accessible form, and have application for the display of other data such as pore size, shape, grain size/shape, orientation and mineral distribution, as well as being of relevance to sandstone, mudrock and other porous media.

Graphite oxidation and SEM as a tool for microstructural investigation

The microstructure of graphite and its oxidation have been individually investigated at length. When any catalytic impurities are removed from graphite, oxidative attack takes place preferentially from the exposed edges, or active sites of graphite crystallites. This provides valuable insights regarding the underlying crystallography and fundamental structure of graphite which are not immediately evident from a raw topographical examination using, for example, microscopy. Using new techniques, such as field emission guns and sensitive detectors, modern scanning electron microscopes are capable of operating down to a few hundred volts. When surface features and effects are being considered this is absolutely critical as the low voltages imply low sample penetration of the electrons, thus the true surface morphology of the material can be resolved. In combination, these methods provide a valuable technique for investigating the microstructures found in graphite. The approach has been applied to natural graphite but is even more relevant to synthetic graphite and therefore nuclear materials, which have an exceedingly complex microstructure. The revealed structural qualities can be related to the manufacturing processes in order to gain additional insights into the material and uncover potential options for improving the properties.

High quality transmission Kikuchi diffraction analysis of deformed alloys - Case study

Modern scanning electron microscopes (SEM) equipped with thermally assisted field emission guns (Schottky FEG) are capable of imaging with a resolution in the range of several nanometers or better. Simultaneously, the high electron beam current can be used, which enables fast chemical and crystallographic analysis with a higher resolution than is normally offered by SEM with a tungsten cathode. The current resolution that limits the EDS and EBSD analysis is related to materials' physics, particularly to the electron-specimen interaction volume. The application of thin, electron-transparent specimens, instead of bulk samples, improves the resolution and allows for the detailed analysis of very fine microstructural features. Beside the typical imaging mode, it is possible to use a standard EBSD camera in such a configuration that only transmitted and scattered electrons are detected. This modern approach was successfully applied to various materials giving rise to significant resolution improvement, especially for the light element magnesium based alloys. This paper presents an insight into the application of the transmission Kikuchi diffraction (TKD) technique applied to the most troublesome, heavily-deformed materials. In particular, the values of the highest possible acquisition rates for high resolution and high quality mapping were estimated within typical imaging conditions of stainless steel and magnesium-yttrium alloy.

Improving Spatial Detection of Twins Achieved by Measuring Individual Kikuchi Band Intensity in EBSD Patterns

Twin boundaries in a crystalline material can be defined by a particular rotation angle about a particular access or a mirrored crystal orientation about a particular plane [1]. For example, copper twins are typically defined by a 60 rotation about where the associated twin plane is of the {111} family. One critical area of twin research looks at deformation twinning as the limiting factor for formability of Mg alloys, such as AZ31 [2]. In AZ31 there are two basic twin modes: compression twinning and tension twinning. The latter phenomenon forms fairly large, easy to detect twinned regions within parent grains, whereas the former tends to form extremely thin twins that are on the order of 100 nm wide. Additionally, the copper which is frequently seen in many microelectronics contains twins on the order of 10 nm [3]. In both cases these features are within the detectable limits for a modern scanning electron microscope (SEM). However, identifying these twins via crystal orientation relations with electron backscatter diffraction (EBSD) in the SEM relies on a larger spatial resolution which makes detecting these twins from crystallographic information difficult in the SEM. This study presents a method whereby improved spatial resolution of thin twins can be achieved with EBSD.

Concepts for an Annular Pole Piece Detector for the Simultaneous Measurement of X-Rays and Backscattered Electrons Inside a SEM

In modern Scanning Electron Microscopes (SEM) a large variety of different signals is collected to create images with various contrasts or to receive compositional information. Among others, Backscattered Electrons (BSE) and characteristic X-rays belong to the major signals which are collected routinely. Both give information about the sample composition and therefore complement each other very good as exemplarily shown in Figure 1. Since electrons and photons follow a straight path out of the sample the collection efficiency is weak if the detectors are far away from the sample resulting in a small solid angle in which they are collected. Hence, in order to collect them with high efficiency modern BSE and Energy Dispersive X-Ray (EDX) detectors use large active areas and are positioned close to the sample.

Fractographic insights into cracking mechanisms and microstructure

ABSTRACTThis Special Issue celebrates the first 30 years of the existence of the Italian Group on Fracture (IGF). In that time, the fractographic imaging capability afforded by scanning electron microscopes had undergone a technological revolution, offering unparalleled opportunities to characterize very fine fracture surface features and to characterize chemical species and microstructure via such techniques as energy dispersive spectroscopy (EDS), wavelength dispersive spectroscopy (WDS) and electron backscatter diffraction (EBSD). A wavelength‐dispersive spectrometer uses the characteristic X‐rays generated by individual elements to enable quantitative analysis (down to trace element levels) to be performed with spot sizes as small as a few micrometres. This complements EDS where a user can acquire a full elemental spectrum in only a few seconds but where energy peaks may overlap among different elements, particularly those corresponding to X‐rays generated by emission from different energy‐level shells (K, L and M) in different elements. It then becomes easier to acquire a quantitative elemental map alongside excellent fracture surface images. This paper considers some of the areas in fractography where the increased capability of modern scanning electron microscopes confers advantages.

High Resolution EBSD/SEM Analysis of PLZT Ferroelectric Crystals in Low Vacuum Conditions - A few Practical Remarks

Modern scanning electron microscopes (SEMs) increase the ability to study a wide range of materials. Especially, an application of low vacuum conditions enables characterization of nonconductive samples without complicated preparation procedure. However, the operator must be aware of several problems he may encounter collecting electron diffractions in the SEM with variable pressure. The charge control and quality of the surface are the challenges when running experiments on insulators. Specimen charging obscures forward scatter electrons images and decreases the EBSD pattern quality making indexing difficult or even impossible. Another crucial question is how to limit the influence of so called "skirt effect" caused by ionization of gas molecules followed by electron beam broading above the sample. The influence of several important parameters (gas pressure, a type of gas, working distance and energy of electron beam) on the EBSD pattern quality must also be considered. When it is properly done, a coupling of crystallographic information with the chemical data obtained from Energy Dispersive Spectroscopy (EDS) in the LV-SEM allows to perform phase identification of insulators. The paper presents some ideas how to deal with the (Pb, La)(Zr, Ti)O3 ceramics in high resolution Quanta 3D SEM (with thermally assisted Schottky type FEG) equipped with EDAX-TSL system in low vacuum environment. The problems occurring during EBSD analysis of the PLZT ceramics are discussed and some solutions are suggested. Paper summarizes the results obtained from PLZT ferroelectric ceramics in the low vacuum FEGSEM and shows how to optimise experimental parameters in order to achieve the best quality of orientation maps acquired from nonconductive samples.

Thermal etching of SiC

Thermal etching of SiC or its decomposition at high temperatures is of significance because of the many industrial applications of SiC at high temperatures. The effect of vacuum annealing at relatively high temperatures (1200–1800°C) on the surface microstructure of 6H-SiC and polycrystalline SiC was investigated using a modern high resolution scanning electron microscope (FEG-SEM) with an in-lens detector. Crystal defects such as stacking faults and twins on the SiC surfaces were easily observed in this system. Thermal etching of SiC already started at 1200°C with evidence of step bunching and grain boundary grooving. Preferred etching occurred on certain crystal surfaces of polycrystalline SiC. Significant decomposition of SiC occurred at 1800°C. The resulting decomposition structures have possible nanotechnological applications.

Characterization of semiconductor detectors of (1–30)-keV monoenergetic and backscattered electrons

Semiconductor detectors of backscattered electrons are basic elements of all modern scanning electron microscopes. Their quality is determined by the properties of planar p-n junctions and the parameters of the protective layer on the detector surface. The main characteristics of semiconductor detectors are considered, their response functions are calculated, and the threshold signal cutoff energies are found both for a monoenergetic electron beam and for detection of the total energy spectrum of backscattered electrons. The experimental results are in good agreement with the computational model data.