This paper presents a statistical method to analyze instabilities that can be introduced during imaging in scanning electron microscopy (SEM). The method is based on the correlation of digital images and it can be used at different length scales. It consists of the evaluation of three different approaches with four parameters in total. The methodology is exemplified with a specific case of internal stress measurements where ion milling and SEM imaging are combined with digital image correlation. It is concluded that before these measurements it is important to test the SEM column to ensure the minimization and randomization of the imaging instabilities. The method has been applied onto three different field emission gun SEMs (Philips XL30, Tescan Lyra, FEI Helios 650) that represent three successive generations of SEMs. Important to note that the imaging instability can be quantified and its source can be identified.

A procedure based on focused ion beam milling and in situ lift-out is introduced for the preparation of high-quality specimens for in situ annealing experiments in the transmission electron microscope. The procedure allows an electron-transparent lamella to be cleaned directly on a heating chip using a low ion energy and back-side milling in order to minimize redeposition and damage. The approach is illustrated through the preparation of an Al–Mn–Fe complex metallic alloy specimen.

A new technique for the preparation of heavily cracked, heavily damaged, brittle materials for examination in a transmission electron microscope (TEM) is described in detail. In this study, cross-sectional TEM samples were prepared from indented silicon carbide (SiC) bulk ceramics, although this technique could also be applied to other brittle and/or multiphase materials. During TEM sample preparation, milling-induced damage must be minimized, since in studying deformation mechanisms, it would be difficult to distinguish deformation-induced cracking from cracking occurring due to the sample preparation. The samples were prepared using a site-specific, two-step ion milling sequence accompanied by epoxy vacuum infiltration into the cracks. This technique allows the heavily cracked, brittle ceramic material to stay intact during sample preparation and also helps preserve the true microstructure of the cracked area underneath the indent. Some preliminary TEM results are given and discussed in regards to deformation studies in ceramic materials. This sample preparation technique could be applied to other cracked and/or heavily damaged materials, including geological materials, archaeological materials, fatigued materials, and corrosion samples.

In the field of electron microscopy the replica technique is known as an indirect method and also as an extraction method that is usually applied on metallurgical samples. This contribution describes a fast and simple transmission electron microscopic (TEM) sample preparation by complete removal of nanoparticles from a substrate surface that allows the study of growth mechanisms of nanostructured coatings. The comparison and combination of advanced diffraction techniques in the TEM and scanning electron microscopy (SEM) provide possibilities for operators with access to both facilities. The analysis of TEM-derived diffraction patterns (convergent beam electron diffraction) in the SEM/electron backscatter diffraction software simplifies the application, especially when the patterns are not aligned along a distinct zone axis. The study of the TEM sample directly by SEM and transmission Kikuchi diffraction allows cross-correlation with the TEM results.

Atom-probe tomography is a materials characterization method ideally suited for the investigation of clustering and precipitation phenomena. To distinguish the clusters from the surrounding matrix, the maximum separation algorithm is widely employed. However, the results of the cluster analysis strongly depend on the parameters used in the algorithm and hence, a wrong choice of parameters leads to erroneous results, e.g., for the cluster number density, concentration, and size. Here, a new method to determine the optimum value of the parameter dmax is proposed, which relies only on information contained in the measured atom-probe data set. Atom-probe simulations are employed to verify the method and to determine the sensitivity of the maximum separation algorithm to other input parameters. In addition, simulations are used to assess the accuracy of cluster analysis in the presence of trajectory aberrations caused by the local magnification effect. In the case of Cu-rich precipitates (Cu concentration 40–60 at% and radius 0.25–1.0 nm) in a bcc Fe–Si–Cu matrix, it is shown that the error in concentration is below 10 at% and the error in radius is <0.15 nm for all simulated conditions, provided that the correct value for dmax, as determined with the newly proposed method, is employed.

The resonant frequency and sensitivity of an atomic force microscope (AFM) with an assembled cantilever probe (ACP) is analyzed utilizing strain gradient theory, and then the governing equation and boundary conditions are derived by a combination of the basic equations of strain gradient theory and Hamilton’s principle. The resonant frequency and sensitivity of the proposed AFM microcantilever are then obtained numerically. The proposed ACP includes a horizontal cantilever, two vertical extensions, and two tips located at the free ends of the extensions that form a caliper. As one of the extensions is located between the clamped and free ends of the AFM microcantilever, the cantilever is modeled as two beams. The results of the current model are compared with those evaluated by both modified couple stress and classical beam theories. The difference in results evaluated by the strain gradient theory and those predicted by the couple stress and classical beam theories is significant, especially when the microcantilever thickness is approximately the same as the material length-scale parameters. The results also indicate that at the low values of contact stiffness, scanning in the higher cantilever modes decrease the accuracy of the proposed AFM ACP.

Atomic force microscopy (AFM) and laser scanning microscopy (LSM) measurements on a series of specially designed roughness artifacts were performed and the results characterized by spectral analysis. As demonstrated by comparisons, both AFM and LSM can image the complex structures with high resolution and fidelity. When the surface autocorrelation length increases from 200 to 500 nm, the cumulative power spectral density spectra of the design, AFM and LSM data reach a better agreement with each other. The critical wavelength of AFM characterization is smaller than that of LSM, and the gap between the measured and designed critical wavelengths is reduced with an increase in the surface autocorrelation length. Topography measurements of surfaces with a near zero or negatively skewed height distribution were determined to be accurate. However, obvious discrepancies were found for surfaces with a positive skewness owing to more severe dilations of either the solid tip of the AFM or the laser tip of the LSM. Further surface parameter evaluation and template matching analysis verified that the main distortions in AFM measurements are tip dilations while those in LSM are generally larger and more complex.

In this paper, the process of pushing rough cylindrical micro/nanoparticles on a surface with an atomic force microscope (AFM) probe is investigated. For this purpose, the mechanics of contact involving adhesion are studied first. Then, a method is presented for estimating the real area of contact between a rough cylindrical particle (whose surface roughness is described by the Rumpf and Rabinovich models) and a smooth surface. A dynamic model is then obtained for the pushing of rough cylindrical particles on a surface with an AFM probe. Afterwards, the process is simulated for different particle sizes and various roughness dimensions. Finally, by reducing the length of the cylindrical particle, the simulation condition is brought closer to the manipulation condition of a smooth spherical particle on a rough substrate, and the simulation results of the two cases are compared. Based on the simulation results, the critical force and time of manipulation diminish for rough particles relative to smooth ones. Reduction in the aspect ratio at a constant cross-section radius and the radius of asperities (height of asperities based on the Rabinovich model) results in an increase in critical force and time of manipulation.

The impact of lubricants on pole-tip recession and surface morphology of hard disk drive heads in the precision lapping process was investigated with atomic force microscopy, scanning electron microscopy, and auger electron spectroscopy. In particular, the effects of deionized water, hydrocarbon oil, ethanediol, isopropanol, and ethanol lubricants were evaluated. The results reveal that proper selection of lubricant is critical for achieving optimal performance in the lapping process. A mixture of 68% hydrocarbon oil, 30% isopropanol, and 2% octadecenoic acid was found to yield the most favorable results, displaying a writer shield recession, first shield of reader recession, and surface roughness of 0.423, 0.581, and 0.242 nm, respectively.

We have studied the influence of experimental factors and specimen geometry on the quality of the mass spectra in copper (Cu) during pulsed-laser atom-probe tomography. We have evaluated the effects of laser pulse energy, laser pulse frequency, specimen base temperature, specimen tip radius, and specimen tip shank half-angle on the effects of mass resolving power, (m/Δm), at full-width at half-maximum and at full-width at tenth-maximum, the tail size after the major mass-to-charge state (m/n) ratio peaks, and the mass spectra. Our results indicate that mass resolving power improves with decreasing pulse energy between 40 and 80 pJ and decreasing base temperature between 20 and 80 K. The mass resolving power also improves with increasing tip radius and shank half-angle. A pulse frequency of 250 kHz slightly improves the mass resolving power relative to 100 or 500 kHz. The tail size decreases with increasing pulse energy. The mass resolving power improves when the cooling time is reduced, which is influenced by the thermal diffusivity of Cu and the specimen base temperature.

The composition of co-precipitated and collocated NbC carbide precipitates, Fe3C iron carbide (cementite), and Cu-rich precipitates are studied experimentally by atom-probe tomography (APT). The Cu-rich precipitates located at a grain boundary (GB) are also studied. The APT results for the carbides are supplemented with computational thermodynamics predictions of composition at thermodynamic equilibrium. Two types of NbC carbide precipitates are distinguished based on their stoichiometric ratio and size. The Cu-rich precipitates at the periphery of the iron carbide and at the GB are larger than those distributed in the α-Fe (body-centered cubic) matrix, which is attributed to short-circuit diffusion of Cu along the GB. Manganese segregation is not observed at the heterophase interfaces of the Cu-rich precipitates that are located at the periphery of the iron carbide or at the GB, which is unlike those located at the edge of the NbC carbide precipitates or distributed in the α-Fe matrix. This suggests the presence of two populations of NiAl-type (B2 structure) phases at the heterophase interfaces in multicomponent Fe–Cu steels.

To unambiguously evaluate the indium and nitrogen concentrations in InxGa1−xNyAs1−y, two independent sources of information must be obtained experimentally. Based on high-resolution scanning transmission electron microscopy (STEM) images taken with a high-angle annular dark-field (HAADF) detector the strain state of the InGaNAs quantum well is determined as well as its characteristic HAADF-scattering intensity. The strain state is evaluated by applying elasticity theory and the HAADF intensity is used for a comparison with multislice simulations. The combination of both allows for determination of the chemical composition where the results are in accordance with X-ray diffraction measurements, three-dimensional atom probe tomography, and further transmission electron microscopy analysis. The HAADF-STEM evaluation was used to investigate the influence of As-stabilized annealing on the InGaNAs/GaAs sample. Photoluminescence measurements show an annealing-induced blue shift of the emission wavelength. The chemical analysis precludes an elemental diffusion as origin of the energy shift—instead the results are in agreement with a model based on an annealing-induced redistribution of the atomic next-neighbor configuration.

Recent studies have shown that when graphene is placed on a thin hexagonal boron nitride (h-BN) substrate, unlike when it is placed on a typical SiO2 surface, it can closely approach the ideal carrier mobility observed in suspended graphene samples. This study further examines the epitaxial relationship between graphene and h-BN substrate with high-resolution transmission electron microscopy simulation. Virtual monolayer and multilayer stacks of h-BN were produced with a monolayer of graphene on top, on bottom, and in between h-BN layers, in order to study this interface. Once the simulations were performed, the phase contrast image and Moiré pattern created by this heterostack were analyzed for local and global intensity minima and maxima. In addition, h-BN substrate thickness and rotations between h-BN and graphene were probed and analyzed. The simulated images produced in this work will be used to help understand subsequent transmission electron microscopy images and electron energy-loss studies.

Here, we report the development of an approach to map atomic resolution images into a convenient matrix representation. Through the combination of two-dimensional Gaussian fitting and the projective standard deviation, atom column locations are projected onto two noncollinear reference lattice vectors that are used to assign each a unique (i, j) matrix index. By doing so, straightforward atomic resolution image analysis becomes possible. Using practical examples, we demonstrate that the matrix representation greatly simplifies categorizing atom columns to different sublattices. This enables a myriad of direct analyses, such as mapping atom column properties and correlating long-range atom column pairs. MATLAB source code can be downloaded from https://github.com/subangstrom/aci.

A connection between microscopic structure and macroscopic properties is expected for almost all material systems. High-resolution transmission electron microscopy is a technique offering insight into the atomic structure, but the analysis of large image series can be time consuming. The present work describes a method to automatically estimate the atomic structure in two-dimensional materials. As an example graphene is chosen, in which the positions of the carbon atoms are reconstructed. Lattice parameters are extracted in the frequency domain and an initial atom positioning is estimated. Next, a plausible neighborhood structure is estimated. Finally, atom positions are adjusted by simulation of a Markov random field model, integrating image evidence and the strong geometric prior. A pristine sample with high regularity and a sample with an induced hole are analyzed. False discovery rate-controlled large-scale simultaneous hypothesis testing is used as a statistical framework for interpretation of results. The first sample yields, as expected, a homogeneous distribution of carbon–carbon (C–C) bond lengths. The second sample exhibits regions of shorter C–C bond lengths with a preferred orientation, suggesting either strain in the structure or a buckling of the graphene sheet. The precision of the method is demonstrated on simulated model structures and by its application to multiple exposures of the two graphene samples.

We report our effort to quantify atomic-scale chemical maps obtained by collecting energy-dispersive X-ray spectra (EDS) using scanning transmission electron microscopy (STEM) (STEM-EDS). With thin specimen conditions and localized EDS scattering potential, the X-ray counts from atomic columns can be properly counted by fitting Gaussian peaks at the atomic columns, and can then be used for site-by-site chemical quantification. The effects of specimen thickness and X-ray energy on the Gaussian peak width are investigated using SrTiO3 (STO) as a model specimen. The relationship between the peak width and spatial resolution of an EDS map is also studied. Furthermore, the method developed by this work is applied to study cation occupancy in a Sm-doped STO thin film and antiphase boundaries (APBs) present within the STO film. We find that Sm atoms occupy both Sr and Ti sites but preferably the Sr sites, and Sm atoms are relatively depleted at the APBs likely owing to the effect of strain.

To date, it is unclear whether chemical order (or disorder) is in any way connected to double exchange, electronic phase separation, or charge ordering (CO) in manganites. In this work, we carry out an atomic resolution study of the colossal magnetoresistant manganite La2−2xSr1+2xMn2O7 (LSMO). We combine aberration-corrected electron microscopy and spectroscopy with spectroscopic image simulations, to analyze cation ordering at the atomic scale in real space in a number of LSMO single crystals. We compare three different compositions within the phase diagram: a ferromagnetic metallic material (x=0.36), an insulating, antiferromagnetic charge ordered (AF-CO) compound (x=0.5), which also exhibits orbital ordering, and an additional AF sample (x=0.56). Detailed image simulations are essential to accurately quantify the degree of chemical ordering of these samples. We find a significant degree of long-range chemical ordering in all cases, which increases in the AF-CO range. However, the degree of ordering is never complete nor can it explain the strongly correlated underlying ordering phenomena. Our results show that chemical ordering over distinct crystallographic sites is not needed for electronic ordering phenomena to appear in manganites, and cannot by itself explain the complex electronic behavior of LSMO.

The dehydrogenated microstructure of the lithium borohydride-yttrium hydride (LiBH4-YH3) composite obtained at 350°C under 0.3 MPa of hydrogen and static vacuum was investigated by transmission electron microscopy combined with a focused ion beam technique. The dehydrogenation reaction between LiBH4 and YH3 into LiH and YB4 takes place under 0.3 MPa of hydrogen, which produces YB4 nano-crystallites that are uniformly distributed in the LiH matrix. This microstructural feature seems to be beneficial for rehydrogenation of the dehydrogenation products. On the other hand, the dehydrogenation process is incomplete under static vacuum, leading to the unreacted microstructure, where YH3 and YH2 crystallites are embedded in LiBH4 matrix. High resolution imaging confirmed the presence of crystalline B resulting from the self-decomposition of LiBH4. However, Li2B12H12, which is assumed to be present in the LiBH4 matrix, was not clearly observed.

Since 1972, when the US Occupational Health and Safety Administration established the first limits on occupational exposure to asbestos fibers, numerous analytical methods employing several microscopy techniques have been developed to identify a group of minerals defined by legislation as asbestos. While transmission electron microscopy (TEM) is implemented in standardized analytical methods, these methods specify the use of selected area electron diffraction. Because of this constraint, the diffraction data a TEM can provide are often underutilized due to challenges associated with collecting and interpreting individual diffraction patterns. It has been shown that transmission electron backscatter diffraction (tEBSD) produces diffraction patterns nearly identical to electron backscatter diffraction, but from smaller crystal domains. This paper explores the utility of tEBSD for characterization of asbestiform particles from reference asbestos materials, a suite of amphibole minerals of varying morphologies to determine if there is a correlation between mineral habit (i.e., crystal form), microscopic particle shape preferred orientation, and mineral specimens from an industrial talc deposit to provide a case study of the utility and limitations of the technique.

Solid oxide fuel cells (SOFCs) are promising candidates for use in alternative energy technologies. A full understanding of the reaction mechanisms in these dynamic material systems is required to optimize device performance and overcome present limitations. Here, we show that in situ transmission electron microscopy (TEM) can be used to study redox reactions and ionic conductivity in SOFCs in a gas environment at elevated temperature. We examine model ultrathin half and complete cells in two environmental TEMs using off-axis electron holography and electron energy-loss spectroscopy. Our results from the model cells provide insight into the essential phenomena that are important for the operation of commercial devices. Changes in the activities of dopant cations in the solid electrolyte are detected during oxygen anion conduction, demonstrating the key role of dopants in electrolyte architecture in SOFCs.