Introducing a Dynamic Reconstruction Methodology for Multilayered Structures in Atom Probe Tomography.

Atom probe tomography (APT) is a powerful three-dimensional nanoanalyzing microscopy technique considered key in modern materials science. However, progress in the spatial reconstruction of APT data has been rather limited since the first implementation of the protocol proposed by Bas et al. in 1995. This paper proposes a simple semianalytical approach to reconstruct multilayered structures, i.e., two or more different compounds stacked perpendicular to the analysis direction. Using a field evaporation model, the general dynamic evolution of parameters involved in the reconstruction of this type of structure is estimated. Some experimental reconstructions of different structures through the implementation of this method that dynamically accommodates variations in the tomographic reconstruction parameters are presented. It is shown both experimentally and theoretically that the depth accuracy of reconstructed APT images is improved using this method. The method requires few parameters in order to be easily usable and substantially improves atom probe tomographic reconstructions of multilayered structures.

A Study of Parameters Affecting Atom Probe Tomography Specimen Survivability.

Specimen survivability is a primary concern to those who utilize atom probe tomography (APT) for materials analysis. The state-of-the-art in understanding survivability might best be described as common-sense application of basic physics principles to describe failure mechanisms. For example, APT samples are placed under near-failure mechanical-stress conditions, so reduction in the force required to initiate field evaporation must provide for higher survivability-a common sense explanation of survivability. However, the interplay of various analytical conditions (or instrumentation) and how they influence survivability (e.g., decreasing the applied evaporation field improves survivability), and which factors have more impact than others has not been studied. In this paper, we report on the systematic analysis of a material composed of a silicon-dioxide layer surrounded on two sides by silicon. In total, 261 specimens were fabricated and analyzed under a variety of conditions to correlate statistically significant survivability trends with analysis conditions and other specimen characteristics. The primary result suggests that, while applied field/force plays an obvious role in survivability for this material, the applied field alone does not predict survivability trends for silicon/silicon-dioxide interfaces. The rate at which ions are extracted from the specimen (both in terms of ions-per-pulse and pulse-frequency) has similar importance.

Modern Focused-Ion-Beam-Based Site-Specific Specimen Preparation for Atom Probe Tomography.

Approximately 30 years after the first use of focused ion beam (FIB) instruments to prepare atom probe tomography specimens, this technique has grown to be used by hundreds of researchers around the world. This past decade has seen tremendous advances in atom probe applications, enabled by the continued development of FIB-based specimen preparation methodologies. In this work, we provide a short review of the origin of the FIB method and the standard methods used today for lift-out and sharpening, using the annular milling method as applied to atom probe tomography specimens. Key steps for enabling correlative analysis with transmission electron-beam backscatter diffraction, transmission electron microscopy, and atom probe tomography are presented, and strategies for preparing specimens for modern microelectronic device structures are reviewed and discussed in detail. Examples are used for discussion of the steps for each of these methods. We conclude with examples of the challenges presented by complex topologies such as nanowires, nanoparticles, and organic materials.

Implementing Transmission Electron Backscatter Diffraction for Atom Probe Tomography.

There are advantages to performing transmission electron backscattering diffraction (tEBSD) in conjunction with focused ion beam-based specimen preparation for atom probe tomography (APT). Although tEBSD allows users to identify the position and character of grain boundaries, which can then be combined with APT to provide full chemical and orientation characterization of grain boundaries, tEBSD can also provide imaging information that improves the APT specimen preparation process by insuring proper placement of the targeted grain boundary within an APT specimen. In this report we discuss sample tilt angles, ion beam milling energies, and other considerations to optimize Kikuchi diffraction pattern quality for the APT specimen geometry. Coordinated specimen preparation and analysis of a grain boundary in a Ni-based Inconel 600 alloy is used to illustrate the approach revealing a 50° misorientation and trace element segregation to the grain boundary.

On the use of simulated field-evaporated specimen apex shapes in atom probe tomography data reconstruction.

The ability to accurately reconstruct original spatial positions of field-evaporated ions emitted from a surface is fundamental to the success of atom probe tomography. As such, a clear understanding of the evolution of specimen shape and the resultant ions' trajectories during field evaporation plays an important role in improving reconstruction accuracy. To further this understanding, field-evaporation simulations of a bilayer specimen composed of two materials having an evaporation field difference of 20% were performed. The simulated field-evaporation patterns qualitatively compare favorably with experimental data, which provides confidence in the accuracy of specimen shapes predicted by the simulation. Correlations of known original atom positions with detector hit positions as a function of lateral detector position and evaporated depth were derived from the simulation. These correlations are contrasted with the current state-of-the-art reconstruction method thus outlining limitations of the current methodology. A pair of transformations are defined that take into account field-evaporated specimen shapes, and the resulting radial magnifications, to relate recorded ion positions in detector space to reconstructed atomic positions in specimen space. This novel process, when applied to simulated data, results in approximately a factor of 2 improvement in accuracy for reconstructions of interfaces with unequal fields (most general interfaces). This method is not constrained by the fundamental assumption of a hemispherical specimen shape.

Atomic-scale phase composition through multivariate statistical analysis of atom probe tomography data.

We demonstrate for the first time that multivariate statistical analysis techniques can be applied to atom probe tomography data to estimate the chemical composition of a sample at the full spatial resolution of the atom probe in three dimensions. Whereas the raw atom probe data provide the specific identity of an atom at a precise location, the multivariate results can be interpreted in terms of the probabilities that an atom representing a particular chemical phase is situated there. When aggregated to the size scale of a single atom (∼0.2 nm), atom probe spectral-image datasets are huge and extremely sparse. In fact, the average spectrum will have somewhat less than one total count per spectrum due to imperfect detection efficiency. These conditions, under which the variance in the data is completely dominated by counting noise, test the limits of multivariate analysis, and an extensive discussion of how to extract the chemical information is presented. Efficient numerical approaches to performing principal component analysis (PCA) on these datasets, which may number hundreds of millions of individual spectra, are put forward, and it is shown that PCA can be computed in a few seconds on a typical laptop computer.

Machine-learning-enhanced time-of-flight mass spectrometry analysis.

Mass spectrometry is a widespread approach used to work out what the constituents of a material are. Atoms and molecules are removed from the material and collected, and subsequently, a critical step is to infer their correct identities based on patterns formed in their mass-to-charge ratios and relative isotopic abundances. However, this identification step still mainly relies on individual users' expertise, making its standardization challenging, and hindering efficient data processing. Here, we introduce an approach that leverages modern machine learning technique to identify peak patterns in time-of-flight mass spectra within microseconds, outperforming human users without loss of accuracy. Our approach is cross-validated on mass spectra generated from different time-of-flight mass spectrometry (ToF-MS) techniques, offering the ToF-MS community an open-source, intelligent mass spectra analysis.

Scolopostethus affinis (Schilling) (Hemiptera, Heteroptera, Rhyparochromidae, Drymini): a new alien established in North America.

Scolopostethus affinis, a species native to the Palearctic region, is reported from two localities in Montreal, Quebec. The species appears established and breeding in Quebec and is a new alien species in North America. A description of S. affinis is given, with illustrations, and details of the life cycle and diagnostic characters.

Dopant Distribution in Atomic Layer Deposited ZnO:Al Films Visualized by Transmission Electron Microscopy and Atom Probe Tomography.

The maximum conductivity achievable in Al-doped ZnO thin films prepared by atomic layer deposition (ALD) is limited by the low doping efficiency of Al. To better understand the limiting factors for the doping efficiency, the three-dimensional distribution of Al atoms in the ZnO host material matrix has been examined on the atomic scale using a combination of high-resolution transmission electron microscopy (TEM) and atom probe tomography (APT). Although the Al distribution in ZnO films prepared by so-called "ALD supercycles" is often presented as atomically flat δ-doped layers, in reality a broadening of the Al-dopant layers is observed with a full-width-half-maximum of ∼2 nm. In addition, an enrichment of the Al at grain boundaries is observed. The low doping efficiency for local Al densities > ∼1 nm-3 can be ascribed to the Al solubility limit in ZnO and to the suppression of the ionization of Al dopants from adjacent Al donors.

Twelve new species and fifty-three new provincial distribution records of Aleocharinae rove beetles of Saskatchewan, Canada (Coleoptera, Staphylinidae).

One hundred twenty species of aleocharine beetles (Staphylinidae) are recognized in the province of Saskatchewan. Sixty-five new provincial records, including twelve new species and one new North American record, are presented. Oligota inflata (Mannerheim), a Palearctic species, is newly recorded for North America. The following twelve species are described as new to science: Acrotona pseudopygmaea Klimaszewski & Larson, sp. n., Agaricomorpha pulchra Klimaszewski & Larson, sp. n. (new genus record for Canadian fauna), Aleochara elisabethae Klimaszewski & Larson, sp. n., Atheta (Dimetrota) larsonae Klimaszewski & Larson, sp. n., Atheta (Microdota) pseudopittionii Klimaszewski & Larson, sp. n., Atheta (Microdota) spermathecorum Klimaszewski & Larson, sp. n., Atheta (sensu lato) richardsoni Klimaszewski & Larson, sp. n., Brachyusa saskatchewanae Klimaszewski & Larson, sp. n., Dochmonota langori Klimaszewski & Larson, sp. n., Dochmonota simulans Klimaszewski & Larson, sp. n., Dochmonota websteri Klimaszewski & Larson, sp. n., and Oxypoda domestica Klimaszewski & Larson, sp. n. Colour images of habitus and black and white images of the median lobe of the aedeagus, spermatheca, and tergite and sternite VIII are presented for all new species, Oligota inflata Mannerheim and Dochmonota rudiventris (Eppelsheim). A new synonymy is established: Tetralina filitarsus Casey, syn. n. = Tetralina helenae Casey, now placed in the genus Brachyusa Mulsant & Rey.

A case report of sporadic ovine listerial menigoencephalitis in Iowa with an overview of livestock and human cases.

A case of ovine listeriosis was examined in a flock of sheep. The index case was a male lamb, which was part of a flock of 85 sheep located in central Iowa. Because the sheep were raised on a premise where soybean sprouts were also cultivated for the organic foods market, the potential of a public health concern was addressed. To identify the source of contaminations, clinical and environmental samples were cultured for Listeria monocytogenes. Isolates were serotyped and analyzed using pulsed-field gel electrophoresis (PFGE). Listeria monocytogenes (serotype 1) was recovered from the brain of a male lamb with clinical signs of listerial encephalitis. Isolates of serotypes 1 and 4 were also cultured from feces of clinically healthy lambs, compost piles, and soybean cleanings. By PFGE, the clinical isolate was distinctly different from the other isolates. Environmental isolates were identified as L. monocytogenes serotypes 1 and 4. However, by PFGE, none matched the profile of the single clinical isolate. Thus, the ultimate source of contamination is unknown.

Electrostatic simulations of a local electrode atom probe: the dependence of tomographic reconstruction parameters on specimen and microscope geometry.

We electrostatically model a local electrode atom probe microscope using the commercial software IES LORENTZ 2D v9.0 to investigate factors affecting the reconstruction parameters. We find strong dependences on the specimen geometry and voltage, and moderate dependences on the tip-aperture separation, which confirm that the current approach to atom probe reconstruction overlooks too many factors. Based on our data, which are in excellent agreement with known trends and experimental results, we derive a set of empirical relations which predict the values of the reconstruction parameters. These may be used to advance current reconstruction protocols by enabling the parameters to be adjusted as the specimen geometry changes.

Review of atom probe FIB-based specimen preparation methods.

Several FIB-based methods that have been developed to fabricate needle-shaped atom probe specimens from a variety of specimen geometries, and site-specific regions are reviewed. These methods have enabled electronic device structures to be characterized. The atom probe may be used to quantify the level and range of gallium implantation and has demonstrated that the use of low accelerating voltages during the final stages of milling can dramatically reduce the extent of gallium implantation.

Spatial distribution maps for atom probe tomography.

A real-space technique for finding structural information in atom probe tomographs, spatial distribution maps (SDM), is described. The mechanics of the technique are explained, and it is then applied to some test cases. Many applications of SDM in atom probe tomography are illustrated with examples including finding crystal lattices, correcting lattice strains in reconstructed images, quantifying trajectory aberrations, quantifying spatial resolution, quantifying chemical ordering, dark-field imaging, determining orientation relationships, extracting radial distribution functions, and measuring ion detection efficiency.

Imaging of arsenic Cottrell atmospheres around silicon defects by three-dimensional atom probe tomography.

Discrete control of individual dopant or impurity atoms is critical to the electrical characteristics and fabrication of silicon nanodevices. The unavoidable introduction of defects into silicon during the implantation process may prevent the uniform distribution of dopant atoms. Cottrell atmospheres are one such nonuniformity and occur when interstitial atoms interact with dislocations, pinning the dislocation and trapping the interstitial. Atom probe tomography has been used to quantify the location and elemental identity of the atoms proximate to defects in silicon. We found that Cottrell atmospheres of arsenic atoms form around defects after ion implantation and annealing. Furthermore, these atmospheres persist in surrounding dislocation loops even after considerable thermal treatment. If not properly accommodated, these atmospheres create dopant fluctuations that ultimately limit the scalability of silicon devices.