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Microscopy and Microanalysis

Nicolas Rolland, François Vurpillot, Sébastien Duguay, Baishakhi Mazumder, James S Speck, Didier Blavette
Accuracy of atom probe tomography measurements is strongly degraded by the presence of phases that have different evaporation fields. In particular, when there are perpendicular interfaces to the tip axis in the specimen, layers thicknesses are systematically biased and the resolution is degraded near the interfaces. Based on an analytical model of field evaporated emitter end-form, a new algorithm dedicated to the 3D reconstruction of multilayered samples was developed. Simulations of field evaporation of bilayer were performed to evaluate the effectiveness of the new algorithm...
March 22, 2017: Microscopy and Microanalysis
Brian Langelier, Hugo P Van Landeghem, Gianluigi A Botton, Hatem S Zurob
Improved understanding of the interactions between solutes and the austenite/ferrite interface can benefit modeling of ferrite growth during austenite decomposition, as the transformation kinetic is significantly affected by solutes that influence interface mobility. Solute-interface interactions dominate solute segregation at the interface in binary systems, but in multi-component alloys, solute-solute interactions may also affect segregation. In this study, interface segregation in Fe-Mn-N is examined and compared with Fe-Mn-C, to reveal the extent to which C affects the segregation of Mn...
March 21, 2017: Microscopy and Microanalysis
Qin Shen, Hao Chen, Wenqing Liu
The microstructural evolution of precipitation in two model alloys, Fe-NiAl and Fe-NiAl-Cu, was investigated during aging at 500°C for different times using atom probe tomography (APT). The APT results reveal that the addition of Cu effectively increases the number density of NiAl precipitates. This is attributed to Cu promoting the nucleation of NiAl particles by increasing the chemical driving force and decreasing the interfacial energy. The NiAl precipitates of the Fe-NiAl-Cu alloy grow and coarsen at a slower rate than that of the Fe-NiAl alloy, mainly due to the slower diffusion rate of the Cu atoms...
March 21, 2017: Microscopy and Microanalysis
Kristina Lindgren, Krystyna Stiller, Pål Efsing, Mattias Thuvander
Radiation induced clustering affects the mechanical properties, that is the ductile to brittle transition temperature (DBTT), of reactor pressure vessel (RPV) steel of nuclear power plants. The combination of low Cu and high Ni used in some RPV welds is known to further enhance the DBTT shift during long time operation. In this study, RPV weld samples containing 0.04 at% Cu and 1.6 at% Ni were irradiated to 2.0 and 6.4×1023 n/m2 in the Halden test reactor. Atom probe tomography (APT) was applied to study clustering of Ni, Mn, Si, and Cu...
March 21, 2017: Microscopy and Microanalysis
Samuel D Keyes, Neil J Gostling, Jessica H Cheung, Tiina Roose, Ian Sinclair, Alan Marchant
The use of in vivo X-ray microcomputed tomography (μCT) to study plant root systems has become routine, but is often hampered by poor contrast between roots, soil, soil water, and soil organic matter. In clinical radiology, imaging of poorly contrasting regions is frequently aided by the use of radio-opaque contrast media. In this study, we present evidence for the utility of iodinated contrast media (ICM) in the study of plant root systems using μCT. Different dilutions of an ionic and nonionic ICM (Gastrografin 370 and Niopam 300) were perfused into the aerial vasculature of juvenile pea plants via a leaf flap (Pisum sativum)...
March 21, 2017: Microscopy and Microanalysis
Michal Dagan, Baptiste Gault, George D W Smith, Paul A J Bagot, Michael P Moody
An automated procedure has been developed for the reconstruction of field ion microscopy (FIM) data that maintains its atomistic nature. FIM characterizes individual atoms on the specimen's surface, evolving subject to field evaporation, in a series of two-dimensional (2D) images. Its unique spatial resolution enables direct imaging of crystal defects as small as single vacancies. To fully exploit FIM's potential, automated analysis tools are required. The reconstruction algorithm developed here relies on minimal assumptions and is sensitive to atomic coordinates of all imaged atoms...
March 20, 2017: Microscopy and Microanalysis
Masoud Rashidi, Hans-Olof Andrén, Fang Liu
In creep resistant Z-phase strengthened 12% Cr steels, MX (M=Nb, Ta, or V, and X=C and/or N) to Z-phase (CrMN, M=Ta, Nb, or V) transformation plays an important role in achieving a fine distribution of Z-phase precipitates for creep strengthening. Atom probe tomography was employed to investigate the phase transformation in a Nb-based Z-phase strengthened trial steel. Using iso-concentration surfaces with different concentration values, and subtracting the matrix contribution enabled us to reveal the core-shell structure of the transient precipitates between MX and Z-phase...
March 20, 2017: Microscopy and Microanalysis
Torben Boll, Kinga A Unocic, Bruce A Pint, Krystyna Stiller
This study applies atom probe tomography (APT) to analyze the oxide scales formed on model NiAlCr alloys doped with Hf, Y, Ti, and B. Due to its ability to measure small amounts of alloying elements in the oxide matrix and its ability to quantify segregation, the technique offers a possibility for detailed studies of the dopant's fate during high-temperature oxidation. Three model NiAlCr alloys with different additions of Hf, Y, Ti, and B were prepared and oxidized in O2 at 1,100°C for 100 h. All specimens showed an outer region consisting of different spinel oxides with relatively small grains and the protective Al2O3-oxide layer below...
March 20, 2017: Microscopy and Microanalysis
Kezhi Ren, Xiaohua Tan, Heyun Li, Hui Xu, Ke Han
We study the effects of Dy, Nb, and Ga additions on the microstructure and magnetic properties of Nd2Fe14B/α-Fe nanocomposites. Dy, Nb, and Ga additions inhibit the growth of the soft magnetic α-Fe phase. Dy and Nb additions are able to refine the microstructure, whereas Ga addition plays only a minor role in prohibiting crystal growth. The magnetic properties are sensitive to Dy, Nb, and Ga additions. The Dy-containing alloy enhances the intrinsic coercivity of 872 kA/m because Dy partially replaces Nd, forming (Nd, Dy)2Fe14B...
March 20, 2017: Microscopy and Microanalysis
Andrey Denisyuk, Tomáš Hrnčíř, Jozef Vincenc Oboňa, Sharang, Martin Petrenec, Jan Michalička
We report on the mitigation of curtaining artifacts during transmission electron microscopy (TEM) lamella preparation by means of a modified ion beam milling approach, which involves altering the incident angle of the Ga ions by rocking of the sample on a special stage. We applied this technique to TEM sample preparation of a state-of-the-art integrated circuit based on a 14-nm technology node. Site-specific lamellae with a thickness <15 nm were prepared by top-down Ga focused ion beam polishing through upper metal contacts...
March 20, 2017: Microscopy and Microanalysis
Zemin Wang, Xulei Fang, Hui Li, Wenqing Liu
The formation of copper-rich precipitates of 17-4 precipitate hardened stainless steel has been investigated, after tempering at 350-570°C for 4 h, by atom probe tomography (APT). The results reveal that the clusters, enriched only with Cu, were observed after tempering at 420°C. Segregation of Ni, Mn to the Cu-rich clusters took place at 450°C, contributing to the increased hardening. After tempering at 510°C, Ni and Mn were rejected from Cu-rich precipitates and accumulated at the precipitate/matrix interfaces...
March 16, 2017: Microscopy and Microanalysis
Andrew J London, Daniel Haley, Michael P Moody
Due to the intrinsic evaporation properties of the material studied, insufficient mass-resolving power and lack of knowledge of the kinetic energy of incident ions, peaks in the atom probe mass-to-charge spectrum can overlap and result in incorrect composition measurements. Contributions to these peak overlaps can be deconvoluted globally, by simply examining adjacent peaks combined with knowledge of natural isotopic abundances. However, this strategy does not account for the fact that the relative contributions to this convoluted signal can often vary significantly in different regions of the analysis volume; e...
March 16, 2017: Microscopy and Microanalysis
Lizhe Qin, Lanying Lin, Feng Fu, Mizi Fan
Emulsion polymer isocyanate (EPI) and urea-formaldehyde (UF) were selected as typical resin systems to investigate the microstructure of wood-adhesive interphases by fluorescence microscopy (FM) and confocal laser scanning microscopy (CLSM). Further, a quantitative micromechanical analysis of the interphases was conducted using nanoindentation. The FM results showed that the UF resin could penetrate the wood to a greater extent than the EPI resin, and that the average penetration depth for these two resin systems was higher in the case of latewood...
March 15, 2017: Microscopy and Microanalysis
Andrew J Breen, Katharina Babinsky, Alec C Day, K Eder, Connor J Oakman, Patrick W Trimby, Sophie Primig, Julie M Cairney, Simon P Ringer
Correlative microscopy approaches offer synergistic solutions to many research problems. One such combination, that has been studied in limited detail, is the use of atom probe tomography (APT) and transmission Kikuchi diffraction (TKD) on the same tip specimen. By combining these two powerful microscopy techniques, the microstructure of important engineering alloys can be studied in greater detail. For the first time, the accuracy of crystallographic measurements made using APT will be independently verified using TKD...
March 14, 2017: Microscopy and Microanalysis
Nicholas W M Ritchie
Secondary fluorescence, the final term in the familiar matrix correction triumvirate Z·A·F, is the most challenging for Monte Carlo models to simulate. In fact, only two implementations of Monte Carlo models commonly used to simulate electron probe X-ray spectra can calculate secondary fluorescence-PENEPMA and NIST DTSA-II a (DTSA-II is discussed herein). These two models share many physical models but there are some important differences in the way each implements X-ray emission including secondary fluorescence...
March 13, 2017: Microscopy and Microanalysis
Michael Mengason, Nicholas Ritchie
The evolution of the energy dispersive spectrometer (EDS) from the lithium-drifted silicon detector [Si(Li)] to the silicon drift detector (SDD) has created new opportunities in the field of electron probe X-ray microanalysis. The SDD permits operation at significantly higher count rates than the Si(Li) and also provides a more stable energy scale. X-ray spectra captured by EDS can now be analyzed qualitatively or quantitatively under the same beam conditions as used for wavelength dispersive spectrometry (WDS)...
March 10, 2017: Microscopy and Microanalysis
Cai Wen
The atomic reconstruction of a misfit dislocation (MD) core causes change in the strain distribution around the core. Several MD cores at the AlSb/GaAs (001) cubic zincblende interface, including a symmetrical glide set Lomer dislocation (LD), a left-displaced glide set LD, a glide set LD with an atomic step, a symmetrical shuffle set LD, and a 60° dislocation pair, were studied using simulated projected potential and aberration-corrected transmission electron microscope images. Image deconvolution was also used to restore structure images from nonoptimum-defocus images...
March 9, 2017: Microscopy and Microanalysis
Landon T Hansen, Brian E Jackson, David T Fullwood, Stuart I Wright, Marc De Graef, Eric R Homer, Robert H Wagoner
Studies of dislocation density evolution are fundamental to improved understanding in various areas of deformation mechanics. Recent advances in cross-correlation techniques, applied to electron backscatter diffraction (EBSD) data have particularly shed light on geometrically necessary dislocation (GND) behavior. However, the framework is relatively computationally expensive-patterns are typically saved from the EBSD scan and analyzed offline. A better understanding of the impact of EBSD pattern degradation, such as binning, compression, and various forms of noise, is vital to enable optimization of rapid and low-cost GND analysis...
March 6, 2017: Microscopy and Microanalysis
Andreas Stoffers, Juri Barthel, Christian H Liebscher, Baptiste Gault, Oana Cojocaru-Mirédin, Christina Scheu, Dierk Raabe
In the course of a thorough investigation of the performance-structure-chemistry interdependency at silicon grain boundaries, we successfully developed a method to systematically correlate aberration-corrected scanning transmission electron microscopy and atom probe tomography. The correlative approach is conducted on individual APT and TEM specimens, with the option to perform both investigations on the same specimen in the future. In the present case of a Σ9 grain boundary, joint mapping of the atomistic details of the grain boundary topology, in conjunction with chemical decoration, enables a deeper understanding of the segregation of impurities observed at such grain boundaries...
February 20, 2017: Microscopy and Microanalysis
Chang-Min Kwak, Young-Tae Kim, Chan-Gyung Park, Jae-Bok Seol
Two challenges exist in laser-assisted atom probe tomography (APT). First, a drastic decline in mass-resolving power is caused, not only by laser-induced thermal effects on the APT tips of bulk oxide materials, but also the associated asymmetric evaporation behavior; second, the field evaporation mechanisms of bulk oxide tips under laser illumination are still unclear due to the complex relations between laser pulse and oxide materials. In this study, both phenomena were investigated by depositing Ni- and Co-capping layers onto the bulk LaAlO3 tips, and using stepwise APT analysis with transmission electron microscopy (TEM) observation of the tip shapes...
February 20, 2017: Microscopy and Microanalysis
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