X-ray diffraction (XRD) characterization of Si powder was carried out using synchrotron and laboratory sources. Microstructural (size-strain) analyses of XRD patterns were carried out using the Rietveld refinement method. Experimentally observed super-Lorentzian shapes of the XRD peaks of Si powder were examined using multimodal profile fitting and bimodal model was found to be adequate. The two components obtained using a bimodal approach are referred as narrow and broad profiles based on their estimated relative peak widths. Peak shapes of crystallite size-dependent parts of narrow and broad profiles were found to be almost Gaussian and Lorentzian in nature, respectively. The simultaneous presence of such peak shapes corresponding to a bimodal microstructure is uncommon in literature. Therefore, in order to explore the role of different natures of XRD peak shapes (size dependent) of the bimodal profiles of Si, detailed microstructural analysis was carried out using the complementary method of whole powder pattern modeling (WPPM) and found to be related to the variance of crystallites' size distribution. Additionally, the effect of instrument resolution (laboratory and synchrotron sources) on the microstructural parameters was also studied. Scanning and transmission electron microscopy were used to characterize the morphology of Si powder and correlate with the microstructural findings of XRD methods.

The aim of this study is to evaluate the potential use of titanium foil coated with sputtered silver and copper films as a novel brazing filler for joining TiAl alloys. For this purpose, a detailed microstructural characterization of the resulting brazing interfaces was carried out. The development of brazing fillers that allow the joining of TiAl alloys without compromising the service temperature is a fruitful prospect. Brazing experiments were performed in a vacuum at 900, 950, and 980°C, with a dwell time of 30 min. Microstructural characterization reveals that brazing joints can be obtained successfully at 950 and 980°C. The interface consists of a large central region of α-Ti with an amount of Al and Ti–Ag compound and thin layers, mainly composed of intermetallic compounds, formed close to the base material. A novel brazing filler consisting of Ti foil coated with sputtered Ag and Cu films inhibits the extensive formation of soft (Ag) zones or coarse brittle Ti–Al–(Cu,Ni) particles. Hence, the need for post-brazing heat treatments for the joining of TiAl alloys was avoided.

The thermomechanical processing of NiTi shape memory alloys usually involves several steps of hot and/or cold deformation. The present work presents the structural characterization of a Ni-rich NiTi alloy bar, produced by vacuum-induced melting and thermomechanical processing in laboratory scale, aiming at massive production in the future. This study focused on the first step of hot working at 800 °C during rotary forging. Microstructural characterization was performed using differential scanning calorimetry, high- and low-temperature X-ray diffraction (XRD) using a laboratory source and synchrotron XRD. Thus, it was possible to obtain the phase transformation characteristics of the material: the transformation temperatures and the transformation sequence. Proposed thermomechanical processing is intended for production of bars and wires that will be subsequently drawn to get thin wires, for different applications, including orthodontic arch wires.

This research focuses on characterization of the impact of dispersion methods on aluminum-carbon nanotubes (Al-CNTs) nanocomposite structure. Nanocomposites were produced by a conventional powder metallurgy process after the dispersion of the CNTs on the Al powders, using two approaches: (1) the dispersion of CNTs and mixture with Al powders were performed in a single step by ultrasonication; and (2) the CNTs were previously untangled by ultrasonication and then mixed with Al powders by ball milling. Microstructural characterization of Al-CNT nanocomposites was performed by optical microscopy, scanning and transmission electron microscopy, electron backscatter diffraction, and high-resolution transmission electron microscopy (HRTEM). Microstructural characterization revealed that the use of ball milling for mixing CNTs with Al powders promoted the formation of CNT clusters of reduced size, more uniformly dispersed in the matrix, and a nanocomposite of smaller grain size. However, the results of HRTEM and Raman spectroscopy show that ball milling causes higher damage to the CNT structure. The strengthening effect of the CNT is attested by the increase in hardness and tensile strength of the nanocomposites.

Archaeological materials present unique records on natural processes allowing the study of long-term material behaviors such as structural modifications and degradation mechanisms. The present work is focused on the chemical and microstructural characterization of four prehistoric arsenical copper artifacts. These artifacts were characterized by micro-energy dispersive X-ray fluorescence spectrometry, optical microscopy, scanning electron microscopy with X-ray microanalysis, micro-X-ray diffraction and synchrotron radiation micro-X-ray diffraction. Cu3As is the expected intermetallic arsenide in arsenical copper alloys, reported in the literature as exhibiting a hexagonal crystallographic structure. However, a cubic Cu3As phase was identified by X-ray diffraction in all of our analyzed archaeological artifacts, while the hexagonal Cu3As phase was clearly identified only in the artifact with higher arsenic content. Occurrence of the cubic arsenide in these particular objects, suggests that it was precipitated due to long-term aging at room temperature, which points to the need of a redefinition of the Cu-As equilibrium phase constitution. These results highlight the importance of understanding the impact of structural aging for the assessment of original properties of archaeological arsenical copper artifacts, such as hardness or color.

Electron-excited X-ray mapping is a key operational mode of the scanning electron microscope (SEM) equipped with energy dispersive X-ray spectrometry (EDS). The popularity of X-ray mapping persists despite the significant time penalty due to the relatively low output count rates, typically less than 25 kHz, that can be processed with the conventional EDS. The silicon drift detector (SDD) uses the same measurement physics, but modifications to the detector structure permit operation at a factor of 5–10 times higher than conventional EDS for the same resolution. Output count rates as high as 500 kHz can be achieved with 217 eV energy resolution (at MnKα). Such extraordinarily high count rates make possible X-ray mapping through the method of X-ray spectrum imaging, in which a complete spectrum is captured at each pixel of the scan. Useful compositional data can be captured in less than 200 s with a pixel density of 160 × 120. Applications to alloy and rock microstructures, ultrapure materials with rare inclusions, and aggregate particles with complex chemistry illustrate new approaches to characterization made practical by high-speed X-ray mapping with the SDD.Note: The Siegbahn notation for characteristic X-rays is commonly used in the field of electron beam X-ray spectrometry and will be used in this article. The equivalent IUPAC notation is indicated in parentheses at the first use.In this article, the following arbitrary definitions will be used when referring to concentration (C) ranges: major: C > 0.1 (10 wt%), minor: 0.01 ≤ C ≤ 0.1 (1–10 wt%), and trace: C < 0.01 (1 wt%).

Mechanical properties, such as hardness and impact toughness, of ferrite-containing stainless steels are greatly affected by long-term aging at intermediate temperatures. It is known that the α-α′ spinodal decomposition occurring in the iron–chromium-based ferrite is responsible for this aging susceptibility. This decomposition can be characterized unambiguously by atom probe analysis, allowing comparison both with the existing theories of spinodal decomposition and the evolution of some mechanical properties. It is then possible to predict the evolution of hardness of industrial components during service, based on the detailed knowledge of the involved aging process.

Atom probe tomography is a technique for the nanoscale characterization of microstructural features. Analytical techniques have been developed to estimate the size, composition, and other parameters of features as small as 1 nm from the atom probe tomography data. These methods are outlined and illustrated with examples of yttrium-, titanium-, and oxygen-enriched particles in a mechanically alloyed, oxide-dispersion-strengthened steel.