The capability of Transmission Kikuchi Diffraction technique for characterizing nano-grained oxide scales formed on a FeCrAl stainless steel

This letter focuses on the capability of Transmission Kikuchi Diffraction (TKD) in Scanning Electron Microscope (SEM) for obtaining microstructural and micro-textural information from nano-grained oxide scales formed on a FeCrAl alloy. Orientation maps, with an indexing rate of 85%, showed the formation of grains in the range 20-300 nm. TKD revealed the existence of an orientation relationship at the alloy/oxide interface as well as the presence of a single grain (40 nm) with spinel structure in the alumina scale. A pre-tilted sample holder was designed for 110 investigations at short working distances with minimized mechanical drift of the thin foils. (C) 2015 The Authors. Published by Elsevier B.V

Should the oxygen source be considered in the initiation of KCl-induced high-temperature corrosion?

The role of two oxygen sources, oxygen and water vapor, in the initiation of KCl-induced high-temperature corrosion was addressed by studying two high-alloyed commercial materials at 550 \ub0C. The differentiation between the two oxygen sources was implemented with 18O-enriched water and 16O2. Based on the results, the solid-solid reaction between KCl(s) and the protective oxide on the alloy surface appeared to be more responsible for corrosion than the gas-solid reaction between KCl(g) and the protective oxide. Water was more involved in the abovementioned reactions than O2: 18O was the main oxygen isotope found in the formed surface oxides and intermediates

Calculated and experimental Schmid factors for chip flow deformation of textured CVD α-alumina coatings

A thorough analysis of Schmid factors (m) for three different (basal and two prismatic) slip systems and three different coating textures, (0001), (011\uaf2) and (112\uaf0), was done in order to understand the influence of CVD α-alumina coating textures on the ability of the coatings to deform plastically at different locations on the rake face of a cutting tool insert during a metal machining operation. Schmid factor diagrams were constructed using MATLAB/MTEX in order to visualize the angular dependence of an external force relative to the α-Al O crystals (grains) on the Schmid factor. The diagrams were also used to extract m-value frequency distributions for different slip systems and textures. In addition, lateral m-value distribution maps were obtained from experimental textured coatings using electron backscatter diffraction. These maps show the ability for neighboring grains to deform plastically in the coatings. Cutting tool inserts with differently textured α-Al2O3 coatings were subjected to dry machining of a quench-tempered steel. Using scanning electron microscopy, the microstructure and surface topography of the worn alumina layers were investigated and it was found that a flatter surface morphology and higher probability of discrete plastic deformation are connected to less wear. This was observed in the (0001)-textured sample, which also exhibited the highest m-values in the wear zone with highest temperatures and external forces. It was observed that basal slip is most easily activated, followed by prismatic slip systems 1 and 2 in this case. For (011\uaf2) and (112\uaf0) textured coatings the differences in m-values for the three slip systems are not that big, and the distributions are relatively wide. It is clear that the Schmid factor analysis forms a basis that is important for understanding crater wear, especially when it is connected to local plastic deformation, of textured CVD α-Al2O3 coatings. The methodology of this work can be expanded to other coating systems and also more generally to applications where it is of interest to analyze the deformation behavior and local plastic anisotropy of textured materials

Deformation and texture evolution of OFHC copper during dynamic tensile extrusion

During dynamic tensile extrusion (DTE) the material is subjected to a complex deformation history, including high strain rates, large strains and elevated temperatures. This technique provides unique means to explore material performance under extreme conditions. In this work, the microstructural evolution of 99.98% commercially pure copper during the DTE test was investigated by means of electron backscatter diffraction (EBSD). The investigation was focused on the segment of the extruded jet that remained in the die, since numerical simulation showed that material points along the longitudinal axis of such segment correspond to different stages of a common temperature compensated deformation history. Therefore, post mortem microstructure information extracted at different locations along the center line is equivalent to in situ real-time measurement during the deformation process. EBSD investigations along the center line showed a progressive elongation of the grains, and an accompanying development of a strong 〈0 0 1〉 + 〈1 1 1〉 dual fiber texture. Meta-dynamic discontinuous dynamic recrystallization (DRX) occurred at larger strains, and it was demonstrated that nucleation occurred during straining, while subsequent grain growth took place during post-deformation cooling in the die. According to strain energy minimization arguments, the recrystallization resulted in an increased 〈0 0 1〉 texture component. The critical strain for recrystallization was well predicted from a power-law dependence on the Zener–Hollomon parameter, including grain size dependence and a temperature dependent activation energy. In addition, it was shown that 〈0 0 1〉 and 〈1 1 1〉oriented grains develop different dislocation substructures during straining, exhibiting elongated cells/micro-bands and typical cell structures, respectively. The present results also confirm that dynamic tensile ductility increases with decreasing initial grain size as a result of grain refinement and lowering of dislocation and twin densities during DRX

Transformation of amorphous calcium phosphate to bone-like apatite

Mineralisation of calcium phosphates in bone has been proposed to proceed via an initial amorphous precursor phase which transforms into nanocrystalline, carbonated hydroxyapatite. While calcium phosphates have been under intense investigation, the exact steps during the crystallisation of spherical amorphous particles to platelet-like bone apatite are unclear. Herein, we demonstrate a detailed transformation mechanism of amorphous calcium phosphate spherical particles to apatite platelet-like crystals, within the confined nanodomains of a bone-inspired nanocomposite. The transformation is initiated under the presence of humidity, where nanocrystalline areas are formed and crystallisation advances via migration of nanometre sized clusters by forming steps at the growth front. We propose that such transformation is a possible crystallisation mechanism and is characteristic of calcium phosphates from a thermodynamic perspective and might be unrelated to the environment. Our observations provide insight into a crucial but unclear stage in bone mineralisation, the origins of the nanostructured, platelet-like bone apatite crystals

Atom probe tomography investigation of 3D nanoscale compositional variations in CVD TiAlN nanolamella coatings

The cubic (Ti1−xAlx)Ny (TiAlN) phase with a nanolamella structure, synthesized via low pressure chemical vapour deposition (LPCVD), has been widely used in wear-resistant coatings during the latest years. The nanolamella structured TiAlN coatings contain periodic and epitaxially grown Ti-rich [denoted as Ti(Al)N] and Al-rich [denoted as Al(Ti)N] lamellae. However, the chemical compositions of these nano-structures have not been fully revealed. In this study, the microstructure of the nanolamella TiAlN coating was studied using scanning and transmission electron microscopy (SEM and TEM), and the chemical content was investigated using atom probe tomography (APT) that provides three-dimensional composition data with good accuracy and a spatial resolution down to the nanometer scale. It was found that over- and under-stoichiometries of N exist for the Ti(Al)N and the Al(Ti)N lamellae, respectively. According to the previous simulation results, such over- and under-stoichiometries are due to metal (Al and Ti) and N vacancies, respectively. The Al(Ti)N lamellae have a chemical formula of (Ti0.12Al0.88)N0.90, and have 10% N vacancies. The Ti(Al)N lamellae have a chemical formula of (Ti0.70Al0.30)0.97N, and have 3% metal (Al and Ti) vacancies. In addition to the nanolamella structure, compositional variations on a scale of a few nm were found in both types of lamellae. In the Ti-richest volumes, the composition corresponds to (Ti0.72Al0.28)0.88N so a maximum of 12% of metal vacancies exists. In the Al-richest volumes, the composition corresponds to (Ti0.07Al0.93)N0.64 so a maximum of 36% N vacancies exists. In addition, a small amount of Cl (around 0.1\ua0at.%) was found in the coating, which could originate from the incomplete dissociation of chloride precursors during the CVD surface reaction

On the capability of in-situ exposure in an environmental scanning electron microscope for investigating the atmospheric corrosion of magnesium

The feasibility of environmental scanning electron microscope (BEM) in studying the atmospheric corrosion behavior of 99.97% Mg was investigated. For reference, ex-situ exposure was performed. A model system was designed by spraying few salt particles on the metal surface and further promoting the corrosion process using platinum (Pt) deposition in the form of 1 x 1 x 1 pm(3) dots around the salt particles to create strong artificial cathodic sites. The results showed that the electron beam play a significant role in the corrosion process of scanned regions. This was attributed to the irradiation damage occurring on the metal surface during the BEM in-situ experiment. After achieving to a reliable process route, in a successful attempt, the morphology and composition of the corrosion products formed in-situ in the ESEM were in agreement with those of the sample exposed ex-situ

Schmid factor analysis for chip flow induced plastic deformation of textured cubic carbonitride coatings

In high-speed metal machining, cutting tools in the form of cemented carbide inserts coated with thin wear-resistant coatings are commonly used. These coatings are often made of metal carbonitrides with cubic rock salt crystal structure and different growth textures. However, the influence of the crystallographic texture of the coatings on their wear by plastic deformation due to the chip flow during machining needs to be revealed further. In this work, in order to analyse the ability of polycrystalline fibre-textured coatings with a rock salt structure to undergo plastic deformation, a method was developed for calculating Schmid factors of such textured coatings as a function of the loading angle of an external force. The Schmid factors were calculated for coatings with 100 and 211 growth textures, and {100} <110>, {110}<110> and {111}<110> as possible slip systems. For the {111}<110> slip systems, the Schmid factors are not much influenced by the force angle and coating texture, which is contrary to the {100}<110> and {110}<110> slip systems. The simulations were compared to wear on the rake face of two textured Ti(C,N) coatings after short longitudinal turning tests. The variation of the degree of plastic deformation of Ti(C,N) coatings with growth texture and external force angle indicates that the dominant activated slip systems are {110}<110> using the machining conditions applied in this work

A new semi-solid casting technique for fabricating SiC-reinforced Mg alloys matrix composites

The capability of the newly developed rheocasting (RC) technique in combination with the RheoMetal process for producing SiC particulate-reinforced AM50 and AZ91D matrix composites (Mg-based MMCs) was investigated. The quality of the MMCs was studied by analyzing the fraction of casting pores, number density of SiC clusters and the uniformity of SiC particles. Solid fraction, particle size and oxidation of SiC particles had strong impacts on the overall quality of the MMCs. The MMCs produced by 40% solid fraction and oxidized micron-sized SiC particles exhibited an excellent casting quality. A low-quality MMC was obtained when non-oxidized sub-micron sized SiC particles were employed. The results showed the formation of various types intermetallic particles and carbides such as MgO, Mg2Si, Al2MgC2, Mg2C3, Al4C3 as the interfacial reaction products of SiC/Mg alloy's melts. Mg hydride (alpha-MgH2) was also identified in inter-dendritic regions of the MMCs for the first time

The effect of additive manufacturing on the initial High temperature oxidation properties of RE-containing FeCrAl alloys

The effect of additive manufacturing on the high temperature oxidation properties of FeCrAl materials was investigated. For this purpose, additively manufactured Kanthal AM100 cut parallel and perpendicular to the building direction and hot-rolled Kanthal AF as a reference were exposed to air at 900 and 1100 \ub0C for 168 h. AM100 performed slightly better than AF in terms of mass gain. Nevertheless, an oxide scale with local differences in thickness formed on AM100 due to the bimodal grain structure of the underlying metal, which was composed of coarse-grained cuboidal repeating units (100 μm wide), separated by fine-grained rims