Annealing Behavior of a Mg-Y-Zn-Al Alloy Processed by Rapidly Solidified Ribbon Consolidation.

Mg-Y-Zn-Al alloys processed by the rapidly solidified ribbon consolidation (RSRC) technique are candidate materials for structural applications due to their improved mechanical performance. Their outstanding mechanical strength is attributed to solute-enriched stacking faults (SESFs), which can form cluster-arranged layers (CALs) and cluster-arranged nanoplates (CANaPs) or complete the long-period stacking ordered (LPSO) phase. The thermal stability of these solute arrangements strongly influences mechanical performance at elevated temperatures. In this study, an RSRC-processed Mg-0.9%, Zn-2.05%, Y-0.15% Al (at%) alloy was heated at a rate of 0.666 K/s up to 833 K, a temperature very close to melting point. During annealing, in situ X-ray diffraction (XRD) measurements were performed using synchrotron radiation in order to monitor changes in the structure. These in situ XRD experiments were completed with ex situ electron microscopy investigations before and after annealing. At 753 K and above, the ratio of the matrix lattice constants, c/a, decreased considerably, which was restored during cooling. This decrease in c/a could be attributed to partial melting in the volumes with high solute contents, causing a change in the chemical composition of the remaining solid material. In addition, the XRD intensity of the secondary phase increased at the beginning of cooling and then remained unchanged, which was attributed to a long-range ordering of the solute-enriched phase. Both the matrix grains and the solute-enriched particles were coarsened during the heat treatment, as revealed by electron microscopy.

Failure mechanisms data analysis during tension of additively manufactured Ti-6Al-4V alloy reinforced with nano-zirconia particles: Investigations of the crack path.

The data presented here aim to show how to analyze crack propagation of a novel metallic matrix composite of Ti-6Al-4V reinforced with 1 wt.% nano-yttria-stabilized zirconia processed by laser powder bed fusion technology. The data was acquired via microstructural observations and electron backscatter diffraction (EBSD) analyses after the quasistatic tensile tests at room temperature. The overall crack path configuration based on the fracture surface observation by scanning electron microscopy (SEM) was first operated, presenting two main regions: (i) local inclined planes (hereafter denoted as "stair-like"), and (ii) region in accordance with the theoretical mode I fracture plane. Thereafter, a series of EBSD data set on a surface obtained after longitudinal cut off operation on one failed piece was conducted at three distinct positions: (i) in the stair-like configuration region, (ii) in the mode I fracture region, and (iii) in the region where the crack path made his transition between these two mechanisms. Since the EBSD data sets were not prone to any post-processing filtering operation, comparison of the observed mechanism with other Ti-6Al-4V alloy processed by additive manufacturing (AM) technology can be easily carried out.

Nanostructuring of Additively Manufactured 316L Stainless Steel Using High-Pressure Torsion Technique: An X-ray Line Profile Analysis Study.

Experiments were conducted to reveal the nanostructure evolution in additively manufactured (AMed) 316L stainless steel due to severe plastic deformation (SPD). SPD-processing was carried out using the high-pressure torsion (HPT) technique. HPT was performed on four different states of 316L: the as-built material and specimens heat-treated at 400, 800 and 1100 °C after AM-processing. The motivation for the extension of this research to the annealed states is that heat treatment is a usual step after 3D printing in order to reduce the internal stresses formed during AM-processing. The nanostructure was studied by X-ray line profile analysis (XLPA), which was completed by crystallographic texture measurements. It was found that the as-built 316L sample contained a considerable density of dislocations (1015 m-2), which decreased to about half the original density due to the heat treatments at 800 and 1100 °C. The hardness varied accordingly during annealing. Despite this difference caused by annealing, HPT processing led to a similar evolution of the microstructure by increasing the strain for the samples with and without annealing. The saturation values of the crystallite size, dislocation density and twin fault probability were about 20 nm, 3 × 1016 m-2 and 3%, respectively, while the maximum achievable hardness was ~6000 MPa. The initial <100> and <110> textures for the as-built and the annealed samples were changed to <111> due to HPT processing.

Modification of the Tensile Performance of an Extruded ZK60 Magnesium Alloy with the Addition of Rare Earth Elements.

The influence of rare earth (RE) elements on the microstructure and mechanical performance of an extruded ZK60 Mg alloy was studied. Two types of RE elements were added to a ZK60 material and then extruded at a ratio of 18:1. The first new alloy contained 2 wt% Y while the second one was produced using 2 wt% Ce-rich mischmetal. The microstructure, the texture, and the dislocation density in a base ZK60 alloy and two materials with RE additives were studied by scanning electron microscopy, electron backscattered diffraction, and X-ray line profile analysis, respectively. It was found that the addition of RE elements caused a finer grain size, the formation of new precipitates, and changes in the initial fiber texture. As a consequence, Y and Ce-rich RE elements increased the strength and reduced the ductility. The addition of these two types of RE elements to the ZK60 alloy decreased the work hardening capacity and the hardening exponent mainly due to grain refinement.

Machine Learning-Based Characterization of the Nanostructure in a Combinatorial Co-Cr-Fe-Ni Compositionally Complex Alloy Film.

A novel artificial intelligence-assisted evaluation of the X-ray diffraction (XRD) peak profiles was elaborated for the characterization of the nanocrystallite microstructure in a combinatorial Co-Cr-Fe-Ni compositionally complex alloy (CCA) film. The layer was produced by a multiple beam sputtering physical vapor deposition (PVD) technique on a Si single crystal substrate with the diameter of about 10 cm. This new processing technique is able to produce combinatorial CCA films where the elemental concentrations vary in a wide range on the disk surface. The most important benefit of the combinatorial sample is that it can be used for the study of the correlation between the chemical composition and the microstructure on a single specimen. The microstructure can be characterized quickly in many points on the disk surface using synchrotron XRD. However, the evaluation of the diffraction patterns for the crystallite size and the density of lattice defects (e.g., dislocations and twin faults) using X-ray line profile analysis (XLPA) is not possible in a reasonable amount of time due to the large number (hundreds) of XRD patterns. In the present study, a machine learning-based X-ray line profile analysis (ML-XLPA) was developed and tested on the combinatorial Co-Cr-Fe-Ni film. The new method is able to produce maps of the characteristic parameters of the nanostructure (crystallite size, defect densities) on the disk surface very quickly. Since the novel technique was developed and tested only for face-centered cubic (FCC) structures, additional work is required for the extension of its applicability to other materials. Nevertheless, to the knowledge of the authors, this is the first ML-XLPA evaluation method in the literature, which can pave the way for further development of this methodology.

Spacer Layer Thickness Dependence of the Giant Magnetoresistance in Electrodeposited Ni-Co/Cu Multilayers.

Electrodeposited Ni65Co35/Cu multilayers were prepared with Cu spacer layer thicknesses between 0.5 nm and 7 nm. Their structure and magnetic and magnetoresistance properties were investigated. An important feature was that the Cu layers were deposited at the electrochemically optimized Cu deposition potential, ensuring a reliable control of the spacer layer thickness to reveal the true evolution of the giant magnetoresistance (GMR). X-ray diffraction indicated satellite reflections, demonstrating the highly coherent growth of these multilayer stacks. All of the multilayers exhibited a GMR effect, the magnitude of which did not show an oscillatory behavior with spacer layer thickness, just a steep rise of GMR around 1.5 nm and then, after 3 nm, it remained nearly constant, with a value around 4%. The high relative remanence of the magnetization hinted at the lack of an antiferromagnetic coupling between the magnetic layers, explaining the absence of oscillatory GMR. The occurrence of GMR can be attributed to the fact that, for spacer layer thicknesses above about 1.5 nm, the adjacent magnetic layers become uncoupled and their magnetization orientation is random, giving rise to a GMR effect. The coercive field and magnetoresistance peak field data also corroborate this picture: with increasing spacer layer thickness, both parameters progressively approached values characteristic of individual magnetic layers. At the end, a critical analysis of previously reported GMR data on electrodeposited Ni-Co/Cu multilayers is provided in view of the present results. A discussion of the layer formation processes in electrodeposited multilayers is also included, together with a comparison with physically deposited multilayers.

Influence of Degree of Severe Plastic Deformation on Thermal Stability of an HfNbTiZr Multi-Principal Element Alloy Processed by High-Pressure Torsion.

Severe plastic deformation (SPD) is an effective route for the nanocrystallization of multi-principal element alloys (MPEAs). The stability of the refined microstructure is important, considering the high temperature applications of these materials. In the present study, the effect of SPD on the stability of a body-centered cubic (bcc) HfNbTiZr MPEA was investigated. SPD was performed using a high-pressure torsion (HPT) technique by varying the number of turns between ½ and 10. The evolution of phase composition and microstructure was studied near the disk centers and edges where the imposed strain values were the lowest and highest, respectively. Thus, the shear strain caused by HPT varies between 3 (½ turn, near the center) and 340 (10 turns, near the edge). It was found that during annealing up to 1000 K, the bcc HfNbTiZr alloy decomposed into two bcc phases with different lattice constants at 740 K. In addition, at high strains a hexagonal close packed (hcp) phase was formed above 890 K. An inhomogeneous elemental distribution was developed at temperatures higher than 890 K due to the phase decomposition. The scale of the chemical heterogeneities decreased from about 10 µm to 30 nm where the shear strain increased from 3 to 340, which is similar to the magnitude of grain refinement. Anneal-induced hardening was observed in the MPEA after HPT for both low and high strains at 740 K, i.e., the hardness of the HPT-processed samples increased due to heat treatment. At low strain, the hardness remained practically unchanged between 740 and 1000 K, while for the alloy receiving high strains there was a softening in this temperature range.

Combinatorial Study of Phase Composition, Microstructure and Mechanical Behavior of Co-Cr-Fe-Ni Nanocrystalline Film Processed by Multiple-Beam-Sputtering Physical Vapor Deposition.

A combinatorial Co-Cr-Fe-Ni compositional complex alloy (CCA) thin film disk with a thickness of 1 µm and a diameter of 10 cm was processed by multiple-beam-sputtering physical vapor deposition (PVD) using four pure metal sources. The chemical composition of the four constituent elements varied between 4 and 64 at.% in the film, depending on the distance from the four PVD sources. The crystal structure, the crystallite size, the density of lattice defects (e.g., dislocations and twin faults) and the crystallographic texture were studied as a function of the chemical composition. It was found that in a wide range of elemental concentrations a face-centered cubic (fcc) structure with {111} crystallographic texture formed during PVD. Considering the equilibrium phase diagrams, it can be concluded that mostly the phase composition of the PVD layer is far from the equilibrium. Body-centered cubic (bcc) and hexagonal-close packed (hcp) structures formed only in the parts of the film close to Co-Fe and Co-Cr sources, respectively. A nanocrystalline microstructure with the grain size of 10-20 nm was developed in the whole layer, irrespective of the chemical composition. Transmission electron microscopy indicated a columnar growth of the film during PVD. The density of as-grown dislocations and twin faults was very high, as obtained by synchrotron X-ray diffraction peak profile analysis. The nanohardness and the elastic modulus were determined by indentation for the different chemical compositions on the combinatorial PVD film. This study is the continuation of a former research published recently in Nagy et al., Materials 14 (2021) 3357. In the previous work, only the fcc part of the sample was investigated. In the present paper, the study was extended to the bcc, hcp and multiphase regions.

Microstructure, Hardness, and Elastic Modulus of a Multibeam-Sputtered Nanocrystalline Co-Cr-Fe-Ni Compositional Complex Alloy Film.

A nanocrystalline Co-Cr-Ni-Fe compositional complex alloy (CCA) film with a thickness of about 1 micron was produced by a multiple-beam-sputtering physical vapor deposition (PVD) technique. The main advantage of this novel method is that it does not require alloy targets, but rather uses commercially pure metal sources. Another benefit of the application of this technique is that it produces compositional gradient samples on a disk surface with a wide range of elemental concentrations, enabling combinatorial analysis of CCA films. In this study, the variation of the phase composition, the microstructure (crystallite size and defect density), and the mechanical performance (hardness and elastic modulus) as a function of the chemical composition was studied in a combinatorial Co-Cr-Ni-Fe thin film sample that was produced on a surface of a disk with a diameter of about 10 cm. The spatial variation of the crystallite size and the density of lattice defects (e.g., dislocations and twin faults) were investigated by X-ray diffraction line profile analysis performed on the patterns taken by synchrotron radiation. The hardness and the elastic modulus were measured by the nanoindentation technique. It was found that a single-phase face-centered cubic (fcc) structure was formed for a wide range of chemical compositions. The microstructure was nanocrystalline with a crystallite size of 10-27 nm and contained a high lattice defect density. The hardness and the elastic modulus values measured for very different compositions were in the ranges of 8.4-11.8 and 182-239 GPa, respectively.

Effect of Heat Treatment on the Microstructure and Performance of Cu Nanofoams Processed by Dealloying.

Cu nanofoams are promising materials for a variety of applications, including anodes in high-performance lithium-ion batteries. The high specific surface area of these materials supports a high capacity and porous structure that helps accommodate volume expansion which occurs as batteries are charged. One of the most efficient methods to produce Cu nanofoams is the dealloying of Cu alloy precursors. This process often yields nanofoams that have low strength, thus requiring additional heat treatment to improve the mechanical properties of Cu foams. This paper provides the effects of heat treatment on the microstructures, mechanical properties, and electrochemical performance of Cu nanofoams. Annealing was conducted under both inert and oxidizing atmospheres. These studies ultimately reveal the underlying mechanisms of ligament coarsening during heat treatment.