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At least 1,117 records · Page 62

In-situ neutron diffraction investigation of two-stage martensitic transformation in a 13%Mn steel with serrated deformation

Two stage austenite →ε-martensite →α-martensite phase transformation, phase-specific lattice strain evolution and load sharing during tensile deformation of a 13%Mn hot-rolled austenitic steel are revealed by in-situ neutron diffraction. In conclusion, direct evidence is provided that serrated deformation behavior is attributed to discontinuous martensitic transformation.

Austenitic steel↗

Electroplated L1{sub 0} CoPt thick-film permanent magnets

The fabrication and magnetic characterization of 15-μm-thick electroplated L1{sub 0} CoPt hard magnets with good magnetic properties is reported in this paper. Experimental study of the dependence of the magnets' properties on annealing temperature reveals that an intrinsic coercivity H{sub ci} = ∼800 kA/m (10 kOe), squareness >0.8, and energy product of >150 kJ/m{sup 3} are obtained for photolithographically patterned structures (250 μm × 2 mm stripes; 15 μm thickness) electroplated on silicon substrates and annealed in hydrogen forming gas at 700 °C. Scanning electron microscopy is used to inspect the morphology of both the as-deposited and annealed magnetic layers, and X-ray Diffractometer analysis on the magnets annealed at 700 °C confirm a phase transformation to an ordered L1{sub 0} CoPt structure, with a minor phase of hcp Co. These thick films are intended for microsystems/MEMS applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

High temperature growth of Ag phases on Ge(111)

The growth of the (3 Multiplication-Sign 1) and ({radical}3 Multiplication-Sign {radical}3)R30 Degree-Sign phases of Ag on Ge(111) on substrates at temperatures from 540 to 660 Degree-Sign C is characterized with low energy electron microscopy (LEEM) and low energy electron diffraction (LEED). From 540 Degree-Sign C to the Ag desorption temperature of 575 Degree-Sign C, LEEM images show that growth of the (3 Multiplication-Sign 1) phase begins at step edges. Upon completion of the (3 Multiplication-Sign 1) phase, the ({radical}3 Multiplication-Sign {radical}3)R30 Degree-Sign phase is observed with a dendritic growth morphology that is not much affected by steps. For sufficiently high deposition rates, Ag accumulates on the sample above the desorption temperature. From 575 to 640 Degree-Sign C, the growth proceeded in a manner similar to that at lower temperatures, with growth of the (3 Multiplication-Sign 1) phase to completion, followed by growth of the ({radical}3 Multiplication-Sign {radical}3)R30 Degree-Sign phase. Increasing the substrate temperature to 660 Degree-Sign C resulted in only (3 Multiplication-Sign 1) growth. In addition, for samples with Ag coverage less than 0.375ML, LEEM and LEED images were used to follow a reversible phase transformation near 575 Degree-Sign C, between a mixed high coverage phase of [(4 Multiplication-Sign 4) + (3 Multiplication-Sign 1)] and the high temperature, lower coverage (3 Multiplication-Sign 1) phase.

36 MATERIALS SCIENCE↗

Helium-bubble-enhanced disordering of intermetallic phase under irradiation

Understanding and controlling phase transformations in metals and alloys under irradiation is vital to the design of irradiation-tolerant materials. The L1 2 -ordered intermetallic phase in nickel-based superalloys provides superior high-temperature mechanical properties and corrosion resistance. Here, we studied the order-disorder transformation kinetics of an L1 2 -structured gamma-prime phase in nickel-based superalloy Rene N4 under krypton ion irradiation and the effect of pre-implanted helium gas bubbles on the kinetics of phase transformation. Furthermore, the presence of pre-implanted helium gas bubbles significantly enhances the order-disorder transformation of L1 2 -structured gamma-prime phase under irradiation at 300 °C. The evolution of pre-implanted helium gas bubbles under irradiation implies that helium gas bubbles could effectively trap irradiation-induced vacancies and impede the reordering process of anti-site defects in gamma-prime phase.

36 MATERIALS SCIENCE↗

Shape Dependence of Pressure-Induced Phase Transition in CdS Semiconductor Nanocrystals

Understanding structural stability and phase transformation of nanoparticles under high pressure is of great scientific interest, as it is one of the crucial factors for design, synthesis, and application of materials. Even though high-pressure research on nanomaterials has been widely conducted, their shape-dependent phase transition behavior still remains unclear. Examples of phase transitions of CdS nanoparticles are very limited, despite the fact that it is one of the most studied wide band gap semiconductors. Here we have employed in-situ synchrotron wide-angle X-ray scattering (WAXS) and transmission electron microscopy (TEM) to investigate the high-pressure behaviors of CdS nanoparticles as a function of particle shapes. We observed that CdS nanoparticles transform from wurtzite to rocksalt phase at elevated pressure in comparison to their bulk counterpart. Phase transitions also vary with particle shape—rod-shaped particles show a partially reversible phase transition and the onset of the structural phase transition pressure decreases with decreasing surface-to-volume ratios, while spherical particles undergo irreversible phase transition with relatively low phase transition pressure. Additionally, TEM images of spherical particles exhibited sintering-induced morphology change after high-pressure compression. Calculations of the bulk modulus reveals that spheres are more compressible than rods in the wurtzite phase. These results indicate that the shape of the particle plays an important role in determining their high-pressure properties. Our study provides important insights into understanding of the phase-structure-property relationship, guiding future design and synthesis of nanoparticles for promising applications.

36 MATERIALS SCIENCE↗

In situ, 3D characterization of the deformation mechanics of a superelastic NiTi shape memory alloy single crystal under multiscale constraint

Microstructural elements in NiTi shape memory alloys (SMAs) – precipitates, phase boundaries, inclusions, grain boundaries – can be viewed as sources of multiscale constraint that influence their deformation response. In this paper, we characterized in situ, and in 3D, the deformation and the evolution of microstructure during a tension test in a superelastic NiTi specimen containing some of these sources of constraint. The method used was far-field high-energy X-ray diffraction microscopy (ff-HEDM), complemented by electron microscopy. We simulated the local stress state in the specimen using a microstructural model informed by the experimental data. Using these combined microstructure, deformation, and stress data, we report three phenomena, and relate them to specific sources of constraint. During initial elastic loading, axial lattice strain in austenite increased monotonically. On partial stress-induced phase transformation to martensite, the stress redistributed to both phases leading to a stress relaxation in austenite. The specimen contained a dense distribution of inclusions, which led to the activation of martensite habit plane variants that produce less than theoretical maximum transformation strain. Large Ni 4 Ti 3 precipitates potentially contributed to the poor transformation response. Under load, proportional gradients in local rotation and elastic stretch developed in the martensite phase, because of the constraint at phase interfaces. Finally, this combined ff-HEDM, electron microscopy, microstructural simulation toolbox provides a versatile method to understand the effect of constraint on inelastic deformation in other alloys with hierarchical microstructure.

36 MATERIALS SCIENCE↗

Formation mechanisms of Sn-rich δ phase and its role in strengthening Cu-10Sn manufactured by laser powder bed fusion

Cu-Sn alloys produced via laser powder bed fusion (L-PBF) additive manufacturing (AM) have gained significant attention because they combine the advantages of AM relevant to intricate component design with outstanding combinations of strength, ductility, and resistance to wear and corrosion. However, a detailed understanding of the microstructure that contributes to the enhancement of the mechanical properties of L-PBF Cu-10Sn alloys remains unclear. In particular, there is a lack of understanding of the formation mechanisms of the Sn-rich δ phase commonly observed in Cu-10Sn. This study reveals two distinct variants of the δ phase possessing unique morphological characteristics. These characteristics are attributed to the local solidification conditions inherent to the melt pool boundaries versus those at the interiors of melt pools. A phase transformation pathway that elucidates the origin of the morphological variants of the δ phase from the Sn-rich metastable phases during the cyclic heating of the AM process is proposed. We report superior mechanical properties in L-PBF Cu-10Sn compared to those of conventionally manufactured counterparts due to the synergistic contributions from grain boundaries, dislocations, and the δ phase. Notably, the δ phase alone contributes approximately 22 % to the overall strength observed in the L-PBF Cu-10Sn alloy. The discovery of two types of distinct Sn-rich δ phase offers key insights into precise microstructural control in AM Cu-Sn alloys to enhance mechanical properties, providing practical strategies for improving material performance for diverse applications in automotive, aerospace, and machinery industries.

36 MATERIALS SCIENCE↗

Fracture toughness of zirconia with a nanometer size notch fabricated using focused ion beam milling

Zirconia with 3 mol% yttria (3Y-TZP) has been used for dental crowns and bridges due to its excellent mechanical behavior. Performing fracture toughness testing on this nanograin material, however, can be a challenge. For reliable results, fracture toughness testing requires an extremely sharp notch in the test specimen that closely approximates a very sharp crack. This study was to investigate an alternative method to produce nanometer-sized notches, which are less than the average grain size of 3Y-TZP, during the preparation of single-edge V-notched beam specimens and report the resulting fracture toughness value. We present a method using focused ion beam (FIB) milling to fabricate nanometer-sized notches in 3Y-TZP. The notch tip is <100 nm wide, which is smaller than the grain size, and is consistent throughout the thickness of the specimen. The FIB-notched specimens show a much reduced average fracture toughness of 5.64 ± 1.14 MPa√m compared to 8.90 ± 0.23 MPa√m for the specimens without FIB-notches. The FIB-milling did not appear to create any monoclinic phase prior to fracture toughness testing. Fractures originated at the FIB-notches, and the notch size can be readily identified post-mortem using a microscope. A considerable amount of tetragonal-to-monoclinic phase transformation was observed throughout the fracture surfaces. FIB milling provides an alternative method to fabricate nanometer-sized notches that are smaller than the grain size of tetragonal zirconia polycrystal. The fracture toughness determined using FIB-notches was ~5.64 MPa√m, smaller than the specimens with V-notches fabricated using saw blades.

36 MATERIALS SCIENCE↗

Probing Dopant Redistribution, Phase Propagation, and Local Chemical Changes in the Synthesis of Layered Oxide Battery Cathodes

Achieving the targeted control of layered oxide properties calls for more fundamental studies to mechanistically probe their evolution during their synthesis. Herein, dopant distribution, phase propagation, and local chemical changes as well as their interplay in multielement-doped LiNiO 2 materials are investigated using spectroscopic, imaging, and scattering techniques. It is shown that dopants undergo dynamic redistribution in the Ni(OH) 2 host lattice at the early stage of calcination (below 300 °C). Such redistribution behavior exhibits strong dopant-dependent characteristics, allowing for targeted surface and bulk doping control. The Ni oxidation process exhibits depth-dependent characteristics and the most rapid Ni oxidation takes place between 300 and 700 °C. Using Ni oxidation state as the proxy for the phase transformation, the buildup of heterogenous phase propagation in the early stage of calcination is shown, especially along the radial direction of secondary particles. Furthermore, the radial heterogenous phase distribution gradually decreases upon completing the calcination. However, a high degree of mosaic-like heterogeneity may still be present in the final product, departing from the perfect layered oxide. Overall, the present study offers fundamental insights into manipulating multiscale materials properties during calcination for obtaining stable, high-energy layered oxide cathodes.

36 MATERIALS SCIENCE↗

Phase stability of iron germanate, FeGeO 3 , to 127 GPa

The high-pressure behavior of germanates is of interest as these compounds serve as analogs for silicates of the deep Earth. Current theoretical and experimental studies of iron germanate, FeGeO 3 , are limited. Here in this paper, we have examined the behavior of FeGeO 3 to 127 GPa using the laser-heated diamond anvil cell combined with in situ synchrotron X-ray diffraction. Upon compression at room temperature, the ambient-pressure clinopyroxene phase transforms to a disordered triclinic phase [FeGeO 3 (II)] at ~ 18 GPa in agreement with earlier studies. An additional phase transition to FeGeO 3 (III) occurs above 54 GPa at room temperature. Laser-heating experiments (~ 1200–2200 K) were conducted at three pressures (33, 54, and 123 GPa) chosen to cover the stability regions of different GeO 2 polymorphs. In all cases, we observe that FeGeO 3 dissociates into GeO 2 + FeO at high pressure and temperature conditions. Neither the perovskite nor the post-perovskite phase was observed up to 127 GPa at ambient or high temperatures. The results are consistent with the behavior of FeSiO 3 , which also dissociates into a mixture of the oxides (FeO + SiO 2 ) at least up to 149 GPa.

36 MATERIALS SCIENCE↗

The nature of the first order isostructural transition in GdRhSn

We present structural, magnetic, thermal, magnetocaloric, and electrical transport properties of polycrystalline GdRhSn. Magnetization data show that it orders antiferromagnetically at TN = 16.2 K. The compound has the ZrNiAl type hexagonal crystal structure at room temperature and undergoes a first order iso-structural transition in the paramagnetic state at 245 K. The unit cell volume change at the transition is small (-0.07 %) but discontinuous, in agreement with the first-order nature of the transition observed by magnetic, transport, and heat capacity measurements. The anisotropic changes of the lattice parameters are Δa/a = 0.28 % and Δc/c = -0.64 % on cooling. A substantial change in the 4f and conduction electron hybridization, giving rise to an increased integrated DOS, occurs when the high temperature phase transforms to the low temperature phase. A moderate magnetocaloric effect at TN (ΔSM = -6.5 J/kg K and ΔTad = 4.5 K for ΔH= 50 kOe) has been measured using both magnetization and heat capacity data

36 MATERIALS SCIENCE↗

Taming the Pseudoelastic Response of Nitinol Using Ion Implantation

Implantation of Ni 50.5 Ti 49.5 wire with 30 MeV Ni 6+ ions at doses (< 0.1 DPA) typically smaller than employed in the literature is shown to systematically alter the pseudoelastic response, with extrema in Berkovich nanoindentation load (+50%), hysteresis (–60%), and recoverable displacement (–19%) occurring at ~ 3.6 μm below the implantation surface. These extraordinary values are attributed to ~ 10 to 20 nm amorphous clusters that constrain the stress-induced B2-B19' phase transformation. This is substantiated by phase field simulations of crystalline-amorphous composites and molecular dynamics simulations of crystalline-vacancy cluster composites showing the spatial refinement of martensite caused by nm-scale defects. Finally, the results suggest that ion implantation may potentially expand the processing and performance space for NiTi, by creating amorphous defects at smaller length scales than dislocation substructures produced by conventional deformation processing.

36 MATERIALS SCIENCE↗

Improved phase stability of formamidinium lead triiodide perovskite by strain relaxation

Though formamidinium lead triiodide (FAPbI 3 ) possesses a suitable band gap and good thermal stability, the phase transition from the pure black perovskite phase (α-phase) to the undesirable yellow nonperovskite polymorph (δ-phase) at room temperature, especially under humid air, hinders its practical application. Here, we investigate the intrinsic instability mechanism of the α-phase at ambient temperature and demonstrate the existence of an anisotropic strained lattice in the (111) plane that drives phase transformation into the δ-phase. Methylammonium bromide (MABr) alloying (or FAPbI 3 -MABr) was found to cause lattice contraction, thereby balancing the lattice strain. This led to dramatic improvement in the stability of α-FAPbI 3 . As a result, solar cells fabricated using FAPbI 3 -MABr demonstrated significantly enhanced stability under the humid air.

14 SOLAR ENERGY↗

Electron-ion plasma modification of Al-based alloys

The paper reports on the study where we analyzed the surface structure and strength properties of coated Al alloys modified by electron-ion plasma treatment. The Al alloys were deposited with a thin (≈0.5 μm) TiCu film coating (TiCu-Al system) and with a hard TiCuN coating (TiCuN–AlSi system) on a TRIO vacuum setup in the plasma of low-pressure arc discharges. The temperature fields and phase transformations in the film–substrate system were estimated by numerical simulation in a wide range of electron energy densities (5–30 J/cm{sup 2}) and pulse durations (50–200 μs). The calculations allowed us to determine the threshold energy density and pulse duration at which the surface structure of the irradiated Al-based systems is transformed in a single-phase state (solid or liquid) and in a two-phase state (solid plus liquid). The elemental composition, defect structure, phase state, and lattice state in the modified surface layers were examined by optical, scanning, and transmission electron microscopy, and by X-ray diffraction analysis. The mechanical characteristics of the modified layers were studied by measuring the hardness and Young’s modulus. The tribological properties of the modified layers were analyzed by measuring the wear resistance and friction coefficient. It is shown that melting and subsequent high-rate crystallization of the TiCu–Al system makes possible a multiphase Al-based surface structure with the following characteristics: crystallite size ranging within micrometer, microhardness of more than 3 times that in the specimen bulk, and wear resistance ≈1.8 times higher compared to the initial material. Electron beam irradiation of the TiCuN–AlSi system allows fusion of the coating into the substrate, thus increasing the wear resistance of the material ≈2.2 times at a surface hardness of ∼14 GPa.

36 MATERIALS SCIENCE↗

Structure, magnetism, and electron-transport properties of Mn{sub 2}CrGa-based nanomaterials

Mn{sub 2}CrGa in the disordered cubic structure has been synthesized using rapid quenching and subsequent annealing. The cubic phase transforms to a stable tetragonal phase when a fraction of Cr or Ga is replaced by Pt or Al, respectively. All samples are ferrimagnetic with high Curie temperatures (T{sub c}); Mn{sub 2}CrGa exhibits the highest T{sub c} of about 813 K. The tetragonal samples have appreciable values of magnetocrystalline anisotropy energy, which leads to an increase in coercivity (H{sub c}) that approaches about 10 kOe in the Pt-doped sample. The H{sub c} linearly increases with a decrease of temperature, concomitant with the anisotropy change with temperature. All samples are metallic and show negative magnetoresistance with room-temperature resistivities on the order of 1 mΩcm. The magnetic properties including high T{sub c} and low magnetic moment suggest that these tetragonal materials have potential for spin-transfer-torque-based devices.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Crystallographic and magnetic investigations of textured bismuth ferrite lead titanate layers

In present work we demonstrate the synthesis of textured 60BiFeO 3 –40PbTiO 3 (60:40 BFPT) by using the templated grain growth technique with platelets of BaTiO 3 . Synthesised 60:40 BFPT has been examined by High-energy x-ray diffraction utilizing a synchrotron x-ray source. The crystallographic structure refinement results revealed the co-existence of monoclinic and tetragonal phases. By employing an external electric field, the mixed monoclinic/tetragonal phases transformed to the predominantly tetragonal phase. In addition, a crystallographic texture refinement was completed on unpoled state of 60:40 BFPT which showed the sample had 1.3 multiples of random distribution (MRD) $\{100\}$ crystallographic textured in tetragonal phase. However, magnetic measurements showed isotropic ferromagnetism for the sample which is not in agreement with the crystallographic texture properties of the sample. Low temperature magnetic transition has been found in zero field cooled—field cooled (ZFC-FC) measurements. This could be due to the possible existence of a secondary magnetic phase, which dominated the magnetic result.

36 MATERIALS SCIENCE↗

Free energy of grain boundary phases: Atomistic calculations for Σ 5 ( 310 ) [ 001 ] grain boundary in Cu

Atomistic simulations are employed to demonstrate the existence of a well-defined thermodynamic phase transformation between grain boundary (GB) phases with different atomic structures. The free energy of different interface structures for an embedded-atom-method model of the Σ5 (310) [001] symmetric tilt boundary in elemental Cu is computed using the nonequilibrium Frenkel-Ladd thermodynamic integration method through molecular dynamics simulations. It is shown that the free-energy curves predict a temperature-induced first-order interfacial phase transition in the GB structure in agreement with computational studies of the same model system. Moreover, the role of vibrational entropy in the stabilization of the high-temperature GB phase is clarified. The calculated results are able to determine the GB phase stability at homologous temperatures less than 0.5, a temperature range particularly important given the limitation of the methods available hitherto in modeling GB phase transitions at low temperatures. Lastly, the calculation of GB free energies complements currently available 0 K GB structure search methods, making feasible the characterization of GB phase diagrams.

36 MATERIALS SCIENCE↗

Topological defect dynamics in operando battery nanoparticles

Topological defects can markedly alter nanomaterial properties. This presents opportunities for "defect engineering," where desired functionalities are generated through defect manipulation. However, imaging defects in working devices with nanoscale resolution remains elusive. We report three-dimensional imaging of dislocation dynamics in individual battery cathode nanoparticles under operando conditions using Bragg coherent diffractive imaging. Dislocations are static at room temperature and mobile during charge transport. During the structural phase transformation, the lithium-rich phase nucleates near the dislocation and spreads inhomogeneously. The dislocation field is a local probe of elastic properties, and we find that a region of the material exhibits a negative Poisson's ratio at high voltage. Operando dislocation imaging thus opens a powerful avenue for facilitating improvement and rational design of nanostructured materials.

25 ENERGY STORAGE↗