Probing the phase transformation and dislocation evolution in dual-phase high-entropy alloys
Not Available
Fang, Qihong↗
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Tensile behavior of dual-phase titanium alloys under high-intensity proton beam exposure: radiation-induced omega phase transformation in Ti-6Al-4V
A high-intensity proton beam exposure with 181 MeV energy has been conducted at Brookhaven Linac Isotope Producer facility on various material specimens for accelerator targetry applications, including titanium alloys as a beam window material. The radiation damage level of the analyzed capsule was 0.25 dpa at the beam center region with an irradiation temperature around 120 oC. Tensile tests showed increased hardness and a large decrease in ductility for the dual a+ß-phase Ti-6Al-4V Grade-5 and Grade-23 extra low interstitial alloys, with the near a-phase Ti-3Al-2.5V Grade-9 alloy still exhibiting uniform elongation of a few % after irradiation. Transmission Electron Microscope analyses on Ti-6Al-4V indicated clear evidence of a high-density of defect clusters with size less than 2 nm in each a-phase grain. The ß-phase grains did not contain any visible defects such as loops or black dots, while the diffraction patterns clearly indicated ?-phase precipitation in an advanced formation stage. The radiation-induced ?-phase transformation in the ß-phase could lead to greater loss of ductility in Ti-6Al-4V alloys in comparison with Ti-3Al-2.5V alloy with less ß-phase.google scho
Tensile Test, titanium, acclerator, proton beam↗
In situ Raman spectroscopy of pressure-induced phase transformations in polycrystalline TbPO 4 , DyPO 4 , and Gd x Dy (1– x ) PO 4 [ In situ Raman spectroscopy of pressure-induced phase transformations in DyPO 4 and Gd x Dy (1– x ) PO 4 ]
Xenotime DyPO 4 and Gd x Dy (1–x) PO 4 (x = 0.4, 0.5, 0.6) (tetragonal I41amd zircon structure) have been studied at ambient temperature under high pressures inside a diamond anvil cell with in situ Raman spectroscopy. The typical Raman–active modes of the xenotime structure were observed at low pressures and the appearance of new Raman peaks at higher pressures indicated a phase transformation to a lower symmetry structure—likely monoclinic. Raman mode softening was observed, resulting in a line crossing at approximately 7–8 GPa for each material and preceding the phase transformation. The onset of phase transformation for DyPO 4 occurred at a pressure of 15.3 GPa. DyPO 4 underwent a reversible phase transformation and returned to the xenotime phase after decompression. The transformation pressures of the solid solutions (Gd x Dy (1–x) PO 4 ) were in the range 10–12 GPa. The GdxDy(1–x)PO 4 solid solutions yielded partially reversible phase transformations, retaining some of the high–pressure phase spectrum while reforming xenotime peaks during decompression. The substitution of Gd into DyPO 4 decreased the transformation pressure relative to pure DyPO 4 . In conclusion, the ability to modify the phase transformation pressures of xenotime rare–earth orthophosphates by chemical variations of solid solutions may provide additional methods to improve the performance of ceramic matrix composites.
36 MATERIALS SCIENCE↗
Temperature-dependent mechanical deformation of silicon at the nanoscale: Phase transformation versus defect propagation
This study uses high-temperature nanoindentation coupled with in situ electrical measurements to investigate the temperature dependence (25–200 °C) of the phase transformation behavior of diamond cubic (dc) silicon at the nanoscale. Along with in situ indentation and electrical data, ex situ characterizations, such as Raman and cross-sectional transmission electron microscopy, have been used to reveal the indentation-induced deformation mechanisms. We find that phase transformation and defect propagation within the crystal lattice are not mutually exclusive deformation processes at elevated temperature. Both can occur at temperatures up to 150 °C but to different extents, depending on the temperature and loading conditions. For nanoindentation, we observe that phase transformation is dominant below 100 °C but that deformation by twinning along (111) planes dominates at 150 °C and 200 °C. This work, therefore, provides clear insight into the temperature dependent deformation mechanisms in dc-Si at the nanoscale and helps to clarify previous inconsistencies in the literature.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Two-dimensional lithium diffusion behavior and probable hybrid phase transformation kinetics in olivine lithium iron phosphate
Olivine lithium iron phosphate is a technologically important electrode material for lithium-ion batteries and a model system for studying electrochemically driven phase transformations. Despite extensive studies, many aspects of the phase transformation and lithium transport in this material are still not well understood. Here we combine operando hard X-ray spectroscopic imaging and phase-field modeling to elucidate the delithiation dynamics of single-crystal lithium iron phosphate microrods with long-axis along the [010] direction. Lithium diffusivity is found to be two-dimensional in microsized particles containing ~3%lithium-iron anti-site defects. Our study provides direct evidence for the previously predicted surface reaction-limited phase-boundary migration mechanism and the potential operation of a hybrid mode of phase growth, in which phase-boundary movement is controlled by surface reaction or lithium diffusion in different crystallographic directions. These findings uncover the rich phase-transformation behaviors in lithium iron phosphate and intercalation com-pounds in general and can help guide the design of better electrodes.
25 ENERGY STORAGE↗
Quantification of High-Temperature Transition Al2O3 and Their Phase Transformations
High temperature exposure of ?-Al2O3 can lead to a series of polymorphic transformations, including the formation of ?-Al2O3 and ?-Al2O3. Quantification of the microstructure in the ?/?-Al2O3 formation range represents a formidable challenge as both phases accommodate a high degree of structural disorder. In this work, we explore the use of XRD recursive stacking formalism for quantification of high temperature transition aluminas. We formulate the recursive stacking methodology for modelling of disorder in ?-Al2O3 and twinning in ?-Al2O3 and show that explicitly accounting for the disorder is necessary to reliably model the XRD patterns of high temperature transition alumina. In the second part, we use the recursive stacking approach to study phase transformation during high temperature (1050 ºC) treatment. We show that the two different intergrowth modes of ?-Al2O3 have different transformation characteristics, and that a significant portion of ?-Al2O3 is stabilized with ?-Al2O3 even after prolonged high-temperature exposures. In discussions, we outline the limitation of the current XRD approach and discuss a possible multimodal XRD and NMR approach which can improve analysis of complex transition aluminas. This work was performed in the Wiley Environmental Molecular Sciences Laboratory (EMSL), a national scientific user facility sponsored by DOEs Office of Biological and Environmental Research and located at PNNL. The work was supported by the U.S. Department of Energy (DOE), Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences, and Biosciences.
Kovarik, Libor↗
Investigation of water assisted phase transformation process from AlPO4-5 to AlPO4-tridymite
Not Available
Xu, Suochang↗
In-situ Experiments to Capture the Evolution of Microstructure During Phase Transformation of Titanium Under Dynamic Loading
Under sufficient stresses, such as during dynamic loading, titanium experiences a phase transformation from hcp alpha phase to hexagonal omega phase. Omega phase is often retained in the microstructure after unloading, and has a strong influence on subsequent mechanical properties. Simulations suggest there are multiple pathways and underlying mechanisms for this transformation. Due to the incredibly short timescales involved, experimental measurements for model validation have been difficult. However, new capabilities at the Advanced Photon Source have enabled diffraction measurements during plate impact experiments to study the evolution of titanium during transformation. These high-rate data allow us to probe the mechanism and kinetics of phase transformations in new ways. Recent results will be presented and compared to post-mortem characterization of soft-recovered shocked specimens. Comparisons are then made with previous tests where material was shock-loaded and soft recovered for microstructural analysis. Together these techniques create a consistent picture of material behavior during the shock-induced α–ω phase transformation in titanium.
36 MATERIALS SCIENCE↗
Phase transformations in Ln 2 O 3 materials irradiated with swift heavy ions
Phase transformations induced in the cubic C-type lanthanide sesquioxides, Ln 2 O 3 (Ln = Sm, Gd, Ho, Tm, and Lu), by dense electronic excitation are investigated. The structural modifications resulting from exposure to beams of 185 MeV Xe and 2246 MeV Au ions are characterized using synchrotron x-ray diffraction and Raman spectroscopy. The formation of a B-type polymorph, an X-type nonequilibrium phase, and an amorphous phase are observed. The specific phase formed and the transformation rate show dependence on the material composition, as well as the ion beam mass and energy. Atomistic mechanisms for these transformations are determined, indicating that formation of the B-type phase results from the production of anti-Frenkel defects and the aggregation of anion vacancies into planar clusters, whereas formation of the X-type and amorphous phases requires extensive displacement of both anions and cations. Here, the observed variations in phase behavior with changing lanthanide ionic radius and deposited electronic energy density are related to the energetics of these transformation mechanisms.
36 MATERIALS SCIENCE↗
In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction
The alloy Cu{sub 25}Au{sub 30}Zn{sub 45} undergoes a huge first-order phase transformation (6% strain) and shows a high reversibility under thermal cycling and an unusual martensitc microstructure in sharp contrast to its nearby compositions. This alloy was discovered by systematically tuning the composition so that its lattice parameters satisfy the cofactor conditions (i.e., the kinematic conditions of compatibility between phases). It was conjectured that satisfaction of these conditions is responsible for the enhanced reversibility as well as the observed unusual fluid-like microstructure during transformation, but so far, there has been no direct evidence confirming that these observed microstructures are those predicted by the cofactor conditions. To verify this hypothesis, we use synchrotron X-ray Laue microdiffraction to measure the orientations and structural parameters of variants and phases near the austenite/martensite interface. The areas consisting of both austenite and multi-variants of martensite are scanned by microLaue diffraction. The cofactor conditions have been examined from the kinematic relation of lattice vectors across the interface. The continuity condition of the interface is precisely verified from the correspondent lattice vectors between two phases.
36 MATERIALS SCIENCE↗
Phase transformations, microstructural refinement and defect evolution mechanisms in Al-Si alloys under non-hydrostatic diamond anvil cell compression
Non-hydrostatic compression of materials using a diamond anvil cell (DAC) can transform equilibrium microstructure of an alloy to novel, potentially metastable states. In this study, in situ synchrotron X-ray diffraction (XRD) during compression up to 24 GPa and subsequent ex situ, high resolution analytical electron microscopy (AEM) after decompression of an Al-Si alloy provided insight into the crystallographic changes during the compression as well as microstructural refinement, and defect structures caused by such a high pressure compression-decompression process. Pressure resolved in-situ synchrotron XRD was used to detail the phase transformation pathway of the eutectic Si phase in Al-Si alloy, from Si-I → Si-XI → Si-V during compression, and a final transformation predominantly to Si-III after decompression. Using scanning and transmission electron microscopy (S/TEM), site specific analysis of the alloy immediately underneath the anvil contact surface demonstrated a highly complex microstructure. A narrow region of thick amorphous Al oxide interspersed with nanocrystalline grains was found at the top surface. Underneath this Al oxide, while the majority the eutectic Si was transformed into highly-deformed, polycrystalline (PC) Si-III, a complex intermediate layer was discovered at the interface between Al and Si, comprised of a small fraction of Al nanocrystals and a majority of nanocrystalline Si-I. This combination of pressure resolved in-situ synchrotron XRD coupled with subsequent high resolution, electron microscopy resolved the phase transformation as well as non-equilibrium microstructures in a metallic alloy induced by a non-hydrostatic high pressure compression followed by decompression.
36 MATERIALS SCIENCE↗
Phase transformation of hydrous ringwoodite to the lower-mantle phases and the formation of dense hydrous silica
In order to understand the effects of H 2 O on the mineral phases forming under the pressure-temperature conditions of the lower mantle, we have conducted laser-heated diamond-anvil cell experiments on hydrous ringwoodite (Mg 2 SiO 4 with 1.1wt% H 2 O) at pressures between 29 and 59 GPa and temperatures between 1200 and 2400 K. Our experimental results show that hydrous ringwoodite (hRw) converts to crystalline dense hydrous silica, stishovite (Stv) or CaCl 2 -type SiO 2 (mStv), containing 1 wt% H 2 O together with Brd and MgO at the pressure-temperature conditions expected for shallow lower-mantle depths between approximately 660 to 1600 km. Considering lack of sign for melting in our experiments, our preferred interpretation of the observation is that Brd partially breaks down to dense hydrous silica and periclase (Pc), forming Brd + Pc + Stv mineralogy. Our experiments may provide an explanation for the enigmatic coexistence of Stv and Fp inclusions in lower-mantle diamonds
58 GEOSCIENCES↗
The roles of kinematic constraint and diffusion in non-equilibrium solid state phase transformations of Ti-6Al-4V
A solid state phase transformation of Ti-6Al-4V was studied using high speed in situ x-ray diffraction measurements made during rapid cooling of a cold metal transfer arc weld bead deposited onto a water cooled substrate. Analysis of body centered cubic (BCC) and hexagonal close packed (HCP) lattices revealed an abrupt, nonlinear shift in the lattice parameters of both phases just after the HCP phase had nucleated. Postmortem transmission electron microscopy confirmed that V diffusion was mostly suppressed during cooling. Together, these results indicate that at this cooling rate of approximately 10 4 K/s, which is representative of cooling rates of many additive manufacturing and welding processes, kinematic coherency of the BCC–HCP interfaces gives rise to the anomalous lattice expansion and contraction behaviors of both phases during the initial nucleation and growth stages of (mostly) martensitic transformation from BCC to HCP; the role of diffusion in such lattice anomalies is shown to be minimal.
36 MATERIALS SCIENCE↗
Role of α → ε → α phase transformation on the spall behavior of iron at atomic scales
Shock compression of iron microstructures above a threshold stress results in a α (BCC) → ε (HCP) transformation and the propagation of the release wave brings the metal back to the α phase following the ε→α transformation. Predicting failure behavior under shock loading conditions (spallation) relies on understanding the evolution of defects in the microstructure as it undergoes the α→ε→α phase transformation. This study uses molecular dynamics (MD) simulations to investigate the role of defect evolution during α→ε→α phase transformation on the spall strength values of single-crystal (sc) Fe microstructures. The MD simulations aim to characterize the ε phase fraction formed during shock compression and the defects during shock release for variations in loading orientations and shock stresses. The simulations are carried out for loading along the [100], [110], [111], and [112] orientations and for impact velocities ranging from 600 m/s to 1 km/s. The ε phase fractions during compression and defects (dislocations, twins) characterized during spall failure show an orientation dependence that affects the spall strength values. Here, the lowest value for spall strength is observed for the <110> loading orientation that shows a high density of twinning at the spall plane, whereas the highest value is observed for the <100> orientation and is associated with a α (BCC) → γ (FCC) transformation at the spall plane. The correlations of the spall strength values with the strain rates and with the ε phase fractions are discussed.
36 MATERIALS SCIENCE↗
Relationships Between the Phase Transformation Kinetics, Texture Evolution, and Microstructure Development in a 304L Stainless Steel Under Biaxial Loading Conditions: Synchrotron X-ray and Electron Backscatter Diffraction Studies
The relationships between the martensitic phase transformation kinetics, texture evolution, and the microstructure development in the parent austenite phase were studied for a 304L stainless steel that exhibits the transformation-induced plasticity effect under biaxial loading conditions at ambient temperature. The applied loading paths included: pure torsion, simultaneous biaxial torsion/tension, simultaneous biaxial torsion/compression, and stepwise loading of tension followed by torsion (i.e., first loading by uniaxial tension and then by pure torsion in sequence). Synchrotron X-ray and electron backscatter diffraction techniques were used to measure the evolution of the phase fractions, textures, and microstructures as a function of the applied strains. The influence of loading character and path on the changes in martensitic phase transformation kinetics is discussed in the context of (1) texture-transformation relationship and the preferred transformation of grains belonging to certain texture components over the others, (2) effects of axial strains on shear band evolutions, and (3) volume changes associated with martensitic transformation.
Complex Loading↗