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At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Effects of Sr, Ce and P on the microstructure and mechanical properties of rapidly solidified Al7Si alloys

Highlights: • Rapid solidification caused formation of nanoscaled Si particle chains. • Sr or Ce induced the columnar transition zone only at extremely high cooling rate. • Enhancement of hardness is attributed to fine dispersion of eutectic Si, grain refinement and the supersaturation of Si. • Sr or Ce caused further enhancement of hardness, attributing to Si modification. - Abstract: A series of Al7Si based alloys with trace addition of Sr, Ce or P were prepared using melt-spinning at two different high cooling rates, and the microstructure as well as the hardness of the ribbons was comprehensively studied. The results show that Sr or Ce induces the formation of columnar transition zone and modifies the morphology of eutectic Si phase from dispersed particle chains to fine fibers only at extremely high cooling rate. However, P has little effect on the microstructure of either α-Al or eutectic Si. Compared with conventional casting, the Al7Si ribbons exhibit extremely high hardness due to the fine dispersion of eutectic Si, the grain refinement and the supersaturation of Si. The hardness is further enhanced by Sr or Ce addition at extremely high cooling rate, especially for columnar and equiaxed zones, attributing to the modification effect on Si phase.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of pre-cold rolling on the evolution of microstructure, microtexture, and mechanical properties of the mushy state rolled in-situ Al-4.5Cu-5TiB2 composite

Highlights: • Microstructure-Microtexture evolution study of the mushy state rolled composite (MRC) and MRC with pre-cold rolling (PCMRC). • The Microstructure and microtexture were characterized using SEM, EBSD, and TEM. • Exactly opposite trends in micro-hardness variation across the thickness of MRC and PCMRC were discussed. • The PCMRC exhibited the best combination of hardness, strength, and ductility. • A proper microstructure-microtexture-property correlation was established with experimental evidence. The mushy state rolling has been found as a promising technique for near-net forming of the cast Al-4.5 wt% Cu-5 wt% TiB{sub 2} in-situ composite to obtain microstructural refinement and moderate mechanical properties. Cold rolling with 30% reduction in thickness was carried out before mushy state rolling, for achieving a relatively more homogeneous distribution of CuAl{sub 2}-TiB{sub 2} particles as well as an appropriate microstructure to enhance the mechanical properties. A comparative investigation on the microstructural and microtextural evolution, along with mechanical properties of both the mushy state rolled composite (MRC) and pre-cold rolled mushy-state rolled composite (PCMRC) was performed, and the microstructure-property correlation was established. The PCMRC exhibited the lowest homogenized lengthscale parameter (L{sub H} 29 μm) indicating the maximum uniformity of particle distribution, computed with the help of multi-scalar analysis of area fractions (MSAAF) technique. Electron back-scattered diffraction (EBSD) and transmission electron microscopy (TEM) studies revealed the presence of fine sub-grains within centrally located deformed Al grains due to dynamic recovery, as well as the particle stimulated nucleation of equiaxed fine Al grains by dynamic recrystallization or rapid solidification of liquid near edges for both the investigated composites. The PCMRC displayed a superior combination of hardness (96.82 ± 4.5 HV{sub 5kgf}), 40% higher ultimate tensile strength (301.4 ± 1.8 MPa), and 68% more uniform elongation (30.8% ± 0.5%), compared to the MRC. The improvement in mechanical properties is attributed to the uniform particle distribution and presence of both higher density of low angle boundaries and recrystallized grains adjacent to the particles, obtained from prior cold rolling.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Process-structure-property considerations for wire-based directed energy deposition of Ti-6Al-4V

Directed energy deposition (DED) is an attractive additive manufacturing (AM) process for large structural components. The rapid solidification and layer-by-layer process associated with DED results in non-ideal microstructures, such as large grains with strong crystallographic textures. These non-ideal microstructures can lead to severe anisotropy in the mechanical properties. Despite these challenges, DED has been identified as a potential solution for the manufacturing of near net shape Ti-6Al-4V preforms, replacing lost casting and forging capabilities. Two popular wire-based directed energy deposition (W-DED) processes were considered for the manufacturing of Ti-6Al-4V with assessments on their respective metallurgical and mechanical properties, as compared to a conventionally processed material. The two W-DED processes explored were wire arc additive manufacturing (WAAM) and electron beam additive manufacturing (EBAM). High throughput inspection and tensile testing procedures were utilized to generate statistically relevant data sets related to each process and sample orientation. The 2 AM technologies produced material with remarkably different microstructures and mechanical properties. Importantly, results revealed key differences in strength and ductility for the two disparate processes which were found to be related to differences in the metallurgical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Investigation of CO2 Sorption Characteristics of Imidazolium Ionic Liquid Crystals

This work is focused on advancing of the understanding the carbon dioxide (CO2) sorption characteristics of imidazolium ionic liquid crystals based on the 1-alkyl-3-methylimidazolium (Cnmim) ionic liquid family. Specifically, the mechanism of sorption across the melting, liquid crystal, and isotropic liquid transitions is investigated for 1-tetradecyl-3-methylimidazolium tetrafluoroborate (BF4-) and hexafluorophosphate (PF6-). A unique reversible CO2 occlusion was observed in 1-tetradecyl-3-methylimidazolium tetrafluoroborate (C14mim BF4) under rapid temperature quench from the liquid phases to the solid phase, while complete desorption occurred upon heating above the melting point (40 degrees C). In situ wide-angle x-ray scattering revealed that the lamellar structure of C14mim BF4 liquid crystal phases provides a high concentration of dynamically accessible anion and cation interaction sites for CO2, facilitating CO2 occlusion upon rapid solidification. The selective occlusion of CO2 in C14mim BF4 suggests a new mechanism for CO2 sorption processes.

08 HYDROGEN↗
DOE OSTI2022

Two-step deformation-induced martensitic transformation in additively manufactured High-Si stainless steel

Deformation-induced phase transformation in the additively manufactured (AM) Fe–18Cr–8Ni-5.5Si (in wt.%) alloy was analyzed using the in-situ electron backscattered diffraction (EBSD) record during uniaxial tensile testing in a scanning electron microscope (SEM). Analysis of EBSD data was focused to investigate phase transformation behavior during deformation with consideration of mechanical interactions among phases and grains in the ultrafine AM microstructure. The initial EBSD phase map illustrated that the as-built microstructure was a duplex structure consisting of major austenite (γ) and minor ferrite phases, some of which showed non-traditional orientation relationship since the rapid solidification in the AM process has produced non-equilibrium state in phase formation. In the deformed as-built AM alloy, the two-step martensitic transformation (γ→ε→α´) was identified as the main deformation-induced transformation mechanism. Martensitic transformation steps were found to be associated with glides of Shockley partial dislocations on closed packed (111) planes under the influence of atomic disturbance in the γ and ε phases, respectively. Using the closed-packed plane pole figures and unit cell orientations, their evolutions and mechanisms accompanying with the transformation were analyzed. Finally, the results indicate that one variant of ε-martensite forms from their parent γ phase, while two variants of α´ form from their parent ε phase.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Selective determination of grain size in the electrodeposition of nanocrystalline nickel foils

There are many synthesis methods through phase space to produce nanostructures in metals. Condensation methods with rapid solidification are extensively explored from the gas or liquid phase. In particular, electrodeposition using pulsed currents favors continuous nucleation in the processing of structures to produce free-standing sheets as well as protective coatings for surfaces. An analysis approach used to develop the method for refining the structure and surface finish for nanocrystalline gold-copper alloy coatings relates the energy in each deposition pulse to the constituent grain size that forms during growth. Application is now pursued to evaluate a select determination of the grain size for nanocrystalline nickel foils synthesized by pulsed electrodeposition. The mechanical behaviors of hardness and rate-sensitivity of strength are assessed as function of grain size.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Scalable Synthesis of Defect Abundant Si Nanorods for High-Performance Li-Ion Battery Anodes

Microsized nanostructured silicon–carbon composite is a promising anode material for high energy Li-ion batteries. However, large-scale synthesis of high-performance nano-Si materials at a low cost still remains a significant challenge. Here we report a scalable low cost method to synthesize Al/Na-doped and defect-abundant Si nanorods that have excellent electrochemical performance with high first-cycle Coulombic efficiency (90%). The unique Si nanorods are synthesized by acid etching the refined and rapidly solidified eutectic Al–Si ingot. To maintain the high electronic conductivity, a thin layer of carbon is then coated on the Si nanorods by carbonization of self-polymerized polydopamine (PDA) at 800 °C. The carbon coated Si nanorods (Si@C) electrode at 0.9 mg cm –2 loading (corresponding to area-specific-capacity of ~2.0 mAh cm –2 ) exhibits a reversible capacity of ~2200 mAh g –1 at 100 mA g –1 current, and maintains ~700 mAh g –1 over 1000 cycles at 1000 mA g –1 with a capacity decay rate of 0.02% per cycle. High Coulombic efficiencies of 87% in the first cycle and ~99.7% after 5 cycles are achieved due to the formation of an artificial Al 2 O 3 solid electrolyte interphase (SEI) on the Si surface, and the low surface area (31 m 2 g –1 ), which has never been reported before for nano-Si anodes. The excellent electrochemical performance results from the massive defects (twins, stacking faults, dislocations) and Al/Na doping in Si nanorods induced by rapid solidification and Na salt modifications; this greatly enhances the robustness of Si from the volume changes and alleviates the mechanical stress/strain of the Si nanorods during the lithium insertion/extraction process. Introducing massive defects and Al/Na doping in eutectic Si nanorods for Li-ion battery anodes is unexplored territory. We venture this uncharted territory to commercialize this nanostructured Si anode for the next generation of Li-ion batteries.

25 ENERGY STORAGE↗
DOE OSTI2024

Critical role of slags in pitting corrosion of additively manufactured stainless steel in simulated seawater

Abstract Pitting corrosion in seawater is one of the most difficult forms of corrosion to identify and control. A workhorse material for marine applications, 316L stainless steel (316L SS) is known to balance resistance to pitting with good mechanical properties. The advent of additive manufacturing (AM), particularly laser powder bed fusion (LPBF), has prompted numerous microstructural and mechanical investigations of LPBF 316L SS; however, the origins of pitting corrosion on as-built surfaces is unknown, despite their utmost importance for certification of LPBF 316L SS prior to fielding. Here, we show that Mn-rich silicate slags are responsible for pitting of the as-built LPBF material in sodium chloride due to their introduction of deleterious defects such as cracks or surface oxide heterogeneities. In addition, we explain how slags are formed in the liquid metal and deposited at the as-built surfaces using high-fidelity melt pool simulations. Our work uncovers how LPBF changes surface oxides due to rapid solidification and high-temperature oxidation, leading to fundamentally different pitting corrosion mechanisms.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Real-time monitoring of laser powder bed fusion process using high-speed X-ray imaging and diffraction

Here, we employ the high-speed synchrotron hard X-ray imaging and diffraction techniques to monitor the laser powder bed fusion (LPBF) process of Ti-6Al-4V in situ and in real time. We demonstrate that many scientifically and technologically significant phenomena in LPBF, including melt pool dynamics, powder ejection, rapid solidification, and phase transformation, can be probed with unprecedented spatial and temporal resolutions. In particular, the keyhole pore formation is experimentally revealed with high spatial and temporal resolutions. The solidification rate is quantitatively measured, and the slowly decrease in solidification rate during the relatively steady state could be a manifestation of the recalescence phenomenon. The high-speed diffraction enables a reasonable estimation of the cooling rate and phase transformation rate, and the diffusionless transformation from β to α’ phase is evident. The data present here will facilitate the understanding of dynamics and kinetics in metal LPBF process, and the experiment platform established will undoubtedly become a new paradigm for future research and development of metal additive manufacturing.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

The structure and properties of boron carbide ceramics modified by high-current pulsed electron-beam

The present work is devoted to numerical simulation of temperature fields and the analysis of structural and strength properties of the samples surface layer of boron carbide ceramics treated by the high-current pulsed electron-beam of the submillisecond duration. The samples made of sintered boron carbide ceramics are used in these investigations. The problem of calculating the temperature field is reduced to solving the thermal conductivity equation. The electron beam density ranges between 8…30 J/cm{sup 2}, while the pulse durations are 100…200 μs in numerical modelling. The results of modelling the temperature field allowed ascertaining the threshold parameters of the electron beam, such as energy density and pulse duration. The electron beam irradiation is accompanied by the structural modification of the surface layer of boron carbide ceramics either in the single-phase (liquid or solid) or two-phase (solid-liquid) states. The sample surface of boron carbide ceramics is treated under the two-phase state (solid-liquid) conditions of the structural modification. The surface layer is modified by the high-current pulsed electron-beam produced by SOLO installation at the Institute of High Current Electronics of the Siberian Branch of the Russian Academy of Sciences, Tomsk, Russia. The elemental composition and the defect structure of the modified surface layer are analyzed by the optical instrument, scanning electron and transmission electron microscopes. Mechanical properties of the modified layer are determined measuring its hardness and crack resistance. Research results show that the melting and subsequent rapid solidification of the surface layer lead to such phenomena as fragmentation due to a crack network, grain size reduction, formation of the sub-grained structure due to mechanical twinning, and increase of hardness and crack resistance.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Ultra-soft magnetic properties and correlated phase analysis by {sup 57}Fe Mössbauer spectroscopy of Fe{sub 74}Cu{sub 0.8}Nb{sub 2.7}Si{sub 15.5}B{sub 7} alloy

A detailed study of magnetic softness has been performed on FINEMENT type of ribbons by investigating the BH loop with maximum applied field of 960 A/m. The ribbon with the composition of Fe{sub 74}Cu{sub 0.8}Nb{sub 2.7}Si{sub 15.5}B{sub 7} was synthesized by rapid solidification technique and the compositions volume fraction was controlled by changing the annealing condition. Detail phase analysis was performed through X-ray diffraction (XRD), Differential scanning calorimetry (DSC), Vibrating sample magnetometer (VSM) and Mössbauer spectroscopy in order to correlate the ultrasoft magnetic properties with the volume fraction of amorphous and α-Fe(Si) soft nano composites. Bright (BF) and dark field (DF) image with selective area diffraction (SAD) patterns by the transmission electron microscopy (TEM) of the sample annealed for the optimized annealed condition at 853 K for 3 min reveals nanocrystals with an average size between 10-15 nm possessing the bcc structure which matches with the grain size revealed by the X-ray diffraction. Kinetics of crystallization of α-Fe(Si) phases has been determined by DSC curves. Extremely small coercivity of 30.9 A/m and core loss of 2.5 W/Kg for the sample annealed at 853 K for 3 min was found. Similar values for other crystalline conditions were determined by using BH loop tracer with a maximum applied field of around 960 A/m. Mössbauer spectroscopy was used to determine chemical shift, hyperfine field distribution (HFD), and peak width of different phases. The volume fractions of the relative amount of amorphous and crystalline phases are also determined by Mössbauer spectroscopy. High saturation magnetization along with ultrasoft magnetic properties exhibits very high potentials technological applications.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effect of layer thickness on device response of silicon heavily supersaturated with sulfur

We report on a simple experiment in which the thickness of a hyperdoped silicon layer, supersaturated with sulfur by ion implantation followed by pulsed laser melting and rapid solidification, is systematically varied at constant average sulfur concentration, by varying the implantation energy, dose, and laser fluence. Contacts are deposited and the external quantum efficiency (EQE) is measured for visible wavelengths. We posit that the sulfur layer primarily absorbs light but contributes negligible photocurrent, and we seek to support this by analyzing the EQE data for the different layer thicknesses in two interlocking ways. In the first, we use the measured concentration depth profiles to obtain the approximate layer thicknesses, and, for each wavelength, fit the EQE vs. layer thickness curve to obtain the absorption coefficient of hyperdoped silicon for that wavelength. Comparison to literature values for the hyperdoped silicon absorption coefficients [S.H. Pan et al. Applied Physics Letters 98, 121913 (2011)] shows good agreement. Next, we essentially run this process in reverse; we fit with Beer’s law the curves of EQE vs. hyperdoped silicon absorption coefficient for those wavelengths that are primarily absorbed in the hyperdoped silicon layer, and find that the layer thicknesses obtained from the fit are in good agreement with the original values obtained from the depth profiles. We conclude that the data support our interpretation of the hyperdoped silicon layer as providing negligible photocurrent at high S concentrations. This work validates the absorption data of Pan et al. [Applied Physics Letters 98, 121913 (2011)], and is consistent with reports of short mobility-lifetime products in hyperdoped layers. It suggests that for optoelectronic devices containing hyperdoped layers, the most important contribution to the above band gap photoresponse may be due to photons absorbed below the hyperdoped layer.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

Influence of minor Ce additions on magnetic and electrical properties in Fe–6.5 wt. % Si alloy

Fe–6.5 wt. % Si alloys exhibit lower core loss at higher frequency than the dominating electrical steel containing 3.2% Si due to its lower magneto-crystalline anisotropy energy (MAE) and higher electrical resistivity. However, compared to nanocrystalline and amorphous soft-magnetic materials, 6.5% Si steel, although being cost effective and having high saturation magnetization, still has much to improve, especially with respect to MAE and resistivity. To explore further improvement, the effects of minor Ce additions (due to its mixed valence 4f-electron configuration) on the microstructure, electrical and magnetic behaviors of Fe–6.5 wt. % Si alloys were investigated. Due to its limited solubility in Fe, Ce exhibits condition-dependent effects on electrical resistivity, showing only marginal improvement under rapid solidification. In contrast, Ce addition degrades magnetic performance, reducing saturation magnetization (from 1.86 to 1.76 T) and increasing coercivity (from 88 to 171 A/m), which results in an 83.4% increase in core loss (W 10/1000 condition). Overall, Ce addition provides limited benefit in electrical resistivity while deteriorating magnetic properties, making it ineffective for enhancing the soft magnetic performance of Fe–6.5 wt. % Si alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Ultrahigh strength and plasticity in laser rapid solidified Al–Si nanoscale eutectics

As-cast Al–20wt.% Si alloys were processed via laser rapid solidification (LRS) techniques to create eutectic microstructures with nanoscale interconnected, nanotwinned Si fibers. LRS morphologies exhibit higher flow stress, exceeding 800 MPa and uniform plastic deformation above 20% compared to as-cast alloy that fractures at strains below 8% at flow strength of approximately 200 MPa. The strengthening mechanisms of LRS morphologies are interpreted in terms of the interfacial constraints: increase in yield strength as well as strain hardening rate due to nanoscale confined slip in fibrous Al–Si eutectic, and load transfer and eventual plasticity in the nanoscale Si fibers.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Beyond the eutectic paradigm: nanolamellar patterns in a rapidly solidified peritectic alloy

Peritectic transformations are central to many structural alloys, yet pattern formation remains poorly understood due to complex growth dynamics and limited three-dimensional data. Here, we report an unusual two-phase microstructure in a Zn–Ag peritectic alloy subjected to rapid solidification by laser surface remelting. Synchrotron X-ray nanotomography reveals a lamellar structure of primary 𝜀-AgZn 3 and peritectic Zn with ∼700 nm spacing. Although resembling a eutectic morphology, this pattern forms without a eutectic reaction through non-steady coupled growth from the liquid. SEM and TEM-EDS confirm interface shapes and phase compositions. These findings expand the design space of peritectics for refined microstructural control.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Modeling mechanical behavior of an additively manufactured metal structure with local texture variations: a study on model form error

Here, the repetitive rapid solidification that occurs in metal additive manufacturing (AM) processes creates microstructures distinctly different from wrought materials. Local variability in AM microstructures (either by design or unintentional) raises questions as to how AM structures should be modeled at the part-scale to minimize modeling error. The key goal of this work is to demonstrate a posteriori error estimation applied to an AM part. It is assumed that the actual microstructure is unknown and an approximate, spatially uniform material model is used. Error bounds are calculated for many reference models based on AM microstructures with elongated grain morphology and localized or global fiber textures during a post-processing step. The current findings promote confidence that a posteriori model form error estimation could be used effectively in mechanical performance simulations of AM parts to quickly obtain quantitative error metrics between an approximate model result and many microstructure-based reference models. The a posteriori error estimation introduces significant time savings compared to computing the full reference model solutions. Tight bounds on model form error are obtained when texture variations in the reference models occur on large length scales. For materials with property variation at small length scales, multi-scale error estimation techniques are needed to properly account for the many interfaces present between areas with different properties.

36 MATERIALS SCIENCE↗