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Results for “spinodal decomposition”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Precipitation-site competition in duplex stainless steels: Cu clusters vs spinodal decomposition interfaces as nucleation sites during thermal aging

Competing microstructural evolution mechanisms can exist simultaneously when duplex stainless steels are operating for several decades in a high temperature service environment. Such competition between different microstructural evolution pathways can be difficult to ascertain using simple model alloy systems necessitating detailed structural and compositional analysis of phase transformation mechanisms in complex alloys Thus, in this study duplex stainless steels with complex but well understood chemistries were used to investigate the relative importance of different heterogeneous nucleation sites – specifically spinodal decomposition and Cu clustering – on precipitation of Ni-Si-Mn particles during long term thermal aging. Precipitation of Ni-Si-Mn particles in duplex stainless steels and ferritic steels during thermal aging and irradiation is known to have profound effect on mechanical properties. Using duplex stainless steels with custom modified compositions along with atom probe tomography characterization and first-passage kinetic Monte Carlo (FPKMC) simulations it is revealed that while the interface between Cr and Fe formed during spinodal decomposition can be a pathway for diffusion of Ni, Si, Mn, and Cu, it is not a site that encourages precipitation of Ni-Si-Mn rich particles. Instead, the presence of a higher concentration of Cu in these steels leads to formation of small Cu clusters with high energy interfaces that act as nucleation sites for Ni-Si-Mn particles because of its strong interaction particularly with Ni increasing the chemical driving force for precipitation. These results will help inform predictive models for the use of duplex stainless steels and other precipitation-hardened alloys for extended operation at high temperatures.

Duplex stainless steel, Thermal aging, Precipitati↗
DOE OSTI2016

High thermoelectric performance of n-type PbTe 1-y S y due to deep lying states induced by indium doping and spinodal decomposition

Good thermoelectric materials should have high engineering figure-of-merit (ZT) eng , not peak ZT, to achieve high conversion efficiency. In this work, we achieved a good (ZT) eng by optimizing the carrier concentration to improve the room temperature ZT using deep lying dopant, indium, in PbTe 1-y S y . It was found that a room temperature ZT as high as ~0.5 and a peak ZT ~1.1 at about 673 K were obtained in Pb 0.98 In 0.02 Te 0.8 S 0.2 due to a lower thermal conductivity by alloy scattering and Spinodal decomposition. The calculated efficiency could be as high as ~12% at cold side 323 K and hot side 773 K. The approach is expected to work in other materials systems too.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

The Effect of Nonisothermality on the Early Stages of Spinodal Decomposition

A nonisothertmal model of spinodal decomposition is proposed for a binary system described by the Ginzburg–Landau energy. The initial stages of spinodal decomposition are investigated for a system of simultaneous equations describing the impurity and temperature redistribution. The dispersion equation and the instability growth rate of spinodal structures are obtained. The temperature dependence of the growth rate and the wave number corresponding to the maximum instability is found. The observed difference in the dispersion relations of isothermal and nonisothermal models shows that a criterion for the effect of temperature fluctuations on the spinodal decomposition is given by a dimensionless parameter Γ; for large values of Γ (Γ ≥ 1000), temperature fluctuations in the form of noise are certainly insufficient for spinodal decomposition due to a change in the dispersion structure of the equations, which suggests the need to take into account the nonisothermal behavior of the system.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

A high-resolution analytical scanning transmission electron microscopy study of the early stages of spinodal decomposition in binary Fe–Cr

Spinodal decomposition (SD) is an important phenomenon in materials science and engineering. For example, it is considered to be responsible for the 475 °C embrittlement of stainless steels comprising the bcc (ferrite) or bct (martensite) phases. Structural characterization of the evolving minute nano-scale concentration fluctuations during SD in the Fe–Cr system is, however, a notable challenge, and has mainly been considered accessible via atom probe tomography (APT) and small-angle neutron scattering. The standard tool for nanostructure characterization, viz. transmission electron microscopy (TEM), has only been successfully applied to late stages of SD when embrittlement is already severe. However, we here demonstrate that the structural evolution in the early stages of SD in binary Fe–Cr, and alloys based on the binary, are accessible via analytical scanning TEM. An Fe–36 wt% Cr alloy aged at 500 °C for 1, 10 and 100 h is investigated using an aberration-corrected microscope and it is found that highly coherent and interconnected Cr-rich regions develop. The wavelength of decomposition is rather insensitive to the sample thickness and it is quantified to 2, 3 and 6 nm after ageing for 1, 10 and 100 h, which is in reasonable agreement with prior APT analysis. The concentration amplitude is more sensitive to the sample thickness and acquisition parameters but the TEM analysis is in good agreement with APT analysis for the longest ageing time. These findings open up for combinatorial TEM studies where both local crystallography and chemistry is required. - Highlights: • STEM-EELS analysis was successfully applied to resolve early stage SD in Fe–Cr. • Compositional wavelength measured with STEM-EELS compares well to previous ATP studies. • Compositional amplitude measured with STEM-EELS is a function of experimental parameters. • STEM-EELS allows for combinatorial studies of SD using complementary techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2021

A Polymer-Assisted Spinodal Decomposition Strategy toward Interconnected Porous Sodium Super Ionic Conductor-Structured Polyanion-Type Materials and Their Application as a High-Power Sodium-Ion Battery Cathode

A general polymer-assisted spinodal decomposition strategy is used to prepare hierarchically porous sodium super ionic conductor (NASICON)-structured polyanion-type materials (e.g., Na 3 V 2 (PO 4 ) 3 , Li 3 V 2 (PO 4 ) 3 , K 3 V 2 (PO 4 ) 3 , Na 4 MnV(PO 4 ) 3 , and Na 2 TiV(PO 4 ) 3 ) in a tetrahydrofuran/ethanol/H 2 O synthesis system. Depending on the boiling point of solvents, the selective evaporation of the solvents induces both macrophase separation via spinodal decomposition and mesophase separation via self-assembly of inorganic precursors and amphiphilic block copolymers, leading to the formation of hierarchically porous structures. We find that the resulting hierarchically porous Na 3 V 2 (PO 4 ) 3 possessing large specific surface area (≈77 m 2 g -1 ) and pore volume (≈0.272 cm 3 g -1 ) shows a high specific capacity of 117.6 mAh g -1 at 0.1 C achieving the theoretical value and a long cycling life with 77% capacity retention over 1000 cycles at 5 C. This method presented here can open a facile avenue to synthesize other hierarchically porous polyanion-type materials.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Evolution of the role of molybdenum in duplex stainless steels during thermal aging: From enhancing spinodal decomposition to forming heterogeneous precipitates

Thermal aging of ferrite in duplex stainless steels leads to a complex microstructural evolution that can give way to large deleterious changes in mechanical properties. The microstructural evolution mechanisms that happen concurrently are strongly linked to minor changes in composition. By characterizing duplex stainless steels with various compositions over a range of aging conditions, it was revealed that adding a modest amount of Mo to cast austenitic stainless steel (such as changing from grade CF3 to grade CF3M) not only increases the kinetics of spinodal decomposition and Ni-Si-Mn-rich G-phase precipitation, but it also forms a separate Mo-rich phase. At shorter equivalent aging times, Mo segregates from Fe and towards Cr accelerating spinodal decomposition. At longer aging times, Mo enriches in the Ni-Si-Mn clusters before phase separating into an adjoined Mo-rich cluster. We found that these phase changes and precipitation events result in a rather steep drop in fracture and impact toughness. These results will inform the design of similar alloys for use at high temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Surface Modes of Coherent Spinodal Decomposition

Here, we use linear stability theory and numerical simulations to show that spontaneous phase separation in elastically coherent solids is fundamentally altered by the presence of free surfaces. Because of misfit stress relaxation near surfaces, phase separation is mediated by unique surface modes of spinodal decomposition that have faster kinetics than bulk modes and are unstable even when spinodal decomposition is suppressed in the bulk. Consequently, in the presence of free surfaces, the limit of metastability of supersaturated solid solutions of crystalline materials is shifted from the coherent to chemical spinodal.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Non-equilibrium theory of arrested spinodal decomposition

The non-equilibrium self-consistent generalized Langevin equation theory of irreversible relaxation [P. E. Ramŕez-González and M. Medina-Noyola, Phys. Rev. E 82, 061503 (2010); 82, 061504 (2010)] is applied to the description of the non-equilibrium processes involved in the spinodal decomposition of suddenly and deeply quenched simple liquids. For model liquids with hard-sphere plus attractive (Yukawa or square well) pair potential, the theory predicts that the spinodal curve, besides being the threshold of the thermodynamic stability of homogeneous states, is also the borderline between the regions of ergodic and non-ergodic homogeneous states. It also predicts that the high-density liquid-glass transition line, whose high-temperature limit corresponds to the well-known hard-sphere glass transition, at lower temperature intersects the spinodal curve and continues inside the spinodal region as a glass-glass transition line. Within the region bounded from below by this low-temperature glass-glass transition and from above by the spinodal dynamic arrest line, we can recognize two distinct domains with qualitatively different temperature dependence of various physical properties. We interpret these two domains as corresponding to full gas-liquid phase separation conditions and to the formation of physical gels by arrested spinodal decomposition. The resulting theoretical scenario is consistent with the corresponding experimental observations in a specific colloidal model system.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Self-Assembled, Nanostructured, Tunable Metamaterials via Spinodal Decomposition

Self-assembly via nanoscale phase separation offers an elegant route to fabricate nanocomposites with physical properties unattainable in single-component systems. One important class of nanocomposites are optical metamaterials which exhibit exotic properties and lead to opportunities for agile control of light propagation. Such metamaterials are typically fabricated via expensive and hard-to-scale top-down processes requiring precise integration of dissimilar materials. In turn, there is a need for alternative, more efficient routes to fabricate large-scale metamaterials for practical applications with deep-subwave length resolution. Here, we demonstrate a bottom-up approach to fabricate scalable nanostructured metamaterials via spinodal decomposition. To demonstrate the potential of such an approach, we leverage the innate spinodal decomposition of the VO 2 -TiO 2 system, the metal-to-insulator transition in VO 2 , and thin-film epitaxy, to produce self-organized nanostructures with coherent interfaces and a structural unit cell down to 15 nm (tunable between horizontally and vertically aligned lamellae) wherein the iso-frequency surface is temperature-tunable from elliptic to hyperbolic dispersion producing metamaterial behavior. These results provide an efficient route for the fabrication of nanostructured metamaterials and other nanocomposites for desired functionalities.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Mechanochemical spinodal decomposition: a phenomenological theory of phase transformations in multi-component, crystalline solids

Here, we present a phenomenological treatment of diffusion-driven martensitic phase transformations in multi-component crystalline solids that arise from non-convex free energies in mechanical and chemical variables. The treatment describes diffusional phase transformations that are accompanied by symmetry-breaking structural changes of the crystal unit cell and reveals the importance of a mechanochemical spinodal, defined as the region in strain-composition space, where the free-energy density function is non-convex. The approach is relevant to phase transformations wherein the structural order parameters can be expressed as linear combinations of strains relative to a high-symmetry reference crystal. The governing equations describing mechanochemical spinodal decomposition are variationally derived from a free-energy density function that accounts for interfacial energy via gradients of the rapidly varying strain and composition fields. A robust computational framework for treating the coupled, higher-order diffusion and nonlinear strain gradient elasticity problems is presented. Because the local strains in an inhomogeneous, transforming microstructure can be finite, the elasticity problem must account for geometric nonlinearity. An evaluation of available experimental phase diagrams and first-principles free energies suggests that mechanochemical spinodal decomposition should occur in metal hydrides such as ZrH 2-2c . The rich physics that ensues is explored in several numerical examples in two and three dimensions, and the relevance of the mechanism is discussed in the context of important electrode materials for Li-ion batteries and high-temperature ceramics.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Unconditionally energy stable time stepping scheme for Cahn–Morral equation: Application to multi-component spinodal decomposition and optimal space tiling

An unconditionally energy stable time stepping scheme is introduced to solve Cahn–Morral-like equations in the present study. It is constructed based on the combination of David Eyre's time stepping scheme and Schur complement approach. Although the presented method is general and independent of the choice of homogeneous free energy density function term, logarithmic and polynomial energy functions are specifically considered in this paper. The method is applied to study the spinodal decomposition in multi-component systems and optimal space tiling problems. A penalization strategy is developed, in the case of later problem, to avoid trivial solutions. Extensive numerical experiments demonstrate the success and performance of the presented method. According to the numerical results, the method is convergent and energy stable, independent of the choice of time stepsize. Its MATLAB implementation is included in the appendix for the numerical evaluation of algorithm and reproduction of the presented results. -- Highlights: •Extension of Eyre's convex–concave splitting scheme to multiphase systems. •Efficient solution of spinodal decomposition in multi-component systems. •Efficient solution of least perimeter periodic space partitioning problem. •Developing a penalization strategy to avoid trivial solutions. •Presentation of MATLAB implementation of the introduced algorithm.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2022

In-Situ Study of Microstructure Evolution of Spinodal Decomposition in an Al-Rich High-Entropy Alloy

High-entropy alloys (HEAs) are materials which leverage the entropy of mixing to motivate the formation of single-phase solid solutions, even of immiscible elements. While these materials are well-recognized for their application to structural engineering, there is increasing interest in the use of HEAs for functional applications such as memory storage and energy devices. The current work investigates the HEA Al 1.3 CoCrCuFeNi, which has been previously shown to be single-phase at high temperatures, but undergoes phase separation at lower temperatures, transforming the structural and the functional properties. This phase separation is investigated at high temperatures with in-situ small angle neutron scattering (SANS) and scanning transmission electron microscopy (EDS). These techniques show that increasing the temperature up to 800°C, the microstructure of the HEA adiabatically disorders and abruptly homogenizes near 700°C, which is consistent with spinodal decomposition. Overall, the microstructural evolution proceeds mainly by the atomistic redistribution of the constituent elements within simple crystal lattices, producing coherent phase mixtures.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Detecting Thermally-Induced Spinodal Decomposition with Picosecond Ultrasonics in Cast Austenitic Stainless Steels

Destructive techniques to monitor nuclear reactor component health may not always be available during service, as they are time-consuming and often require pre-installed inspection coupons. Non-destructive evaluation (NDE) techniques can bridge this gap by rapidly identifying the state of mission-critical reactor components, via inference between NDE-measurable material properties and those of ultimate interest, such as ductility and toughness. Here, we demonstrate one such inference about the health of thermally aged cast austenitic stainless steels. Observations of surface acoustic wave peak (SAW) splitting correlate with spinodal decomposition-induced embrittlement as destructively measured by Charpy impact energy. Elastodynamic calculations and molecular dynamics simulations of the effects of spinodal decomposition on elastic moduli support that the new acoustic modes present are due to stiffening in the δ-ferrite domains. Finally, this discovery enables one to probe structure-property relationships in materials in a greatly accelerated manner, suggesting that similar inference methods can be used to determine material fitness-for-service, or to quickly uncover new structure-property relationships.

304-type stainless steel↗
DOE OSTI2015

Early stages of spinodal decomposition in Fe–Cr resolved by in-situ small-angle neutron scattering

In-situ, time-resolved small-angle neutron scattering (SANS) investigations of the early stages of the spinodal decomposition process in Fe–35Cr were performed at 773 and 798 K. The kinetics of the decomposition, both in terms of characteristic distance and peak intensity, followed a power-law behaviour from the start of the heat treatment (a′{sup }= 0.10–0.11 and a″ = 0.67–0.86). Furthermore, the method allows tracking of the high–Q slope, which is a sensitive measure of the early stages of decomposition. Ex-situ SANS and atom probe tomography were used to verify the results from the in-situ investigations. Finally, the in-situ measurement of the evolution of the characteristic distance at 773 K was compared with the predictions from the Cahn-Hilliard-Cook model, which showed good agreement with the experimental data (a′{sup }= 0.12–0.20 depending on the assumed mobility)

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2011

Spinodal Decomposition of Ga{sub x}In{sub 1-x}As{sub y}P{sub 1-y}Quaternary Alloys

Using X-ray structural analysis, scanning electron microscopy, atomic force microscopy, and photoluminescent spectroscopy, it is shown that it is possible to obtain a small-scale domain structure on the surface of liquid-phase epitaxial heterostructures. The domain structure emerges as a result of spinodal decomposition of the Ga{sub x}In{sub 1-x}As{sub y}P{sub 1-y} quaternary alloy due to immiscibility of its components and relaxation of its lattice parameter to surrounding layers.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Impact of symmetry energy on sound speed and spinodal decomposition in dense neutron-rich matter

Using a meta model for nuclear Equation of State (EOS) with its parameters constrained by astrophysical observations and terrestrial nuclear experiments, we examine effects of nuclear EOS especially its symmetry energy $E$ sym ($ρ$) term on the speed of sound squared $C$ $^2_s$($ρ$) and the critical density ρt where $C$ $^2_s$($ρ_t$) vanishes (indicating the onset of spinodal decomposition) in both dense neutron-rich nucleonic matter relevant for relativistic heavy-ion collisions and the cold $n$ + $p$ + $e$ + $μ$ matter in neutron stars at $β$- equilibrium. Unlike in nucleonic matter with fixed values of the isospin asymmetry $δ$, in neutron stars with a density dependent isospin profile $δ$($ρ$) determined consistently by the $β$-equilibrium and charge neutrality conditions, the $C$ $^2_s$($ρ$) almost always show a peak and then vanishes at $ρ_t$. Furthermore, the latter strongly depends on the high-density behavior of $E$ sym ($ρ$) if the skewness parameter $J$ 0 characterizing the stiffness of high-density symmetric nuclear matter (SNM) EOS is not too far above its currently known most probable value of about -190 MeV inferred from recent Bayesian analyses of neutron star observables. Moreover, in the case of having a super-soft $E$ sym ($ρ$) that is decreasing with increasing density above about twice the saturation density of nuclear matter, the $ρ$ $t$ is significantly lower than the density where the $E$ sym ($ρ$) vanishes (indicating the onset of isospin-separation instability and pure neutron matter formation) in neutron star cores.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2020

Detecting Thermally Induced Spinodal Decomposition with Picosecond Ultrasonics in Cast Austenitic Stainless Steels

Given the existential climate crisis faced by mankind and the world, the lifetime and sustainability of nuclear reactors as a carbon-free source of renewable energy depend on the susceptibility of their structural components to environmental degradation. In particular, critical components for light water reactors (LWRs) evolve over decades in service, losing ductility and toughness due to thermal and irradiation aging. Techniques to monitor their health cannot be easily applied in the field due to their destructive, expensive, or immobile nature. Thus, non-destructive evaluation (NDE) methods are sought to monitor and evaluate the health of major LWR components such as core barrels, steam generator tubes, or primary coolant pipes and are often required by policy, such as NRC policy #10-CFR-50.65. In this work we demonstrate the use of gigahertz, non-contact ultrasonics to gauge the state of cast austenitic stainless steels (CASS), used in some of the largest components in LWR primary systems. We do so by linking changes in their surface acoustic wave (SAW) characteristics using transient grating spectroscopy (TGS) to transmission electron microscopy (TEM)-verified evidence of spinodal decomposition and G-phase precipitation. In this thesis, thermal aging is shown to induce SAW peak splitting in spinodally decomposed CASS alloys, correlated strongly with lowered toughness and decreased ductility. Furthermore, statistical testing on the number of SAW peak splits observed show that the second SAW peak significantly appears more frequently and is significantly different in frequency in comparison to counts and frequencies measured in unaged specimens. The ability of this technique to non-destructively detect microstructural degradation at a distance in a predictive manner in the case of CASS motivates extending gigahertz ultrasonics to detect other LWR material degradation modes as an in-vessel inspection technique, such as reactor pressure vessel (RPV) embrittlement. This allows for the greater use of NDE techniques for confident monitoring of LWR structural material health to 80 years and beyond, saving costs by minimizing structural replacements until needed and maximizing energy production by preventing early decommission until necessary.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Spinodal Decomposition in InSb/AlAs Heterostructures

The atomic structure and energy spectrum of heterostructures formed in a system of InAs/AlAs binary compounds are studied. The In{sub x}Al{sub 1–x}Sb{sub y}As{sub 1–y} alloy, from which quantum wells are formed in InSb/AlAs structures, decomposes into two phases with different compositions. The characteristic dimensions of regions containing separate phases of the alloy in the structure plane are 5–7 nm. Spinodal decomposition of the alloy brings about the formation of coexisting indirect-gap regions with type-I and type-II energy spectra in quantum wells of the heterostructures.

36 MATERIALS SCIENCE↗