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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 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Phase Pattern Formation in Grain Boundaries

Here, in this Letter, we derive conditions that predict the existence of two-phase periodic-pattern grain boundary structures that are stable against coarsening. While previous research has established that elastic effects can lead to phase pattern formation on crystal surfaces, the possibility of stable grain boundary structures composed of alternating grain boundary phases has not been previously analyzed. Our theory identifies the specific combination of grain boundary and materials properties that enable the emergence of patterned grain boundary states and shows that the dislocation content of grain boundary phase junctions, absent in surface phenomena, weakens the stability of the patterned structures. The predictions of the theory are tested using a model copper grain boundary that exhibits multiple phases and two-phase pattern formation. We discuss how, similarly to surfaces, elastic effects associated with grain boundary phase junctions have profound implications for how grain boundary phases transform.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Complexions at the iron-magnetite interface

Synthesizing distinct phases and controlling crystalline defects are key concepts in materials design. These approaches are often decoupled, with the former grounded in equilibrium thermodynamics and the latter in nonequilibrium kinetics. By unifying them through defect phase diagrams, we can apply phase equilibrium models to thermodynamically evaluate defects—including dislocations, grain boundaries, and phase boundaries—establishing a theoretical framework linking material imperfections to properties. Using scanning transmission electron microscopy (STEM) with differential phase contrast (DPC) imaging, we achieve the simultaneous imaging of heavy Fe and light O atoms, precisely mapping the atomic structure and chemical composition at the iron-magnetite (Fe/Fe 3 O 4 ) interface. We identify a well-ordered two-layer interface-stabilized phase state (referred to as complexion) at the Fe[001]/Fe 3 O 4 [001] interface. Using density-functional theory (DFT), we explain the observed complexion and map out various interface-stabilized phases as a function of the O chemical potential. The formation of complexions increases interface adhesion by 20% and alters charge transfer between adjacent materials, impacting transport properties. Our findings highlight the potential of tunable defect-stabilized phase states as a degree of freedom in materials design, enabling optimized corrosion protection, catalysis, and redox-driven phase transitions, with applications in materials sustainability, efficient energy conversion, and green steel production.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Data-Efficient Methods for Determining Flory–Huggins χ Parameters in Multicomponent Polymer Formulations

Polymer formulations are essential in diverse applications including personal care products, coatings, paints, adhesives, and plastic materials. Designing these formulations requires navigating large, complex design spaces, where phase and self-assembly behavior critically impact performance. The Flory–Huggins χ parameter, which quantifies segmental miscibility, is widely used to parametrize the excess free energy of mixing in formulation models. In this work, we introduce two data-efficient, top-down methods for estimating χ parameters using the Random Phase Approximation (RPA): (i) Boundary Nonlinear Regression (Boundary-NLR), which fits theoretical spinodal boundaries to experimental phase boundaries, and (ii) Surrogate Model Inverse Parameter Estimation (SMIPE), which uses a Gaussian Process Classifier to fit sparse phase maps via a surrogate model. Both methods allow rapid parametrization of polymer field-theoretic models without the need for additional experiments. We evaluate these approaches on data sets involving polymer–solvent–nonsolvent ternary mixtures and block copolymer–solvent systems, demonstrating their robustness to experimental noise and their relevance for real-world formulation design.

copolymers↗
NASA NTRS2000

Solid Freeform Fabrication of Continuous Fiber Reinforced Composites for Propulsion Applications

For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500'C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible- manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. This is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths With carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites-, they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP process.

Vaidyanathan, R.↗
NASA NTRS2001

Solid Free-Form Fabrication of Continuous Fiber Reinforced Composites for Propulsion Application

For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500 C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible-manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. M is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths with carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites; they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP processes.

Vaidyanathan, R.↗
NASA NTRS1976

Vacuum thermal-mechanical fatigue behavior of two iron-base alloys

The present study extends the concept of in-phase grain boundary ratcheting to two iron-base alloys (Type 304 stainless steel and A286 alloy) and provides a clearer interpretation of out-of-phase grain boundary ratcheting effects observed in the A286 alloy which does not exhibit geometric instability. Elevated-temperature low-cycle thermal-mechanical fatigue tests in an ion-pumped ultrahigh vacuum chamber revealed significant effects of frequency and combined temperature-strain cycling on fatigue life. In-phase thermal cycling (tension at high temperature and compression at low temperature) caused large life reductions in both materials due to grain boundary cavitation caused by unreversed grain boundary sliding (grain boundary ratcheting). Out-of-phase thermal cycling (tension at low temperature and compression at high temperature) also caused large cyclic life reductions in both materials. In the A286 alloy, out-of-phase life reductions are attributed to compressive ratcheting.

Sheffler, K. D.↗
DOE OSTI2025

Nucleation and Growth of Blue Phase 3D Cubic Structure Under Continuously Changing Curved Boundary Conditions

The blue phase of liquid crystals (BPLCs) with a cubic lattice of disclination lines and 3D nanostructure enables the modulation of photonic bandgap thus casting them in the category of photonic crystals. Its unique nature promises applications in display technologies, electro‐optics, and sensors. To integrate these ordered materials into wearable devices a fundamental understanding of curvature, and spatial confinement is necessary. Although continuous confinement in flat geometries have been studied, confining curvature has shown to induce strong destabilization effects on the cubic structure and formation of topological defects, thereby deteriorating their optical performance. Moreover, limitations in controlling the curvature of droplets further hinder studies of nucleation and growth of BPLCs. Here, to address these challenges, micro‐scale patterned surfaces of concentric cylinders are exploited to systematically control curvatures. The impact of curvature on the confined BPLCs is revealed in terms of phase transition temperature, nucleation and growth, morphology, as well as phase transformation. This research offers valuable insights into the stability, and structural characteristics of BPLCs in adaptive photonic devices, paving the way for future advancements in flexible displays, sensors, and other technologies leveraging liquid crystal (LC) materials.

3D Cubic Structure↗
NASA NTRS1988

The high temperature creep deformation of Si3N4-6Y2O3-2Al2O3

The creep properties of silicon nitride containing 6 wt percent yttria and 2 wt percent alumina have been determined in the temperature range 1573 to 1673 K. The stress exponent, n, in the equation epsilon dot varies as sigma sup n, was determined to be 2.00 + or - 0.15 and the true activation energy was found to be 692 + or - 25 kJ/mol. Transmission electron microscopy studies showed that deformation occurred in the grain boundary glassy phase accompanied by microcrack formation and cavitation. The steady state creep results are consistent with a diffusion controlled creep mechanism involving nitrogen diffusion through the grain boundary glassy phase.

Todd, J. A.↗
NASA NTRS1989

The high temperature creep deformation of Si3N4-6Y2O3-2Al2O3

The creep properties of silicon nitride containing 6 wt percent yttria and 2 wt percent alumina have been determined in the temperature range 1573 to 1673 K. The stress exponent, n, in the equation epsilon dot varies as sigma sup n, was determined to be 2.00 + or - 0.15 and the true activation energy was found to be 692 + or - 25 kJ/mol. Transmission electron microscopy studies showed that deformation occurred in the grain boundary glassy phase accompanied by microcrack formation and cavitation. The steady state creep results are consistent with a diffusion controlled creep mechanism involving nitrogen diffusion through the grain boundary glassy phase.

Todd, J. A.↗
NASA NTRS2008

Role of Hf on Phase Formation in Ti45Zr(38-x)Hf(x)Ni17 Liquids and Solids

Hafnium and zirconium are very similar, with almost identical sizes and chemical bonding characteristics. However, they behave differently when alloyed with Ti and Ni. A sharp phase formation boundary near 18-21 at.% Hf is observed in rapidly-quenched and as-cast Ti45Zr38-xHfxNi17 alloys. Rapidly-quenched samples that contain less than 18 at.% Hf form the icosahedral quasicrystal phase, whiles samples containing more than 21 at.% form the 3/2 rational approximant phase. In cast alloys, a C14 structure is observed for alloys with Hf lower than the boundary concentration, while a large-cell (11.93 ) FCC Ti2Ni-type structure is found in alloys with Hf concentrations above the boundary. To better understand the role of Hf on phase formation, the structural evolution with supercooling and the solidification behavior of liquid Ti45Zr38-xHfxNi17 alloys (x=0, 12, 18, 21, 38) were studied using the Beamline Electrostatic Levitation (BESL) technique using 125keV x-rays on the 6ID-D beamline at the Advanced Photon Source, Argonne National Laboratory. For all liquids primary crystallization was to a BCC solid solution phase; interestly, an increase in Hf concentration leads to a decrease in the BCC lattice parameter in spite of the chemical similarity between Zr and Hf. A Reitveld analysis confirmed that as in the cast alloys, the secondary phase that formed was the C14 below the phase formation boundary and a Ti2Ni-type structure at higher Hf concentrations. Both the liquidus temperature and the reduced undercooling change sharply on traversing the phase formation boundary concentration, suggesting a change in the liquid structure. Structural information from a Honeycutt-Anderson index analysis of reverse Monte Carlo fits to the S(q) liquid data will be presented to address this issue.

Wessels, V.↗
NASA NTRS1974

Improved toughness of refractory compounds

The concept of grain-boundary-engineering through elimination of the grain-boundary silicate phase in silicon nitride was developed. The process involved removal of the silica from the nitride powder via a thermal treatment coupled with the use of nitride additives to compensate the remaining oxygen. Magnesium and aluminum nitrides are found to be the most effective additive for use as oxygen compensators. Strength decreases at elevated temperatures are not observed in the alumina containing material. The creep rate of a dual additive sialon composition was two orders of magnitude lower at 1400 C than commercial silicon nitride. A cursory analysis of the creep mechanism indicate that grain-boundary sliding is avoided through elimination of the grain-boundary silicate phase.

Wright, T. R.↗
NASA NTRS2013

Calcium-Magnesium-Aluminosilicate (CMAS) Reactions and Degradation Mechanisms of Advanced Environmental Barrier Coatings

The thermochemical reactions between calcium-magnesium-aluminosilicate- (CMAS-) based road sand and several advanced turbine engine environmental barrier coating (EBC) materials were studied. The phase stability, reaction kinetics and degradation mechanisms of rare earth (RE)-silicates Yb2SiO5, Y2Si2O7, and RE-oxide doped HfO2 and ZrO2 under the CMAS infiltration condition at 1500 C were investigated, and the microstructure and phase characteristics of CMAS-EBC specimens were examined using Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD). Experimental results showed that the CMAS dissolved RE-silicates to form crystalline, highly non-stoichiometric apatite phases, and in particular attacking the silicate grain boundaries. Cross-section images show that the CMAS reacted with specimens and deeply penetrated into the EBC grain boundaries and formed extensive low-melting eutectic phases, causing grain boundary recession with increasing testing time in the silicate materials. The preliminary results also showed that CMAS reactions also formed low melting grain boundary phases in the higher concentration RE-oxide doped HfO2 systems. The effect of the test temperature on CMAS reactions of the EBC materials will also be discussed. The faster diffusion exhibited by apatite and RE-doped oxide phases and the formation of extensive grain boundary low-melting phases may limit the CMAS resistance of some of the environmental barrier coatings at high temperatures.

Ahlborg, Nadia L.↗
NASA NTRS1982

Improvement of Rocket Engine Plume Analysis Techniques

A nozzle plume flow field code was developed. The RAMP code which was chosen as the basic code is of modular construction and has the following capabilities: two phase with two phase transonic solution; a two phase, reacting gas (chemical equilibrium reaction kinetics), supersonic inviscid nozzle/plume solution; and is operational for inviscid solutions at both high and low altitudes. The following capabilities were added to the code: a direct interface with JANNAF SPF code; shock capturing finite difference numerical operator; two phase, equilibrium/frozen, boundary layer analysis; a variable oxidizer to fuel ratio transonic solution; an improved two phase transonic solution; and a two phase real gas semiempirical nozzle boundary layer expansion.

Smith, S. D.↗
DOE OSTI2024

Creep and failure at metal-oxide interfaces

Small-scale bicrystal creep experiments were performed on contacts formed via in situ high-temperature diffusion bonding of metal-oxide interfaces including Ag-ZrO 2 , Pd-ZrO 2 , Pt-ZrO 2 , and Ag-high entropy oxide. This work characterizes deformation and failure at metal-oxide interfaces during mechanical loading. Interfacial sliding can be activated easily, while tensile interfacial creep was not observed at any condition of stress or temperature measured. Plastic strain, instead, localizes within the metal under tensile loading. A variety of mechanisms for plastic strain occur in the metal including lattice dislocation-mediated plasticity, twinning, low-angle grain boundary formation, and low-angle grain boundary creep. Surface and low-angle grain boundary diffusion occur under conditions where no metal-oxide tensile creep is observed, highlighting the significant differences in their interfacial mechanical response. High-temperature interfacial failure occurs when the mean curvature at the contact neck is approximately zero and the applied stresses comparable to brittle fracture stresses. The brittle fracture stresses were measured to be σ ƒ = 180 ± 90 MPa at the Ag-ZrO 2 interface at 225 °C, σ ƒ = 460 ± 160 MPa at the Pd-ZrO 2 interface at 680 °C, and σ ƒ = 640 ± 440 MPa at the Pt-ZrO 2 interface at 1010 °C.

Creep↗
NASA NTRS2007

Development of Hairpin Vortices in Turbulent Spots and End-Wall Transition

The end-stage phase of boundary layer transition is characterized by the development of hairpin-like vortices which evolve rapidly into patches of turbulent behavior. In general, the characteristics of the evolution form this hairpin stage to the turbulent stage is poorly understood, which has prompted the present experimental examination of hairpin vortex development and growth processes. Two topics of particular relevance to the workshop focus will be covered: 1) the growth of turbulent spots through the generatio and amalgamation of hairpin-like vortices, and 2) the development of hairpin vortices during transition in an end-wall junction flow. Brief summaries of these studies are described below. Using controlled generation of hairpin vortices by surface injection in a critical laminar boundary layer, detailed flow visualization studies have been done of the phases of growth of single hairpin vortices, from the initial hairgin generation, through the systematic generation of secondary hairpin-like flow structures, culminating in the evolution to a turbulent spot. The key to the growth process is strong vortex-surface interactions, which give rise to strong eruptive events adjacent to the surface, which results in the generation of subsequent hairpin vortex structures due to inviscid-viscuous interactions between the eruptive events and the free steam fluid. The general process of vortex-surface fluid interaction, coupled with subsequent interactions and amalgamation of the generated multiple hairpin-type vortices, is demonstrated as a physical mechanism for the growth and development of turbulent spots. When a boundary layer flow along a surface encounters a bluff body obstruction extending from the surface (such as cylinder or wing), the strong adverse pressure gradients generated by these types of flows result in the concentration of the impinging vorticity into a system of discrete vortices near the end-wall juncture of the obstruction, with the extensions of the vortices engirdling the obstruction to form "necklace" or "horseshoe" vortices. Recent hydrogen bubble and particle image visualization have shown that as Reynolds number is increased for a laminar approach flow, the flow will become critical, and a destabilization of the necklace vortices results in the development of an azimuthal waviness, or "kinks", in the vortices. These vortex kinks are accentuated by Biot-Savart effects, causing portions of a distorted necklace vortex to make a rapid approach to the surface, precipitating processes of localized, three-dimensional surface interactions. These interactions result in the rapid generation, focussing, and ejection of thin tongues of surface fluid, which rapidly roll-over and appear as hairpin vortices in the junction region. Subsequent amalgamation of these hairpin vortices with the necklace vortices produces a complex transitional-type flow. A presentation of key results from both these studies will be done, emphasizing both the ubiquity of such hairpin-type flow structures in manifold transitional-type flows, and the importance of vortex-surface interactions n the development of hairpin vortices.

Smith, Charles R.↗
NASA NTRS1989

Further Improvements to Nozzle Boundary Layer Calculations in BLIMPJ

Further improvements made to advance the current Boundary Layer Integral Matrix Procedure - Version J (BLIMPJ) containing previously modeled simplified calculation methods by accounting for condensed phase, thick boundary layer and free stream turbulence effects are discussed. The condensed phase effects were included through species composition effect considered via input to the code and through particle damping effect considered via a turbulence model. The thrust loss calculation procedure for thick boundary layer effects was improved and the optimization of net thrust with respect to nozzle length was performed. The effects of free stream turbulence were approximately modeled in the turbulence model.

Praharaj, S. C.↗