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DOE OSTI2023

Engineering Relaxor Behavior in (BaTiO 3 ) n /(SrTiO 3 ) n Superlattices

Complex-oxide superlattices provide a pathway to numerous emergent phenomena because of the juxtaposition of disparate properties and the strong interfacial interactions in these unit-cell-precise structures. This is particularly true in superlattices of ferroelectric and dielectric materials, wherein new forms of ferroelectricity, exotic dipolar textures, and distinctive domain structures can be produced. Here, in this study, relaxor-like behavior, typically associated with the chemical inhomogeneity and complexity of solid solutions, is observed in (BaTiO 3 ) n /(SrTiO 3 ) n (n = 4–20 unit cells) superlattices. Dielectric studies and subsequent Vogel–Fulcher analysis show significant frequency dispersion of the dielectric maximum across a range of periodicities, with enhanced dielectric constant and more robust relaxor behavior for smaller period n. Bond-valence molecular-dynamics simulations predict the relaxor-like behavior observed experimentally, and interpretations of the polar patterns via 2D discrete-wavelet transforms in shorter-period superlattices suggest that the relaxor behavior arises from shape variations of the dipolar configurations, in contrast to frozen antipolar stripe domains in longer-period superlattices (n = 16). Moreover, the size and shape of the dipolar configurations are tuned by superlattice periodicity, thus providing a definitive design strategy to use superlattice layering to create relaxor-like behavior which may expand the ability to control desired properties in these complex systems.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Interfacial Hydrogen-Bond Dynamics in Transition Metal Compounds

Understanding how water behaves when confined within atomic layers of active transition-metal carbides, nitrides, and carbonitrides is essential for uncovering the fundamental principles needed to engineer solid–liquid interfaces at the atomic scale. Yet, how lattice element chemistry and surface termination groups collectively regulate the structure and mobility of such interlayer water remains poorly understood. Here, we present a composition-controlled investigation of interlayer water dynamics in layered transition-metal nitride, carbide, and carbonitride systems using a systematic integration of quasi-elastic neutron scattering (QENS), ab initio molecular dynamics (AIMD) simulations, and density functional theory (DFT) calculations. QENS measurements show that nitride-rich systems host mobile, translationally diffusing water with thermally activated self-diffusion coefficients on the order of 10 –10 m 2 s –1 , whereas mixed C/N lattices confine water to localized, nontranslational motion that is insensitive to temperature. AIMD and DFT reveal that lattice C/N chemistry and surface functional group composition reshape the first hydration layer by modulating the surface electronic structure and termination-dependent hydrogen-bond networks, leading to pronounced differences in water ordering and thermal resilience. On the other hand, fully carbide systems exhibit intermediate behavior, highlighting that water mobility is not primarily controlled by the hydration level alone but by the coupling between lattice composition and surface chemistry. Overall, this study establishes how surface chemistry and lattice composition jointly control interfacial hydrogen bond dynamics, offering a mechanistic framework for designing transition-metal layered materials with tailored interfacial transport properties.

Hydration↗

DOE OSTI2018

Measurement of Interfacial Fracture Toughness of Surface Coatings Using Pulsed-Laser-Induced Ultrasonic Waves

This research develops a new technique for the measurement of interfacial fracture toughness of films/surface coatings using laser-induced ultrasonic waves. Using pulsed laser ablation on the bottom substrate surface, strong stress waves are generated leading to interfacial fractures and coating delamination. Simultaneously, a laser ultrasonic interferometer is used to measure the normal (out-of-plane) displacement of the top surface coating in order to detect coating delamination in a non-destructive manner. We can thus determine the critical laser energy for delamination, yielding the critical stress (that is, the interfacial strength). Subsequently, to examine the interfacial fracture toughness, additional pulsed laser irradiation is applied to a pre-delaminated specimen to show that the delamination area expands. This type of interfacial crack growth can be visualized using laser ultrasonic scanning. Furthermore, the calculation of elastic wave propagation was carried out using a finite-difference time-domain method) in order to accurately estimate the interfacial stress field. In this calculation, the stress distribution around the initial delamination is calculated to obtain the stress intensity factor. Based on the experimental and computational results, interfacial fracture toughness can be quantitatively evaluated. Since this technique relies on a two-laser system in a non-contact approach, it may be useful for a quantitative evaluation of adhesion/bonding quality (including both interfacial fracture strength and toughness) in various environments.

42 ENGINEERING↗

DOE OSTI2019

Pseudoplasticity and Dynamic Interfacial Tension Relaxation Effects on Nucleate Pool Boiling in Aqueous Polymeric Liquids

Nucleate pool boiling heat transfer and its ebullient dynamics in polymeric solutions at atmospheric pressure saturated conditions are experimentally investigated. Three grades of hydroxyethyl cellulose (HEC) are used, which have intrinsic viscosity in the range 5.29 ≤ [ η ] ≤ 10.31 [dl/g]. Their aqueous solutions in different concentrations, with zero-shear viscosity in the range 0.0021 ≤ η 0 ≤ 0.0118 [N∙s/m 2 ], exhibit shear-thinning rheology in varying degrees, as well as gas–liquid interfacial tension relaxation and wetting. Boiling heat transfer in solutions with constant molar concentrations of each additive, which are greater than their respective critical polymer concentration C * , is seen to have anomalous characteristics. There is degradation in the heat transfer at low heat fluxes, relative to that in the solvent, where the postnucleation bubble dynamics in the partial boiling regime is dominated by viscous resistance of the polymeric solutions. At higher heat fluxes, however, there is enhancement of boiling heat transfer due to a complex interplay of pseudoplasticity and dynamic surface tension effects. The higher frequency vapor bubbling train with high interfacial shear rates in this fully developed boiling regime tends to be influenced by increasing shear-thinning and time-dependent differential interfacial tension relaxation at the dynamic gas–liquid interfaces.

Engineering↗

DOE OSTI2019

Light Induced Interfacial Phenomena in Atomically thin 2D Van der Waals Material Hybrids and Heterojunctions

Atomically thin 2D van Der Waals (2D-vDW) materials have attracted significant attention for optoelectronic applications in photodetectors, photovoltaics, quantum information science. Their atomically thin thickness, however, renders them poor absorbers. Hybrid structures of 2D-vDW materials assembled with other semiconducting materials, such as quantum dots, nanowires, polymers, other 2D-vDW materials or 3D bulk materials, have provided an elegant way to increase light harvesting and carrier generation via interfacial charge and energy transfer interactions. Here we present recent examples focused on the characterization of interfacial charge transfer and energy transfer in 2D-vDW hybrids and heterostructures and methods to modulate and control these processes through bandgap engineering, morphology engineering and external factors. Lastly, we discuss potential future directions of research, including scalability from micron-sized flake-based devices to wafer size for commercial deployment, issues with long term stability and performance and the ability to extend the spectral range of these 2D hybrids.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2018

Nanostructural and Electrochemical Evolution of the Solid-Electrolyte Interphase on CuO Nanowires Revealed by Cryogenic-Electron Microscopy and Impedance Spectroscopy

Battery performance is critically dependent on the nanostructure and electrochemical properties of the solid-electrolyte interphase (SEI)—a passivation film that exists on most lithium-battery anodes. However, knowledge of how the SEI nanostructure forms and its impact on ionic transport remains limited due to its sensitivity to transmission electron microscopy and difficulty in accurately probing the SEI impedance. Here, we track the voltage-dependent, stepwise evolution of the nanostructure and impedance of the SEI on CuO nanowires using cryogenic-electron microscopy (cryo-EM) and electrochemical impedance spectroscopy (EIS). In carbonate electrolyte, the SEI forms at 1.0 V vs Li/Li + as a 3 nm thick amorphous SEI and grows to 4 nm at 0.5 V; as the potential approaches 0.0 V vs Li/Li + , the SEI on the CuO nanowires forms an 8 nm thick inverted multilayered nanostructure in ethylene carbonate/diethyl carbonate (EC/DEC) electrolyte with 10 vol % fluoroethylene carbonate (FEC) and a mosaic nanostructure in EC/DEC electrolyte. Upon Li deposition, the total SEI thickness grows to 16 nm, and significant growth of the inner amorphous layer takes place in the inverted multilayered nanostructure, indicating that electrolyte permeates the SEI. Using a refined EIS methodology, we isolate the SEI impedance on Cu and find that the SEI nanostructure directly correlates to macroscopic Li-ion transport through the SEI. The inverted layered nanostructure decreases the interfacial impedance upon formation, whereas the mosaic nanostructure continually increases the interfacial impedance during growth. Furthermore these structural and electrochemical findings illustrate a more complete portrait of SEI formation and guide further improvements in engineered SEI.

25 ENERGY STORAGE↗

DOE OSTI2022

Understanding Phase and Interfacial Effects of Spall Fracture in Additively Manufactured Ti-5Al-5V-5Mo-3Cr

Additive manufactured Ti-5Al-5V-5Mo-3Cr (Ti-5553) is being considered as an AM repair material for engineering applications because of its superior strength properties compared to other titanium alloys. Here, we describe the failure mechanisms observed through computed tomography, electron backscatter diffraction (EBSD), and scanning electron microscopy (SEM) of spall damage as a result of tensile failure in as-built and annealed Ti-5553. We also investigate the phase stability in native powder, as-built and annealed Ti-5553 through diamond anvil cell (DAC) and ramp compression experiments. We then explore the effect of tensile loading on a sample containing an interface between a Ti-6Al-V4 (Ti-64) baseplate and additively manufactured Ti-5553 layer. Post-mortem materials characterization showed spallation occurred in regions of initial porosity and the interface provides a nucleation site for spall damage below the spall strength of Ti-5553. Preliminary peridynamics modeling of the dynamic experiments is described. Finally, we discuss further development of Stochastic Parallel PARticle Kinteic Simulator (SPPARKS) Monte Carlo (MC) capabilities to include the integration of alpha (α)-phase and microstructural simulations for this multiphase titanium alloy.

36 MATERIALS SCIENCE↗

NASA NTRS2004

Improved BN Coatings on SiC Fibers in SiC Matrices

Modifications of BN-based coatings that are used as interfacial layers between the fibers and matrices of SiCfiber/SiC-matrix composite materials have been investigated to improve the thermomechanical properties of these materials. Such interfacial coating layers, which are also known as interphases (not to be confused with interphase in the biological sense), contribute to strength and fracture toughness of a fiber/matrix composite material by providing for limited amounts of fiber/matrix debonding and sliding to absorb some of the energy that would otherwise contribute to the propagation of cracks. Heretofore, the debonding and sliding have been of a type called inside debonding because they have taken place predominantly on the inside surfaces of the BN layers that is, at the interfaces between the SiC fibers and the interphases. The modifications cause the debonding and sliding to include more of a type, called outside debonding, that takes place at the outside surfaces of the BN layers that is, at the interfaces between the interphases and the matrix (see figure). One of the expected advantages of outside debonding is that unlike in inside debonding, the interphases would remain on the crack-bridging fibers. The interphases thus remaining should afford additional protection against oxidation at high temperature and should delay undesired fiber/fiber fusion and embrittlement of the composite material. A secondary benefit of outside debonding is that the interphase/matrix interfaces could be made more compliant than are the fiber/interphase interfaces, which necessarily incorporate the roughness of the SiC fibers. By properly engineering BN interphase layers to favor outside debonding, it should be possible, not only to delay embrittlement at intermediate temperatures, but also to reduce the effective interfacial shear strength and increase the failure strain and toughness of the composite material. Two techniques have been proposed and partially experimentally verified as candidate means to promote outside debonding in state-of-the-art SiC/SiC composites.

Morscher, Gregory N.↗

DOE OSTI2026

Low-cost, Highly Efficient and Fast Thermally Pressed Scalable Carbon-based Planar Perovskite Solar Cells

This Final Technical Report summarizes work completed under Award Number DEEE0009833, titled "Low-cost, Highly Efficient and Fast Thermally Pressed Scalable Carbon-based Planar Perovskite Solar Cells." The project addressed the central technical problem that carbon-electrode perovskite solar cells (C-PSCs) can reduce electrode costs and improve environmental durability, but they have historically lagged noble-metalcontact devices due to poor carbon/perovskite contact, high carbon-electrode resistance, imperfect hole extraction, and insufficient operational stability. The Statement of Project Objectives (SOPO), therefore, required systematic engineering of thermally pressed carbon-based planar perovskite solar cells by improving the carbon/perovskite interface quality, improving carbon-electrode conductivity, and further increasing device stability. The work advanced understanding of carbon-based perovskite photovoltaics by connecting device performance to three coupled mechanisms: interfacial recombination at the perovskite/hole-transport-layer/carbon stack; lateral and vertical transport losses in carbon contacts; and instability driven by moisture, heat, illumination, ion migration, and slow/variable manufacturing steps.

14 SOLAR ENERGY↗

DOE OSTI2021

High-speed impact of micron-sized diesel drop trains—Splashing dynamics, secondary droplet formation, and effects of pre-existing film thickness

This work investigates surface impingement of monodispersed diesel drop trains using computational simulations. The three-dimensional simulations include high-speed impact of micrometer-sized fuel drops onto initially dry and wetted stainless steel substrates. The drop size and impact velocity are representative of fuel injection conditions in internal combustion engines (ICEs). The drop trains serve as a simplified representation of fuel spray. To accurately capture the film that naturally develops on initially dry substrates, a dynamic diesel-stainless steel contact angle model was developed using experiments of single drop impact under ICE representative temperature. Simulations are presented for a highly splashing case and the effects of a pre-existing film on splashing dynamics were investigated, including the temporal evolution of splashed mass and film thickness. It was concluded that for thin films, the effect of pre-existing film thickness is less significant than in single drop impingement. Secondary droplet characterization was performed on simulation results, leading to instantaneous and time-averaged distributions of secondary droplet size, velocity magnitude, and trajectory angle. It was found that for each drop impingement, approximately 58% of the splashed mass is from the impinging drop itself, while the remainder of the splashed mass is composed of film liquid. From a high resolution case, details of secondary droplet formation are observed and three distinct phases of secondary droplet formation are identified. The detailed analysis of drop train impingement under engine-relevant conditions serves as a first step toward a robust understanding of fuel impingement and the development of cleaner and more efficient ICEs.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2019

Development of an Advanced Finite Element Model and Parametric Study to Evaluate Cement Sheath Barrier

Cement failure is known as one of the major causes for loss of well control events. Cement design is considered as one of the top technological knowledge gaps in high-pressure high-temperature oil and gas exploration. The primary objective of this paper is to perform a parametric analysis and identify critical parameters affecting the mechanical integrity of the set cement sheath. To achieve the objective, three-dimensional finite element models consisting of concentric casings and annular cement sheath were created. The finite element model was validated by analytical calculations. Performance of cement sheath was assessed by analyzing radial, hoop, and maximum shear stresses at different loading conditions. A parametric study was conducted by individually varying influencing factors such as cement material properties, sheath dimensions, and wellbore pressure loads. Values of all parameters were normalized and represented on the same plot against mechanical stresses. Such response curves can be used to estimate whether cement will structurally fail because of various operational loads or material aging. The plot can also be utilized to rank various factors in terms of influence on cement’s performance. Sensitivity response reveals that wellbore pressure, cement material properties, and annulus pressure are major parameters influencing mechanical stresses in neat class G cement. The order of importance depends on the type of stress. Results indicate interfacial bond failure and radial cracking to be the more likely modes of failure for class G cement. Cement response curves can help design engineers and regulators alike in quickly evaluating short-term or long-term fitness-for-service of cement sheath from the perspective of structural integrity. Industry standards and guidelines can be improved by adding performance curves for standard cement recipes.

Energy & Fuels↗

NASA NTRS1984

Analytical and experimental investigation of rubbing interaction in labyrinth seals for a liquid hydrogen fuel pump

Cracking of the titanium knife edges on the labyrinth seals of the liquid hydrogen fuel pump in the Space Shuttle main engine is considered. Finite element analysis of the thermal response of the knife edge in sliding contact with the wear ring surface shows that interfacial temperatures can be quite high and they are significantly influenced by the thermal conductivity of the surfaces in rubbing contact. Thermal shock experiments on a test specimen similar to the knife edge geometry demonstrate that cracking of the titanium alloy is possible in a situation involving repeated thermal cycles over a wide temperature range, as might be realized during a rub in the liquid hydrogen fuel pump. High-speed rub interaction tests were conducted using a representative knife edge and seal geometry over a broad range of interaction rates and alternate materials were experimentally evaluated. Plasma-sprayed aluminum-graphite was found to be significantly better than presently used aluminum alloy seals from the standpoint of rub performance. Ion nitriding the titanium alloy knife-edges also improved rub performance compared to the untreated baseline.

Dolan, F. X.↗

NASA NTRS1994

Solid Surface Wetting and the Deployment of Drops in Microgravity

surface↗

DOE OSTI2018

Atomic layer deposition for membrane interface engineering

In many applications, interfaces govern the performance of membranes. Structure, chemistry, electrostatics, and other properties of interfaces can dominate the selectivity, flux, fouling resistance, and other critical aspects of membrane functionality. Control over membrane interfacial properties, therefore, is a powerful means of tailoring performance. In this minireview, we discuss the application of atomic layer deposition (ALD) and related techniques in the design of novel membrane interfaces. We discuss recent literature in which ALD is used to 1) modify the surface chemistry and interfacial properties of membranes, 2) tailor the pore sizes and separation characteristics of membranes, and 3) enable novel advanced functional membranes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Accelerating Manufacturing of Powder-Processed Strong, Lightweight and Thermally Stable Bulk Nanocrystalline Al Alloys via Engineered Interface States

The overarching goal of this program is to develop an integrated materials by design framework enabling a simple, scalable, and efficient manufacturing route for thermally stable nanocrystalline Al-based alloys with high specific strength over a range of service temperatures. The central scientific principle underpinning this program is the elucidation, and ultimately implementation in novel alloy design, of unique interfacial structures and chemistries driven by segregation in multi-component systems that give rise to unprecedented processability and properties. This program targeted nanocrystalline Al-based ternary alloys produced by mechanical alloying of powders followed by compaction and sintering with hot pressing, which are inherently scalable and inexpensive manufacturing routes, but when applied to nanocrystalline alloys are usually plagued by low density and/or poor retention of the intended nanostructures during processing. This program successfully demonstrated manufacturing of a bulk (>1 cm 3 ) nanocrystalline Al-based alloy with a combination of thermal stability, high temperature strength retention, and specific strength that exceeds the current-state-of-the-art of Al alloys. It is anticipated that the greatest technological impact will occur by demonstration of rapid and scalable manufacturing of bulk nanocrystalline Al alloys with exceptional thermal stability and mechanical performance, thus enabling increased energy efficiency in high performance power generation systems via: (i) replacement of existing components with lightweight Al-based alloys and (ii) increasing operating temperatures with property retention. The program focused on the development of a simple and efficient manufacturing route for thermally stable nanocrystalline Al-based alloys with high specific strength over a range of service temperatures. The program is expected to have direct impact on scalable and economic manufacturing of bulk nanocrystalline alloys. This program profited from the recent discovery by the project team of segregation-driven amorphous intergranular films in nanocrystalline metallic alloys that can be kinetically frozen-in at sub-solidus temperatures. These interfacial states (also known as amorphous complexions) comprise a large fraction of the total material in nanocrystalline alloys and are responsible for two beneficial characteristics that anchor the proposed work: (1) activated sintering leading to high density and (2) retained nanostructures leading to high strengths that approach a substantial fraction of the theoretical limit. More specifically, these engineered interfaces led to a three-fold benefit: (i) high-throughput materials processing with low energy budget and cost, (ii) exceptional thermal stability, and (iii) high specific strength at both room temperature and intermediate temperatures experienced during service.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

NASA NTRS1994

Solid surface wetting and the deployment of drops in microgravity

The complete or partial deployment of liquid samples in low gravity is primarily influenced by the interfacial properties of the specific liquid and solid materials used because the overwhelming bias of the Earth gravitational acceleration is removed. This study addresses the engineering aspects of injecting and deploying drops of prescribed volume into an acoustic positioning chamber in microgravity. The specific problems of interest are the design, testing, and implementation of injector tips to be used in a simultaneously retracting dual-injector system in the Drop Physics Module microgravity experiment facility. Prior to release, the liquid to be deployed must be retained within a restricted area at the very end of the injectors under dynamic stimuli from the continuous injection flow as well as from the stepped motion of the injectors. The final released drop must have a well determined volume and negligible residual linear or angular momentum. The outcome of Earth-based short-duration low gravity experiments had been the selection of two types of injector tips which were flown as back-up parts. They were successfully utilized during the USML-1 Spacelab mission as the primary tips. The combination of a larger contact surface, liquid pinning with a sharp edge, and selective coating of strategic tip surfaces with a non-wetting compound has allowed a significant increase in the success rate of deployment of simple and compound drops of aqueous solutions of glycerol and silicone oil. The diameter of the samples studied in the Drop Physics Module range between 0.3 and 2.7 cm. The tests conducted on-orbit with a manually operated small device have allowed the calibration of the volume deployed for a few drop sizes. The design for improved tips to be used during the next USML flight is based on these results.

Trinh, E. H.↗

NASA NTRS1994

Solid Surface Wetting and the Deployment of Drops in Microgravity

The complete or partial deployment of liquid samples in low gravity is primarily influenced by the interfacial properties of the specific liquid and solid materials used because the overwhelming bias of the Earth gravitational acceleration is removed. This study addresses the engineering aspects of injecting and deploying drops of prescribed volume into an acoustic positioning chamber in microgravity. The specific problems of interest are the design, testing, and implementation of injector tips to be used in a simuttaneously retracting dual-injector system used in the Drop Physics Module microgravity experiment facility. Prior to release, the liquid to be deployed must be retained within a restricted area at the very end of the injectors even under dynamic stimuli due to continuous injection flow as well as to the stepped motion of the injectors, and the final released drop must have a well determined volume as well as negligible residual linear or angular momentum from the deployment process. The outcome of Earthbased short-duration low gravity experiments had been the selection of two types of injector tips which were flown as back-up parts and were successfully utilized during the USML-1 Spacelab mission. The combination of a larger contact surface, liquid pinning with a sharp edge, and selective coating of strategic tip surfaces with a non-wetting compound has allowed a significant increase in the success rate of deployment of simple and compound drops of aqueous solutions of glycerol and silicone oil. The diameter of the samples studied in the Drop Physics Module ranged between 0.3 and 2.7 cm. The tests conducted onsrbit with a manually operated small device have allowed the calibration of the volume deployed for a few drop sizes. The design for improved tips to be used during the next USML flight is based on these results.

Trinh, E. H.↗

NASA NTRS2003

Alloy Design Workbench-Surface Modeling Package Developed

NASA Glenn Research Center's Computational Materials Group has integrated a graphical user interface with in-house-developed surface modeling capabilities, with the goal of using computationally efficient atomistic simulations to aid the development of advanced aerospace materials, through the modeling of alloy surfaces, surface alloys, and segregation. The software is also ideal for modeling nanomaterials, since surface and interfacial effects can dominate material behavior and properties at this level. Through the combination of an accurate atomistic surface modeling methodology and an efficient computational engine, it is now possible to directly model these types of surface phenomenon and metallic nanostructures without a supercomputer. Fulfilling a High Operating Temperature Propulsion Components (HOTPC) project level-I milestone, a graphical user interface was created for a suite of quantum approximate atomistic materials modeling Fortran programs developed at Glenn. The resulting "Alloy Design Workbench-Surface Modeling Package" (ADW-SMP) is the combination of proven quantum approximate Bozzolo-Ferrante-Smith (BFS) algorithms (refs. 1 and 2) with a productivity-enhancing graphical front end. Written in the portable, platform independent Java programming language, the graphical user interface calls on extensively tested Fortran programs running in the background for the detailed computational tasks. Designed to run on desktop computers, the package has been deployed on PC, Mac, and SGI computer systems. The graphical user interface integrates two modes of computational materials exploration. One mode uses Monte Carlo simulations to determine lowest energy equilibrium configurations. The second approach is an interactive "what if" comparison of atomic configuration energies, designed to provide real-time insight into the underlying drivers of alloying processes.

Abel, Phillip B.↗