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At least 397 records · Page 22

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DOE OSTI2025

Friction surface layer deposition of triple-phase Al 10 Cr 12 Fe 35 Mn 23 Ni 20 high entropy alloy: Process optimization and microstructural evolution

A high-strength Co-free triple-phase Al 10 Cr 12 Fe 35 Mn 23 Ni 20 high-entropy alloy (HEA) was successfully fabricated using Friction Surface Layer Deposition (FSLD), a bulk manufacturing method. Multiple single-layer deposits were produced by varying forging force (F) and traverse speeds (T r ) to optimize the process parameters. The optimized conditions (F = 40 kN & T r = 200 mm/min) were then applied to manufacture a scaled-up multi-layer specimen. The initial microstructure of the HEA consisted of coarse grains of the soft FCC-phase, long columnar dendrites of the hard BCC-phase, and small precipitates of the harder B2-phase within the BCC-dendrites. During FSLD, the FCC-matrix underwent continuous dynamic recrystallization due to high-temperature severe plastic deformation, forming finer equiaxed grains. Simultaneously, the BCC-dendrites fractured into smaller fragments, some of which experienced partial growth and coarsening under applied stress, resulting in an hourglass morphology. In contrast, the small B2-precipitates within the BCC-fragments dissolved during the elevated temperatures of FSLD and reprecipitated as substantially finer precipitates during continuous cooling post-FSLD. Additionally, the orientation relationships between the FCC and BCC/B2 phases were completely destroyed by the severe thermoplastic deformation inherent to FSLD. The microstructural refinements led to a substantial improvement in hardness from 177 HV to 283 HV, driven by Hall-Petch strengthening. The increased number of interfaces, including coherent BCC-B2 interfaces, potentially enhances the sink strength and radiation tolerance of the HEA, making it a promising candidate for nuclear applications. In conclusion, this study also highlights FSLD as a versatile technique for achieving tunable properties in HEAs, with detailed schematics illustrating the complex mechanisms of phase transformations during processing.

Additive Manufacturing↗

DOE OSTI2026

Influence of Surface Treatment on the Interfacial and Mechanical Performance of Metal-Insert Overmolded Composites

Structural composites with metal inserts are gaining increasing interest enabling light weight design for energy efficiency, provide insulation, corrosion protection without compromising mechanical integrity. Such over molded metal-polymer composites show strong potential in many automotive and aerospace component parts, e.g. car bumper, chassis, door, brackets, fasteners, etc. Despite several advantages, metal-polymer dissimilar interface remains a weak spot in structural design, requiring further investigation to improve interfacial interlocking. The current work focuses on enhancing the metal-polymer adhesion between stainless steel inserts and polymer matrices (e.g. acrylonitrile butadiene styrene resin (ABS), and polyamide 66 (PA66) through surface treatment via chemical etching and mechanical roughening. In the chemical etching process, metal substrates were treated with aqua regia solution for different time intervals to evaluate surface roughness measured by water contact angle and morphology analysis. For mechanical roughening approach, metal inserts were subjected to blasting for surface abrasion. Treated samples were also functionalized with aminosilane coupling agent which showed successful grafting on the surface measured by water contact angle. Metal inserts with micro level surface roughness through etching exhibited significant 21% improvement in adhesion strength compared to untreated inserts; however, the effect of silane treatment on the interfacial strength was found to be highly matrix dependent.

Saha, Subhabrata [ORNL] (ORCID:000000033966064X)↗

NASA NTRS1991

Skeletal responses to spaceflight

The role of gravity in the determination of bone structure is elucidated by observations in adult humans and juvenile animals during spaceflight. The primary response of bone tissue to microgravity is at the interface of the mineral and matrix in the process of biomineralization. This response is manifested by demineralization or retarded growth in some regions of the skeleton and hypermineralization in others. The most pronounced effects are seen in the heelbone and skull, the most distally located bones relative to the heart. Ground based flight simulation models that focus on changes in bone structure at the molecular, organ, and whole body levels are described and compared to flight results. On Earth, the morphologic and compositional changes in the unloaded bones are very similar to changes during flight; however, the ground based changes appear to be more transient. In addition, a redistribution of bone mineral in gravity-dependent bones occurs both in space and during head down positioning on Earth. Longitudinal data provided considerable information on the influence of endocrine and muscular changes on bone structure after unloading.

Morey-Holton, Emily↗

NASA NTRS1999

Characterization of In-Situ BN Interface Formed by Nitridation of Nextel 312

Treatment of Nextel (TM) 312 in a reactive environment has been used as a low cost approach to the formation of BN on the fiber surface. Although the BN enriched surface region is extremely thin (less than 40 run), it is effective in providing debonding and composite behavior. Variation in mechanical behavior of Nextel (TM) 312/BN/Blackglas (TM) composites has been noted among panels fabricated with AF-10 cloth treated in different nitridation runs, Understanding this variation became the rationale for undertaking a detailed characterization of the nitrided fiber using field emission scanning electron microscopy, low voltage energy dispersive x-ray and Auger electron spectroscopy. Chemical composition and surface morphology are discussed in relation to observed mechanical behavior of NeXtel (TM) 312/Blackglas (TM) composites tested in bending.

Hurwitz, Fances I.↗

NASA NTRS2001

Characterization of Carbon Nanotubes Grown by Chemical Vapor Deposition

Since the superior properties of multi-wall carbon nanotubes (MWCNT) could improve numerous devices such as electronics and sensors, many efforts have been made in investigating the growth mechanism of MWCNT to synthesize high quality MWCNT. Chemical vapor deposition (CVD) is widely used for MWCNT synthesis, and scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS) are useful methods for analyzing the structure, morphology and composition of MWCNT. Temperature and pressure are two important growth parameters for fabricating carbon nanotubes. In MWCNT growth by CVD, the plasma assisted method is normally used for low temperature growth. However a high temperature environment is required for thermal CVD. A systematic study of temperature and pressure-dependence is very helpful to understanding MWCNT growth. Transition metal particles are commonly used as catalysis in carbon nanotube growth. It is also interesting to know how temperature and pressure affect the interface of carbon species and catalyst particles

Cochrane, J. C.↗

NASA NTRS2000

Growth and Morphology of Supercritical Fluids Studied in Microgravity on Mir

The Growth and Morphology of Supercritical Fluids (GMSF) is an international experiment facilitated by the NASA Glenn Research Center at Lewis Field and under the guidance of U.S. principal investigator Professor John Hegseth of the University of New Orleans and three French coinvestigators Daniel Beysens, Yves Garrabos, and Carole Chabot. In early 1999, GMSF experiments were operated for 20 days on the Russian Space Station Mir. Mir astronauts performed experiments One through Seven, which spanned the three science themes of near-critical phase separation rates, interface dynamics in near-critical boiling, and measurement of the spectrum of density fluctuation length scales very close to the critical point. The fluids used were pure CO2 or SF6. Three of the five thermostats used could adjust the sample volume with the scheduled crew time. Such a volume adjustment enabled variable sample densities around the critical density as well as pressure steps (as distinct from the usual temperature steps) to be applied to the sample.

Wilkinson, R. Allen↗

NASA NTRSDate not supplied

Morphological evolution and transition at nanoscale in BSTO ceramic materials

Considerable efforts have been devoted for the development of low cost ferroelectric and clean energy storage multifunctional materials. Modification in design and production of a low cost material with well proven process provides pathway for high energy density dielectric energy storage. We studied fluorine doped a commercially well-established material system barium strontium titanate with two different concentrations of dopants and studied the morphological transition and its effect on properties. It was observed that sample with higher concentration transitioned much faster into glassy state, followed by growth of fibers which turned into a self-arranged bird nest type shape. The sample with lower concentration changed slowly into glassy state and only few fibers were farmed. Dielectric was highly dependent on processing methods and shows variation with crystallinity of material, temperature and cooling conditions during processing. In the higher concentration range, we observed nano-scale interface breakdown very similar to that of solid-liquid interface breakdown during crystal growth.

dielectric↗

DOE OSTI2026

Atomic- and Molecular-Scale Interphase Engineering for High-Performance Solid-State Batteries

Solid-state batteries (SSBs) promise a decisive advance beyond conventional Li-ion systems, yet their development remains constrained by persistent solid–solid interfacial instabilities that degrade performance and durability. Interfaces between solid electrolytes and both cathodes and Li metal often exhibit poor wettability, limited physical contact, and high charge–transfer resistance, leading to chemical decomposition, mechanical failure, and impedance growth. Overcoming these limitations requires interphase engineering with atomic-scale precision—capabilities that conventional coating methods cannot reliably deliver. Atomic layer deposition (ALD) and molecular layer deposition (MLD) uniquely meet this need by enabling ultrathin, conformal, and composition-tunable films that stabilize reactive surfaces, suppress parasitic reactions, and regulate Li-metal morphology. Importantly, this Perspective highlights ALD/MLD systems that have already demonstrated effectiveness in liquid-electrolyte cells and discusses how these validated strategies can be deliberately translated to solid-state architectures. By grounding future directions in experimentally proven concepts rather than speculative hypotheses, we outline how atomic- and molecular-scale design principles can accelerate the development of robust, high-performance SSB technologies.

atomic and molecular layer deposition↗

NASA NTRS2001

How Cyanobacterial Distributions Reveal Flow and Irradiance Conditions of Photosynthetic Biofilm Formation

Microbial life on Earth is enormously abundant at sediment-water interfaces. The fossil record in fact contains abundant evidence of the preservation of life on such surfaces. It is therefore critical to our interpretation of early Earth history, and potentially to history of life on other planets, to be able to recognize life forms at these interfaces. On Earth this life often occurs as organized structures of microbes and their extracellular exudates known as biofilms. When such biofilms occur in areas receiving sunlight photosynthetic biofilms are the dominant form in natural ecosystems due to selective advantage inherent in their ability to utilize solar energy. Cyanobacteria are the dominant phototrophic microbes in most modern and ancient photosynthetic biofilms, microbial mats and stromatolites. Due to their long (3.5 billion year) evolutionary history, this group has extensively diversified resulting in an enormous array of morphologies and physiological abilities. This enormous diversity and specialization results in very specific selection for a particular cyanobacterium in each available photosynthetic niche. Furthermore these organisms can alter their spatial orientation, cell morphology, pigmentation and associations with heterotrophic organisms in order to fine tune their optimization to a given micro-niche. These adaptations can be detected, and if adequate knowledge of the interaction between environmental conditions and organism response is available, the detectable organism response can be used to infer the environmental conditions causing that response. This presentation will detail two specific examples which illustrate this point, Light and water are essential to photosynthesis in cyanobacteria and these organisms have specific detectable behavioural responses to these parameters. We will present cyanobacterial responses to quantified flow and irradiance to demonstrate the interpretative power of distribution and orientation information. This study presents new results, but many such examples are already found in the literature.

Prufert-Bebout, Lee↗

NASA NTRS2001

How Cyanobacterial Distributions Reveal Flow and Irradiance Conditions of Photosynthetic Biofilm Formation

Microbial life on Earth is enormously abundant at sediment-water interfaces. The fossil record in fact contains abundant evidence of the preservation of life on such surfaces. It is therefore critical to our interpretation of early Earth history, and potentially to history of life on other planets, to be able to recognize life forms at these interfaces. On Earth this life often occurs as organized structures of microbes and their extracellular exudates known as biofilms. When such biofilms occur in areas receiving sunlight photosynthetic biofilms are the dominant form in natural ecosystems due to selective advantage inherent in their ability to utilize solar energy. Cyanobacteria are the dominant phototrophic microbes in most modern and ancient photosynthetic biofilms, microbial mats and stromatolites. Due to their long (3.5 billion year) evolutionary history, this group has extensively diversified resulting in an enormous array of morphologies and physiological abilities. This enormous diversity and specialization results in very specific selection for a particular cyanobacterium in each available photosynthetic niche. Furthermore these organisms can alter their spatial orientation, cell morphology, pigmentation and associations with heterotrophic organisms in order to fine tune their optimization to a given micro-niche. These adaptations can be detected, and if adequate knowledge of the interaction between environmental conditions and organism response is available, the detectable organism response can be used to infer the environmental conditions causing that response. This presentation will detail two specific examples which illustrate this point. Light and water are essential to photosynthesis in cyanobacteria and these organisms have specific detectable behavioral responses to these parameters. We will present cyanobacterial responses to quantified flow and irradiance to demonstrate the interpretative power of distribution and orientation information. This study presents new results, but many such examples are already found in the literature. However this information exists in such a wide variety of journals, spanning decades of research that the utility of the vast storehouse of information is limited, not by the ability of cyanobacteria to respond in recognizable ways to environmental stimuli, but by our ability to compile and use this information. Recent advances in information technology will soon allow us to overcome these difficulties and utilize the detailed responses of cyanobacteria to environmental microniches as powerful records of the interaction between the biosphere and lithosphere.

Prufert-Bebout, Lee↗

NASA NTRSDate not supplied

Fabrication and Performance Characterization of Electrospun Nanofibers for Terrestrial and Space Applications

Passive thermal control is vital in space, especially for extended missions involving cryogen storage needing protection from sunlight. This presentation covers the development of a thermal coating with wavelength-selective characteristics using polymeric materials that scatter sunlight with minimal absorption, resulting in high solar reflectance. Furthermore, these coatings allow emission in infrared wavelengths, making them suitable for deep-space missions requiring extended storage. The study chose polymer and surface morphology suitable as solar reflectors that are lightweight, compact, and easily manufacturable, focusing on different multilayered nanofibers made using polytetrafluoroethylene and polyethylene-oxide (PTFE-PEO), polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP), and silica (SiO2). To understand how these materials interact with sunlight, we analyze light propagation through several layers of electrospun nanofibers to determine spectral reflectance, absorptance, and transmittance by solving the Maxwell equations. The model is also compared with measurements of spectral reflectance and transmittance of the various electrospun nanofibers using spectrophotometers interfaced with integrating spheres in the ultraviolet, visible, near-infrared, and mid-infrared wavelengths. The presentation will also describe the design and analysis, fabrication of the nanofibers using electrospinning, and several experimental characterization techniques to determine suitability for space applications. The nanofibers are tested using various tools to determine their suitability for cryogenic applications in space. Lastly, the samples were tested under low vacuum conditions and exposing them to sunlight inside a vacuum chamber maintained at 300 K. Relative to the incoming solar flux (1000 W/m2), only 1% of the energy was absorbed under these operating conditions. With further optimization and testing under high vacuum cryogenic environments, the samples could demonstrate much lower absorption or higher reflection of incoming solar radiation, which can translate to low temperatures suitable for cryogen storage.

Chieloka Ibekwe↗

DOE OSTI2025

Gas Hydrate Film Growth in Microfluidic Channels for Carbon Dioxide Capture and Sequestration Applications

Gas or clathrate hydrates are a solid, crystalline compound composed of water and guest molecules that typically form at high pressure and low temperature conditions. Carbon dioxide (CO2) hydrates may be involved in several carbon dioxide capture and sequestration (CCS) applications, including CO2 pipeline transportation and CO2 offshore sequestration. Within these applications, the formation mechanism and kinetics must be well understood to manage the CCS processes, either by preventing or promoting hydrate formation. In this work, a high-pressure glass microfluidic reactor is used in tandem with visual microscopy and in-situ Raman spectroscopy to study both the morphological and kinetic behavior of gas hydrate crystals. Subcooling, pressure, and CO2 flow rate are investigated for their impact on the thickening behavior of pure CO2 hydrates, with flow rate being the only parameter to have a significant effect. Visual and Raman spectroscopy evidence show that both a dense hydrate layer and a porous hydrate layer form, and the latter may provide a path for mass transfer to continue hydrate crystallization. A first principles mass transfer model is developed to describe CO2 hydrate crystal thickening at the interface between gas and water. The impacts of gas impurities and channel wettability are also studied. This method is further applied to investigate the conversion of methane hydrate to CO2 hydrate for combined energy recovery and methane hydrate formation. The authors acknowledge the US Department of Energy Basic Energy Science award # DE-SC0022162.

Wadsworth, Lindsey [Colorado School of Mines, Gold↗

DOE OSTI2024

Endothermic Charge Separation Occurs Spontaneously in Non–Fullerene Acceptor/Polymer Bulk Heterojunction

Organic photovoltaics (OPVs) based on non-fullerene acceptors (NFAs) have achieved a power conversion efficiency close to 20%. These NFA OPVs can generate free carriers efficiently despite a very small energy level offset at the donor/acceptor interface. Why these NFAs can enable efficient charge separation (CS) with low energy losses remains an open question. Here, the CS process in the PM6:Y6 bulk heterojunction is probed by time-resolved two-photon photoemission spectroscopy. It is found that the CS, the conversion from bound charge transfer (CT) excitons to free carriers, is an endothermic process with an enthalpy barrier of 0.15 eV. The CS can occur spontaneously despite being an endothermic process, which implies that it is driven by entropy. It is further argued that the morphology of the PM6:Y6 film and the anisotropic electron delocalization restrict the electron and hole wavefunctions within the CT exciton such that they can primarily contact each other through point-like junctions. Furthermore, this configuration can maximize the entropic driving force.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Characterizing the surface compositions of supported bimetallic PtSn clusters: Effects of cluster-support interactions and surface adsorbates

PtSn bimetallic clusters on TiO2(110) and highly oriented pyrolytic graphite (HOPG) surfaces have been characterized by scanning tunneling microscopy, low energy ion scattering (LEIS), Xray photoelectron spectroscopy, and temperature programmed desorption (TPD); density functional theory (DFT) calculations have also been performed to better understand adsorption of CO and D2 on the PtSn surfaces. On TiO2 at coverages of 2 ML of Pt and 2 ML of Sn, exclusively bimetallic clusters are formed for both orders of deposition because clusters of the first metal completely cover the surface such that all atoms of the second metal are incorporated into the existing clusters. In contrast, on HOPG, the high mobility and weak cluster-support interactions on HOPG result in much larger 2 ML monometallic clusters (~30 Å high) that do not completely cover the surface, and deposition of the second metal produces larger clusters as well as smaller ones. Despite the difference in cluster morphologies for the different orders of deposition and supports, the LEIS experiments demonstrate that in all cases, the PtSn clusters are rich in Sn at the surface, as expected based on the lower surface free energy for Sn compared to Pt. Furthermore, the +0.2 eV shift in the Sn(3d5/2) binding energy observed on all surfaces in the presence of Pt is consistent with PtSn alloy formation. Deposition of 2 ML of Sn on TiO2 produces two-dimensional clusters with oxidation of Sn and reduction of titania at the clustersupport interface, but addition of Pt to the Sn clusters causes Sn to diffuse away from this interface, leaving Sn in the metallic state. TPD experiments on 2 ML Pt/TiO2 with increasing coverages of Sn show that the number of adsorption sites for D2 sharply decreases to nearly zero at 0.5 ML, while CO adsorption decreases to zero only at much higher Sn coverages of 2 ML. DFT studies for Sn modified Pt surfaces and bulk structures demonstrate that for CO adsorption at low Sn coverages (<0.25 ML), the strong Pt-CO interactions induce diffusion of Pt to the cluster surface and the formation of a bulk Pt3Sn alloy, whereas D2 adsorption does not lead to interactions with the Pt surface that are strong enough to induce alloy formation. A single Sn adatom prevents D2 adsorption on four neighboring Pt atoms via site-blocking and the donation of electron density to Pt.

Li, Fangliang↗

NASA NTRS1986

Kinetics and mechanism of corrosion of SiC by molten salts

Corrosion of sintered alpha-SiC under thin films of Na2CO3/CO2, Na2SO4/O2, and Na2SO4/SO3 was investigated at 1000 C. Chemical analysis was used to follow silicate and silica evolution as a function of time. This information coupled with morphology observations leads to a detailed corrosion mechanism. In all cases the corrosion reactions occur primarily in the first few hours. In the Na2CO3/CO2 case, rapid oxidation and dissolution lead to a thick layer of silicate melt in about 0.25 h. After this, silica forms a protective layer on the carbide. In the Na2SO4/O2 case, a similar mechanism occurs. In the Na2SO4/SO3 case, a porous nonprotective layer of SiO2 grows directly on the carbide, and a silicate melt forms above this. In addition, SiO2 and regenerated Na2SO4 form at the melt/gas interface due to reaction of silicate with SO3 and SO2 + O2. The reaction slows when the lower silica layer becomes nonporous.

Jacobson, N. S.↗

DOE OSTI2024

Fundamental benchmarking of the discharge properties of negative electrodes in lead acid batteries

The unprecedented scale of energy storage deployment needed to allow high penetration of intermittent renewable energy sources into the electrical grid places significant economic cost and performance targets on battery technologies. Lead batteries, owing to their highly abundant and inexpensive raw materials, can be considered an important solution to grid storage as long as they achieve high material utilization, fast recharge rates, and long cycle life. To address the limitations in material utilization, we need to revisit the electrochemical processes during the discharge step and answer the following question: what are the fundamental limits of the discharge reaction? In this work we discuss how well-defined lead metal surfaces with nanometer scale roughness allow us to resolve the accessible discharge capacity for both faradaic and non-faradaic processes as a function of electrolyte concentration and in the presence of traditional additives. The direct connection between PbSO 4 layer morphology and discharge rates gives us important insights on the mechanism of discharge as related to the dissolution and passivation events. In conclusion, this work sets the stage for reimagining the design of lead batteries with implications to grid storage applications.

25 ENERGY STORAGE↗

NASA NTRS1987

Effect of LID (Registered) processing on the microstructure and mechanical properties of Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo titanium foil-gauge materials

A study was undertaken to determine the mechanical properties and microstructures resulting from Liquid Interface Diffusion (LID -Registered) processing of foil-gauge specimens of Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo coated with varying amounts of LID material. In addition, the effects of various elevated temperature exposures on the concentration profiles of the LID alloying elements were investigated, using specimens with a narrow strip of LID material applied to the surface. Room and elevated temperature tensile properties were determined for both coated and uncoated specimens. Optical microscopy was used to examine alloy microstructures, and scanning electron microscopy to examine fracture surface morphologies. The chemical concentration profiles of the strip-coated specimens were determined with an electron microprobe.

Balckburn, Linda B.↗

DOE OSTI2025

Dual-Responsive Macromolecular Surfaces with Binary Patterns

The development of nanopatterned interfaces incorporating multiple stimuli-responsive polymers has great potential for advancing smart sensors and molecular capture devices, yet it remains challenging due to limitations in patterning techniques and “grafting from” methods. Here, we present a binary-patterned surface featuring honeycomb-shaped photothermal polypyrrole (PPy) and thermally responsive poly(ethylene glycol methyl ether acrylate-co-poly(ethylene glycol) methyl ether acrylate) [poly(EGMEA-co-PEGMEA)] brushes within the cavities, fabricated using colloidal lithography and surface-initiated photoinduced electron transfer-reversible addition–fragmentation chain transfer (SI-PET-RAFT) polymerization. The morphology of the surface can be precisely tuned by adjusting the height of each domain. This design integrates unique topographical features with the stimuli-responsiveness of the polymer, enabling the collapse of the copolymer brushes through direct heating or photothermal conversion of PPy under near-IR light. In conclusion, this innovative system offers potential capture-release functionality, providing versatility for diverse applications and enhancing adaptability across different functional scenarios.

Copolymers↗