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At least 37 records · Page 2

REFRACTORY COMPACT HEAT EXCHANGERS WITH EMBEDDED SENSORS ENABLED BY HYBRID ADVANCED SINTERING AND ADDITIVE APPROACH

Structural health monitoring (SHM) of compact heat exchangers (CHXs) operating in extreme environments is essential for ensuring system reliability, safety, and longevity. This study presents the development of high-temperature sensors fabricated via aerosol jet printing (AJP) using platinum ink, selected for its exceptional thermal stability, oxidation resistance, and electrical conductivity. AJP enables precise deposition of fine-feature sensor patterns onto complex geometries, making it well-suited for integration within CHX architectures. To enhance sensor durability, an alumina-based ceramic protective layer was printed over the platinum sensing elements. The sensors demonstrated stable, repeatable performance up to 900?°C during extended thermal cycling. A custom test setup was developed to evaluate sensor accuracy and robustness under steady-state and transient conditions. Substrate screening identified HG-1 ceramic-coated stainless steel as the most effective platform, offering strong adhesion and low resistance. Furthermore, electric field-assisted sintering (EFAS) was employed to embed the sensors into stainless steel 316L matrices without degrading their functionality. Post-embedding electrical tests confirmed sensor integrity, and initial characterization suggests strong potential for in-situ monitoring. This work provides a scalable strategy for integrating high-performance temperature sensors directly into refractory components, advancing embedded SHM technologies for harsh operating environments.

36 - MATERIALS SCIENCE↗

Friction behavior of members of the platinum metals group with gold

The adhesion and friction behavior of the platinum metals group was examined with clean surfaces and surfaces selectively contaminated with oxygen, vinyl chloride (C2H3Cl), and methyl mercaptan (CH3SH). A pin or disk specimen configuration was used with the pin being a single crystal of gold of the (111) orientation and with the platinum metal disks also being single crystals of the (111) or (0001) orientation. Loads applied ranged from 1 to 10 g and a sliding velocity of 0.7 mm/min was employed. Results indicate adhesion and transfer of gold to all of the platinum metals. Despite this observation friction differences existed among the metals in the group. These differences are related to surface chemical activity. Adsorption of various friction reducing species was selective. With some adsorbates present strong adhesive forces between metals were still observed.

Buckley, D. H.↗

Residual Silicone Detection

Both photoelectron emission and ellipsometry proved successful in detecting silicone contamination on unpainted and epoxy painted metal surfaces such as those of the external tank and the solid rocket booster. Great success was achieved using photoelectron emission (PEE). Panels were deliberately contaminated to controlled levels and then mapped with PEE to reveal the areas and levels that were contaminated. The panels were then tested with regard to adhesive properties. Tapes were bonded over the contaminated and uncontaminated regions and the peel force was measured, or the contaminated panels were bonded (with CPR 483 foam) to uncontaminated panels and made into lap shear specimens. Other panels were bonded and made into wedge specimens for hydrothermal stress endurance tests. Strong adhesion resulted if the PEE signal fell within an acceptance window, but was poor outside the acceptance window. A prototype instrument is being prepared which can automatically be scanned over the external liquid hydrogen tank and identify those regions that are contaminated and will cause bond degradation.

Smith, T.↗

Truss beam having convex-curved rods, shear web panels, and self-aligning adapters

A truss beam comprised of a plurality of joined convex-curved rods with self-aligning adapters (SAA) adhesively attached at each end of the truss beam is disclosed. Shear web panels are attached to adjacent pairs of rods, providing buckling resistance for the truss beam. The rods are disposed adjacent to each other, centered around a common longitudinal axis, and oriented so that adjacent rod ends converge to at least one virtual convergence point on the common longitudinal axis, with the rods' curvature designed to increase prevent buckling for the truss beam. Each SAA has longitudinal bores that provide self-aligning of the rods in the SAA, the self-aligning feature enabling creation of strong adhesive bonds between each SAA and the rods. In certain embodiments of the present invention, pultruded unidirectional carbon fiber rods are coupled with carbon fiber shear web panels and metal SAA(s), resulting in a lightweight, low-cost but strong truss beam that is highly resistant to buckling.

Fernandez, Ian M.↗

Reflector coatings development (FY2020 End of Year Report)

X-ray detection instrumentation has been developed and manufactured at LANL for various DOE programs. One way to improve light collection efficiency, for a scintillator type detector, is to apply suitable reflectors. The coating capability and fabrication procedure for Al reflective coatings was established in FY19 at MST-7. Al reflective coatings with good stability, good adhesion to LSO, and reflectivity (R) up to 78% were fabricated. Materials with higher diffuse reflectivity (such as Teflon tape R=99%) are desirable. A literature search revealed a number of materials in the form of paint or free standing tape with diffuse R = 98- 99%. However, for the intended application such reflectors have to be applied in the form of a coating with strong adhesion to LSO crystals. The purpose of the FY20 project was to develop thin film coating techniques for PTFE (known as Teflon) reflectors and fabricate reflective coatings on provided LSO crystals.

36 MATERIALS SCIENCE↗

Adhesion and friction of iron and gold in contact with elemental semiconductors

Adhesion and friction experiments were conducted with single crystals of iron and gold in contact with single crystals of germanium and silicon. Surfaces were examined in the sputter cleaned state and in the presence of oxygen and a lubricant. All experiments were conducted at room temperature with loads of 1 to 50 grams, and sliding friction was at a sliding velocity of 0.7 mm/min. Results indicate that the friction nature of metals in contact with semiconductors is sensitive to orientation, that strong adhesion of metals to both germanium and silicon occurs, and that friction is lower with silicon than with germanium for the same orientation. Surface effects are highly sensitive to environment. Silicon, for example, behaves in an entirely brittle manner in the clean state, but in the presence of a lubricant the surface deforms plastically.

Buckley, D. H.↗

Vertically Aligned Carbon Nanotubes Grown on Copper Foil as Electrodes for Electrochemical Double Layer Capacitors

This study reports a binder-free, catalyst-free method for fabricating vertically aligned carbon nanotubes (VACNTs) directly on copper (Cu) foil using plasma-enhanced chemical vapor deposition (PECVD) for electrochemical double-layer capacitor (EDLC) applications. This approach eliminates the need for catalyst layers, polymeric binders, or substrate pre-treatments, simplifying electrode design and enhancing electrical integration. The resulting VACNTs form a dense, uniform, and porous array with strong adhesion to the Cu substrate, minimizing contact resistance and improving conductivity. Electrochemical analysis shows gravimetric specific capacitance (C grav ) and areal specific capacitance (C areal ) of 8 F g −1 and 3.5 mF cm −2 at a scan rate of 5 mV/s, with low equivalent series resistance (3.70 Ω) and charge transfer resistance (0.48 Ω), enabling efficient electron transport and rapid ion diffusion. The electrode demonstrates excellent rate capability and retains 92% of its initial specific capacitance after 3000 charge–discharge cycles, indicating strong cycling stability. These results demonstrate the potential of directly grown VACNT-based electrodes for high-performance EDLCs, particularly in applications requiring rapid charge–discharge cycles and sustained energy delivery.

25 ENERGY STORAGE↗

Broadband and omnidirectional polymer antireflection coatings

A method for generating antireflective coatings for polymeric substrates using a deposition process and/or a dissolving process can provide a coating onto the outer surface of the substrate. Some embodiments can include a GLAD generated fluoropolymer coating or a co-evaporated fluoropolymer coating on a substrate that may achieve ultralow refractive index as well as improved adhesion and durability properties on polymeric substrates. In some embodiments, the deposition process is performed such that a fluoropolymer can be evaporated to form chain fragments of the fluoropolymer. The chain fragments diffused into the substrate can subsequently re-polymerize, interlocking with the polymer chains of the substrate. In some embodiments, the co-evaporation process can form a nanoporous polymer chain scaffold of the fluoropolymer, from which a sacrificial material can be dissolved out. The formed coating can be a multilayer or continuously-graded antireflective coating that has strong adhesion with the substrate.

36 MATERIALS SCIENCE↗

Broadband and omnidirectional polymer antireflection coatings

A method for generating antireflective coatings for polymeric substrates using a deposition process and/or a dissolving process can provide a coating onto the outer surface of the substrate. Some embodiments can include a GLAD generated fluoropolymer coating or a co-evaporated fluoropolymer coating on a substrate that may achieve ultralow refractive index as well as improved adhesion and durability properties on polymeric substrates. In some embodiments, the deposition process is performed such that a fluoropolymer can be evaporated to form chain fragments of the fluoropolymer. The chain fragments diffused into the substrate can subsequently re-polymerize, interlocking with the polymer chains of the substrate. In some embodiments, the co-evaporation process can form a nanoporous polymer chain scaffold of the fluoropolymer, from which a sacrificial material can be dissolved out. The formed coating can be a multilayer or continuously-graded antireflective coating that has strong adhesion with the substrate.

Wang, Baomin↗

Tough and circular glass fiber composites via a tailored dynamic boronic ester interface

Glass fiber reinforced polymer (GFRP) composites are valued for their strength and cost-effectiveness. However, traditional GFRPs often face challenges for end-of-life recycling due to their non-depolymerizable thermoset matrices, and long-term performance due to inadequate interfacial adhesion, which can lead to fiber–matrix delamination. Here, in this work, we have designed dynamic fiber–matrix interfaces to allow tough and closed-loop recyclable GFRPs by utilizing a vitrimer, derived from upcycled polystyrene-b-poly(ethylene-co-butylene)-b-polystyrene (SEBS) with boronic ester (S-Bpin) and amine-based diol crosslinker. The boronic ester groups in S-Bpin form dynamic covalent bonds with the naturally present hydroxyl groups on the unsized GF surface, which eliminates the need for fiber sizing and enables facile closed-loop recyclability of both the fibers and the vitrimer matrix. The resulting strong fiber–matrix interface, depicted by the Raman mapping, leads to a 552% increase in-plane shear toughness (6.2 ± 0.3 MJ m -3 ) and 27% ultimate tensile strength (361 ± 89.2 MPa) compared to those of the conventional epoxy-based matrix (0.95 ± 0.05 MJ m -3 and 264 ± 59.7 MPa, respectively). The network rearrangement through dynamic boronic ester exchange enables fast thermoformability and repairability of micro-cracks at elevated temperatures. Additionally, both the matrix and composite demonstrate strong adhesion to various surfaces including steel and glasses exhibiting ≥6 MPa lap shear strength, which expands their suitability for diverse industrial applications. The readily created dynamic interface between boronic ester functionalized vitrimer and neat GFs presents a promising strategy for developing closed-loop recyclable, multifunctional structural materials, offering a sustainable alternative to non-recyclable thermoset GFRPs and contributes to a circular economy in composite materials.

36 MATERIALS SCIENCE↗

In‐Scribe Silane Bonding for Mechanical Reinforcement of Perovskite Photovoltaic Modules

Despite the extraordinary rise in power conversion efficiency over the last decade, metal halide perovskite (MHP) photovoltaics remain more mechanically fragile than other PV technologies. In this work, the scribe area, created by the monolithic interconnection of thin-film solar cells, is used to extrinsically reinforce the mechanical robustness of packaged MHP solar modules. In contrast to the epoxy-based chemistries often leveraged in the MHP literature, silane-grafted polyolefin encapsulants are designed to form strong covalent bonds to oxide surfaces, specifically to glass and the transparent conductive oxide at the base of the scribe line. Pseudo-modules encapsulated with silane-grafted polyolefin are measured with more than an order-of-magnitude enhancement infracture energy from 0.27 ± 0.01 J·m −2 (no scribes) to 5.97 ± 0.42 J·m −2 (scribes perpendicular to delamination directioncovering ≈2.2% of the module area). The silane-grafted polyolefin retains strong adhesion even after undergoing an accelerated IEC 61215 thermal cycling test consisting of 250 cycles. We find that the in-scribe bonding allows perovskite modules to have adhesion strength comparable to commercial c-Si and CdTe technologies with only 5% reduction in the active module area. This manufacturing-compatible approach offers a practical solution to address the mechanical integrity challenges in MHP solar modules, regardless of cell architecture.

14 SOLAR ENERGY↗

Electrolyte design for Li metal-free Li batteries

Li metal, with the lowest thermodynamically achievable negative electrochemical potential and the highest specific capacity (3860 mAh g -1 ), is the ultimate anode choice for Li batteries. However, the highest reported Li plating/stripping Coulombic efficiency (CE) of 99.5% after extensive efforts is still too low for the Li metal-free (all the Li metal in cycling comes from cathode, without anode pre-lithiation) Li metal batteries. The low CE is attributed to both non-uniform Li plating/stripping on the lithiophobic Cu current collector and Li dendrite growth through lithiophilic organic–inorganic solid electrolyte interphase (SEI) formed in carbonate electrolytes. Here, we use a lithiophilic Bismuth graphite blend (Bi–Gr) substrate to replace lithiophobic Cu current collector to seed a uniform Li nucleation, and form a lithiophobic LiF-rich SEI rather than lithiophilic organic-rich SEI to suppress Li dendrite growth. Molecular dynamics simulations reveal the preferential reduction of anions in 2.0 M LiPF 6 in tetrahydrofuran/2-methyl tetrahydrofuran (2.0 M LiPF 6 –mixTHF) electrolyte to generate LiF-rich SEI on plated Li. Bi–Gr substrate and 2.0 M LiPF 6 –mixTHF electrolyte enable the Li anodes to achieve a record high CE of 99.83% at a high capacity of 1.0 mAh cm -2 and current of 0.5 mA cm -2 . The Bi particles serve as dispersed nucleation centers that promote uniform Li deposition with strong adhesion to the substrate to avoid dead Li, while the lithiophobic LiF-rich SEI promotes lateral Li growth and suppresses the vertical Li dendrite growth even at a high current density of 3.0 mA cm -2 and high areal capacities of 3.0 mAh cm -2 . The regulation of Li nucleation and growth enables the Li metal-free LiFePO 4 full cells to achieve 100 cycles at a practical areal capacity of >2.0 mAh cm -2 . This article highlights the benefits of simultaneous substrate design to improve Li nucleation and electrolyte design to promote lithiophobic SEI growth, enabling a promising and practical route Li metal-free Li metal batteries.

36 MATERIALS SCIENCE↗

Tuning Fabrication Factors for Reduced Graphene Oxide Forward Osmosis Membranes

Forward osmosis (FO) may serve as a near-zero energy approach for wastewater management and selective chemical enrichment with an appropriate FO membrane. There is a need for novel FO membranes with better physical stability, chemical compatibility, and enhanced reverse flux selectivity. In this work, we have systematically studied a variety of factors for fabricating thermally reduced graphene oxide (RGO) FO filtration membranes and have demonstrated that with a comparable water flux, the RGO membranes have an exceptionally large reverse flux selectivity with 1.5 M sodium sulfate draw solution, about 7 times larger than that of cellulose triacetate membranes under the same testing condition. The interlayer spacing of the membranes can be fine-tuned by varying temperatures, so that the free interlayer spacing is less than 0.7 nm after exposure to water. The RGO-based membranes offer a few advantages with high reverse flux selectivity, mechanical robustness with strong adhesion to nylong support membranes without damage after FO tests and tape peel tests, and enhanced chromate and chlorine resistance. Finally, we have further demonstrated that in the FO processes, one can concentrate waste brine while simultaneously harvesting the osmotic energy as electricity, offering potential applications of forward osmosis-based osmotic batteries for powering electronic devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Understanding why poly(acrylic acid) works: decarbonylation and cross-linking provide an ionically conductive passivation layer in silicon anodes

Poly(acrylic acid) (PAA) is commonly used as a binder for fabricating silicon (Si) anode active materials in lithium-ion batteries due to its useful properties including high polar solvent solubility, good rheology, and strong adhesive properties. However, the role and evolution of PAA during electrode fabrication, cycling, and calendar aging are not well understood. In this work, we reveal the evolution of PAA during electrode curing and relate its chemical change to the final electrode properties and performance. These studies are made possible using two types of in situ attenuated total reflectance-infrared Fourier transform (ATR-FTIR) spectroscopy: thermal ATR-FTIR to probe the cross-linking reaction, and ATR-FTIR spectroelectrochemistry of three-dimensional composite electrodes, a unique technique developed herein that probes the solvation dynamics of lithium ions at the silicon anode interface under electrochemical polarization. Specifically, we show that PAA undergoes a thermally-mediated, cross-linking decarbonylation reaction to form an ether-based network polymer. To show the importance of the polyether moieties, we synthesize partially esterified PAA analogues that do not undergo this cross-linking decarbonylation reaction and correlate the degree of cross-linking to half-cell performance metrics. Finally, we unveil the mechanism of the polyether binder performance through in situ ATR-FTIR spectroelectrochemistry and show that PAA acts as an interfacial material that conducts lithium-ions, limits solvent molecule access to the Si surface, and stabilizes the electrode against parasitic lithium inventory loss at high state of charge for an extended period of time.

25 ENERGY STORAGE↗

Structured for success: conjugated polymer binders with tailored composition and architecture for lithium-ion batteries

Conjugated polymer binders are replacing conventional binders in lithium-ion batteries. Herein, we examine how molecular engineering and hierarchical nanostructuring govern binder functionality and electrochemical performance. Lithium-ion batteries (LIBs) are the leading energy storage technology, yet enhancing their energy density and cycle life remains critical. Significant progress has been made in high-capacity anodes and high-voltage cathodes, but their performance is hindered by electrode degradation, where it is related to the behaviors of binders at the surface and interface. Conventional non-conductive binders like poly(vinylidene difluoride) (PVDF), combined with conductive additives, often fail to maintain electrical pathways under repeated volume changes. Alternatively, conjugated polymer binders have emerged as a superior alternative, simultaneously offering intrinsic conductivity, mechanical flexibility, and strong adhesion through π-conjugated backbones and functional groups. Their tunable molecular structure enables efficient electron/ion transport while mitigating electrode cracking. Additionally, the development of hierarchically ordered nanostructures in conjugated polymer binder can further enhance their electrochemical performance. This review examines the design principles of conjugated polymer binders, focusing on molecular engineering and nanostructural control to optimize their performance in high-loading electrodes, such as silicon-based anodes. By addressing key challenges in binder functionality, these advanced materials pave the way for next-generation high-energy-density LIBs.

Jin, Xiuyu↗

Full-film dry transfer of MBE-grown van der Waals materials

Abstract Molecular beam epitaxy (MBE) has been used to create high-quality, large-scale two-dimensional van der Waals (2D vdW) materials. However, due to the strong adhesion between the substrate and deposited materials, the peel-off and dry transfer of MBE-grown vdW films onto other substrates has been challenging. This limits the study and use of MBE films for heterogeneous integration including stacked and twisted heterostructures. In this work, we develop a polymer-assisted dry transfer method and successfully perform full-film transfer of various MBE-grown 2D vdW materials including transition metal dichalcogenides, topological insulators and 2D magnets. In particular, we transfer air-sensitive 2D magnets, characterize their magnetic properties, and compare them with as-grown materials. The results show that the transfer technique does not degrade the magnetic properties, with the Curie temperature and hysteresis loops exhibiting similar behaviors after the transfer. Our results enable further development of heterogeneous integration of 2D vdW materials based on MBE growth.

Li, Ziling (ORCID:0000000203537036)↗

Bioadhesive polymer semiconductors and transistors for intimate biointerfaces

The use of bioelectronic devices relies on direct contact with soft biotissues. For transistor-type bioelectronic devices, the semiconductors that need to have direct interfacing with biotissues for effective signal transduction do not adhere well with wet tissues, thereby limiting the stability and conformability at the interface. Here we report a bioadhesive polymer semiconductor through a double-network structure formed by a bioadhesive brush polymer and a redox-active semiconducting polymer. The resulting semiconducting film can form rapid and strong adhesion with wet tissue surfaces together with high charge-carrier mobility of ~1 square centimeter per volt per second, high stretchability, and good biocompatibility. Further fabrication of a fully bioadhesive transistor sensor enabled us to produce high-quality and stable electrophysiological recordings on an isolated rat heart and in vivo rat muscles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Polymer-assisted transfer of MBE-grown van der Waals materials

Molecular beam epitaxy (MBE) has been used to create high-quality, large-scale two-dimensional van der Waals (2D vdW) materials. However, due to the strong adhesion between the substrate and deposited materials, the peel-off and dry transfer of MBE-grown vdW films onto other substrates has been challenging. This limits the study and use of MBE films for heterogeneous integration including stacked and twisted heterostructures. In this work, we develop a polymer-assisted dry transfer method and successfully perform full-film transfer of various MBE-grown 2D vdW materials including transition metal dichalcogenides (TMD), topological insulators (TI) and 2D magnets. In particular, we transfer air-sensitive 2D magnets, characterize their magnetic properties, and compare them with as-grown materials. The results show that the transfer technique does not degrade the magnetic properties, with the Curie temperature and hysteresis loops exhibiting similar behaviors after the transfer. Our results enable further development of heterogeneous integration of 2D vdW materials based on MBE growth.

Li, Ziling [The Ohio State University]↗