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DOE OSTI2024

Spontaneous Supercrystal Formation During a Strain‐Engineered Metal–Insulator Transition

Abstract Mott metal–insulator transitions possess electronic, magnetic, and structural degrees of freedom promising next‐generation energy‐efficient electronics. A previously unknown, hierarchically ordered, and anisotropic supercrystal state is reported and its intrinsic formation characterized in‐situ during a Mott transition in a Ca 2 RuO 4 thin film. Machine learning‐assisted X‐ray nanodiffraction together with cryogenic electron microscopy reveal multi‐scale periodic domain formation at and below the film transition temperature ( T Film ≈ 200–250 K) and a separate anisotropic spatial structure at and above T Film . Local resistivity measurements imply an intrinsic coupling of the supercrystal orientation to the material's anisotropic conductivity. These findings add a new degree of complexity to the physical understanding of Mott transitions, opening opportunities for designing materials with tunable electronic properties.

Gorobtsov, Oleg Yu.↗

DOE OSTI2021

Thermomechanical and sequential stress performance of photovoltaic backsheets

Photovoltaic backsheet technology is utilized to protect the interior components of solar modules from environmental stress as well as provide electrical insulation to the module. The growing demand for solar energy and longer module service life requirements have brought backsheet performance into focus. Despite being a protective packaging material, many backsheets have exhibited failure in the field, limiting the performance and service life of entire modules. Most backsheets consist of multiple polymeric layers laminated together using adhesives. A new backsheet, with a high performance polyamide structure, has been developed as the solution to module failure. Primarily, it contains a unique polyamide-ionomer alloy targeted at improved weather resistance. In this study, several photovoltaic industry standard backsheets, and the novel polyamide compositions of multilayered backsheets fabricated from the coextrusion process, were examined using thermomechanical analysis (TMA). The coefficient of thermal expansion (CTE) for entire backsheets and their constituent layers was used to model the thermomechanical behavior of various backsheet constructions. Subsequently, thermal cycling was performed in the TMA to examine the intrinsic thermal behavior of the backsheets. Thermal cycling in the TMA indicates the resilience and dimensional stability in the coextruded structures as opposed to the laminated structures. Lastly, results from a Module Accelerated Sequential Testing (MAST), are included to show the mechanical integrity of these backsheets after sequential exposure to stressors including damp heat, ultra-violet (UV) light radiation, and thermal cycling. The laminate backsheets deteriorated extensively after sequential exposure to these stressors, while the novel coextruded structures retained their physical properties.

14 SOLAR ENERGY↗

DOE OSTI2024

Giant Anisotropic Magnetoresistance in Few-Layer α-RuCl 3 Tunnel Junctions

The spin–orbit-assisted Mott insulator α-RuCl 3 is proximate to the coveted quantum spin liquid (QSL) predicted by the Kitaev model. In the search for the pure Kitaev QSL, reducing the dimensionality of this frustrated magnet by exfoliation has been proposed as a way to enhance magnetic fluctuations and Kitaev interactions. Here, in this work, we perform angle-dependent tunneling magnetoresistance (TMR) measurements on ultrathin α-RuCl 3 crystals with various layer numbers to probe their magnetic, electronic, and crystal structures. We observe a giant change in resistance, as large as ~2500%, when the magnetic field rotates either within or out of the α-RuCl 3 plane, a manifestation of the strongly anisotropic spin interactions in this material. In combination with scanning transmission electron microscopy, this tunneling anisotropic magnetoresistance (TAMR) reveals that few-layer α-RuCl 3 crystals remain in the high-temperature monoclinic phase at low temperatures. It also shows the presence of a zigzag antiferromagnetic order below the critical temperature T N ≃ 14 K, which is twice the one typically observed in bulk samples with rhombohedral stacking. Our work offers valuable insights into the relation between the stacking order and magnetic properties of this material, which helps lay the groundwork for creating and electrically probing exotic magnetic phases such as QSLs via van der Waals engineering.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1985

Transformation toughened ceramics for the heavy duty diesel engine technology program, phase 2

The objective of this program is to develop an insulating structural ceramic for application in a heavy duty adiabatic diesel engine. The approach is to employ transformation toughening (TT) by additions of zirconia-hafnia solid solution (ZHSS). The feasibility of using ZHSS as a toughening agent in mullite and alumina has been demonstrated in Phase 1 of this work. Based on Phase 1 results, a decision was made to concentrate the Phase 2 effort on process optimization of the TT mullite. A strong factor in that decision was the low thermal conductivity and high thermal shock resistance of the mullite. Results of the Phase 2 effort indicate that optimum toughening of mullite by additions of ZHSS is difficult to achieve due to apparent sensitivity to morphology. The 48 ksi room temperature modulus-of-rupture (MOR) achieved in selected specimens is approximately 50% of the original strength target. The MOR deteriorated to 34 ksi at 800 C.

Musikant, S.↗

DOE OSTI2024

Tailoring-Orientated Deposition of Li 2 S for Extreme Fast-Charging Lithium–Sulfur Batteries

Precipitation/dissolution of insulating Li 2 S has long been recognized as the rate-determining step in lithium-sulfur (Li-S) batteries, which dramatically undermines sulfur utilization at elevated charging rates. Herein, we present an orientated Li 2 S deposition strategy to achieve extreme fast charging (XFC, ≤15 min) through synergistic control of porosity, electronic conductivity, and anchoring sites of electrode substrate. Via magnesiothermic reduction of a zeolitic imidazolate framework, a nitrogen-doped and hierarchical porous carbon with highly graphitic phase was developed. This design effectively reduces interfacial resistance and ensures efficient sequestration of polysulfides during deposition, leading to (110)-preferred growth of Li 2 S nanocrystalline between (002)-dominated graphitic layers. Our approach directs an alternative Li 2 S deposition pathway to the commonly reported lateral growth and 3D thickening growth mode, ameliorating the electrode passivation. Therefore, a Li-S cell capable of charging/discharging at 5C (12 min) while maintaining excellent cycling stability (82% capacity retention) for 1000 cycles is demonstrated. In conclusion, even under high S loading (8.3 mg cm -2 ) and low electrolyte/sulfur ratio (3.8 mL mg -1 ), the sulfur cathode still delivers a high areal capacity of >7 mAh cm -2 for 80 cycles.

25 ENERGY STORAGE↗

DOE OSTI2024

Magnetotransport of Sm 2 Ir 2 O 7 across the pressure-induced quantum-critical phase boundary

Rare-earth pyrochlore iridates host two interlocking magnetic sublattices of corner-sharing tetrahedra and can harbour a unique combination of frustrated moments, exotic excitations and highly correlated electrons. They are also the first systems predicted to display both topological Weyl semimetal and axion insulator phases. We have measured the transport and magnetotransport properties of single-crystal Sm 2 Ir 2 O 7 up to and beyond the pressure-induced quantum critical point for all-in-all-out (AIAO) Ir order at p c = 63 kbar previously identified by resonant X-ray scattering and close to which Weyl semimetallic behavior has been previously predicted. Our findings overturn the accepted expectation that the suppression of AIAO order should lead to metallic conduction persisting down to zero temperature. Instead, the resistivity-minimum temperature, which tracks the decrease in the AIAO ordering temperature for pressures up to 30 kbar, begins to increase under further application of pressure, pointing to the presence of a second as-yet unidentified mechanism leading to non-metallic behavior. The magnetotransport does track the suppression of Ir magnetism, however, with a strong hysteresis observed only within the AIAO phase boundary, similar to that found for Ho 2 Ir 2 O 7 and attributed to plastic deformation of Ir domains. Around pc we find the emergence of a new type of electronic phase, characterized by a negative magnetoresistance with small hysteresis at the lowest temperatures, and hysteresis-free positive magnetoresistance above approximately 5K. The temperature dependence of our low-temperature transport data are found to be best described by a model consistent with a Weyl semimetal across the entire pressure range.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Magnetotransport of Sm 2 Ir 2 O 7 across the pressure-induced quantum-critical phase boundary

Rare-earth pyrochlore iridates host two interlocking magnetic sublattices of corner-sharing tetrahedra and can harbour a unique combination of frustrated moments, exotic excitations and highly correlated electrons. They are also the first systems predicted to display both topological Weyl semimetal and axion insulator phases. We have measured the transport and magnetotransport properties of single-crystal Sm 2 Ir 2 O 7 up to and beyond the pressure-induced quantum critical point for all-in-all-out (AIAO) Ir order at $p_c$ = 63 kbar previously identified by resonant X-ray scattering and close to which Weyl semimetallic behavior has been previously predicted. Our findings overturn the accepted expectation that the suppression of AIAO order should lead to metallic conduction persisting down to zero temperature. Instead, the resistivity-minimum temperature, which tracks the decrease in the AIAO ordering temperature for pressures up to 30 kbar, begins to increase under further application of pressure, pointing to the presence of a second as-yet unidentified mechanism leading to non-metallic behavior. The magnetotransport does track the suppression of Ir magnetism, however, with a strong hysteresis observed only within the AIAO phase boundary, similar to that found for Ho 2 Ir 2 O 7 and attributed to plastic deformation of Ir domains. Around $p_c$ we find the emergence of a new type of electronic phase, characterized by a negative magnetoresistance with small hysteresis at the lowest temperatures, and hysteresis-free positive magnetoresistance above approximately 5 K. The temperature dependence of our low-temperature transport data are found to be best described by a model consistent with a Weyl semimetal across the entire pressure range.

36 MATERIALS SCIENCE↗

NASA NTRS2005

Pressure Vessel with Impact and Fire Resistant Coating and Method of Making Same

An impact and fire resistant coating laminate is provided which serves as an outer protective coating for a pressure vessel such as a composite overwrapped vessel with a metal lining. The laminate comprises a plurality of fibers (e.g., jute twine or other, stronger fibers) which are wound around the pressure vessel and an epoxy matrix resin for the fibers. The epoxy matrix resin including a plurality of microspheres containing a temperature responsive phase change material which changes phase in response to exposure thereof to a predetermined temperature increase so as to afford increased insulation and hear absorption.

Thomas K DeLay↗

NASA NTRS2005

Pressure vessel with impact and fire resistant coating and method of making same

DeLay, Thomas K.↗

NASA NTRS2007

Thermal Properties of Double-Aluminized Kapton at Low Temperatures

Double-aluminized kapton (DAK) is commonly used in multi-layer insulation blankets in cryogenic systems. NASA plans to use individual DAK sheets in lightweight deployable shields for satellites carrying instruments. A set of these shields will reflect away thermal radiation from the sun, the earth, and the instrument's warm side and allow the instrument's cold side to radiate its own heat to deep space. In order to optimally design such a shield system, it is important to understand the thermal characteristics of DAK down to low temperatures. We describe experiments which measured the thermal conductivity and electrical resistivity down to 4 Kelvin and the emissivity down to 10 Kelvin.

Tuttle, J.↗

NASA NTRS1984

Ceramic-coated metals can survive contact with hot working fluid

Thermal barrier coatings (TBCs) have been developed as a means of protecting turbine blades and other engine hot section components whose surfaces are exposed to the most extreme operating conditions. By adding a thin, insulating ceramic oxide layer to an air-cooled turbine blade, the difference between the gas temperature and the metal temperature is further increased as a function of ceramic coating thickness, heat flux, and oxide thermal conductivity. An 0.04-cm thick ceramic layer can typically yield a 100-300 C temperature drop. Of the various techniques available for the deposition of thermal barrier coatings, the most common is that of plasma spraying. Significant improvements have been made in TBC durability through the use of bond coat compositions with increased oxidation resistance.

Levine, S. R.↗

NASA NTRS2008

The Characterization of the Selected Materials for Space Shuttle

The harsh conditions to which the Space Shuttles are exposed during flight required the development and use of many unique materials. These materials were specially designed to withstand extreme temperatures, in some cases over 1600 C, while other material must withstand the cryogenic conditions of -253 C, and others must operate while under extreme loads. All of these materials must not only operate in the harsh condition but they must be light weight as well. The Space Shuttle is composed of three major components when configured for launch, Figure 1; the Shuttle, solid rocket boosters, and external tank (ET). The different heat shields of the Shuttle make up the thermal protection system (TPS); this system consists of many different types of components designed to operate on various parts of the vehicle. The body of the Shuttle and ET are composed mainly of aluminum alloy and graphite epoxy. The TPS consists of reinforced carbon-carbon (RCC) used on the wing leading edges and nose cap areas while the upper forward fuselage areas, the entire underside of the Shuttle, the Orbiter maneuvering system, and reaction control system utilize blacc high temperature reusable surface insulation (HRSI) tiles, Figure 2. Other areas of the Orbiter are protected by fibrous refractory composite insulation (FRCI) tiles. Areas where the temperature stays below 649 C, such as the forward fuselage, mid-fuselage, aft fuselage, vertical tail, and upper wing, are protected by other material such as, white low temperature reusable surface insulation (LRSI) tiles, advanced flexible reusable surface insulation (AFRSI) blankets, and felt reusable surface insulation (FRSI) white blankets. The RCC is a pyrolized laminated carbon with the outer surface converted to silicon carbide to prevent oxidation. The FiRST tiles are made of a low-density, high purity silica 99.8-percent amorphous fiber insulation that is made rigid by ceramic bonding resulting in 90-percent void and 10-percent materials. The RCC and HRSI are used in areas where the temperature rises above 1260 T. The FRCI tiles are high strength tiles derived by adding alumina-bososilicate fiber to the pure silica tile slurry that welds the micron-sizes fibers of pure silica into a rigid structure during sintering. The FRCI is composed of 20-percent alumina-borosilicate fibers and 80-percent silica fibers, and provided improved strength, durability and resistance to coating cracking and weight reduction than HRSI.

Kim, Hae-Soo↗

DOE OSTI2021

Method and apparatus for an insulating glazing unit and compliant seal for an insulating glazing unit

A vacuum insulating glazing unit (VIGU) comprises two or more glass lites (panes) spaced apart from one another and hermetically bonded to an edge seal assembly therebetween. The resulting cavity between the lites is evacuated to create at least one insulating vacuum cavity within which are disposed a plurality of stand-off members to maintain separation between the lites. The edge seal assembly is preferably compliant in the longitudinal (i.e., edgewise) direction to allow longitudinal relative motion between the two lites (e.g., from thermal expansion). The longitudinal compliance may be obtained by imprinting a three-dimensional pattern into the edge seal material. The edge seal assembly is preferably bonded to the lites with a first bond portion that is hermetic and a second bond portion that is load-resistant. Methods for producing VIGUs and/or compliant edge seal assemblies and VIGU and edge seal apparatus are disclosed.

Francis, William H.↗

DOE OSTI2021

From weak antilocalization to Kondo scattering in a magnetic complex oxide interface

Quantum corrections to electrical resistance can serve as sensitive probes of the magnetic landscape of a material. For example, interference between time-reversed electron paths gives rise to weak localization effects, which can provide information about the coupling between spins and orbital motion, while the Kondo effect is sensitive to the presence of spin impurities. In this work, we use low-temperature magnetotransport measurements to reveal a gradual transition from weak antilocalization (WAL) to Kondo scattering in the quasi-two-dimensional electron gas formed at the interface between SrTiO 3 and the Mott insulator NdTiO 3 . This transition occurs as the thickness of the NdTiO 3 layer is increased. Analysis of the Kondo scattering and WAL points to the presence of atomic-scale magnetic impurities coexisting with nanoscale magnetic regions that affect transport via a strong magnetic exchange interaction. This leads to distinct magnetoresistance behaviors that can serve as a sensitive probe of magnetic properties in two dimensions.

36 MATERIALS SCIENCE↗

NASA NTRS1981

A test and instrumentation system for the investigation of degradation of electrical insulating materials

A comprehensive test apparatus has been developed for the evaluation of the effects of thermal cycling, high temperatures and high electric fields on the quality and stability of electrical insulating materials used in spacecraft systems. The system includes a test chamber in which the specimen can be subjected to thermal and electrical stresses encountered in the space environment (temperatures from -50 to 200 C and voltages from 0 to 10 kV rms, respectively) simultaneously. The system instrumentation includes provisions for the measurement of the change in capacitance, the thermal dissipation factor of the material, and complex dielectric constants with changes in temperature, corona intensity and voltages at frequencies from 22 kHz to 70 MHz, as well as the volume and surface resistivities of the materials.

Doreswamy, C. V.↗

NASA NTRS2000

Experimental and Numerical Characterization of a Cylindrical Blackbody Cavity

During hypersonic flight, high temperatures and high heat fluxes are generated on the surfaces of vehicles. The Flight Loads Laboratory (FLL) at Dryden Flight Research Center (DFRC) is equipped with a calibration furnace, capable of calibrating heat flux gages up to 1100kW per square meters, and temperature sensors up to 2600 C. One heating configuration of the calibration furnace is a cylindrical blackbody cavity. Throughout the blackbody there are temperature gradients due to various boundary conditions. These boundary conditions include resistance heating, radiant heat transfer, and conduction to water-cooled electrodes. Also, an inert gas is purged through the graphite blackbody to prevent it from oxidizing. Consequently, the various modes of heat transfer present during operation of the blackbody cavity must be well understood in order to produce accurate heat flux gage and temperature sensor calibrations for use in ground testing or flight testing of hypersonic vehicles. The first step towards understanding the heat transfer in the blackbody cavity was to perform experiments at 1100 C, with and without outer surface insulation, while taking detailed temperature measurements inside the blackbody cavity. Steady state thermal models of the blackbody cavity were then developed. These models included detailed thermal analysis using commercial thermal analysis software. Conduction, radiation, and convection were considered in the thermal models for two cases: one with the outside of the blackbody cavity insulated and the second without insulation. This paper describes the experimental and numerical efforts used to characterize the steady state operation of the blackbody cavity. It describes the analysis of the test measurements, the boundary conditions used in the numerical models, and how the models were calibrated to fit the experimental data. Effects of various uncertainties, such as material properties, and convection are discussed.Initial thermal models predicted temperatures in the deepest part of the blackbody cavity within 7 C of the measured value and produced trends comparable to the experimental data, throughout the models. Adjustment of the boundary conditions, which were included in the thermal models, produced good agreement with measured temperatures. Free and forced convection of the purge gas inside the blackbody was found to be insignificant.

Abdelmessih, Amanie N.↗

NASA NTRS2000

Polymeric Coatings for Electrodynamic Tethers

Two polymeric coatings have been developed for the Propulsive Small Expendable Deployer System (ProSEDS) mission. ProSEDS is designed to provide an on-orbit demonstration of the electrodynamic propulsion capabilities of tethers in space. The ProSEDS experiment will be a secondary payload on a Delta II unmanned expendable booster scheduled for launch in August 2000. A 5-km conductive tether is attached to the Delta 11 second stage and collects current from the low Earth orbit (LEO) plasma to facilitate de-orbit of the spent stage. The conductive tether is attached to a 10-km non-conductive tether, the other end of which is attached to an endmass containing several scientific instruments. A bare metal tether would have the best conductivity but thermal concerns preclude this design. A conductive polymer developed by Triton Systems has been optimized for conductivity and thermo-optical properties. The current design for the ProSEDS conductive tether is seven strands of 28 AWG aluminum wire individually coated with 8.7 micrometers (0.35 mil) of an atomic oxygen-resistant conductive polymer composed of a mixture of 87% Clear Oxygen-Resistant polymer (COR) and 13% polyanaline (PANi), wrapped around a braided Kevlar (TM) 49 core. Extensive testing has been performed at the Marshall Space Flight Center (MSFC) to qualify this material for flight on ProSEDS. Atomic oxygen exposure was performed, with solar absorptance and infrared emittance measured before and after exposure. Conductivity was measured before and after atomic oxygen exposure. High voltage tests, up to 1500 V, of the current collecting ability of the COR/PANi have been completed. Approximately 160 meters of the conductive tether closest to the Delta 11 second stage is insulated to prevent any electron reconnection to the tether from the plasma contactor. The insulation is composed of polyimide overcoated with TOR-BP, another polymeric coating developed by Triton for this mission. TOR-BP acts as both insulator and a protective coating against atomic oxygen erosion. The insulation has been tested to withstand 5000 V.

Vaughn, Jason A.↗

NASA NTRS1994

Modeling Thermal Contact Resistance

One difficulty in using cryocoolers is making good thermal contact between the cooler and the instrument being cooled. The connection is often made through a bolted joint. The temperature drop associated with this joint has been the subject of many experimental and theoretical studies. The low temperature behavior of dry joints have shown some anomalous dependence on the surface condition of the mating parts. There is also some doubts on how well one can extrapolate from the test samples to predicting the performance of a real system. Both finite element and analytic models of a simple contact system have been developed. The model assumes (a) the contact is dry (contact limited to a small portion of the total available area and the spaces in-between the actual contact patches are perfect insulators), (b) contacts are clean (conductivity of the actual contact is the same as the bulk), (c) small temperature gradients (the bulk conductance may be assumed to be temperature independent), (d) the absolute temperature is low (thermal radiation effects are ignored), and (e) the dimensions of the nominal contact area are small compared to the thickness of the bulk material (the contact effects are localized near the contact). The models show that in the limit of actual contact area much less than the nominal area (a much less than A), that the excess temperature drop due to a single point of contact scales as a(exp -1/2). This disturbance only extends a distance approx. A(exp 1/2) into the bulk material. A group of identical contacts will result in an excess temperature drop that scales as n(exp -1/2), where n is the number of contacts and n dot a is constant. This implies that flat rough surfaces will have a lower excess temperature drop than flat polished surfaces.

Kittel, Peter↗