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DOE OSTI2023

Heterogeneous Structural Evolution of In–Zn–O Thin Films during Annealing

Amorphous In-Zn-O (a-IZO) thin films are among the most promising transparent conducting materials. Applications of a-IZO include thin film transistors for display technology and photovoltaic devices. However, the use of this material in practical devices has been impeded by limitations in our understanding of the relationship between a-IZO film structure and electrical properties. Here, we use in situ X-ray reflectivity to provide experimental evidence for a vertically heterogeneous, thermally induced structural relaxation that had been predicted for amorphous oxide films but not previously observed. The structural relaxation is shown to be dependent on the thermal annealing environment. Complementary in situ current-voltage curves and ex situ Van der Pauw measurements further show that thermal annealing also influences the electrical performance of the films. Here our results suggest that both oxygen uptake and structural relaxation contribute to the reduction in free carriers within a-IZO films during postdeposition processing. The structural heterogeneity and loss of carriers that occur during thermal annealing are only partly reversible. We anticipate that this insight into the structure-processing-property relationships within a-IZO will help to enable a-IZO-based devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2018

Optimization of Thin-Film Solar Cells for Lunar Surface Operations

Thin-film solar cells have been in production for decades, but technology has only recently advanced enough to allow for comparable efficiencies to traditional rigid cells. Some of the benefits of thin-films, such as lighter weight and being foldable, are particularly advantageous to space applications since mass and volume are key considerations of any flight project. Using these thin-film cells in space, however, is outside of their ground-based design criteria. This requires special care to be taken in designing the power generation system of a spacecraft around a thin-film solar cell, particularly in regards to thermal management. Without the diffusion of an atmosphere to mitigate solar load, the temperature of the panels can rapidly exceed their design specification. In this paper a design solution is presented that allows for thin-film solar cells to be used in a robotic lunar lander. Due to the low thermal mass and in-plane conductivity of thin films, it is difficult to remove waste heat by any other method than radiation. On the lunar surface this means angling the arrays to increase their view factor to space, which has the negative consequence of decreasing their power generation. An optimization was developed to balance the heat rejection and power generation of the cells, using constraints on the maximum cell temperature and minimum spacecraft power requirements. The resulting solar panel angle was then used as an input to the Thermal Desktop model to verify the final panel temperatures.

Breeding, Shawn↗

DOE OSTI2020

Temperature and processing effects on lithium ion conductivity of solution‐deposited lithium zirconium phosphate (LiZr 2 P 3 O 12 ) thin films

Abstract Lithium zirconium phosphate (LiZr 2 P 3 O 12 ) thin films have been prepared on platinized silicon substrates via a chemical solution deposition approach with processing temperatures between 700°C and 775°C. Films that were subject to a single high‐temperature anneal were found to crystallize at temperatures above 725°C. Crystallization was observed in films annealed after each deposited layer at 700°C and above. In both cases, grain size was found to increase with annealing temperature. Ion conductivity was found to increase with annealing temperature in singly annealed films. In per‐layer annealed films ion conductivity was found to initially increase then decrease with increasing annealing temperature. A maximum ion conductivity of 1.6 × 10 −6 S/cm was observed for the singly annealed 775°C condition, while a maximum ion conductivity of 5.8 × 10 −7 S/cm was observed for the 725°C per‐layer annealed condition. These results are consistent with an increasing influence of cross‐plane, internal interface resistance and vapor phase carrier loss in the per‐layer annealed samples. This work demonstrates that post‐deposition processing methods can strongly affect the ion conducting properties of LiZr 2 P 3 O 12 thin films.

Brummel, Ian A.↗

DOE OSTI2021

Instrument for spatially resolved, temperature-dependent electrochemical impedance spectroscopy of thin films under locally controlled atmosphere

We demonstrate an instrument for spatially resolved measurements (mapping) of electrochemical impedance under various temperatures and gas environments. Automated measurements are controlled by a custom LabVIEW program, which manages probe motion, sample motion, temperature ramps, and potentiostat functions. Sample and probe positioning is provided by stepper motors. Dry or hydrated atmospheres (air or nitrogen) are available. The configurable heater reaches temperatures up to 500 °C, although the temperature at the sample surface is moderated by the gas flow rate. The local gas environment is controlled by directing flow toward the sample via a glass enclosure that surrounds the gold wire probe. Software and hardware selection and design are discussed. Reproducibility and accuracy are quantified on a Ba(Zr,Y)O 3-δ proton-conducting electrolyte thin film synthesized by pulsed laser deposition. The mapping feature of the instrument is demonstrated on a compositionally graded array of electrocatalytically active Ba(Co,Fe,Zr,Y)O 3-δ thin film microelectrodes. The resulting data indicate that this method proficiently maps property trends in these materials, thus demonstrating the reliability and usefulness of this method for investigating electrochemically active thin films.

47 OTHER INSTRUMENTATION↗

DOE OSTI2025

Controlled phosphate doping into nanoscopic SiO 2 proton conducting membranes

This article describes a method to introduce phosphate (PO 4 ) into SiO 2 atomic layer deposition (ALD) films in a self-limiting fashion. The method involves the use of a less common phosphate precursor, trimethyl phosphite [P(OMe) 3 ], to introduce PO 4 as a low-level dopant, <1 at. %, into a SiO 2 ALD process using bis(ethylmethylamino)silane and a modified O 3 conversion. P(OMe) 3 does not deposit a film with typical oxygen sources but incorporates as PO 4 in an ABC-type ALD scheme at deposition temperatures ranging from 100 to 300 °C. Addition of up to ∼1 at. % of PO 4 does not significantly impact the film density or concentrations of carbon and nitrogen impurities, which are both <0.4 at. %. Despite the relatively low dopant concentrations, PO 4 incorporation is shown to have a large impact on transport properties of the film. When explored as proton (H + )-conducting membranes, undoped SiO 2 ALD films showed H + conductivities (3 × 10 −6 –8 × 10 −5 S cm −1 ) and low H 2 permeabilities (<10 −9 cm 2 s −1 ) when measured at room temperature. The addition of PO 4 is shown to increase H + conductivity to 2 × 10 −4 S cm −1 , while maintaining low H 2 permeability of <10 −9 cm 2 s −1 . The ratio of H + conductivity to H 2 permeability, a key performance metric for H + -conducting membranes used in water electrolyzers, exceeds that of commercial Nafion-117 membranes. Here, the moderate H + conductivity and very low H 2 permeability of PO 4 -doped SiO 2 films make them promising candidates as fluorine-free replacements for Nafion in applications such as water electrolysis, hydrogen fuel cells, and redox flow batteries.

Atomic layer deposition↗

NASA NTRS2002

Development of Chemically and Thermally Robust Lithium Fast Ion Conducting Chalcogenide Glasses

In this project, a new research thrust into the development of an entirely new class of FIC glasses has begun that may lead to a new set of optimized thin-film lithium ion conducting materials. New chemically robust FIC glasses are being prepared that are expected to exhibit unusually high chemical and electrochemical stability. New thermally robust FIC glasses are being prepared that exhibit softening points in excess of 500 C which will dramatically expand the usable operating temperature range of batteries, fuel-cells, and sensors using such electrolytes. Glasses are being explored in the general compositional series xLi2S+ yGa2S3 + (1-x-y)GeS2. Li2S is added as the source of the conductive lithium ions. GeS2 is the base glass-forming phase and the trivalent sulfides, Ga2S3, is added to increase the "refractoniness" of the glass, that is to significantly increase the softening point of the glass as well as its chemical stability. By optimizing the composition of the glass, new glasses and glass-ceramic FIC materials have been prepared with softening points in excess of 500 C and conductivities above 10(exp -3)/Ohm cm at room temperature. These latter attributes are currently not available in any FIC glasses to date.

Martin, Steve W.↗

NASA NTRS1991

Investigation of throat film coolant for advanced LOX/RP-1 thrust chambers

The use of throat film coolant as a method to reduce peak combustion heat flux was investigated. Hot-fire tests were performed using a subscale LOX/RP-1 combustor at a nominal chamber pressure of 2000 psia. A special injection manifold was fabricated to introduce the film coolant into the chamber. Four tests were conducted with RP-1 film coolant injected 4.4 inches upstream of the throat. In order to determine the effect of chamber length on the film coolant, four additional tests were performed with the injection point moved 16.4 inches upstream of the throat. Results from the test program are discussed. Methods for incorporating throat film cooling into a flightweight combustion chamber are also discussed.

Volkmann, Jon C.↗

NASA NTRS1990

Thermal diffusivity of diamond films

A laser pulse technique to measure the thermal diffusivity of diamond films deposited on a silicon substrate is developed. The effective thermal diffusivity of diamond film on silicon was measured by observing the phase and amplitude of the cyclic thermal waves generated by the laser pulses. An analytical model is developed to calculate the effective in-plane (face-parallel) diffusivity of a two layer system. The model is used to reduce the effective thermal diffusivity of the diamond/silicon sample to a value for the thermal diffusivity and conductivity of the diamond film. Phase and amplitude measurements give similar results. The thermal conductivity of the films is found to be better than that of type 1a natural diamond.

Albin, Sacharia↗

NASA NTRS2004

Implementation of a Thick-Film Composite Li-Ion Microcathode Using Carbon Nanotubes as the Conductive Filler

This paper describes the development of a thick-film microcathode for use in Li-ion microbatteries in order to provide increased power and energy per area. These cathodes take advantage of a composite porous electrode structure, utilizing carbon nanotubes (CNT) as the conductive filler. The use of carbon nanotubes was found to significantly reduce the measured resistance of the electrodes, increase active material accessibility, and improve electrode performance. In particular, the cycling and power performance of the thick-film cathodes was significantly improved, and the need for compression was eliminated. Cathode thickness and CNT content were optimized to maximize capacity and power performance. Power capability of >50 mW/sq cm (17 mA/sq cm) with discharge capacity of >0.17 mAh/sq cm was demonstrated. The feasibility of fabricating thick-film microcathodes capable of providing the power and capacity needed for use in autonomous microsensor systems was also demonstrated.

Lin, Qian↗

DOE OSTI2021

Design, Flow Field, and Heat Transfer Characterization of the Conjugate Aero-Thermal Test Facility at NETL

A new aerothermal test facility was constructed for the purpose of studying film cooling performance in an environment that accurately simulates conjugate heat transfer characteristics that exist in engine operation. Here, this paper details the design of the facility and the plan for conducting steady state film cooling experiments to improve the understanding of conjugate heat transfer scaling from laboratory to engine conditions. The test facility consists of two separate low channels (hot gas/coolant) and each gas path has a flow conditioning section, a convergent nozzle and a test section/channel with viewports. Numerical simulations were conducted to predict flow field characteristics supporting the design of the flow loop facility. Preliminary experiments were conducted to characterize the flow field using velocity and temperature profile measurements. In addition, infrared (IR) thermography methods were developed to measure surface temperatures on the hot side of the test plate. The IR measurement methods including calibration of the IR camera is explained in detail. It was concluded that appropriate hot gas path flow conditioning could be achieved using a strainer-like tube, a perforated plate, and a honeycomb-mesh screen system upstream of the test section. Flow field measurements from preliminary experiments showed that the boundary layer profile follows the law of the wall.

47 OTHER INSTRUMENTATION↗

DOE OSTI2023

Plasmonic Terahertz Devices and Sensors Based on Carbon Electronics

Tunable terahertz (THz) photonic devices are imperative in a wide range of applications ranging from THz signal modulation to molecular sensing. One of the currently prevailing methods is based on arrays of metallic or dielectric resonators integrated with functional materials in response to an external stimulus, in which for the purpose of sensing the external stimuli may introduce inadvertent undesirable effects into the target samples to be measured. Here we developed an alternative approach by postprocessing nanothickness macro-assembled graphene (nMAG) films with widely tunable THz conductivity, enabling versatile solid-state THz devices and sensors, showing multifunctional nMAG-based applications. The THz conductivities of free-standing nMAGs showed a broad range from 1.2 x 10 3 S/m in reduced graphene oxide before annealing to 4.0 x 10 6 S/m in a nMAG film annealed at 2800 °C. We fabricated nMAG/dielectric/metal and nMAG/dielectric/nMAG THz Salisbury absorbers with broad reflectance ranging from 0% to 80%. The highly conductive nMAG films enabled THz metasurfaces for sensing applications. Taking advantage of the resonant field enhancement arising from the plasmonic metasurface structures and the strong interactions between analyte molecules and nMAG films, we have successfully detected diphenylamine with a limit of detection of 4.2 pg. Those wafer-scale nMAG films present promising potential in high-performance THz electronics, photonics, and sensors.

36 MATERIALS SCIENCE↗

NASA NTRS1972

Analysis of DuPont and Kodak duplicating films and chemistries in a Fultron spray processor

A test program was conducted with duPont duplicating film type SR 112 and SCOLOR developer and Kodak duplicating film types 2430, 2422, and FE 2628 (SO-467) and MX-641 developer to determine sensitometric and image quality characteristics of these materials when used with a fultron spray processor. The test results show that the SCOLOR developer foams excessively in the fultron processor when used with or without the addition of an antifoaming agent. The Kodak type FE 2628 film with MX-641 chemistry had the longest linear Log E range at a 1.0 gamma. Sensitometric curves and granularity traces for all film process combinations tested are included.

Weinstein, M. S.↗

NASA NTRS1999

Vortex-State Complex Hall Conductivity of Superconducting YBa(2)Cu(3)0(7) Epitaxial Films at Radio Frequencies

Explore the source record for details and available documents.

Vortex-State Hall Conductivity Epitaxial Films Rad↗

DOE OSTI2025

Autonomous platform for solution processing of electronic polymers

The manipulation of electronic polymers’ solid-state properties through processing is crucial in electronics and energy research. Yet, efficiently processing electronic polymer solutions into thin films with specific properties remains a formidable challenge. We introduce Polybot, an artificial intelligence (AI) driven automated material laboratory designed to autonomously explore processing pathways for achieving high-conductivity, low-defect electronic polymers films. Leveraging importance-guided Bayesian optimization, Polybot efficiently navigates a complex 7-dimensional processing space. In particular, the automated workflow and algorithms effectively explore the search space, mitigate biases, employ statistical methods to ensure data repeatability, and concurrently optimize multiple objectives with precision. The experimental campaign yields scale-up fabrication recipes, producing transparent conductive thin films with averaged conductivity exceeding 4500 S/cm. Feature importance analysis and morphological characterizations reveal key design factors. This work signifies a significant step towards transforming the manufacturing of electronic polymers, highlighting the potential of AI-driven automation in material science.

Wang, Chengshi [Argonne National Laboratory (ANL),↗

NASA NTRS2004

Preparation of Proton Exchange Membranes and Lithium Batteries from Melamine-containing Ormosils

Our laboratory has recently reported a series of rodcoil polymers for lithium batteries that display dimensionally stable films with good ionic conductivity. The rod segments consist of rigid linear and branched polyimides and the coil segments are polyethylene oxides (PEO). It has been proposed that good mechanical and transport properties are due to phase separation between the rod and coil segments. It was also observed that increased branching and molecular weight lead to increased conductivity. The following study was undertaken to assess the effects of phase separation in polyalkylene oxides connected by melamine linkages. Melamine was chosen as the linking unit because it provides a branching site, cation binding sites to help ionic transport between polymer chains, and the opportunity for self assembly through hydrogen bonding. Polymers were made by the reaction of cyanuric chloride with a series of amine-terminated alkylene oxides. A linear polymer was first made, followed by reaction of the third site on cyanuric chloride with varying ratios of monofunctional Jeffamine and (3-aminopropyl)triethoxysilane. The lithium trifluoromethane sulfonamide-doped polymers are then crosslinked through a sol-gel process to form free-standing films. Initial results have shown mechanically strong films with lithium conductivities on the order of 2 x 10(exp -5) S/cm at ambient temperature. In a separate study, organically modified silanes (Ormosils) that contain sulfonic acid derivatized melamines have been incorporated into proton exchange membranes. The membranes are made by reaction of the primary amine groups of various ratios of melamine derivative and difunctional Jeffamine (MW = 2000) with the epoxide group of (3-Glycidyloxypropyl)trimethoxysilane. The films were then cross-linked through a sol-gel process. Resulting sulfuric acid doped films are strong, flexible, and have proton conductivities on the order of 2 x l0(exp -2) S/cm (120 C, 25% relative humidity). Our best results have been observed when films contain 60% PEO and 40% sulfonated melamine.

Tigelaar, Dean M.↗

NASA NTRS1989

Molecular beam epitaxial growth of high-quality InSb on InP and GaAs substrates

Epitaxial layers of InSb were grown on InP and GaAs substrates by molecular beam epitaxy. The dependence of the epilayer quality on flux ratio, J sub Sb4/J sub In, was studied. Deviation from an optimum value of J sub Sb4/J sub In (approx. 2) during growth led to deterioration in the surface morphology and the electrical and crystalline qualities of the films. Room temperature electron mobilities as high as 70,000 and 53,000 sq cm /V-s were measured in InSb layers grown on InP and GaAs substrates, respectively. Unlike the previous results, the conductivity in these films is n-type even at T = 13 K, and no degradation of the electron mobility due to the high density of dislocations was observed. The measured electron mobilities (and carrier concentrations) at 77 K in InSb layers grown on InP and GaAs substrates are 110,000 sq cm/V-s (3 x 10(15) cm(-3)) and 55,000 sq cm/V-s (4.95 x 10(15) cm(-3)), respectively, suggesting their application to electronic devices at cryogenic temperatures.

Oh, J. E.↗

NASA NTRS1989

Molecular beam epitaxial growth of high-quality InSb on InP and GaAs substrates

Oh, J. E.↗

NASA NTRS1997

Organometallic Polymeric Conductors

For aerospace applications, the use of polymers can result in tremendous weight savings over metals. Suitable polymeric materials for some applications like EMI shielding, spacecraft grounding, and charge dissipation must combine high electrical conductivity with long-term environmental stability, good processability, and good mechanical properties. Recently, other investigators have reported hybrid films made from an electrically conductive polymer combined with insulating polymers. In all of these instances, the films were prepared by infiltrating an insulating polymer with a precursor for a conductive polymer (either polypyrrole or polythiophene), and oxidatively polymerizing the precursor in situ. The resulting composite films have good electrical conductivity, while overcoming the brittleness inherent in most conductive polymers. Many aerospace applications require a combination of properties. Thus, hybrid films made from polyimides or other engineering resins are of primary interest, but only if conductivities on the same order as those obtained with a polystyrene base could be obtained. Hence, a series of experiments was performed to optimize the conductivity of polyimide-based composite films. The polyimide base chosen for this study was Kapton. 3-MethylThiophene (3MT) was used for the conductive phase. Three processing variables were identified for producing these composite films, namely time, temperature, and oxidant concentration for the in situ oxidation. Statistically designed experiments were used to examine the effects of these variables and synergistic/interactive effects among variables on the electrical conductivity and mechanical strength of the films. Multiple linear regression analysis of the tensile data revealed that temperature and time have the greatest effect on maximum stress. The response surface of maximum stress vs. temperature and time (for oxidant concentration at 1.2 M) is shown. Conductivity of the composite films was measured for over 150 days in air at ambient temperature. The conductivity of the films dropped only half an order of magnitude in that time. Films aged under vacuum at ambient temperature diminished slightly in conductivity in the first day, but did not change thereafter. An experimental design approach will be applied to maximize the efficiency of the laboratory effort. The material properties (initial and long term) will also be monitored and assessed. The experimental results will add to the existing database for electrically conductive polymer materials. Attachments: 1) Synthesis Crystal Structure, and Polymerization of 1,2:5,6:9,10-Tribenzo-3,7,11,13-tetradehydro(14) annulene. 2) Reinvestigation of the Photocyclization of 1,4-Phenylene Bis(phenylmaleic anhydride): Preparation and Structure of (5)Helicene 5,6:9,10-Dianhydride. 3) Preparation and Structure Charecterization of a Platinum Catecholate Complex Containing Two 3-Ethynyltheophone Groups. and 4) Rigid-Rod Polymers Based on Noncoplanar 4,4'-Biphenyldiamines: A Review of Polymer Properties vs Configuration of Diamines.

Youngs, Wiley J.↗