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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Impact of Processing on Structural and Compositional Evolution in Mixed Metal Halide Perovskites during Film Formation

Understanding crystallization processes and their pathways in metal-halide perovskites is of crucial importance as this strongly affects the film microstructure, its stability, and device performance. While many approaches are developed to control perovskite formation, the mechanisms of film formation are still poorly known. Using time-resolved in situ grazing incidence wideangle X-ray scattering, the film formation of perovskites is investigated with average stoichiometry Cs 0.15 FA 0.85 PbI 3 , where FA is formamidinium, using the popular antisolvent dropping and gas jet treatments and this is contrasted with untreated films. i) The crystallization pathways during spin coating, ii) the subsequent postdeposition thermal annealing, and iii) crystallization during blade coating are studied. The findings reveal that the formation of a nonperovskite FAPbI 3 phase during spin coating is initially dominant regardless of the processing and that the processing treatment (e.g., antisolvent dropping, gas jet) has a significant impact on the as-cast film structure and affects the phase evolution during subsequent thermal treatment. It is shown that blade coating can be used to overcome the nonperovskite phase formation via solvothermal direct crystallization of perovskite phase. This work shows how real-time investigation of perovskite formation can help to establish processing–microstructure–functionality relationships.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Grid-assisted magnetron sputtering deposition of nitrogen graded TiN thin films

Titanium Nitride (TiN) films were obtained using the grid-assisted magnetron sputtering deposition technique on Al substrates in two conditions: under constant and variable nitrogen concentration along the thin solid film thickness. The formation of a film with variable N concentration (herein referred as graded film) was confirmed using energy filtered transmission electron microscopy, X-ray photoelectron spectroscopy and grazing incidence X-ray diffraction. The TiN thin films microstructures were also analysed using scanning and transmission electron microscopies (SEM and TEM). Finally, the viability of synthesizing TiN thin films with variable N concentration is herein proposed as an alternative method for tailoring the properties of such functional coating materials.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Dielectric relaxation analysis of Pb(Zr{sub 0.54},Ti{sub 0.46})O{sub 3} thin films: Electric field dependence

350 nm-thick Perovskite PbZr{sub 0.54}Ti{sub 0.46}O{sub 3} (PZT) thin films were deposited on Al{sub 2}O{sub 3} substrates by sputtering with and without an additional 10-nm-thick TiO{sub x} buffer layer. X-ray diffraction patterns showed that in presence of TiO{sub x} buffer layer, PZT film was highly oriented along the (111) direction film, whereas the unbuffered, counterpart was polycrystalline. A full wave electromagnetic analysis using a vector finite element method was performed to determine the tunability and the complex permittivity up to 67 GHz. A comparison between the electromagnetic analysis and Cole-Cole relaxation model was proposed. Through an original study of the relaxation time as a function of the electric field, values, such as 2 ps and 0.6 ps, were estimated for E{sub DC} = 0 kV/cm and 235 kV/cm, respectively, and in both cases (111)-PZT and polycrystalline-PZT. The distribution of relaxation times is found to be larger for (111)-PZT film, which is probably related to the film microstructure.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2018

Nb3Sn Multilayer Sequential Sputtering at Jefferson Lab

Nb3Sn-coated Nb SRF cavities are studied due to their potential of providing a higher accelerating gradient over Nb SRF cavities. Magnetron sputtering can be a feasible alternative to conventional tin vapor diffusion process to fabricate Nb3Sn for SRF cavities. By depositing Nb and Sn layers separately and annealing afterwards, the stoichiometry of the coated films can be controlled to create Nb3Sn. To understand the formation of Nb3Sn at higher annealing temperatures, a comparative study of deposition and processing conditions is required. We have sputtered Nb and Sn multilayers and post-deposition annealed at 850, 950, 1000, 1100 and 1200 °C for 3 hours. The structural properties of the annealed films were characterized by X-ray diffraction (XRD) and compared to as-coated films. The film microstructures and compositions were examined by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). The superconducting transition of the films were measured by surface resistivity data obtained down to cryogenic temperatures. A new cavity deposition system with a cylindrical magnetron has been designed to implement the sequential sputtering technique onto a single-cell cavity.

Eremeev, Grigory↗
DOE OSTI2015

Investigations on Ni-Co-Mn-Sn thin films: Effect of substrate temperature and Ar gas pressure on the martensitic transformations and exchange bias properties

We report the effect of substrate temperature (T{sub S}) and Ar gas pressure (P{sub D}) on the martensitic transformations, magnetic and exchange bias (EB) properties in Heusler type Ni-Co-Mn-Sn epitaxial thin films. Martensitic transformation temperatures and EB fields at 5 K were found to increase with increasing T{sub S}. The observed maximum EB value of 320 Oe after field cooling in the film deposited at 650 {sup ∘}C is high among the values reported for Ni-Mn-Sn thin films which is attributed to the coexistence of ferromagnetic (FM) and antiferromagnetic (AF) phases in the martensitic state. In the case of P{sub D} variation, with increase in P{sub D}, martensitic transformation temperatures were increased and a sharp transformation was observed in the film deposited at 0.06 mbar. Magnetization values at 5 K were higher for increasing P{sub D}. These observations are attributed to the compositional shift. EB effect is also present in these films. Microstructural features observed using atomic force microscopy (AFM) shows a fine twinning and reduced precipitation with increase in P{sub D}, which is also confirmed from the scanning electron microscopy (SEM) images. EB effects in both series were confirmed from the training effect. Target ageing effect has been observed in the films deposited before and after ninety days of time interval. This has been confirmed both on substrate temperature and Ar gas pressure variations.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Aligned Conjugated Polymer Nanofiber Networks in an Elastomer Matrix for High-Performance Printed Stretchable Electronics

Conjugated polymer films are promising in wearable X-ray detection. However, achieving optimal film microstructure possessing good electrical and detection performance under large deformation via scalable printing remains challenging. Herein, we report bar-coated high-performance stretchable films based on a conjugated polymer P(TDPP-Se) and elastomer SEBS blend by optimizing the solution-processing conditions. The moderate preaggregation in solution and prolonged growth dynamics from a solvent mixture with limited dissolving capacity is critical to forming aligned P(TDPP-Se) chains/crystalline nanofibers in the SEBS phase with enhanced π–π stacking for charge transport and stress dissipation. The film shows a large elongation at break of >400% and high mobilities of 5.29 cm 2 V –1 s –1 at 0% strain and 1.66 cm 2 V –1 s –1 over 500 stretch–release cycles at 50% strain, enabling good X-ray imaging with a high sensitivity of 1501.52 μC Gy air –1 cm –2 . Finally, our work provides a morphology control strategy toward high-performance conjugated polymer film-based stretchable electronics.

36 MATERIALS SCIENCE↗
DOE OSTI2020

A pathway to synthesizing single-crystal Fe and FeCr films

Nuclear reactor environments provide a unique scientific and engineering challenge wherein materials must tolerate prolonged exposure to concurrent irradiation, elevated temperatures, and corrosive media. However, uncontrolled variability in material composition and structure often prohibits truly single-variable experiments that can reveal basic aspects of environmental damage. Here, Magnetron sputtering is used to provide a more controlled model system for these fundamental studies, yielding reproducible single-crystal Fe and FeCr thin films containing 8 and 18 at.% Cr. Electron microscopy is used to determine the systematic correlations between growth conditions and the resulting film microstructure and surface morphology. It is found that the substrate temperature and applied radio frequency (RF) bias can be tuned to obtain consistent homogeneous and single crystal films with a minimal amount of Ar impurities from the RF bias process. Epitaxial, single-crystal Fe films are obtained on MgO substrates at 500 °C with 10 Watt (W) RF bias deposition. However, when Cr is alloyed with Fe, higher substrate temperatures (600 °C) and applied RF biases (15 W) are required to achieve a similar epitaxial single-crystal FeCr film. Accelerated molecular dynamics simulations reveal that Cr impedes surface transport, explaining the need for higher temperature and bias during the growth of the Cr-bearing films.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Effects of growth rate and dynamic substrate tilt on properties of Au-Ta alloy films deposited by high-power impulse magnetron sputtering

Gold-tantalum (Au—Ta) alloys are promising for next-generation hohlraums for magnetically-assisted indirect-drive inertial confinement fusion. Hohlraum fabrication involves sputter deposition of ultrathick coatings on sphero-cylindrical substrates. The control of physical properties of such coatings remains a challenge. Here, in this work, we systematically study effects of the growth rate and dynamic substrate tilt on properties of AuTa 4 films deposited onto rotating planar substrates mounted at different tilt angles to mimic different regions of the sphero-cylindrical surface of a hohlraum. We use high-power impulse magnetron sputtering (HiPIMS) in the constant charge per pulse mode with a pulse duration of 100 μs, a charge per pulse of 190 μC, a peak target current of about 3 A, and the pulse frequency varied in the range of 400–1400 Hz. The Langmuir probe, mass-resolved ion energy spectrometry, and optical emission spectroscopy are used to monitor plasma discharge characteristics in order to isolate and study effects of the growth rate. The deposition rate and the ballistics and energetics of depositing species are estimated by Monte Carlo simulations. Results show that the film microstructure, crystallographic phase, residual stress, and electrical resistivity strongly depend on both the deposition rate and substrate tilt, highlighting their critical role in tailoring properties of Au—Ta films during hohlraum fabrication.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Unconventional Molecular Weight Dependence of Charge Transport in the High Mobility n‐type Semiconducting Polymer P(NDI2OD‐T2)

The charge transport and microstructural properties of five different molecular weight (MW) batches of the naphthalenediimide‐thiophene copolymer P(NDI2OD‐T2) are investigated. In particular, the field‐effect transistor (FET) performance and thin‐film microstructure of samples with MW varying from M n = 10 to 41 kDa are studied. Unlike conventional semiconducting polymers such as poly(3‐hexylthiophene) where FET mobility dramatically drops with decreasing molecular weight, the FET mobility of P(NDI2OD‐T2)‐based transistors processed from 1,2‐dichlorobenzene is found to increase with decreasing MW. Using a combination of grazing‐incidence wide‐angle X‐ray scattering, near‐edge X‐ray absorption fine‐structure spectroscopy, atomic force microscopy, and resonant soft X‐ray scattering, the increase in FET mobility with decreasing MW is attributed to the pronounced increase in the orientational correlation length (OCL) with decreasing MW. In particular, the OCL is observed to systematically increase from <100 nm for the highest MW samples to ≈1 µm for the lowest MW samples. The improvement in OCL and hence mobility for low MW samples is attributed to the lack of aggregation of low MW chains in solution promoting backbone ordering, with the pre‐aggregation of chains in 1,2‐dichlorobenzene found to suppress longer‐range liquid crystalline order.

Nahid, Masrur M.↗
DOE OSTI2021

Understanding Reproducibility of Sputter‐Deposited Metastable Ferroelectric Wurtzite Al 0.6 Sc 0.4 N Films Using In Situ Optical Emission Spectrometry

High‐Sc Al 1– x Sc x N thin films are of tremendous interest because of their attractive piezoelectric and ferroelectric properties, but overall film quality and reproducibility are widely reported to suffer as x increases. In this study, structural and electrical properties of metastable Al 0.6 Sc 0.4 N films are connected with plasma changes during film growth, identified via glow discharge optical emission spectroscopy (GD‐OES), and linked to the target mode changes. This in situ GD‐OES technique uses changes in the N 2 (I) intensity, correlated with DC bias hysteresis behavior of a Al 0.6 Sc 0.4 target in metallic and poisoned modes, to identify films that subsequently exhibit unacceptable structural and electrical performance. Two representative samples deposited under identical conditions but possessing distinct properties related to phases present in the films are focused on. Films sputtered under a poisoned target mode produce pure wurtzite ferroelectric Al 0.6 Sc 0.4 N with a reversible 80 μC cm −1 polarization and 3.1 MV cm −1 coercive field. When identical chamber settings are used but the process starts in metallic mode, a mixed wurtzite/rocksalt film is deposited which exhibits nanometer‐scale changes to the film microstructure and a nonferroelectric response. These results illustrate the utility of optical emission spectroscopy for tracking target mode fluctuations when fabricating metastable materials such as high‐Sc Al 1– x Sc x N films.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Carrier mobilities of (001) cadmium arsenide films

We investigate (001)-oriented films of the topological semimetal cadmium arsenide (Cd 3 As 2 ) grown by molecular beam epitaxy on lattice-matched III–V Al x In 1-x Sb buffer layers. Magnetotransport studies and analysis of thin film microstructures are used to determine the influence of dislocations on their carrier mobilities. We show that only a minority of the threading dislocations present in the buffer layers extend into the Cd 3 As 2 films. Threading dislocations are shown to reduce the mobilities of carriers residing in the topological surface states, while bulk transport was unaffected by a change in the dislocation density across an order of magnitude. Thick (001) Cd 3 As 2 films exhibit electron mobilities of up to 41 000 cm 2 V -1 s -1 at 2 K. The results provide insights into the influence of extended defects on the transport properties of a prototype topological semimetal.

36 MATERIALS SCIENCE↗
DOE OSTI2025

High-rate magnetron sputter deposition of low-stress boron carbide films on tilted substrates

Boron carbide is attractive for several applications, including nuclear fuel capsules for inertial confinement fusion (ICF). The fabrication of ICF capsules involves the deposition of ultrathick coatings with density and thickness uniformity on submicron length scales on non-planar (spherical) substrates. Such a deposition requires control of the deposition rate, residual stress, and film microstructure. Here, we systematically study the direct-current magnetron sputter deposition of B 4 C coatings with a full-face-erosion magnetron source as a function of substrate tilt and Ar working gas pressure. Film properties are correlated with results of plasma diagnostics and predictions of Monte Carlo simulations of ballistic sputtering and gas-phase transport. The fabrication of low-stress amorphous B 4 C films with deposition rates of 7μm/h is demonstrated.

Kawasaki, K. [Lawrence Livermore National Laborato↗
DOE OSTI2017

Morphology controls the thermoelectric power factor of a doped semiconducting polymer

The electrical performance of doped semiconducting polymers is strongly governed by processing methods and underlying thin-film microstructure. We report on the influence of different doping methods (solution versus vapor) on the thermoelectric power factor (PF) of PBTTT molecularly p-doped with F n TCNQ (n = 2 or 4). The vapor-doped films have more than two orders of magnitude higher electronic conductivity (s) relative to solution-doped films. On the basis of resonant soft x-ray scattering, vapor-doped samples are shown to have a large orientational correlation length (OCL) (that is, length scale of aligned backbones) that correlates to a high apparent charge carrier mobility (m). The Seebeck coefficient (a) is largely independent of OCL. This reveals that, unlike s, leveraging strategies to improve m have a smaller impact on a. Our best-performing sample with the largest OCL, vapor-doped PBTTT: F 4 TCNQ thin film, has a s of 670 S/cm and an a of 42 mV/K, which translates to a large PF of 120 mW m -1 K -2 . In addition, despite the unfavorable offset for charge transfer, doping by F 2 TCNQ also leads to a large PF of 70 mW m -1 K -2 , which reveals the potential utility of weak molecular dopants. Overall, our work introduces important general processing guidelines for the continued development of doped semiconducting polymers for thermoelectrics.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Dendritic microstructures observed in electron-beam deposited hafnia films

Dendritic microstructures inside hafnia dielectric coatings fabricated via electron-beam deposition are investigated. These structures are observable with different optical characterization tools, including atomic force microscopy, fluorescence microscopy, Raman microscopy, and differential interference contrast microscopy. Long-term monitoring of individual samples over a seven-year time span revealed that the dendrite-like structures evolve over time, while the hafnia material in the dendrite structure—as compared to the rest of the coating—shows a decrease in crystallinity and an increase in defect density.

Hoffman, B. N. [Univ. of Rochester, NY (United Sta↗
DOE OSTI2018

Modeling solvent evaporation during thin film formation in phase separating polymer mixtures

Preparation of thin films by dissolving polymers in a common solvent followed by evaporation of the solvent has become a routine processing procedure. However, modeling of thin film formation in an evaporating solvent has been challenging due to a need to simulate processes at multiple length and time scales. In this paper, we present a methodology based on the principles of linear non-equilibrium thermodynamics, which allows systematic study of various effects such as the changes in the solvent properties due to phase transformation from liquid to vapor and polymer thermodynamics resulting from such solvent transformations. The methodology allows for the derivation of evaporative flux and boundary conditions near each surface for simulations of systems close to the equilibrium. We apply it to study thin film microstructural evolution in phase segregating polymer blends dissolved in a common volatile solvent and deposited on a planar substrate. Finally, effects of the evaporation rates, interactions of the polymers with the underlying substrate and concentration dependent mobilities on the kinetics of thin film formation are studied.

36 MATERIALS SCIENCE↗
NASA NTRS1998

Tunable Dielectric Materials and Devices for Broadband Wireless Communications

Wireless and satellite communications are a rapidly growing industries which are slated for explosive growth into emerging countries as well as countries with advanced economies. The dominant trend in wireless communication systems is towards broadband applications such as multimedia file transfer, video transmission and Internet access. These applications require much higher data transmission rates than those currently used for voice transmission applications. To achieve these higher data rates, substantially larger bandwidths and higher carrier frequencies are required. A key roadblock to implementing these systems at K-band (18-26.5 GHz) and Ka-band (26.5-40 GHz) is the need to develop hardware which meets the requirements for high data rate transmission in a cost effective manner. In this chapter, we report on the status of tunable dielectric thin films for devices, such as resonators, filters, phased array antennas, and tunable oscillators, which utilize nonlinear tuning in the control elements. Paraelectric materials such as Barium Strontium Titanate ((Ba, Sr)TiO3) have dielectric constants which can be tuned by varying the magnitude of the electric field across the material. Therefore, these materials can be used to control the frequency and/or phase response of various devices such as electronically steerable phased array antennas, oscillators, and filters. Currently, tunable dielectric devices are being developed for applications which require high tunability, low loss, and good RF power-handling capabilities at microwave and millimeter-wave frequencies. These properties are strongly impacted by film microstructure and device design, and considerable developmental work is still required. However, in the last several years enormous progress has occurred in this field, validating the potential of tunable dielectric technology for broadband wireless communication applications. In this chapter we summarize how film processing techniques, microwave test configurations, and prototype devices have combined to drive the field to its current stage of development.

Mueller, Carl H.↗
DOE OSTI2020

Synthesis and Characterization of MoNb Films Superconducting at 100-200 mK

We have developed a new transition-edge sensor material with critical temperature (T-c) in the range 100-200 mK. The new material is a solid solution of two superconducting components, MoxNb1-x, co-sputtered from two high-purity single-component targets (Mo and Nb). The T-c has a minimum (dT(c)/dx = 0) at an intermediate concentration of the components. We have optimized the deposition parameters and composition to provide films with a sharp superconducting transition at ~ 150 mK. We investigated structural features of the films and surface morphology using X-ray diffraction (XRD) and scanning electron microscopy. The XRD measurements indicate that the grown films are polycrystalline, with a preferred orientation along the (110) crystal direction and a clear correlation between superconducting properties and film microstructure.

superconducting alloys↗
DOE OSTI2020

In situ X-ray measurements over large Q-space to study the evolution of oxide thin films prepared by RF sputter deposition

Sputter deposition is a versatile and industrially important deposition technique for thin films, with increasing demand for matching the characteristics of thin film materials to specific requirements. Additionally, the actual film properties are largely determined by sputtering parameters such as pressure conditions, temperature and power settings. By means of various X-ray diffraction and scattering techniques, it is shown that the characterization of film formation and growth is feasible in real time at synchrotron sources, thus adding an important dimension to the fundamental understanding of the evolution of thin film microstructure. In particular, grazing incidence small-angle X-ray scattering, grazing incidence X-ray powder diffraction and X-ray reflectometry are used in a complementary manner to study the influence of deposition temperature and substrate choice on the crystallization kinetics and growth of polycrystalline BaTiO 3 films.

36 MATERIALS SCIENCE↗