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DOE OSTI2023

Machine-learning-assisted analysis of transition metal dichalcogenide thin-film growth

In situ reflective high-energy electron diffraction (RHEED) is widely used to monitor the surface crystalline state during thin-film growth by molecular beam epitaxy (MBE) and pulsed laser deposition. With the recent development of machine learning (ML), ML-assisted analysis of RHEED videos aids in interpreting the complete RHEED data of oxide thin films. The quantitative analysis of RHEED data allows us to characterize and categorize the growth modes step by step, and extract hidden knowledge of the epitaxial film growth process. In this study, we employed the ML-assisted RHEED analysis method to investigate the growth of 2D thin films of transition metal dichalcogenides (ReSe2) on graphene substrates by MBE. Principal component analysis (PCA) and K-means clustering were used to separate statistically important patterns and visualize the trend of pattern evolution without any notable loss of information. Using the modified PCA, we could monitor the diffraction intensity of solely the ReSe2 layers by filtering out the substrate contribution. These findings demonstrate that ML analysis can be successfully employed to examine and understand the film-growth dynamics of 2D materials. Further, the ML-based method can pave the way for the development of advanced real-time monitoring and autonomous material synthesis techniques.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Structure and Dynamics of Domains in Ferroelectric Nanostructures – Phase-Field Modeling (Final Technical Report)

Domain pattern formation is one of the most common phenomena in nature and is a topic of immense interest in many fields ranging from materials science and physics to chemistry and biology. This DOE sponsored research project explored the basic science concerning the thermodynamic stability of mesoscale polarization domain patterns and their temporal evolution mechanisms during formation and subsequent switching in ferroelectric nanostructures and heterostructures. The project employed the computational phase-field method in combination of microelasticity and electrostatic theories. The research was carried out in close collaboration with a number of experimental groups who used High Resolution Transmission Electron Microscopy (HRTEM), in situ TEM with Scanning Probe Microscopy (SPM), or Piezoresponse Force Microscopy (PFM) to characterize the domain structures and dynamics of ferroelectric thin films and heterostructures and who grow high-quality ferroelectric and multiferroic thin films using advanced growth techniques such as Molecular Beam Epitaxy (MBE), Pulsed Laser Deposition (PLLD), and sputtering. The research efforts of the project help establish the phase-field method as the most powerful method for understanding and predicting domain structures in ferroelectric thin films and nanostructures. The findings of the project led to the basic understanding of stability and switching mechanisms of ferroelectric domains under different mechanical boundary conditions and under either homogeneous capacitor configurations or local fields using metallic probes as electrodes and the emergence of charged domain walls during domain switching. The project predicted the spatial length scales, temperature ranges, and electromechanical conditions for different polar states in heterostructures and guided the discovery of both transient and stable novel polarization states containing vortex lattices in oxide superlattices. The project resulted in 134 journal publications and 6 PhD theses with all the PhD graduates currently working in either academia or industry within the United States. The basic understanding on the stability of mesoscale polar states and pattern evolution achieved by the project improved our ability to control and engineer properties of ferroelectric thin films and heterostructures for potential applications in nanoscale electronic devices.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Growth and Development of Quantum Materials

Topological insulators (TIs) display a new state of quantum matter, which is broadly known as quantum materials. The TIs have a unique property of being an insulator as a bulk property and having conducting surface states, which are symmetry-protected Dirac Fermions and well isolated from the bulk valence and conduction bands. Ideally, these topological surface states and bulk electronic states should act independently. The degree to which they intermix depends on the crystalline quality, composition and defects present in the material. These materials thus demand very high-quality crystals to observe the desired quantum properties. We proposed growth of high-quality single crystals and thin films to enhance the ability to fabricate devices with unique performance attributes. Two separate approaches will be made to make the thin films, one is exfoliation of 2D monolayer from the grown single crystals and the second is thin films grown by pulsed laser deposition. Both techniques will subsequently allow for fabrication of meso structures using a Focused Ion Beam technique.

36 MATERIALS SCIENCE↗

DOE OSTI2024

ZnO-Au Hybrid Metamaterial Thin Films with Tunable Optical Properties

ZnO-Au nanocomposite thin films have been previously reported as hybrid metamaterials with unique optical properties such as plasmonic resonance properties and hyperbolic behaviors. In this study, Au composition in the ZnO-Au nanocomposites has been effectively tuned by target composition variation and thus resulted in microstructure and optical property tuning. Specifically, all the ZnO-Au nanocomposite thin films grown through the pulsed laser deposition (PLD) method show obvious vertically aligned nanocomposite (VAN) structure with the Au nanopillars embedded in the ZnO matrix. Moreover, the average diameter of Au nanopillars increases as Au concentration increases, which also leads to the redshifts in the surface plasmon resonance (SPR) wavelength and changes in the hyperbolic behaviors of the films. As a whole, this work discusses how strain-driven tuning of optical properties and microstructure resulted through a novel Au concentration variation approach which has not been previously attempted in the ZnO-Au thin film system. These highly ordered films present great promise in the areas of sensing, waveguides, and nanophotonics to name a few.

Bhatt, Nirali A.↗

DOE OSTI2023

Anisotropic Properties of Epitaxial Ferroelectric Lead-Free 0.5[Ba(Ti 0.8 Zr 0.2 )O 3 ]-0.5(Ba 0.7 Ca 0.3 )TiO 3 Films

As the energy demand is expected to double over the next 30 years, there has been a major initiative towards advancing the technology of both energy harvesting and storage for renewable energy. In this work, we explore a subset class of dielectrics for energy storage since ferroelectrics offer a unique combination of characteristics needed for energy storage devices. We investigate ferroelectric lead-free 0.5[Ba(Ti 0.8 Zr 0.2 )O 3 ]-0.5(Ba 0.7 Ca 0.3 )TiO 3 epitaxial thin films with different crystallographic orientations grown by pulsed laser deposition. We focus our attention on the influence of the crystallographic orientation on the microstructure, ferroelectric, and dielectric properties. Our results indicate an enhancement of the polarization and strong anisotropy in the dielectric response for the (001)-oriented film. The enhanced ferroelectric, energy storage, and dielectric properties of the (001)-oriented film is explained by the coexistence of orthorhombic-tetragonal phase, where the disordered local structure is in its free energy minimum.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Transformation of TiN to TiNO Films via In-Situ Temperature-Dependent Oxygen Diffusion Process and Their Electrochemical Behavior

Titanium oxynitride (TiNO) thin films represent a multifaceted material system applicable in diverse fields, including energy storage, solar cells, sensors, protective coatings, and electrocatalysis. This study reports the synthesis of TiNO thin films grown at different substrate temperatures using pulsed laser deposition. A comprehensive structural investigation was conducted by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Non-Rutherford backscattering spectrometry (N-RBS), and X-ray absorption spectroscopy (XAS), which facilitated a detailed analysis that determined the phase, composition, and crystallinity of the films. Structural control was achieved via temperature-dependent oxygen in-diffusion, nitrogen out-diffusion, and the nucleation growth process related to adatom mobility. The XPS analysis indicates that the TiNO films consist of heterogeneous mixtures of TiN, TiNO, and TiO2 phases with temperature-dependent relative abundances. The correlation between the structure and electrochemical behavior of the thin films was examined. The TiNO films with relatively higher N/O ratio, meaning less oxidized, were more electrochemically active than the films with lower N/O ratio, i.e., more oxidized films. Films with higher oxidation levels demonstrated enhanced crystallinity and greater stability under electrochemical polarization. These findings demonstrate the importance of substrate temperature control in tailoring the properties of TiNO film, which is a fundamental part of designing and optimizing an efficient electrode material.

Cherono, Sheilah↗

DOE OSTI2020

Epitaxial Stabilization of Single-Crystal Multiferroic YCrO 3 Thin Films

We report on the growth of stoichiometric, single-crystal YCrO 3 epitaxial thin films on (001) SrTiO 3 substrates using pulsed laser deposition. X-ray diffraction and atomic force microscopy reveal that the films grew in a layer-by-layer fashion with excellent crystallinity and atomically smooth surfaces. Magnetization measurements demonstrate that the material is ferromagnetic below 144 K. The temperature dependence of dielectric permittivity shows a characteristic relaxor-ferroelectric behavior at T C = 375–408 K. A dielectric anomaly at the magnetic transition temperature indicates a close correlation between magnetic and electric order parameters in these multiferroic YCrO 3 films. These findings provide guidance to synthesize rare-earth, chromite-based multifunctional heterostructures and build a foundation for future studies on the understanding of magnetoelectric effects in similar material systems.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Single-Step Fabrication of Au-Fe-BaTiO3 Nanocomposite Thin Films Embedded with Non-Equilibrium Au-Fe Alloyed Nanostructures

Nanocomposite thin film materials present great opportunities in coupling materials and functionalities in unique nanostructures including nanoparticles-in-matrix, vertically aligned nanocomposites (VANs), and nanolayers. Interestingly the nanocomposites processed through a non-equilibrium processing method, e.g., pulsed laser deposition (PLD), often possess unique metastable phases and microstructures that could not achieve using equilibrium techniques, and thus lead to novel physical properties. In this work, a unique three-phase system composed of BaTiO3 (BTO), with two immiscible metals, Au and Fe, is demonstrated. By adjusting the deposition laser frequency from 2 Hz to 10 Hz, the phase and morphology of Au and Fe nanoparticles in BTO matrix vary from separated Au and Fe nanoparticles to well-mixed Au-Fe alloy pillars. This is attributed to the non-equilibrium process of PLD and the limited diffusion under high laser frequency (e.g., 10 Hz). The magnetic and optical properties are effectively tuned based on the morphology variation. This work demonstrates the stabilization of non-equilibrium alloy structures in the VAN form and allows for the exploration of new non-equilibrium materials systems and their properties that could not be easily achieved through traditional equilibrium methods.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Electronic structure of compressively strained thin film La$_2$PrNi$_2$O$_7$

The discovery of superconductivity in the bulk nickelates under high pressure is a major advance in physics. The recent observation of superconductivity at ambient pressure in compressively strained bilayer nickelate thin films has now enabled direct characterization of the superconducting phase through angle resolved photoemission spectroscopy (ARPES). Here we present an in-situ ARPES study of compressively strained La$_2$PrNi$_2$O$_7$ films grown by oxide molecular beam epitaxy, and the ozone treated counterparts with an onset T$_c$ of 40 K, supplemented with results from pulsed laser deposition films with similar T$_c$. We resolve a systematic strain-driven electronic band shift with respect to that of bulk crystals, in qualitative agreement with density functional theory (DFT) calculations. However, the strongly renormalized flat 3$d_{z2}$ band shifts a factor of 5-10 smaller than anticipated by DFT. Furthermore, it stays ~70 meV below the Fermi level, contradicting the expectation that superconductivity results from the high density of states of this band at the Fermi level. We also observed a non-trivial k$_z$ dispersion of the cuprate-like 3$d_{x2-y2}$ band. Combined with results from both X-ray diffraction and DFT, we suggest that the strained films are under ~5 GPa effective pressure, considerably larger than the naïve expectation from the DFT relaxed structure. Finally, the ~70 meV energy position is intriguingly close to the collective mode coupling more prominently seen in thin films, in the energy range of both oxygen related phonons and the maximum of the spin excitation spectrum.

FOS: Physical sciences↗

DOE OSTI2026

Self-driving thin film laboratory: autonomous epitaxial atomic-layer synthesis via real-time computer vision analysis of electron diffraction

Emerging materials science platforms with the ability to make autonomous decisions on the fly are fundamentally changing the outlook and protocols for materials optimization and discovery. Because AI-driven self-navigating schemes can effectively reduce the total number of iterations needed to arrive at the "answer" (i.e. the best stochiometric composition for a desired physical property, optimum materials processing parameters, etc.) by significant margins, they have the potential to revolutionize materials and chemical manufacturing processes at large in research laboratory settings as well as in industrial plants. Here, we demonstrate a successful implementation of real-time closed-loop autonomous navigation of a multi-dimensional materials synthesis parameter space for fabricating phase-pure epitaxial films of a metastable phase of a functional oxide in a combinatorial pulsed laser deposition chamber. Sequential epitaxial growth iterations in search of the optimized recipe to stabilize the desired crystal phase were performed using frame-by-frame quantitative computer vision analysis of reflection high-energy electron diffraction (RHEED) images of the unit-cell level film being deposited. The autonomous scheme regularly resulted in > 30-fold reduction in the number of required experiments compared to a comprehensive mapping of the parameter space. The real-time workflow developed here can be readily extended to a variety of thin film synthesis platforms opening the door for self-driving atomic-level materials design as well as autonomous optimization of semiconductor manufacturing.

36 MATERIALS SCIENCE↗

NASA NTRS1990

Perspectives on high temperature superconducting electronics

The major challenges in making high temperature superconducting (HTSC) electronics viable are predominantly materials problems. Unlike their predecessors the metal oxide-based superconductors are integratable with other advanced technologies such as opto-electronics and micro-electronics. The materials problems to be addressed relate to the epitaxial growth of high quality films, highly oriented films on non-lattice matched substrates, heterostructures with atomically sharp interfaces of junctions and other novel devices, and the processing of these films with negligible deterioration of the superconducting properties. These issues are illustrated with results based on films prepared in-situ by a pulsed laser deposition process. Films with zero-transition temperatures of 90 K and critical current densities of 5 x 10(exp 6) A/sq cm at 77 K have been prepared by this technique. Ultra-thin films, less than 100 A show T(sub c) is greater than 80 K, supporting the idea of two-dimensional transport in these materials. By the use of appropriate buffer layers, films with T(sub c) of 87 K and J(sub c) of 6 x 10(exp 4) A/sq cm were fabricated on silicon substrates. Submicron structures with J(sub c) is greater than 2 x 10(exp 7) at 10 K were fabricated. Results on nonlinear switching elements, IR detectors, and microwave studies will be briefly summarized.

Venkatesan, T.↗

NASA NTRS1990

Superconductivity applications for infrared and microwave devices; Proceedings of the Meeting, Orlando, FL, Apr. 19, 20, 1990

Various papers on superconductivity applications for IR and microwave devices are presented. The individual topics addressed include: pulsed laser deposition of Tl-Ca-Ba-Cu-O films, patterning of high-Tc superconducting thin films on Si substrates, IR spectra and the energy gap in thin film YBa2Cu3O(7-delta), high-temperature superconducting thin film microwave circuits, novel filter implementation utilizing HTS materials, high-temperature superconductor antenna investigations, high-Tc superconducting IR detectors, high-Tc superconducting IR detectors from Y-Ba-Cu-O thin films, Y-Ba-Cu0-O thin films as high-speed IR detectors, fabrication of a high-Tc superconducting bolometer, transition-edge microbolometer, photoresponse of YBa2Cu3O(7-delta) granular and epitaxial superconducting thin films, fast IR response of YBCO thin films, kinetic inductance effects in high-Tc microstrip circuits at microwave frequencies.

Bhasin, Kul B.↗

NASA NTRS1991

Perspectives on high temperature superconducting electronics

The major challenges in making high temperature superconducting (HTSC) electronics viable are predominantly materials problems. Unlike their predecessors, the metal oxide-based superconductors are integratable with other advanced technologies such as opto-electronics and micro-electronics. The materials problems to be addressed relate to the epitaxial growth of high quality films, highly oriented films on non-lattice matched substrates, heterostructures with atomically sharp interfaces of junctions and other novel devices, and the processing of these films with negligible deterioration of the superconducting properties. These issues are illustrated with results based on films prepared in-situ by a pulsed laser deposition process. Films with zero-transition temperatures of 90 K and critical current densities of 5 x 10(exp 6) A/sq cm at 77 K have been prepared by this technique. Ultra-thin films, less than 100 A show T(sub c) is greater than 80 K, supporting the idea of two-dimensional transport in these materials. By the use of appropriate buffer layers, films with T(sub c) of 87 K and J(sub c) of 6 x 10(exp 4) A/sq cm were fabricated on silicon substrates. Submicron structures with J(sub c) is greater than 2 x 10(exp 7) at 10 K were fabricated. Results on nonlinear switching elements, IR detectors, and microwave studies will be briefly summarized.

Venkatesan, T.↗

NASA NTRS1991

High temperature superconductor materials and applications

One of the areas concerned itself with the investigation of the phenomena involved in formulating and making in the laboratory new and better superconductor material with enhanced values of critical current and temperature. Of special interest were the chemistry, physical processes, and environment required to attain these enhanced desirable characteristics. The other area concerned itself with producing high temperature superconducting thin films by pulsed laser deposition techniques. Such films are potentially very useful in the detection of very low power signals. To perform this research high vacuum is required. In the course of this effort, older vacuum chambers were maintained and used. In addition, a new facility is being brought on line. This latter activity has been replete with the usual problems of bringing a new facility into service. Some of the problems are covered in the main body of this report.

Doane, George B., III.↗

NASA NTRS1995

Effect of Nb2O5 and V2O5 addition on the superconducting properties of YBa2Cu3O(y) thin films

The effect of Nb2O5 and V2O5 addition on the superconducting properties and microstructure of YBa2Cu3O(y) has been studied in thin films. Polycrystalline targets for laser ablation were prepared by mixing high purity V2O5 or Nb2O5 powders with a well characterized YBa2Cu3O(y) powder in the range 0 to 4 wt percent by solid state reaction method. Thin films (approximately 1500 A thickness) of the above targets were grown on (100) SrTiO3 (STO) and (100) LaAlO3 (LAO) substrates at 700 C temperature by pulsed laser deposition (PLD) technique. In the case of Nb2O5 addition we have noticed an increase in J(sub c) up to 0.5 wt percent and higher additive concentration (greater than 0.5 wt percent) have degraded the superconducting properties. However, in the case of V2O3 addition, there is an improvement in current density and microstructural properties up to 1 wt percent and the superconducting properties degrade for concentrations greater than 1 wt percent. The best J(sub c) for 0.5 wt percent of Nb2O5 added YBCO thin film is 1.6 x 10(exp 6) A/sq cm and for that of V2O5 added sample is 3.4 x 10(exp 6) A/sq cm at 77 K as compared to the pure YBa2Cu3O(y) (YBCO) film J(sub c) (1.2 x 10(exp 6) A/sq cm) observed on STO substrates. The reason for improvement in J(sub c) and microstructural properties in the case of V2O5 addition could be due to the low melting of V2O5 (690 C) which can act as a very good surfactant during deposition. Over all, we have realized that Nb2O5 addition or V2O5 addition to YBCO have shown significant improvement over the undoped YBa2Cu3O(7-x) films grown under identical conditions.

Srinivas, S.↗

NASA NTRS1995

Effects of oxygen stoichiometry on the scaling behaviors of YBa2Cu3O(x) grain boundary weak-links

The effects of oxygen stoichiometry on the transport properties of the pulsed laser deposited YBa2Cu3O(x) bicrystalline grain boundary weak-link junctions were studied. It is found that not only the cross boundary resistive transition foot structure can be manipulated repeatedly with oxygen annealing processes but the junction behaviors are also altered in accordance. In the fully oxygenated state i.e with x = 7.0 in YBa2Cu3O(x) stoichiometry, the junction critical current exhibits a power of 2 scaling behavior with temperature. In contrast, when annealed in the conditions of oxygen-deficient state (e.g with x = 6.9 in YBa2Cu3O(x) stoichiometry) the junction critical current switches to a linear temperature dependence behavior. The results are tentatively attributed to the modification of the structure in the boundary area upon oxygen annealing, which, in turn, will affect the effective dimension of the geometrically constrained weak-link bridges. The detailed discussion on the responsible physical mechanisms as well as the implications of the present results on device applications will be given.

Wu, K. H.↗

NASA NTRS1995

Superconducting materials processing

The effects of materials processing on the properties and behavior of high temperature yttrium barium copper oxide (YBCO) superconductors were investigated. Electrical, magnetic, and structural characteristics of thin films (300 nm) YBA2CU3O(delta) structures grown by pulsed laser deposition on LaAlO3 and SrTiO3 substrates were used to evaluate processing. Pole projection and thin film diffraction measurements were used to establish grain orientation and verify structural integrity of the samples. Susceptibility magnetization, and transport measurements were used to evaluate the magnetic and electrical transport properties of the samples. Our results verified that an unfortunate consequence of processing is inherent changes to the internal structure of the material. This effect translates into modifications in the properties of the materials, and undesired feature that makes it very difficult to consistently predict material behavior. The results show that processing evaluation must incorporate a comprehensive understanding of the properties of the materials. Future studies will emphasize microstructural characteristics of the materials, in particular, those microscopic properties that map macroscopic behavior.

Hurley, John S.↗

NASA NTRS1996

[?]Nonlinear Issues in the Aerothermochemistry of Gases and Materials and the Associated Physics and Dynamics of Interfaces

Our research and technology are focused on nonlinear issues in the aerothermochemistry of gases and materials and the associated physics and dynamics of interfaces. Our program is now organized to aggressively support the NASA Aeronautics Enterprise so as to: (a) develop a new generation of environmentally compatible, economic subsonic aircraft; (b) develop the technology base for an economically viable and environmentally compatible high-speed civil transport; (c) develop the technology options for new capabilities in high-performance aircraft; (d) develop hypersonic technologies for air-breathing flight; and (e) develop advanced concepts, understanding of physical phenomena, and theoretical, experimental, and computational tools for advanced aerospace systems. The implications from our research for aeronautical and aerospace technology have been both broad and deep. For example, using advanced computational techniques, we have determined exact solutions for the Schrodinger equation in electron-molecule scattering allowing us to evaluate atmospheric models important to reentry physics. We have also found a new class of exact solutions for the Navier Stokes equations. In experimental fluid dynamics, we have found explicit evidence of turbulence modification of droplet sizes in shock tube flow with condensation. We have developed a new diagnostic tool for the direct estimation of flow velocities at MHz sampling rates in quasi-one dimensional turbulent flow. This procedure suggests an unexpected confirmation of the possibility of 'natural' closure in Reynolds stresses with deep implications for the development of turbulent models. A transient increase is observed in both the spectral energy decay rate and the degree of chaotic complexity at the interface of a shock wave and a turbulent ionized gas. Even though the gas is apparently brought to rest by the shock wave, no evidence is found either of the expected relaminarization. A unique diamond-shaped nozzle has been designed for a detailed investigation of the effect of significant streamwise vorticity on the acoustic and IR characteristics of supersonic jets. Our results provide convincing evidence of the significant effect of vorticity on the far-field noise for the diamond jet as compared to the conventional round jets. We have found that the countercurrent shear layer mixes much more efficiently than conventional coflowing shear layers. We also developed the fluid thrust vectoring procedures which use counter flow to vector a jet. Our materials research has shown that the steep stress gradients at the fiber-matrix interface could be the primary cause of interface cracks after the processing of metallic and intermetallic matrix composites. New techniques have been evolved for: the microcharacterization of materials including microplastic strain and, point by point, the misorientation and plasticity for matrix composites; thermally induced stress measurements and load relaxation; the growth and characterization of metallic matrix composite interfaces; and for the growth of ferrite materials by pulsed laser deposition. The FAMU commitment to the HBCU Research Center also continues to be broad and deep.

Johnson, Joseph A., III↗