DLTS Measurements of Thin-Oxide MOS Capacitors
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Ray, Michael↗
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DLTS Measurements of Thin-Oxide MOS Capacitors
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Allemang, Christopher Richard [Sandia National Lab↗
Influence of Oxygen Flow and Sub-Stoichiometry on the Optical and Damage Resistance Properties of Hafnium Oxide Thin Films
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Guediche, Amira [Lawrence Livermore National Labor↗
Gold Nanoparticle Incorporated Oxide Thin Films for Gas Sensing at High Temperature
2021 MRS Fall Meeting and Exhibit, Virtual, December 6-8, 2021.
Wuenschell, Jeffrey↗
Hydrogen Diffusion Coefficient Measures on Thin Film Uranium Oxide
Thin films of uranium oxides, putatively UO 2 and U 3 O 8 , were deposited on palladium/silver (75/25) foil discs (10 μm thick, 10 mm diameter). Methodology for sealing these foils, applying a hydrogen pressure (~ 1 atm) to the oxide side, and measuring the pressure on the permeate side (opposite side of foil) is reported. The experimental apparatus is held at 100 °C to speed diffusion, aided by the pressure differential across the foil (~1 atm (750 torr) on oxide side, initially low vacuum on permeate side, ~1x 10 -4 torr). Early results indicate an effective diffusion coefficient of roughly 7.66 x 10 -17 +/- 2.22 x 10 -17 cm 2 /sec for UO 2 . These values are in line with expectations and prior measures relative to large lag times for system baseline (substrate only). Evaluation of the technique for U 3 O 8 thin films suggests further development will be needed to extend the technique to more oxidized films (U 3 O 8 , UO 3 ). Characterization of the foils (thickness and speciation) post diffusion experiments will be carried out by SIGMA (Eric Tegtmeier and Andy Richards) in FY24 which will sharpen the uncertainty quantification for UO 2 diffusion coefficients, aiding the nucleation model for DRACO.
36 MATERIALS SCIENCE↗
Assessing factors that determine adatom migration and clustering on a thin film oxide; Pt 1 and Rh 1 on the “29” Cu x O/Cu(1 1 1) surface
The dynamical nature of single-site catalysts under non-equilibrium conditions poses significant challenges in the full characterization of their active sites. The “29” oxide is a thin Cu x O film grown on Cu(111) which provides a well-defined surface on which to study the structure and chemistry of atomically dispersed precious metals. A combination of experimental and first-principles approaches is used to investigate the factors that influence the mobility of metal adatoms and their clustering tendencies. Our work elucidates how a homogenous coordination environment of neutral single-atoms can be obtained when its tendency to break oxide bonds within its vicinity is low. Herein we demonstrate that this in turn affects the chemical atomically dispersed species on thin-film oxides, as defects on the oxide would in fact allow such species to be more accessible to CO. We thus highlight the importance of understanding the relationship between defects and atomically dispersed active sites upon designing single-site catalysts.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Epitaxial Thin Film Growth on Recycled SrTiO 3 Substrates Toward Sustainable Processing of Complex Oxides
Complex oxide thin films cover a range of physical properties and multifunctionalities that are critical for logic, memory, and optical devices. Typically, the high‐quality epitaxial growth of these complex oxide thin films requires single crystalline oxide substrates such as SrTiO 3 (STO), MgO, LaAlO 3 , a‐Al 2 O 3, and many others. Recent successes in transferring these complex oxides as free‐standing films not only offer great opportunities in integrating complex oxides on other devices, but also present enormous opportunities in recycling the deposited substrates after transfer for cost‐effective and sustainable processing of complex oxide thin films. In this work, the surface modification effects introduced on the recycled STO are investigated, and their impacts on the microstructure and properties of subsequently grown epitaxial oxide thin films are assessed and compared with those grown on the pristine substrates. Detailed analyses using high‐resolution scanning transmission electron microscopy and geometric phase analysis demonstrate distinct strain states on the surfaces of the recycled STO versus the pristine substrates, suggesting a pre‐strain state in the recycled STO substrates due to the previous deposition layer. These findings offer opportunities in growing highly mismatched oxide films on the recycled STO substrates with enhanced physical properties. Specifically, yttrium iron garnet (Y 3 Fe 5 O 12 ) films grown on recycled STO present different ferromagnetic responses compared to that on the pristine substrates, underscoring the effects of surface modification. The study demonstrates the feasibility of reuse and redeposition using recycled substrates. Via careful handling and preparation, high‐quality epitaxial thin films can be grown on recycled substrates with comparable or even better structural and physical properties toward sustainable process of complex oxide devices.
pre-strained STO surfaces↗
Order-disorder behavior at thin film oxide interfaces
Order-disorder processes fundamentally determine the structure and properties of many important oxide systems for energy and computing applications. While these processes have been intensively studied in bulk materials, they are less investigated and understood for nanostructured oxides in highly non-equilibrium conditions. These systems can now be realized through a range of deposition techniques and probed at exceptional spatial and chemical resolution, leading to a greater focus on interface dynamics. In this work, we survey a selection of recent studies of order-disorder behavior at thin film oxide interfaces, with a particular emphasis on the emergence of order during synthesis and disorder in extreme irradiation environments. We summarize key trends and identify directions for future study in this growing research area.
36 MATERIALS SCIENCE↗
Substrate oxygen sponge effect: A parameter for epitaxial manganite thin film growth
The emergent phenomena in complex oxide thin films are strongly tied to the oxygen content, which is often engineered by the oxygen partial pressure during growth. However, such oxygen control by the growth pressure is challenging to synthesize for some oxide films, which requires a subtle control of the oxygen content. A parameter of controlling the oxygen content independent of the growth pressure is desired. Here, we propose a method of controlling the oxygen content of films by engineering the substrate before the growth. The oxide substrate serves as an oxygen sponge, which provides a tunable oxygen environment ranging from oxygen-rich to oxygen-poor for the film growth, depending on the pre-substrate annealing (PSA) conditions. Using manganite as a model system, we demonstrate that this simple PSA method leads to remarkable changes in the structure and physical properties of the as-grown films. Finally, this substrate oxygen sponge effect, driven by the large oxygen concentration gradient at high temperatures, can be applied to explore not only emergent interfacial phenomena but also the growth of a variety of functional oxide thin films and nanocomposites.
36 MATERIALS SCIENCE↗
A DFT-based kinetic Monte Carlo simulation of multiphase oxide-metal thin film growth
Functional thin films of nanoscale metal pillars in oxide or nitride matrices known as vertically aligned nanocomposite (VAN) have gained much interest owing to their unique strain-coupled and highly anisotropic properties. So far, the deposition of these films has been explored mostly experimentally. In this work, a density functional theory (DFT)-based kinetic Monte Carlo simulation model using Bortz–Kalos–Lebowitz algorithm was developed to understand the growth of VAN films deposited by pulsed laser technique on mismatching substrates. The model has been parameterized and applied to understand the kinetics of growth thin films consisting of Au pillars in CeO2 matrix deposited on SrTiO3 substrates. The effects of pulsed laser deposition (PLD) conditions including the pulse frequency, deposition flux, and substrate temperature were explored. The simulations indicate that the Au pillar size and shape exhibit significant dependence on the PLD conditions. Namely, increasing the temperature increases the average pillar size and lowers the pillar density, and vice versa. In addition, the simulations revealed that increasing the deposition rate results in lowering the average pillar size and increasing the density. Particularly, the DFT results suggest that Au pillar size can be tuned during the initial growth of the first monolayer due to the significantly low activation barrier. Our analysis showed that the relationship between the average pillar size and pillar density is influenced by the kinetics. Furthermore, autocorrelation analysis showed that pillars self-organize in quasi-ordered patterns at certain windows of the deposition conditions, which is attributed to the complex nature of the chemical interactions in the system, the kinetics, and the deposition parameters.
Physics↗
A generalized 3D elastic model for nanoscale, self-assembled oxide-metal thin films with pillar-in-matrix configurations
In recent years, functional oxide-metal based vertically aligned nanocomposite (VAN) thin films have gained interest due to their intriguing physical properties and multifunctionalities stemming from the complex interactions between the two phases in the film and the substrate. In this work, we develop a model for studying the energetics of these thin film systems, including the effects of both lattice mismatch and capillary forces due to interface curvature. Each phase is incorporated into the model using a phase indicator function, and we introduce the capillary forces as body forces using a vector density representation of the interface. The model is implemented using the finite element method to study the deformation of the thin film which is composed of Au nanopillars embedded in a La 0.7 Sr 0.3 MnO 3 (LSMO) matrix on an SrTiO 3 (STO) substrate. Further, the results suggest that the total energy is lowest for random configurations of pillars compared to ordered square and hexagonal lattice configurations, consistent with the random distribution of pillars found in experiments. Furthermore, we find that the interfacial energy dominates the total energy of each configuration, suggesting that interfacial energy in the system is an important design parameter for nanocomposite growth, along with the lattice mismatch.
36 MATERIALS SCIENCE↗
Catalytic open-circuit passivation by thin metal oxide films of p-Si anodes in aqueous alkaline electrolytes
Ni and NiO x -based protective thin films are shown to catalyze the oxidation of Si in the presence of O 2 in strongly alkaline KOH(aq) even in the absence of illumination. The O 2 in solution drove the open-circuit potential of the electrode to >0.4 V, which is positive of the Si passivation potential. The elevated electrochemical potential of the surface promoted formation of passive oxides on exposed Si regions of Si/Ni electrodes. Catalytic passivation of Si extended the durability of an np + -Si(100)/NiO x photoanode to >400 h while operating under simulated day/night cycles. In contrast, electrodes without a Ni(O x ) layer and/or without O 2 in solution displayed direct etching of the Si and corrosion pitting during non-illuminated, simulated nighttime episodes of day/night cycling. The O 2 -derived catalyzed passivation of Si using thin films can be generalized to multiple phases of NiO x as well as to materials other than Ni. Finally, relative to operation in aqueous alkaline conditions, decreasing the pH of the electrolyte decreased the dissolution rate of the protective oxide layer formed by the catalyzed passivation process, and consequently increased the durability of the photoanode, but yielded lower photoelectrode fill factors for water oxidation due to the relatively large kinetic overpotentials for the electrocatalyzed oxygen-evolution reaction at near-neutral pH.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Shifting Valencies and Magnetic Responses in La-Based High-Entropy Oxide Perovskite Thin Films with Variable Mn Presence
Chemical disorder in compositionally complex perovskite oxides generates a broad distribution of exchange pathways and spin states, but the microscopic origin and spatial homogeneity of the resulting magnetic phases remain debated. Here, we tune the Mn fraction (x = 0.2–0.6) in epitaxial La(Cr, Mn, Fe, Co, Ni)O3 thin films and resolve the coupled evolution of valence, spin state, and magnetism using element-specific x-ray absorption spectroscopy and x-ray magnetic circular dichroism (XMCD). Mn enrichment drives an internal redistribution of charge, in which Mn evolves toward a Mn3+-rich mixed valence, while Co converts from predominantly Co3+ to high-spin Co2+. This valence/spin-state coupling amplifies the Mn- and Co-derived ferromagnetic response by nearly an order of magnitude while increasing the magnetic onset temperature to at least 250 K, whereas Fe and Cr remain essentially trivalent with weak dichroism. Depth-resolved low-energy muon spin spectroscopy (LE-μSR) shows magnetic homogeneity through the film thickness, with a secondary relaxation maximum near 25 K indicating a low-temperature dynamical crossover consistent with frustrated magnetism in a strongly disordered spin lattice.
Miertschin, Duncan [Baylor University]↗
Controlling antiferromagnetic domains in patterned La0.7Sr0.3FeO3 thin films
Transition metal oxide thin films and heterostructures are promising platforms to achieve full control of the antiferromagnetic (AFM) domain structure in patterned features as needed for AFM spintronic devices. In this work, soft x-ray photoemission electron microscopy was utilized to image AFM domains in micromagnets patterned into La0.7Sr0.3FeO3 (LSFO) thin films and La0.7Sr0.3MnO3 (LSMO)/LSFO superlattices. A delicate balance exists between magnetocrystalline anisotropy, shape anisotropy, and exchange interactions such that the AFM domain structure can be controlled using parameters such as LSFO and LSMO layer thickness, micromagnet shape, and temperature. In LSFO thin films, shape anisotropy gains importance only in micromagnets where at least one extended edge is aligned parallel to an AFM easy axis. In contrast, in the limit of ultrathin LSFO layers in the LSMO/LSFO superlattice, shape anisotropy effects dominate such that the AFM spin axes at micromagnet edges can be aligned along any in-plane crystallographic direction.
Lee, Michael S. (ORCID:0000000177852189)↗
Scalable thin graphene oxide membranes enabled by polydopamine gutter layer
Two-dimensional (2D) nanosheets have been widely used to fabricate thin-film composite membranes for dye desalination. However, they often need to be thick to mitigate the defects resulting from their random stacking and rough support surface. Herein, bio-adhesive polydopamine (PDA) is used as a gutter layer to prepare graphene oxide (GO)-based membranes by improving the adhesion between the GO and porous support and providing a smooth surface to form thin, highly selective layers. For example, the PDA priming reduces the GO layer thickness by 57 %, from 447 to 190 nm, while achieving similar dye desalination properties. The effect of the dopamine concentration, exposure time, and GO layer thickness on the membrane structure and desalination performance are thoroughly investigated using various techniques, such as scanning electron microscopy (SEM), x-ray photoelectron spectroscopy (XPS), and x-ray diffraction (XRD). The PDA gutter layer is also applied for hollow fiber membranes, achieving water permeance of 79 L m -2 h −1 bar−1 and rejection of ∼99 % for Direct red 80. The membranes were challenged by simulated dye/salt mixtures to elucidate the complicated effect of the compositions on the desalination performance. Furthermore, this study unveils a new avenue to improve separation performance and large-scale manufacturability of 2D material-based membranes.
Dye desalination↗
Theoretical Analysis of Experimental Data of Sodium Diffusion in Oxidized Molybdenum Thin Films
In this work, the diffusion process of sodium (Na) in molybdenum (Mo) thin films while it was deposited on soda lime glass (SLG) was studied. A small amount of oxygen was present in the chamber while the direct-current (DC) magnetron sputtering was used for the deposition. The substrate temperatures were varied to observe its effect. Such molybdenum films, with or without oxidations, are often used in thin film solar cells, either as back contact or as hole transport layers. Secondary ion mass spectrometry (SIMS) was used to quantify the concentration of the species. A grain diffusion mechanistic model incorporating the effect of grain and grain boundary geometrical shape and size was developed. The model was used to provide an in-depth theoretical analysis of the sodium diffusion in molybdenum thin films that lead to the measured SIMS data. It was observed that not only diffusion coefficients should be considered when analyzing diffusion processes in thin films but also the ratio of grain boundary size to grain size. Both depend on substrate temperature and directly affect the amount of diffused species in the film. The data were analyzed under the light of the film growth speed versus diffusion front speed, the effect of oxygen content, and the effect of substrate temperature on the overall diffusion process. The temperature inversely affects the ratio of grain boundary size and grain size and directly affects the diffusion coefficient, which leads to a preferable temperature at which the highest amount of alkali can be found in the film.
36 MATERIALS SCIENCE↗
Multifunctional Metal–Oxide Nanocomposite Thin Film with Plasmonic Au Nanopillars Embedded in Magnetic La 0.67 Sr 0.33 MnO 3 Matrix
Searching for multifunctional materials with tunable magnetic and optical properties has been a critical task toward the implementation of future integrated optical devices. Vertically aligned nanocomposite (VAN) thin films provide a unique platform for multifunctional material designs. In this work, a new metal–oxide VAN has been designed with plasmonic Au nanopillars embedded in a ferromagnetic La 0.67 Sr 0.33 MnO 3 (LSMO) matrix. Such Au–LSMO nanocomposite presents intriguing plasmon resonance in the visible range and magnetic anisotropy property, which are functionalized by the Au and LSMO phase, respectively. Furthermore, the vertically aligned nanostructure of metal and dielectric oxide results in the hyperbolic property for near-field electromagnetic wave manipulation. Such optical and magnetic response could be further tailored by tuning the composition of Au and LSMO phases.
36 MATERIALS SCIENCE↗
Temperature dependence of nickel ion release from nitinol medical devices
Abstract Nitinol exhibits unique (thermo)mechanical properties that make it central to the design of many medical devices. However, nitinol nominally contains 50 atomic percent nickel, which if released in sufficient quantities, can lead to adverse health effects. While nickel release from nitinol devices is typically characterized using in vitro immersion tests, these evaluations require lengthy time periods. We have explored elevated temperature as a potential method to expedite this testing. Nickel release was characterized in nitinol materials with surface oxide thickness ranging from 12 to 1564 nm at four different temperatures from 310 to 360 K. We found that for three of the materials with relatively thin oxide layers, ≤ 87 nm nickel release exhibited Arrhenius behavior over the entire temperature range with activation energies of 80 to 85 kJ/mol. Conversely, the fourth ''black–oxide'' material, with a much thicker, complex oxide layer, was not well characterized by an Arrhenius relationship. Power law release profiles were observed in all four materials; however, the exponent from the thin oxide materials was approximately 1/4 compared with 3/4 for the black–oxide material. To illustrate the potential benefit of using elevated temperature to abbreviate nickel release testing, we demonstrated that a > 50 day 310 K release profile could be accurately recovered by testing for less than 1 week at 340 K. However, because the materials explored in this study were limited, additional testing and mechanistic insight are needed to establish a protective temperature scaling that can be applied to all nitinol medical device components.
Saylor, David M.↗