Tuning Ionic Conductivity in Fluorite Gd-Doped CeO 2 -Bixbyite RE 2 O 3 (RE = Y and Sm) Multilayer Thin Films by Controlling Interfacial Strain
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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
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Methods for dc to ac conversion Semiannual status report
Thin film deposition on metal oxide semiconductor devices, and dc to ac conversion methods
ALTERNATING CURRENT /AC/↗
Electrically Variable Resistive Memory Devices
Nonvolatile electronic memory devices that store data in the form of electrical- resistance values, and memory circuits based on such devices, have been invented. These devices and circuits exploit an electrically-variable-resistance phenomenon that occurs in thin films of certain oxides that exhibit the colossal magnetoresistive (CMR) effect. It is worth emphasizing that, as stated in the immediately preceding article, these devices function at room temperature and do not depend on externally applied magnetic fields. A device of this type is basically a thin film resistor: it consists of a thin film of a CMR material located between, and in contact with, two electrical conductors. The application of a short-duration, low-voltage current pulse via the terminals changes the electrical resistance of the film. The amount of the change in resistance depends on the size of the pulse. The direction of change (increase or decrease of resistance) depends on the polarity of the pulse. Hence, a datum can be written (or a prior datum overwritten) in the memory device by applying a pulse of size and polarity tailored to set the resistance at a value that represents a specific numerical value. To read the datum, one applies a smaller pulse - one that is large enough to enable accurate measurement of resistance, but small enough so as not to change the resistance. In writing, the resistance can be set to any value within the dynamic range of the CMR film. Typically, the value would be one of several discrete resistance values that represent logic levels or digits. Because the number of levels can exceed 2, a memory device of this type is not limited to binary data. Like other memory devices, devices of this type can be incorporated into a memory integrated circuit by laying them out on a substrate in rows and columns, along with row and column conductors for electrically addressing them individually or collectively.
Liu, Shangqing↗
Suppressed paramagnetism in amorphous Ta 2 O 5 − x oxides and its link to superconducting-qubit performance
Amorphous-oxide layers in thin-film capacitors are linked to reduced transmon-qubit T 1 coherence times. Ta -based capacitors outperform Nb -based ones, suggesting that amorphous Ta 2 O 5 − x is less lossy than Nb 2 O 5 − x . We investigate the microscopic features of these amorphous oxides using ab initio molecular dynamics and density functional theory, revealing the origins of the superior performance of Ta 2 O 5 − x . We establish that oxygen deficiency is less likely to occur in amorphous Ta 2 O 5 − x than in Nb 2 O 5 − x for 0 ≤ x ≤ 0.25 and that for a given oxygen deficiency x , metal Ta — Ta bond formation is enhanced. Such bonds, which are accommodated by structural flaws in the amorphous network, capture electrons better than in amorphous Nb 2 O 5 − x . These thermochemical differences quench or highly suppress magnetic moments in amorphous Ta 2 O 5 − x and eliminate a potential source of quasiparticles and magnetic flux noise. We also show that hyperfine couplings between Nb nuclei and local magnetic moments in Nb 2 O 5 − x can form “two-level systems” (TLSs) or “two-level fluctuators” with energy splittings of 100–1000 MHz or higher. This reveals a TLS mechanism in amorphous Nb 2 O 5 − x oxide layers that is likely inactive in Ta 2 O 5 − x . Our work provides a fundamental understanding of the materials chemistry and limitations imposed by native oxides of superconducting qubits that can be used to guide materials selection and processing.
Pritchard, P. Graham [Northwestern U.] (ORCID:0000↗
Oxidation of metals and alloys in controlled atmospheres using in situ transmission electron microscopy and Auger spectrography
Single-crystalline thin films of copper were oxidized at an isothermal temperature of 425 C and at an oxygen partial pressure of .005 Torr in situ in a high-resolution electron microscope. The specimens were prepared by epitaxial vapor deposition onto polished 100 and 110 faces of rocksalt and mounted in a hot stage inside an ultra-high-vacuum specimen chamber of the microscope. Large amounts of sulfur, carbon, and oxygen were detected by Auger electron spectroscopy on the surface of the as-received films and were removed in situ by ion-sputter etching immediately prior to the oxidation. The nucleation and growth characteristics of Cu2O on Cu were studied. Results show that neither stacking faults nor dislocations are associated with the Cu2O nucleation sites. The growth of Cu2O nuclei is linear with time. The experimental findings, including results from oxygen dissolution experiments and from repetitive oxidation-reduction-oxidation sequences, fit well into the framework of an oxidation process involving (a) the formation of a surface-charge layer, (b) oxygen saturation in the metal and (c) nucleation, followed by surface diffusion of oxygen and bulk diffusion of copper for lateral and vertical oxide growth, respectively.
Rao, D. B.↗
Process for Making a Noble Metal on Tin Oxide Catalyst
To produce a noble metal-on-metal oxide catalyst on an inert, high-surface-area support material (that functions as a catalyst at approximately room temperature using chloride-free reagents), for use in a carbon dioxide laser, requires two steps: First, a commercially available, inert, high-surface-area support material (silica spheres) is coated with a thin layer of metal oxide, a monolayer equivalent. Very beneficial results have been obtained using nitric acid as an oxidizing agent because it leaves no residue. It is also helpful if the spheres are first deaerated by boiling in water to allow the entire surface to be coated. A metal, such as tin, is then dissolved in the oxidizing agent/support material mixture to yield, in the case of tin, metastannic acid. Although tin has proven especially beneficial for use in a closed-cycle CO2 laser, in general any metal with two valence states, such as most transition metals and antimony, may be used. The metastannic acid will be adsorbed onto the high-surface-area spheres, coating them. Any excess oxidizing agent is then evaporated, and the resulting metastannic acid-coated spheres are dried and calcined, whereby the metastannic acid becomes tin(IV) oxide. The second step is accomplished by preparing an aqueous mixture of the tin(IV) oxide-coated spheres, and a soluble, chloride-free salt of at least one catalyst metal. The catalyst metal may be selected from the group consisting of platinum, palladium, ruthenium, gold, and rhodium, or other platinum group metals. Extremely beneficial results have been obtained using chloride-free salts of platinum, palladium, or a combination thereof, such as tetraammineplatinum (II) hydroxide ([Pt(NH3)4] (OH)2), or tetraammine palladium nitrate ([Pd(NH3)4](NO3)2).
Davis, Patricia↗
Flow-Tagging Velocimetry for Hypersonic Flows Using Fluorescence of Nitric Oxide
We demonstrate a new variation of molecular-tagging velocimetry for hypersonic flows based on laser-induced fluorescence. A thin line of nitric-oxide molecules is excited with a laser beam and then, after a time delay, a fluorescence image of the displaced line is acquired. One component of velocity is determined from the time of flight. This method is applied to measure the velocity profile in a Mach 8.5 laminar, hypersonic boundary layer in the Australian National University s T2 free-piston shock tunnel. The single-shot velocity measurement uncertainty in the freestream was found to be 3.5%, based on 90% confidence. The method is also demonstrated in the separated flow region forward of a blunt fin attached to a flat plate in a Mach 7.4 flow produced by the Australian National University s T3 free-piston shock tunnel. The measurement uncertainty in the blunt fin experiment is approximately 30%, owing mainly to low fluorescence intensities, which could be improved significantly in future experiments. This velocimetry method is applicable to very high-speed flows that have low collisional quenching of the fluorescing species. It is particularly convenient in facilities where planar laser-induced fluorescence is already being performed.
Danehy, Paul M.↗
Ultradense Arrays of Sub-100 nm Co/CoO Nanodisks for Spintronics Applications
Sub-100 nm ferromagnetic/antiferromagnetic nanodisks present enhanced magnetic properties with respect to their thin film counterparts. Co/CoO disks were fabricated over large areas by a transferring process of an anodic aluminum oxide membrane, electron beam evaporation of Co, and subsequent oxidation to CoO. This method reveals exchange bias fields up to 4 times larger than that in thin films and higher blocking temperatures for the same oxidation protocol. The significant improvement of the magnetic properties is attributed to finite-size effects in nanostructures and might be exploited in diverse areas such as the magnetic stabilization of ultradense arrays or the scalability process of patterned heterostructures in spintronic phenomena.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
The Mars oxidant experiment (MOx) for Mars '96
The MOx instrument was developed to characterize the reactive nature of the martian soil. The objectives of MOx were: (1) to measure the rate of degradation of organics in the martian environment; (2) to determine if the reactions seen by the Viking biology experiments were caused by a soil oxidant and measure the reactivity of the soil and atmosphere: (3) to monitor the degradation, when exposed to the martian environment, of materials of potential use in future missions; and, finally, (4) to develop technologies and approaches that can be part of future soil analysis instrumentation. The basic approach taken in the MOx instrument was to place a variety of materials composed as thin films in contact with the soil and monitor the physical and chemical changes that result. The optical reflectance of the thin films was the primary sensing-mode. Thin films of organic materials, metals, and semiconductors were prepared. Laboratory simulations demonstrated the response of thin films to active oxidants.
Flight Experiment↗
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↗
Optimization of La 2–x Sr x CuO 4 Single Crystal Film Growth via Molecular Beam Epitaxy
Atomic layer-by-layer molecular beam epitaxy (ALL-MBE) combined with ozone is one of the best methods to fabricate single-crystal thin films of complex oxides. Cuprate such as La 2-x Sr x CuO 4 (LSCO) is a representative complex-oxide high-temperature superconductor (HTS) material. Our group utilizes this method to produce high-quality single-crystal HTS films with atomically smooth surfaces and interfaces. In addition, ALL-MBE enables us to engineer multilayer heterostructures with atomic precision. This allows the fabrication of tunnel junctions, various nanostructures, and other HTS devices of interest for superconducting electronics. We have synthesized over three thousand LSCO thin films in the past two decades. These films’ structural and electronic properties have been studied and characterized by various methods. Here, we distill the extensive experience we accumulated into a step-by-step protocol to fabricate atomically perfect LSCO films. The recipe includes substrate preparation, ozone generation and distillation, source calibration, the in situ monitoring of the film synthesis, post-growth annealing, and ex situ characterization. It discloses a reproducible way to fabricate single-crystal LSCO films for basic research and HTS electronic applications.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Reversible Oxidation Quantified by Optical Properties in Epitaxial Fe2CrO4+d Films on (001) MgAl2O4
We report on the structural and optical properties of Fe2CrO4+d epitaxial films grown by molecular beam epitaxy on MgAl2O4 (001) as a function of ?. The average Fe valence can be correlated with the out-of-plane lattice parameter and the extent of light absorption in the infrared spectral region. Over-oxidized films (0 < d < 0.5) exhibit reduced lattice parameters and suppressed infrared absorption. We discuss the behavior of a novel infrared transition at ~0.6 eV in stoichiometric Fe2CrO4 films deposited on MgAl2O4 (MAO) at or above 400 °C. This research provides new insight into the atomic structure, optical processes, oxidation states, electronic structure, and application potentials of Fe2CrO4+d.
ellipsometry, Epitaxy, thin film, oxidation, reduc↗
CCD imaging sensors
A method for promoting quantum efficiency (QE) of a CCD imaging sensor for UV, far UV and low energy x-ray wavelengths by overthinning the back side beyond the interface between the substrate and the photosensitive semiconductor material, and flooding the back side with UV prior to using the sensor for imaging. This UV flooding promotes an accumulation layer of positive states in the oxide film over the thinned sensor to greatly increase QE for either frontside or backside illumination. A permanent or semipermanent image (analog information) may be stored in a frontside SiO.sub.2 layer over the photosensitive semiconductor material using implanted ions for a permanent storage and intense photon radiation for a semipermanent storage. To read out this stored information, the gate potential of the CCD is biased more negative than that used for normal imaging, and excess charge current thus produced through the oxide is integrated in the pixel wells for subsequent readout by charge transfer from well to well in the usual manner.
Janesick, James R.↗
Combinatorial Growth of Vertically Aligned Nanocomposite Thin Films for Accelerated Exploration in Composition Variation
Combinatorial growth is capable of creating a compositional gradient for thin film materials and thus has been adopted to explore composition variation mostly for metallic alloy thin films and some dopant concentrations for ceramic thin films. This study uses a combinatorial pulsed laser deposition method to successfully fabricate two‐phase oxide–oxide vertically aligned nanocomposite (VAN) thin films of La 0.7 Sr 0.3 MnO 3 (LSMO)‐NiO with variable composition across the film area. The LSMO‐NiO compositional gradient across the film alters the two‐phase morphology of the VAN through varying nanopillar size and density. Additionally, the magnetic anisotropy and magnetoresistance properties of the nanocomposite thin films increase with increasing NiO composition. This demonstration of a combinatorial method for VAN growth can increase the efficiency of nanocomposite thin film research by allowing all possible compositions of thin film materials to be explored in a single deposition.
36 MATERIALS SCIENCE↗
Light Weight Ceramic Ablators for Mars Follow-on Mission Vehicle Thermal Protection System
New Light Weight Ceramic Ablators (LCA) were produced by using ceramic and carbon fibrous substrates, impregnated with silicone and phenolic resins. The special infiltration techniques (patent pending) were developed to control the amount of organic resins in the highly porous fiber matrices so that the final densities of LCA's range from 0.22 to 0.24 g/cc. This paper presents the thermal and ablative performance of the Silicone Impregnated Reusable Ceramic Ablators (SIRCA) in simulated entry conditions for Mars-Pathfinder in the Ames 60 MW Interaction Heating Facility (I HF). Arc jet test results yielded no evidence of char erosion and mass loss at high stagnation pressures to 0.25 atm. Minimal silica melt was detected on surface char at a stagnation pressure of 0.31 atm. Four ceramic substrates were used in the production of SIRCA's to obtain the effective of boron oxide present in substrate so the thermal performance of SIRCA's. A sample of SIRCA was also exposed to the same heating condition for five cycles and no significant mass loss or recession was observed. Tensile testing established that the SIRCA tensile strength is about a factor of two higher than that of the virgin substrates. Thermogravimetric Analysis (TGA) of the char in nitrogen and air showed no evidence of free carbon in the char. Scanning Electron Microscopy of the post test sample showed that the char surface consists of a fibrous structure that was sealed with a thin layer of silicon oxide melt.
Tran, Huy K.↗
Meniscus Guided Coating and Evaporative Crystallization of UiO-66 Metal Organic Framework Thin Films
Thin-film fabrication of metal organic frameworks (MOFs) has been explored for a range of applications, including separations, catalysis, sensing, and charge transport. However, many fabrication techniques have obstacles, including slow crystallization, control over film thickness, and control over crystallinity. Recently, a meniscus-guided coating technique, called solution shearing, has been shown to create MOF thin films within minutes and with control over the film thickness. However, there have been no previous reports of solution shearing based evaporative crystallization of zirconium-based MOFs, which have been widely studied for the aforementioned applications. In this work, for the first time, we show that (i) the zirconium 1,4-dicarboxybenzene MOF, UiO-66, can be formed using evaporative crystallization during solution shearing, and (ii) a wide range of parameters can be tuned to control the film thickness, coverage, and crystallinity. Finally, we bring the solution shearing technique closer to separation applications by growing a full film of UiO-66 crystals up to the resolution of scanning electron microscopy (SEM) on anodic alumina oxide (AAO). This is the first instance of UiO-66 crystals being formed using an evaporative crystallization-based flow coating method, and solution shearing shows the promise to be applicable to form large area zirconium-based MOF crystals in a rapid manner (within seconds to minutes).
42 ENGINEERING↗
Ceramic Composite Thin Films
A ceramic composite thin film or layer includes individual graphene oxide and/or electrically conductive graphene sheets dispersed in a ceramic (e.g. silica) matrix. The thin film or layer can be electrically conductive film or layer depending the amount of graphene sheets present. The composite films or layers are transparent, chemically inert and compatible with both glass and hydrophilic SiOx/silicon substrates. The composite film or layer can be produced by making a suspension of graphene oxide sheet fragments, introducing a silica-precursor or silica to the suspension to form a sol, depositing the sol on a substrate as thin film or layer, at least partially reducing the graphene oxide sheets to conductive graphene sheets, and thermally consolidating the thin film or layer to form a silica matrix in which the graphene oxide and/or graphene sheets are dispersed.
Ruoff, Rodney S.↗
Mechanism of incipient oxidation of bulk chemical vapor deposited Si3N4
X-ray photoelectron spectroscopy was employed, in conjunction with ion bombardment, to analyze the chemical composition profile across thin (less than 50 nm) oxide films on chemically vapor deposited Si3N4. The thermal oxides were grown in dry oxygen at 1100 C on samples with or without native oxide film (formed in room air). The results show that the thermal oxidation product was silicon oxynitride of graded N:O ratio, and that the presence of a native oxide film promotes the formation of a SiO2 crust over the oxynitride. It is proposed that the fundamental mechanism of Si3N4 oxidation is progressive O-for-N substitution in the silicon oxynitride unit tetrahedron, which is best designated SiN(2-x)O(2+x), where x is also an index of depth. The corresponding equation for nonstoichiometric oxidation of Si3N4 describes a bulk (rather than an interface) reaction process, with significant implications for O2 and N2 fluxes and diffusivities.
Ogbuji, L. U. T.↗