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At least 433 records · Page 24

Commissioning of a modulated pulse-power magnetron sputtering system for depositing niobium thin films

A modulated pulse-power magnetron sputtering system (MPPMS) was commissioned and used to deposit niobium on copper. MPPMS utilizes a modulated pulse train with high peak-to-average energy ratios, thereby increasing the energy density leading to the production of the energetic ions. The MPPMS modulator was designed and constructed based on large voltage/current IGBT modules, which can be externally modulated, produce bi-polar waveforms, and are readily available. A high voltage power supply provides moderate current to the IGBT module to create the precise pulse structure. The MPPMS system was used to deposit ~1 mm thick, niobium film on a copper substrate held at ~77 K to minimize Nb atom surface diffusion and maximize intrinsic film energy. Finally, the Nb film had an average grain size of ~8 nm.

42 ENGINEERING↗

Electrochemical Formation of Li-M-(M')-Si Phases Using Multivalent Electrolyte Salt Additives

Lithium-rich silicides (Li 15 Si 4 ), formed during the electrochemical lithiation of silicon, show high reactivity with electrolyte components that contribute to capacity decay, formal lithium loss, and low coulombic efficiency. Recently, the reactivity of lithium silicides was found to be suppressed by substituting a multivalent cation (i.e. Mg, Ca) for lithium that results in the room temperature formation of a ternary Li-M-Si phase. In this study, we explored a range of multivalent electrolyte salt additives (M = Ni, Cu, La, Ce, Sr, Ba, and Ca-Mg mixed salt) in a lithium-ion cell configuration and identified a room temperature electrochemical route to the formation of new ternary and quaternary lithium silicides. Using this method, both nickel and copper salts were found to plate onto the silicon electrode surface upon lithiation. Further, based on refined synchrotron XRD data, multivalent cations with an ionic radius similar to Na (~1.03 Å) or smaller can be inserted electrochemically into a formally cation-deficient Li 15 Si 4 host lattice to form new ternary (or quartenary) phases. The electrochemical synthesis of a new quaternary Li-M-M’-Si phase represents a facile route to preparing and scaling materials isostructural to the Heusler phase and electron-precise Li 14 MgSi 4 phase that results in enhanced cycling and calendar life performance.

25 ENERGY STORAGE↗

Morphological stability and fluid dynamics of vapor crystal growth

Progress is reported in establishing the capabilities of thermal deflection spectroscopy for measurements of the concentration field around a growing crystal. Work was completed on the inclusion of the next nearest neighbor interaction into a surface roughness model and the resulting formalism was applied to copper, zinc, and lead. Other work in mass spectroscopy and vapor transport is discussed.

Rosenberger, F. E.↗

Quick Access Rocket Exhaust Rig Testing of Coated GRCop-84 Sheets Used to Aid Coating Selection for Reusable Launch Vehicles

The design of the next generation of reusable launch vehicles calls for using GRCop-84 copper alloy liners based on a composition1 invented at the NASA Glenn Research Center: Cu-8(at.%)Cr-4%Nb. Many of the properties of this alloy have been shown to be far superior to those of other conventional copper alloys, such as NARloy-Z. Despite this considerable advantage, it is expected that GRCop-84 will suffer from some type of environmental degradation depending on the type of rocket fuel utilized. In a liquid hydrogen (LH2), liquid oxygen (LO2) booster engine, copper alloys undergo repeated cycles of oxidation of the copper matrix and subsequent reduction of the copper oxide, a process termed "blanching". Blanching results in increased surface roughness and poor heat-transfer capabilities, local hot spots, decreased engine performance, and premature failure of the liner material. This environmental degradation coupled with the effects of thermomechanical stresses, creep, and high thermal gradients can distort the cooling channel severely, ultimately leading to its failure.

Raj, Sai V.↗

Mechanical Properties and Microstructure Investigation of Lead Free Solder

While the electronics industry appears to be focusing on Sn-Ag-Cu as the alloy of choice for lead free electronics assembly, ,the exact composition varies by geographic region, supplier and user. Add to that dissolved copper and silver from the printed circuit board traces and surface finish, and there can be significant variation in the final solder joint composition. A systematic study of the mechanical and microstructural properties of Sn-Ag-Cu alloys with Ag varying from 2wt% to 4wt% and Cu varying from 0.5wt% to lSwt%, was undertaken in this research study. Different sample preparation techniques (water quenched, oil quenched and water quenched followed by reflow) were explored and the resulting microstructure compared to that of a typical reflowed lead free chip scale package (CSP) solder joint. Tensile properties (modulus, 0.2% yield strength and the ultimate tensile strength) and creep behavior of selected alloy compositions (Sn-4Ag-1 X u , Sn-4Ag-OSCu, Sn- 2Ag-1 X u , Sn-2Ag-OSCu, Sn-3.5Ag-O.SCu) were determined for three conditions: as- cast; aged for 100 hours at 125OC; and aged for 250 hours at 125OC. There was no significant difference in Young's Modulus as a function of alloy composition. After an initial decrease in modulus after 100 hours at 125"C, there was an insignificant change with further aging. The distribution of 0.2% strain yield stress and ultimate tensile strength as a function of alloy composition was more significant and decreased with aging time and temperature. The microstructures of these alloys were examined using light and scanning electron microscopy (LM and SEM) respectively and SEM based energy dispersive x-ray spectroscopy (EDS). Fracture surface and cross-section analysis were performed on the specimens after creep testing. The creep testing results and the effect of high temperature aging on mechanical properties is presented for the oil quenched samples. In general the microstructure of oil quenched specimen exhibited a eutectic region of Sn with moderately dispersed Ag3Sn intermetallic, surrounded by a dendritic Sn-rich phase. The SEM images of the fracture surface indicated the presence of a tough shear surface at the initial cavity break area and a break line in the middle of specimen along the failure direction. A hyperbolic-sine creep model was adopted and used to fit the creep experiment data. The effect on the mechanical properties by adding the quaternary element bismuth to the Sn-3.5Ag-0.8Cu alloy was measured and compared with the mechanical properties of the ternary alloys. The results of this research study provide necessary data for the modeling of solder joint reliability for a range of Sn-Ag-Cu compositions and a baseline for evaluating the effects of subsequent quaternary additions.

Wang, Qing↗

Hermetically sealable package for hybrid solid-state electronic devices and the like

A light-weight, inexpensively fabricated, hermetically sealable, repairable package for small electronic or electromechanical units, having multiple connections, is described. A molded ring frame of polyamide-imide plastic (Torlon) is attached along one edge to a base plate formed of a highly heat conducting material, such as aluminum or copper. Bores are placed through a base plate within the area of the edge surface of ring frame which result in an attachment of the ring frame to the base plate during molding. Electrical leads are molded into the ring frame. The leads are L-shaped gold-plated copper wires imbedded within widened portions of the side wall of the ring frame. Within the plastic ring frame wall the leads are bent (typically, though not necessarily at 90 deg) so that they project into the interior volume of the ring frame for connection to the solid state devices.

Miller, Wilson N.↗

Auger electron spectroscopy study of initial stages of oxidation in a copper - 19.6-atomic-percent-aluminum alloy

Auger electron spectroscopy was used to examine the initial stages of oxidation of a polycrystalline copper - 19.6 a/o-aluminum alloy. The growth of the 55-eV aluminum oxide peak and the decay of the 59-, 62-, and 937-eV copper peaks were examined as functions of temperature, exposure, and pressure. Pressures ranged from 1x10 to the minus 7th power to 0.0005 torr of O2. Temperatures ranged from room temperature to 700 C. A completely aluminum oxide surface layer was obtained in all cases. Complete disappearance of the underlying 937-eV copper peak was obtained by heating at 700 C in O2 at 0.0005 torr for 1 hr. Temperature studies indicated that thermally activated diffusion was important to the oxidation studies. The initial stages of oxidation followed a logarithmic growth curve.

Ferrante, J.↗

Assessing the quality of large-area monolayer graphene grown on liquid copper for size-selective ionic/molecular membrane separations

Monolayer graphene growth on liquid copper (Cu) has attracted attention due to advantages of a flat/smooth catalytic growth surface, high synthesis temperature (>1080 °C) as well as the possibility of forming graphene domains that are mobile on the liquid Cu with potential to minimize grain boundary defects and self-assemble into a continuous monolayer film. However, the quality of monolayer graphene grown on liquid copper and its suitability for size-selective ionic/molecular membrane separations has not been evaluated/studied. Here, we probe the quality of monolayer graphene grown on liquid Cu (via a metallurgical process, HSMG ® ) using Scanning Electron Microscope (SEM), High-resolution transmission electron microscope (HR-TEM), Raman spectroscopy and report on a facile approach to assess intrinsic sub-nanometer to nanometer-scale defects over centimeter-scale areas. We demonstrate high transfer yields of monolayer graphene (>93% coverage) from the growth substrate to polyimide track etched membrane (PITEM, pore diameter ~200 nm) supports to form centimeter-scale atomically thin membranes. Next, we use pressure-driven transport of ethanol to probe defects > 60 nm and diffusion-driven transport of analytes (KCl ~0.66 nm, L-Tryptophan ~0.7–0.9 nm, Vitamin B12 ~1–1.5 nm and Lysozyme ~3.8–4 nm) to probe nanoscale and sub-nanometer scale defects. Diffusive transport confirms the presence of intrinsic sub-nanometer to nanometer scale defects in monolayer graphene grown on liquid Cu are no less than that in high-quality graphene synthesized via chemical vapor deposition (CVD) on solid Cu. Our work not only benchmarks quality of graphene grown on liquid copper for membrane applications but also provides fundamental insights into the origin of intrinsic defects in large-area graphene synthesized via bottom-up processes for membrane applications.

36 MATERIALS SCIENCE↗

Thin film strain transducer

A strain transducer system and process for making the same is disclosed. A beryllium copper ring having four strain gages is electrically connected in Wheatstone bridge fashion to the output instrumentation. Tabs are bonded to a balloon or like surface with strain on the surface causing bending of a ring which provides an electrical signal through the gages proportional to the surface strain. A photographic pattern of a one half ring segment as placed on a sheet of beryllium copper for chem-mill etch formation is illustrated.

Rand, J. L.↗

Interaction of atomic oxygen with thin film and bulk copper: An XPS, AES, XRD, and profilometer study

The University of Alabama in Huntsville (UAH) experiment A-0114 was designed primarily to study degradation of material surfaces due to low earth orbital (LEO) atmospheric oxygen. The experiment contained 128 one inch circular samples: metals, polymers, carbons, and semiconductors. Among metal samples, copper has shown some interesting new results. Two types of copper samples, a film sputter coated on fused silica and a bulk piece of OFHC copper, were characterized employing a variety of techniques such as X-ray and Auger electron spectroscopies, X-ray diffraction, and high resolution profilometry. Cu 2p core level spectra were used to characterize the presence of Cu2O and CuO in addition to Cu Auger LMM lines. These results are supported by our recent X-ray diffraction studies which clearly establish the presence of Cu oxides which we were unable to prove in our earlier work. Profilometry showed an increase in thickness of the film sample where exposed to 106.7 +/- 0.5 nm from an initial thickness of 74.2 +/- 1.1 nm. Further studies with SEM and ellipsometry are underway.

Raikar, Genesh N.↗

Wear of single-crystal silicon carbide in contact with various metals in vacuum

Sliding friction experiments were conducted in vacuum with single crystal silicon carbide (0001) surface in contact with transition metals (tungsten, iron, rhodium, nickel, titanium, and cobalt), copper, and aluminum. The hexagon shaped cracking and fracturing of silicon carbide that occurred is believed to be due to cleavages of both the prismatic and basal planes. The silicon carbide wear debris, which was produced by brittle fracture, slides or rolls on both the metal and silicon carbide and produces grooves and indentations on these surfaces. The wear scars of aluminum and titanium, which have much stronger chemical affinity for silicon and carbon, are generally rougher than those of the other metals. Fracturing and cracking along the grain boundary of rhodium and tungsten were observed. These may be primarily due to the greater shear moduli of the metals.

Miyoshi, K.↗

CO 2 Adsorption and Hydrogenation on Inverse InO x /Cu(111) Catalysts: Active Role of the Oxide–Metal Interface

The direct conversion of carbon dioxide (CO 2 ) into methanol via hydrogenation is essential for industrial applications. Recent studies on catalysts that contain an inverse oxide/metal configuration have shown very good catalytic performance for the CO 2 hydrogenation to methanol process. Here, in this study, we investigated the behavior of indium oxide-Cu(111) interfaces under pure CO 2 and CO 2 /H 2 mixtures using synchrotron-based ambient-pressure X-ray photoelectron spectroscopy (AP-XPS). Initially, a single layer of copper oxide (Cu x O) was grown on the Cu(111) surface by controlled oxidation. On this surface, indium was deposited at room temperature. Oxygen atoms transferred from Cu x O/Cu(111) to the indium metal upon deposition, forming In-O-Cu bonds and active interfaces. Although Cu(111) is not very active for the binding and activation of CO 2 , the formed InO x -Cu(111) interfaces had no problem adsorbing and dissociating the molecule at room temperature. Reaction of CO 2 with H 2 on InO x -Cu(111) yielded surface-bound H 3 CO, CO 2 δ− , CO 3 , and CH x species that are typical intermediates in the production of methanol and other oxygenates. The InO x -Cu(111) interface underwent dynamic chemical changes under reaction conditions, forming In-Cu alloys at low indium coverages (< 0.05 monolayer), while at higher indium coverages a mixture of an In-Cu and InO x was detected in XPS. These findings indicate that InO x /In-Cu interfaces can play a key role in processes aimed at the trapping and valorization of CO 2 .

36 MATERIALS SCIENCE↗

Innovative Electrostatic Adhesion Technologies

Developing specialized Electro-Static grippers (commercially used in Semiconductor Manufacturing and in package handling) will allow gentle and secure Capture, Soft Docking, and Handling of a wide variety of materials and shapes (such as upper-stages, satellites, arrays, and possibly asteroids) without requiring physical features or cavities for a pincher or probe or using harpoons or nets. Combined with new rigid boom mechanisms or small agile chaser vehicles, flexible, high speed Electro-Static Grippers can enable compliant capture of spinning objects starting from a safe stand-off distance. Electroadhesion (EA) can enable lightweight, ultra-low-power, compliant attachment in space by using an electrostatic force to adhere similar and dissimilar surfaces. A typical EA enabled device is composed of compliant space-rated materials, such as copper-clad polyimide encapsulated by polymers. Attachment is induced by strong electrostatic forces between any substrate material, such as an exterior satellite panel and a compliant EA gripper pad surface. When alternate positive and negative charges are induced in adjacent planar electrodes in an EA surface, the electric fields set up opposite charges on the substrate and cause an electrostatic adhesion between the electrodes and the induced charges on the substrate. Since the electrodes and the polymer are compliant and can conform to uneven or rough surfaces, the electrodes can remain intimately close to the entire surface, enabling high clamping pressures. Clamping pressures of more than 3 N/cm2 in shear can be achieved on a variety of substrates with ultra-low holding power consumption (measured values are less than 20 microW/Newton weight held). A single EA surface geometry can be used to clamp both dielectric and conductive substrates, with slightly different physical mechanisms. Furthermore EA clamping requires no normal force be placed on the substrate, as conventional docking requires. Internally funded research and development has demonstrated that EA can function effectively in space, even in the presence of strong ultraviolet radiation, atomic oxygen, and free electrons. We created a test setup in an existing vacuum chamber to simulate low-Earth-orbit conditions. An EA mechanism was fabricated and installed in the chamber, instrumented, operated in a vacuum, and subjected to ultraviolet photons and free electrons generated by an in-chamber multipactor electron emitter. Extensions to EA that can add value include proximity and contact sensing and transverse motion or rotation, both of which could enhance docking or assembly applications. Possible next steps include development of targeted applications for ground investigation or on-orbit subsystem performance demonstrations using low cost access to space such as CubeSats.

Bryan, Tom↗

Millimeter-wave surface resistance of laser-ablated YBa2Cu3O(7-delta) superconducting films

The millimeter-wave surface resistance of YBa2Cu3O(7-delta) superconducting films was measured in a gold-plated copper host cavity at 58.6 GHz between 25 and 300 K. High-quality laser-ablated films of 1.2-micron thickness were deposited on SrTiO3 and LaGaO3 substrates. Their transition temperatures were 90.0 and 88.9 K, with a surface resistance at 70 K of 82 and 116 milliohms, respectively. These values are better than the values for the gold-plated cavity at the same temperature and frequency.

Miranda, F. A.↗

First-principles design of a single-atom–alloy propane dehydrogenation catalyst

The complexity of heterogeneous catalysts means that a priori design of new catalytic materials is difficult, but the well-defined nature of single-atom–alloy catalysts has made it feasible to perform unambiguous theoretical modeling and precise surface science experiments. Herein we report the theory-led discovery of a rhodium-copper (RhCu) single-atom–alloy catalyst for propane dehydrogenation to propene. Although Rh is not generally considered for alkane dehydrogenation, first-principles calculations revealed that Rh atoms disperse in Cu and exhibit low carbon-hydrogen bond activation barriers. Surface science experiments confirmed these predictions, and together these results informed the design of a highly active, selective, and coke-resistant RhCu nanoparticle catalyst that enables low-temperature nonoxidative propane dehydrogenation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

An ultra-compact x-ray free-electron laser

In the field of beam physics, two frontier topics have taken center stage due to their potential to enable new approaches to discovery in a wide swath of science. These areas are: advanced, high gradient acceleration techniques, and x-ray free electron lasers (XFELs). Further, there is intense interest in the marriage of these two fields, with the goal of producing a very compact XFEL. In this context, recent advances in high gradient radio-frequency cryogenic copper structure research have opened the door to the use of surface electric fields between 250 and 500 MV m -1 . Such an approach is foreseen to enable a new generation of photoinjectors with six-dimensional beam brightness beyond the current state-of-the-art by well over an order of magnitude. This advance is an essential ingredient enabling an ultra-compact XFEL (UC-XFEL). In addition, one may accelerate these bright beams to GeV scale in less than 10 m. Such an injector, when combined with inverse free electron laser-based bunching techniques can produce multi-kA beams with unprecedented beam quality, quantified by 50 nm-rad normalized emittances. The emittance, we note, is the effective area in transverse phase space (x, p x /m e c) or (y, p y /m e c) occupied by the beam distribution, and it is relevant to achievable beam sizes as well as setting a limit on FEL wavelength. These beams, when injected into innovative, short-period (1–10 mm) undulators uniquely enable UC-XFELs having footprints consistent with university-scale laboratories. We describe the architecture and predicted performance of this novel light source, which promises photon production per pulse of a few percent of existing XFEL sources. We review implementation issues including collective beam effects, compact x-ray optics systems, and other relevant technical challenges. To illustrate the potential of such a light source to fundamentally change the current paradigm of XFELs with their limited access, we examine possible applications in biology, chemistry, materials, atomic physics, industry, and medicine—including the imaging of virus particles—which may profit from this new model of performing XFEL science.

47 OTHER INSTRUMENTATION↗

Heating of Cs2Te photocathode via field emission and radiofrequency pulsed heating: Implication toward breakdown

The occurrence of radiofrequency (RF) breakdown limits operational electromagnetic gradients in accelerator structures. Experimental evidence often suggests that breakdown events are associated with temperature and dark current spikes on the surface of RF devices. In the past decade, there has been increased interest in unveiling the mechanism behind breakdown initiation in metal copper and copper alloys; however, efforts regarding a breakdown phenomenon in photocathode-relevant semiconductors have been more limited. In this work, we explore field-emission-assisted heating via Nottingham and Joule processes, as a possible candidate for breakdown initiation. For this, field emission from an intrinsic Cs2Te ultrathin film coated on a copper substrate was modeled within the Stratton–Baskin–Lvov–Fursey formalism, describing the processes and effects in the bulk and on the surface of a photocathode exposed to high RF electromagnetic fields. It is shown that a field-emission characteristic deviates significantly from the classical Fowler–Nordheim (FN) theory, whereby predicting that dark current is orders of magnitude lower than the one expected by FN law. Conventional pulsed heating was also found to impose negligible heating to the photocathode. Both conclusions suggest that a Cs2Te photocathode coated on a metal substrate would be insensitive to catastrophic thermal-material runaway breakdown, unlike what is observed for metal surfaces. Finally, a few unconventional breakdown candidate scenarios are identified and discussed, including thermoelastic deformation and avalanche breakdown.

Shinohara, Ryo (ORCID:0000000276995732)↗