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Modification of LiMn 2 O 4 surfaces by controlling the Acid–Base surface chemistry of atomic layer deposition
In this combined theoretical and experimental study, we report the effects of Al precursor selection on the growth chemistry, interfacial structure, and electrochemistry of Al 2 O 3 coatings on spinel LiMn 2 O 4 (LMO) surfaces by atomic layer deposition (ALD). Five Al precursors, exhibiting a range of Lewis acid-base properties, were used to establish trends in the ALD Al 2 O 3 growth chemistry on LMO powders in comparison to redox-inactive planar silicon substrates. We show that the Lewis acid-base properties of the Al precursor ligands can be used to tune both the Mn oxidation states and the Al 2 O 3 coverage on the LMO surface. Density functional theory calculations are used to examine the reaction mechanism of each precursor on LMO surfaces, elucidating a correlation between the Lewis acidity of the ligands and the decomposition thermochemistry. In-depth X-ray photoelectron spectroscopy and in situ Fourier transform infrared spectroscopy measurements support these theoretical predictions and further reveal how different Al precursors modify the atomic and electronic structure near the LMO surface during ALD. While the Mn oxidation state is strongly influenced by the Lewis acidity of the precursor ligand, the surface coverage and thickness of the Al 2 O 3 coating are a more representative descriptor of the electrochemical performance measured in coin cell experiments. Finally, we show how the ligand acid-base properties of ALD precursors can be used to rationally tailor atomic layer growth mechanisms, which may enable atomic level control over the structure of functionalized interfaces for various applications related to catalysis, semiconductors, and energy storage.
Low resistance Ohmic contact to p-type crystalline silicon via nitrogen-doped copper oxide films
This work explores the application of transparent nitrogen doped copper oxide (CuO{sub x}:N) films deposited by reactive sputtering to create hole-selective contacts for p-type crystalline silicon (c-Si) solar cells. It is found that CuO{sub x}:N sputtered directly onto crystalline silicon is able to form an Ohmic contact. X-ray photoelectron spectroscopy and Raman spectroscopy measurements are used to characterise the structural and physical properties of the CuO{sub x}:N films. Both the oxygen flow rate and the substrate temperature during deposition have a significant impact on the film composition, as well as on the resulting contact resistivity. After optimization, a low contact resistivity of ∼10 mΩ cm{sup 2} has been established. This result offers significant advantages over conventional contact structures in terms of carrier transport and device fabrication.
Polarized tip-enhanced Raman spectroscopy at liquid He temperature in ultrahigh vacuum using an off-axis parabolic mirror
Tip-enhanced Raman spectroscopy (TERS) combines inelastic light scattering well below the diffraction limit down to the nanometer range and scanning probe microscopy and, possibly, spectroscopy. In this way, topographic and spectroscopic as well as single- and two-particle information may simultaneously be collected. While single molecules can now be studied successfully, bulk solids are still not meaningfully accessible. It is the purpose of the work presented here to outline approaches toward this objective. We describe a home-built, liquid helium cooled, ultrahigh vacuum TERS. The setup is based on a scanning tunneling microscope and, as an innovation, an off-axis parabolic mirror having a high numerical aperture of ~0.85 and a large working distance. The system is equipped with a fast load-lock chamber, a chamber for the in situ preparation of tips, substrates, and samples, and a TERS chamber. Base pressure and temperature in the TERS chamber were ~3 × 10 –11 mbar and 15 K, respectively. Polarization dependent tip-enhanced Raman spectra of the vibration modes of carbon nanotubes were successfully acquired at cryogenic temperature. The new features described here including very low pressure and temperature and the external access to the light polarizations, thus the selection rules, may pave the way toward the investigation of bulk and surface materials.
GoAmazon 2014/15 Particle Sampling Field Campaign Report
As a part of the GoAmazon 2014/15 field deployments, samples of atmospheric particles were collected at the T3 field site (3° 12' 46.70" S, 60° 35' 53.0, Manacapuru, Brazil) established in the Amazonian region. The site was located downwind from Manaus and therefore, experienced clean conditions when winds were from northwest and polluted conditions when winds were from Manaus. During the second intensive operational period of GoAmazon 2014/15 (09/06/2014-10/02/2014), multiple samples of particles were collected using a cascade Multi-Orifice Uniform Deposition Impactor (MOUDI-110). Size-resolved samples by MOUDI (0.056-0.1, 0.1-0.18, 0.18-0.32, 0.32-0.56, 0.56-1.0, 1.0-1.8 μm) were collected for 6-12 hours. A variety of substrates, compatible with different spectro-microscopy methods of analysis, were arranged on the impactor stages. Collected aerosol samples are now stored pending laboratory analysis using multi-modal methods of chemical imaging. Our approach is to analyze only the samples of specific interest. We use the field campaign records and data on meteorology, as well as in situ measurements of gases and aerosols, to select the subset of samples for the in-depth laboratory analysis for selected episodes where changes in chemical composition of particles can be correlated with other data recorded at the site. Hence, we do not expect to perform detailed measurements on all samples—rather, only those samples with the greatest potential to provide scientific insight into aerosol chemistry.
Interconnnect and bonding technologies for large flexible solar arrays
Thermocompression bonding and conductive adhesive bonding are developed and evaluated as alternate methods of joining solar cells to their interconnect assemblies. Bonding materials and process controls applicable to fabrication of large, flexible substrate solar cell arrays are studied. The primary potential use of the techniques developed is on the solar array developed by NASA/MSFC and LMSC for solar electric propulsion (SEP) and shuttle payload applications. This array is made up of flexible panels approximately 0.7 by 3.4 meters. It is required to operate in space between 0.3 and 6 AU for 5 years with limited degradation. Materials selected must be capable of enduring this space environment, including outgassing and radiation.
Evaluation available encapsulation materials for low-cost long-life silicon photovoltaic arrays
Experimental evaluation of selected encapsulation designs and materials based on an earlier study which have potential for use in low cost, long-life photovoltaic arrays are reported. The performance of candidate materials and encapsulated cells were evaluated principally for three types of encapsulation designs based on their potentially low materials and processing costs: (1) polymeric coatings, transparent conformal coatings over the cell with a structural-support substrate; (2) polymeric film lamination, cells laminated between two films or sheets of polymeric materials; and (3) glass-covered systems, cells adhesively bonded to a glass cover (superstrate) with a polymeric pottant and a glass or other substrate material. Several other design types, including those utilizing polymer sheet and pottant materials, were also included in the investigation.
Cubic GaS: A Surface Passivator For GaAs
Thin films of cubic form of gallium sulfide (GaS) formed on surfaces of gallium arsenide (GaAs) substrates via metal/organic chemical vapor deposition (MOCVD). Deposited cubic GaS, crystalline lattice matched to substrate GaAs, neutralizes electrically active defects on surfaces of both n-doped and p-doped GaAs. Enabling important GaAs-based semiconducting materials to serve as substrates for metal/insulator/semiconductor (MIS) capacitors. Cubic GaS enables fabrication of ZnSe-based blue lasers and light-emitting diodes. Because GaS is optically transparent, deposited to form window layers for such optoelectronic devices as light-emitting diodes, solar optical cells, and semiconductor lasers. Its transparency makes it useful as interconnection material in optoelectronic integrated circuits. Also useful in peeled-film technology because selectively etched from GaAs.
Rotatable crucible for rapid solidification process
This invention relates to an apparatus for producing filament, fiber, ribbon or film from a molten material, comprising a preferably heat extracting crucible which contains a pool of molten material at a selected horizontal level in the pool. The crucible has an opening extending from above the free surface level to a bottom edge of the opening, the bottom edge being sufficiently below the free surface level so that the molten material cannot form and hold a meniscus by surface tension between the edge and the level of the free surface and further comprises a heat extracting substrate laterally disposed with respect to the crucible and which rotates about an axis of rotation. The substrate is positioned adjacent the edge of the opening which confines the molten material and prevents it from overflowing downwardly out of the crucible. The invention features rotating means which includes a first drive means for tiltably rotating the crucible about an axis of rotation which is coaxial with the axis of rotation of the substrate, so the crucible edge can be maintained a predetermined constant distance from the substrate. The distance chosen is suitable for depositing molten material on the substrate and the apparatus also has a second drive means which is drivingly connected to the substrate for continuously moving the surface of the substrate upwardly past the edge and a melt front formed at the interface of the molten material and the substrate surface.
Laboratory Simulation of Impacts upon Aluminum Foils of the Stardust Spacecraft: Calibration of Dust Particle Size from Comet Wild 2
Metallic aluminium alloy foils exposed on the forward, comet-facing surface of the aerogel tray on the Stardust spacecraft are likely to have been impacted by the same cometary particle population as the dedicated impact sensors and the aerogel collector. The ability of soft aluminium alloy to record hypervelocity impacts as bowl-shaped craters offers an opportunistic substrate for recognition of impacts by particles of a wide potential size range. In contrast to impact surveys conducted on samples from low Earth orbit, the simple encounter geometry for Stardust and Wild 2, with a known and constant spacecraft-particle relative velocity and effective surface-perpendicular impact trajectories, permits closely comparable simulation in laboratory experiments. For a detailed calibration programme we have selected a suite of spherical glass projectiles of uniform density and hardness characteristics, with well-documented particle size range from 10 microns to nearly 100 microns. Light gas gun buckshot firings of these particles at approximately 6km s)exp -1) onto samples of the same foil as employed on Stardust have yielded large numbers of craters. Scanning electron microscopy of both projectiles and impact features has allowed construction of a calibration plot, showing a linear relationship between impacting particle size and impact crater diameter. The close match between our experimental conditions and the Stardust mission encounter parameters should provide another opportunity to measure particle size distributions and fluxes close to the nucleus of Wild 2, independent of the active impact detector instruments aboard the Stardust spacecraft.
Application of CO2 Snow Jet Cleaning in Conjunction with Laboratory Based Total Reflection X-Ray Fluorescence
The Genesis mission was the first mission returning solar material to Earth since the Apollo program [1,2]. Unfortunately the return of the space craft on September 8, 2004 resulted in a crash landing, which shattered the samples into small fragments and exposed them to desert soil and other debris. Thus only small fragments of the original collectors are available, each having different degrees of surface contamination. Thorough surface cleaning is required to allow for subsequent analysis of solar wind material embedded within. An initial cleaning procedure was developed in coordination with Johnson Space Center which focused on removing larger sized particulates and a thin film organic contamination acquired during collection in space [3]. However, many of the samples have additional residues and more rigorous and/or innovative cleaning steps might be necessary. These cleaning steps must affect only the surface to avoid leaching and re-distribution of solar wind material from the bulk of the collectors. To aid in development and identification of the most appropriate cleaning procedures each sample has to be thoroughly inspected before and after each cleaning step. Laboratory based total reflection X-ray fluorescence (TXRF) spectrometry lends itself to this task as it is a non-destructive and surface sensitive analytical method permitting analysis of elements from aluminum onward present at and near the surface of a flat substrate [4]. The suitability of TXRF has been demonstrated for several Genesis solar wind samples before and after various cleaning methods including acid treatment, gas cluster ion beam, and CO2 snow jet [5 - 7]. The latter one is non-invasive and did show some promise on one sample [5]. To investigate the feasibility of CO2 snow jet cleaning further, several flown Genesis samples were selected to be characterized before and after CO2 snow application with sample 61052 being discussed below.
Additively Manufactured Strain Sensing for Nuclear Reactor Applications
Real-time monitoring of materials in harsh environments is a crucial technique towards reducing innovation time in nuclear systems. The successful measurement of real time, in-situ strain measurements during nuclear reactor operation requires innovative sensing solutions, including novel sensing strategies as well as advanced sensor design, manufacturing, and materials selection. In this paper, we will discuss two primary strategies for in-situ strain measurement strategies: additively manufactured (AM) capacitive strain gauges (CSGs) and digital image correlation (DIC). Current commercial strain gauges have limited applications in reactors due to the harsh operating conditions and non-trivial attachment strategies (i.e., welding, epoxy-adhesive) that can affect both the sensing performance and the underlying substrate under testing. AM CSGs are a viable solution as they have a low profile, low hysteresis, and wireless sensing integration capabilities that will enhance nuclear sensing technologies. In this work, the mechanical and thermal performance of the AM CSGs were tested up to 300 °C using ASTM standardized testing procedures to simulate the temperatures found in existing light water reactors. The AM CSGs had a similar performance across multiple samples which correlates to analytical models. This work leads towards the development of CSGs designed for higher temperatures and additional environmental factors found in Generation-IV reactors. Non-contact sensors, such as DIC, offer a less destructive way to measure deformation of materials when compared to alternative methods of in-situ strain determination, such as weldable strain gauges. However, DIC requires high contrast surfaces, which often relies on the implementation of artificial patterns. Using traditional splatter techniques to fabricate these patterns have limitations, including poor surface adhesion and reproducibility. In this work, AM fabrication techniques were implemented to avoid such limitations. Accordingly, aerosol jet printing (AJP) was used to print small scale periodic patterns of silver on stainless steel and aluminum tensile specimens. DIC was employed to monitor strain (up to 1100 µe) during temperature cycling from 23-600 °C. The results validated the use of AJP to better control pattern parameters for small fields of view applications at high temperatures.
Controlled Selective CVD Growth of ZnO Nanowires Enabled by Mask‐Free Fabrication Approach using Aqueous Fe Catalytic Inks
Abstract Fabrication process that enables selective growth of vertically oriented zinc oxide (ZnO) nanowires (NWs) via chemical vapor deposition method and mask‐free patterning approach is reported. It is shown that synthesis of high‐quality ZnO nanowires in various architectures is achievable by optimizing the growth conditions and by precise patterning of catalytic ink precursors. Parallel direct‐write patterning method is utilized to fabricate arrays of different architectures on Si/SiO 2 substrates and directly on devices at preselected locations. The production of high‐quality, crystalline ZnO NWs is demonstrated using aqueous iron catalytic inks. The composition of the ink and the lateral size of the patterns deposited on substrates are shown to affect the resulting nanowires and thus, allowing to control the geometry (length and diameter) of the individual ZnO NWs in the patterned assemblies. The results indicate that our protocols are tailored to the fabrication of ZnO NWs with specific surface geometries and interface functionalities for variety of targeted device applications.
Optimizing the Synthetic Potential of O 2 : Implications of Overpotential in Homogeneous Aerobic Oxidation Catalysis
Molecular oxygen is the quintessential oxidant for organic chemical synthesis, but many challenges continue to limit its utility and breadth of applications. Extensive historical research has focused on overcoming kinetic challenges presented by the ground-state-triplet electronic structure of O 2 and the various reactivity and selectivity challenges associated with reactive oxygen species derived from O 2 reduction. This Perspective will analyze thermodynamic principles underlying catalytic aerobic oxidation reactions, borrowing concepts from the study of the oxygen reduction reaction (ORR) in fuel cells. This analysis is especially important for "oxidase"-type liquid-phase catalytic aerobic oxidation reactions, which proceed by a mechanism that couples two sequential redox half-reactions: (1) substrate oxidation, and (2) oxygen reduction, typically affording H 2 O 2 or H 2 O. The catalysts for these reactions feature redox potentials that lie between the potentials associated with the substrate oxidation and oxygen reduction reactions, and changes in the catalyst potential lead to variations in effective overpotentials for the two half reactions. Catalysts that operate at low ORR overpotential retain more thermodynamic driving force for the substrate oxidation step, enabling O 2 to be used in more challenging oxidations. While catalysts that operate at high ORR overpotential have less driving force available for substrate oxidation, they often exhibit different or improved chemoselectivity relative to the high-potential catalysts. The concepts are elaborated in a series of case studies to highlight their implications for chemical synthesis. Examples include comparisons of (a) NO x /oxoammonium and Cu/nitroxyl catalysts, (b) high-potential quinones and amine oxidase biomimetic quinones, and (c) Pd aerobic oxidation catalysts, with or without NO x cocatalysts. In addition, we show how reductive activation of O 2 provides a means to access potentials not accessible with conventional oxidase-type mechanisms. Altogether, this analysis highlights the central role of catalyst overpotential in guiding the development of aerobic oxidation reactions.
Application of functional genomics for domestication of novel non-model microbes
Abstract With the expansion of domesticated microbes producing biomaterials and chemicals to support a growing circular bioeconomy, the variety of waste and sustainable substrates that can support microbial growth and production will also continue to expand. The diversity of these microbes also requires a range of compatible genetic tools to engineer improved robustness and economic viability. As we still do not fully understand the function of many genes in even highly studied model microbes, engineering improved microbial performance requires introducing genome-scale genetic modifications followed by screening or selecting mutants that enhance growth under prohibitive conditions encountered during production. These approaches include adaptive laboratory evolution, random or directed mutagenesis, transposon-mediated gene disruption, or CRISPR interference (CRISPRi). Although any of these approaches may be applicable for identifying engineering targets, here we focus on using CRISPRi to reduce the time required to engineer more robust microbes for industrial applications. One-Sentence Summary The development of genome scale CRISPR-based libraries in new microbes enables discovery of genetic factors linked to desired traits for engineering more robust microbial systems.
Microwave integrated circuit for Josephson voltage standards
A microwave integrated circuit comprised of one or more Josephson junctions and short sections of microstrip or stripline transmission line is fabricated from thin layers of superconducting metal on a dielectric substrate. The short sections of transmission are combined to form the elements of the circuit and particularly, two microwave resonators. The Josephson junctions are located between the resonators and the impedance of the Josephson junctions forms part of the circuitry that couples the two resonators. The microwave integrated circuit has an application in Josephson voltage standards. In this application, the device is asymmetrically driven at a selected frequency (approximately equal to the resonance frequency of the resonators), and a d.c. bias is applied to the junction. By observing the current voltage characteristic of the junction, a precise voltage, proportional to the frequency of the microwave drive signal, is obtained.
The sugar model: catalytic flow reactor dynamics of pyruvaldehyde synthesis from triose catalyzed by poly-l-lysine contained in a dialyzer
The formation of pyruvaldehyde from triose sugars was catalyzed by poly-l-lysine contained in a small dialyzer with a 100 molecular weight cut off (100 MWCO) suspended in a much larger triose substrate reservoir at pH 5.5 and 40 degrees C. The polylysine confined in the dialyzer functioned as a catalytic flow reactor that constantly brought in triose from the substrate reservoir by diffusion to offset the drop in triose concentration within the reactor caused by its conversion to pyruvaldehyde. The catalytic polylysine solution (400 mM, 0.35 mL) within the dialyzer generated pyruvaldehyde with a synthetic intensity (rate/volume) that was 3400 times greater than that of the triose substrate solution (12 mM, 120 mL) outside the dialyzer. Under the given conditions the final yield of pyruvaldehyde was greater than twice the weight of the polylysine catalyst. During the reaction the polylysine catalyst was poisoned presumably by reaction of its amino groups with aldehyde reactants and products. Similar results were obtained using a dialyzer with a 500 MWCO. The dialyzer method of catalyst containment was selected because it provides a simple and easily manipulated experimental system for studying the dynamics and evolutionary development of confined autocatalytic processes related to the origin of life under anaerobic conditions.
Rhombohedral cubic semiconductor materials on trigonal substrate with single crystal properties and devices based on such materials
Growth conditions are developed, based on a temperature-dependent alignment model, to enable formation of cubic group IV, group II-V and group II-VI crystals in the [111] orientation on the basal (0001) plane of trigonal crystal substrates, controlled such that the volume percentage of primary twin crystal is reduced from about 40% to about 0.3%, compared to the majority single crystal. The control of stacking faults in this and other embodiments can yield single crystalline semiconductors based on these materials that are substantially without defects, or improved thermoelectric materials with twinned crystals for phonon scattering while maintaining electrical integrity. These methods can selectively yield a cubic-on-trigonal epitaxial semiconductor material in which the cubic layer is substantially either directly aligned, or 60 degrees-rotated from, the underlying trigonal material.