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At least 721 records · Page 40

Inhibition of Micro-pitting by Tribofilm-Forming ZrO 2 Nanocrystal Lubricant Additives: A Micro-pitting Rig and Transmission Electron Microscope Study

The drive to reduce fuel consumption in transportation has encouraged the emergence of low viscosity lubricants to reduce viscous losses in the engine, drivetrain, and other components. However, viscosity reduction increases the risk of surface damage, thus motivating the development of new anti-wear (AW) additives. Capped ZrO 2 nanocrystals (NCs) in base oils have been shown to form AW tribofilms within microscale sliding contacts. However, the potential of ZrO 2 NCs to protect surfaces subjected to rolling-sliding contact from macroscale damage, such as micro-pitting, remains unexplored. Here, we explore the ability of ZrO 2 NCs to form protective tribofilms under harsh conditions using a micro-pitting rig (MPR), consisting of a three ring-on-roller configuration. The experiments were conducted in polyalphaolephin (PAO) base oil, with and without 5 nm diameter ZrO 2 NCs, at two levels of slide-to-roll ratio (SRR) (30% and 0%) and at variable test durations up to long durations (119 h). MPR results showed the use of ZrO 2 NCs gives rise to the formation of a tribofilm covering the roller surfaces and decreases the initiation and propagation of micro-pits compared to tests in pure PAO base stock. Transmission electron microscopy (TEM) performed on focused ion beam (FIB) milled cross-sectional samples of the roller surfaces revealed the growth of dense and 50–100 nm thick ZrO 2 -based tribofilms independent of (SRR), indicating the potential for robust micro-pitting fatigue protection. Nevertheless, small cracks localized within the near surface region of the roller tested at the most severe conditions (30% SRR and 119 h) were observed. The initiation of these cracks was directly related to the presence of manganese sulphide (MnS) inclusions in the steel, revealed using TEM combined with energy dispersive spectroscopy (EDS). Furthermore, the results highlight the benefits of the protective tribofilms formed by ZrO 2 NCs and suggest approaches for further optimizing their use.

36 MATERIALS SCIENCE↗

Thermo-mechanical characterization of shale using nanoindentation

Abstract Shale can be a potential buffer for high-level radioactive nuclear wastes. To be an effective buffer while subject to waste heat, shale's mechanical response at elevated temperature must be known. Many researchers have experimentally characterized the mechanical behavior of various shales at different length scales in adiabatic conditions. However, its mechanical performance at elevated temperatures at the nano-scale remains unknown. To investigate the temperature dependency of nanomechanical properties of shale, we conducted both experimental and numerical studies. In this study, we measured mechanical and fracture properties of shale, such as hardness, elastic modulus, anisotropy, and fracture toughness from 25 °C up to 300 °C at different bedding planes. Statistical analysis of the results suggests that hardness and fracture toughness significantly increased at temperatures from 100 to 300 °C; while, temperature does not have a significant impact on elastic modulus. Data also shows that the bedding plane orientations have a substantial impact on both mechanical and fracture properties of shale at the nano-scale leading to distinct anisotropic behavior at elevated temperature below 100 °C. Additionally, we numerically investigated the mechanical performance of the shale samples at room temperature to gain an insight into its mechanical response through the thickness. Numerical results were validated against the experimental results, confirming the simulation can be used to predict shale deformation at the nano-scale or potentially be used in multi-scale simulations.

36 MATERIALS SCIENCE↗

Heat-driven acoustic phonons in lamellar nanoplatelet assemblies

Colloidal CdSe nanoplatelets, with the electronic structure of quantum wells, self-assemble into lamellar stacks due to large co-facial van der Waals attractions. These lamellar stacks are shown to display coherent acoustic phonons that are detected from oscillatory changes in the absorption spectrum observed in infrared pump, electronic probe measurements. Rather than direct electronic excitation of the nanocrystals using a femtosecond laser, impulsive transfer of heat from the organic ligand shell, excited at C–H stretching vibrational resonances, to the inorganic core of individual nanoplatelets occurs on a time-scale of <100 ps. This heat transfer drives in-phase longitudinal acoustic phonons of the nanoplatelet lamellae, which are accompanied by subtle deformations along the nanoplatelet short axes. The frequencies of the oscillations vary from 0.7 to 2 GHz (3–8 μeV and 0.5–1 ns oscillation period) depending on the thickness of the nanoplatelets—but not their lateral areas—and the temperature of the sample. Temperaturedependence of the acoustic phonon frequency conveys a substantial stiffening of the organic ligand bonds between nanoplatelets with reduced temperature. Overall, these results demonstrate a potential for acoustic modulation of the excitonic structure of nanocrystal assemblies in self-assembled anisotropic semiconductor systems at temperatures at or above 300 K.

36 MATERIALS SCIENCE↗

Accurate quantification of lattice temperature dynamics from ultrafast electron diffraction of single-crystal films using dynamical scattering simulations

In ultrafast electron diffraction (UED) experiments, accurate retrieval of time-resolved structural parameters, such as atomic coordinates and thermal displacement parameters, requires an accurate scattering model. Unfortunately, kinematical models are often inaccurate even for relativistic electron probes, especially for dense, oriented single crystals where strong channeling and multiple scattering effects are present. This article introduces and demonstrates dynamical scattering models tailored for quantitative analysis of UED experiments performed on single-crystal films. As a case study, we examine ultrafast laser heating of single-crystal gold films. Comparison of kinematical and dynamical models reveals the strong effects of dynamical scattering within nm-scale films and their dependence on sample topography and probe kinetic energy. Applying to UED experiments on an 11 nm thick film using 750 keV electron probe pulses, the dynamical models provide a tenfold improvement over a comparable kinematical model in matching the measured UED patterns. Also, the retrieved lattice temperature rise is in very good agreement with predictions based on previously measured optical constants of gold, whereas fitting the Debye–Waller factor retrieves values that are more than three times lower. Altogether, these results show the importance of a dynamical scattering theory for quantitative analysis of UED and demonstrate models that can be practically applied to single-crystal materials and heterostructures.

36 MATERIALS SCIENCE↗

Industrial deposition of wavelength-shifting films for liquid argon photon detection systems

The Deep Underground Neutrino Experiment (DUNE) Phase-II Far Detector is considering an approximately 2000 m 2 photon detection system to achieve a target mean light yield of 180 PE/MeV. Meeting this requirement demands scalable, cost-effective, and high-quality wavelength-shifter (WLS) coatings capable of converting 127 nm liquid-argon scintillation light into visible photons with controlled and reproducible optical performance. We report on the successful realization of an industrial physical vapor deposition (PVD) process forp-terphenyl (pTP) coatings, adapted from vacuum deposition techniques developed for OLED display manufacturing, to produce uniform WLS layers on large-area inorganic substrates, a task traditionally challenged by adhesion and uniformity issues at organic-inorganic interfaces. Surface characterization by profilometry and spectroscopic measurements demonstrates edge-region thickness variation below 10% and emission spectra consistent with high-quality pTP reference samples. The industrial process demonstrates reproducibility, scalability, and significantly reduced production time compared to laboratory-based methods, while maintaining optical characteristics consistent with established pTP reference samples. These results establish a viable pathway for mass production of high-performance pTP coatings for DUNE FD3 and future neutrino experiments, from a coating manufacturing and process standpoint. Detector-level performance validation, including quantitative VUV conversion efficiency measurements at 127 nm, is identified as future work.

47 OTHER INSTRUMENTATION↗

Characterizing electron-collecting CdTe for use in a 77 ns burst-rate imager

The Keck-PAD (pixel array detector) was developed at Cornell as a burst-rate imager capable of recording images from successive electron bunches (153 ns period) from the Advanced Photon Source (APS). Both Si and hole-collecting Schottky CdTe have been successfully bonded to this ASIC (application-specific integrated circuit) and used with this frame rate. The facility upgrades at the APS will lower the bunch period to 77 ns, which will require modifications to the Keck-PAD electronics to image properly at this reduced period. In addition, operation at high X-ray energies will require a different sensor material having a shorter charge collection time. For the target energy of 40 keV for this project, simulations have shown that electron-collecting CdTe should allow >90% charge collection within 35 ns. This collection time will be sufficient to sample the signal from one frame and prepare for the next. 750 µm-thick electron-collecting Schottky CdTe has been obtained from Acrorad and bonded to two different charge-integrating ASICs developed at Cornell, the Keck-PAD and the CU-APS-PAD. Carrier mobility has been investigated using the detector response to single X-ray bunches at the Cornell High Energy Synchrotron Source and to a pulsed optical laser. The tests indicate that the collection time will meet the requirements for 77 ns imaging.

36 MATERIALS SCIENCE↗

Fundamentals of Scalable Nanoparticle Assembly in Engineering Polymres

Systematically improving the properties of polymer nanocomposites is contingent on effectively controlling nanoparticle (NP) dispersion; further, it is necessary to attain this at scale if these methods are to impact practical applications. While most past work has focused on amorphous polymers, ≈ 70% of all polymers sold annually are semicrystalline. Inspired by this apparent disconnect, our work in the current DOE funded grant and this renewal proposal employs a novel handle, polymer crystallization, to organize NPs into the various amorphous zones of the lamellar semicrystalline morphology (interlamellar, interfibrillar and interspherulitic domains) of stereoregular polymers. We hypothesize that the isothermal crystallization rate of a polymer host, G, and NP diffusivity, are the two relevant control parameters in this context. In the case where the NPs are miscible in the melt, they remain spatially well-dispersed when the polymer is crystallized at a rate that is fast relative to NP diffusion. In contrast, monolayer-thick NP sheets with intersheet spacing of ~10-100nm form in slowly crystallized samples. This sheet stacking is remarkably similar to that seen in natural materials, e.g., Nacre. There is also ordering of the NPs at the larger interfibrillar scale. Importantly, the relative fraction of engulfed, interlamellar and interfibrillar NPs is determined by G. Further, the modulus of these materials can increase by a factor of 2-3 due to the organization state of the NPs, while leaving fracture toughness unaffected. We have established the broad applicability of this approach in two polymers, polyethylene (PE) and polyethyleneoxide (PEO). To achieve this goal we developed a method for grafting long PE chains from NPs with controlled graft density and molecular weight, giving us the ability to tailor their dispersion in the PE melt prior to crystallization. In this renewal proposal, we will develop the fundamental, quantitative understanding that will allow us to independently tailor polymer crystallization rate, NP diffusivity and NP agglomeration state in semicrystalline polymers so as to facilely control NP ordering and hence properties. A program that tightly integrates experiment and theory is proposed, and a key outcome of this research will be a three-dimensional design map for different regimes of NP organization (and hence properties) that can be achieved by polymer crystallization. A second independent outcome is the role of directional solidification and how it competes with the rates of polymer crystallization and NP mobility to affect the organization of the NP.

36 MATERIALS SCIENCE↗

Study of helium emissions from active solar regions

A theoretical study is made of the visible and UV line radiation of He I atoms and He II ions from a plane-parallel model flare layer. Codes were developed for the solution of the statistically steady state equation for a 30 level He I - II - III model, and the line and continuum transport equations. These codes are described and documented in the report along with sample solutions. Optical depths and some line intensities are presented for a 1000 km thick layer. Solutions of the steady state equations are presented for electron temperatures 10,000 to 50,000 K and electron densities 10 to the 10th power to 10 to the 14th power/cu cm.

Kulander, J. L.↗

Measurement of subcoat thickness by characteristic x-rays

Technique employs x-ray scanning system to measure thickness of topcoat and subcoat of heat shields and other ceramic materials. System scans sample in raster pattern and depicts image of structure on cathode-ray-tube for viewing or photocopying within seconds.

Harris, W. J.↗

Use of basaltic magmas to characterize processes in planetary interiors: A test case in the southwestern United States

Whether or not basaltic rocks can be used as mantle probes depends upon the degree to which their compositions reflect their source regions rather than their subsequent histories. Mantle heterogeneities in the central Arizona Transition Zone were studied, and the degree to which interaction with the crust has modified the lavas masking these original variations was examined. Basalts from a thick sequence of basaltic flows in the Hickey Formation and two younger flows were sampled in order to provide a time transgressive suite of rocks. These rocks were dated and an extensive set of analytical data is now available for them.

Wittke, J.↗

Analysis of Nonvolatile Residue (NVR) from Spacecraft Systems

Organic contamination on critical spacecraft surfaces can cause electronic problems, serious attenuation of various optical signals, thermal control changes, and adhesion problems. Such contaminants can be detected early by the controlled use of witness mirrors, witness plates, wipe sampling, or direct solvent extraction. Each method requires careful control of variables of technique and materials to attain the ultimate sensitivities inherent to that procedure. Subsequent chemical analysis of the contaminant sample by infrared and mass spectrometry identifies the components, gives semiquantitative estimates of contaminant thickness, indicates possible sources of the nonvolatile residue (NVR), and provides guidance for effective cleanup procedures.

Colony, J. A.↗

Effects of 12-Crown-4 ether on the ionic conductivity and electrode kinetics of electrolytes in polyethylene oxide

Results are described of investigations of the electrical and electrochemical properties of thin films of polyethylene oxide (PEO) electrolytes with and without 12-Crown-4 ether (12Cr4) as a function of temperature and in the frequency regime 100 kHz-0.1 Hz. These measurements were made for LiCF3SO3, LiBF4, and LiClO4 salts. At a given temperature, the bulk conductivity, sigma, (S/cm), for a particular salt, depends on the 12Cr4 concentration with sigma reaching a maximum at about 3 mM 12Cr4. Of the three salts studied, the sigma is the highest for PEO/LiBF4 with 3 mM 12Cr4. The ac and dc measurements yield a lower charge transfer resistance for 12Cr4-incorporated samples than for samples without. Plating/stripping of Li occurs at a potential closer to Li(+)/Li for 12Cr4 samples than those without. The conductivities of a thin (about 100 microns) and a thick (400 microns) films are similar.

Nagasubramanian, G.↗

Study of density distribution in a near-critical simple fluid (19-IML-1)

This experiment uses visual observation, interferometry, and light scattering techniques to observe and analyze the density distribution in SF6 above and below the critical temperature. Below the critical temperature, the fluid system is split up into two coexisting phases, liquid and vapor. The spatial separation of these phases on earth, liquid below and vapor above, is not an intrinsic property of the fluid system; it is merely an effect of the action of the gravity field. At a fixed temperature, the density of each of the coexisting phases is in principle fixed. However, near T sub c where the fluid is strongly compressible, gravity induced hydrostatic forces will result in a gradual decrease in density with increasing height in the sample container. This hydrostatic density profile is even more pronounced in the one phase fluid at temperatures slightly above T sub c. The experiment is set up to study the intrinsic density distributions and equilibration rates of a critical sample in a small container. Interferometry will be used to determine local density and thickness of surface and interface layers. The light scattering data will reveal the size of the density fluctuations on a microscopic scale.

Michels, Teun↗

The diatom record from beneath the West Antarctic Ice Sheet and the global proxy perspective

Recent glaciological evaluation and modeling of the marine-based West Antarctic Ice Sheet (WAIS) support the possibility that the WAIS disintegrated during one or more Pleistocene interglacial period(s). The magnitude of sea level and oxygen isotope variation during certain late-Pleistocene interglacial periods is also consistent with the possibility of major retreat of the WAIS. Although oxygen isotopes from deep-sea sediments provide the best available proxy record for global ice volume (despite the ambiguities in the record), the source of ice volume changes must be hypothesized. Based on the intensity of interglacial isotopic shifts recorded in Southern Ocean marine sedimentary records, stage 11 (400,000 years ago) is the strongest candidate for WAIS collapse, but the records for stages 9, 7, and 5.5 are all consistent with the possibility of multiple late-Pleistocene collapses. Seismic reflection studies through the WAIS have revealed thick successions of strata with seismic characteristics comparable to upper Tertiary marine sediments. Small samples of glacial diamictons from beneath the ice sheet have been collected via hot-water drilled access holes. These sediments include mixed diatom assemblages of varying ages. Late-Miocene diatoms dominate many samples, probably reflecting marine deposition in West Antarctic basins prior to development of a dominantly glacial phase in West Antarctica. In addition to late-Miocene diatoms, samples from Upstream B (1988/89) contain rare post-Miocene diatoms, many of which imply deposition in the West Antarctic interior during one or more Pleistocene deglaciation periods. Age-diagnostic fossils in glacial sediments beneath ice sheets provide relatively coarse chronostratigraphic control, but they do contain direct evidence of regional deglaciation. Thus, sub-glacial till samples provide the evidence regarding the source of ice sheet variability seen in well-dated proxy records. Combined, these independent data sets can provide a more comprehensive and less speculative interpretation of the history of past glacial minima in currently glaciated polar regions.

Scherer, Reed P.↗

Laboratory Simulations: The Primordial Comet Mantle

Laboratory data are needed to understand the formation of organics in cometary and precometary materials and for deciding on the fate of the volatiles. Appropriate experiments were described in the talk at Milipitas. Because of its importance for the comet sample return mission, I discuss here the relevance of this data for predicting the thickness, nature, and ability to survive of the cosmic-ray produced primordial comet mantle ('crust'). That part of the mantle which becomes predominantly refractory is approx. 30 gm/sq cm thick. The tensile strength of this outer mantle is such that it might survive the comet's entrance into the inner solar system. In addition, important modifications to the ices occur to depths approx. 300 gm/cu cm. Based on this it is expected that a deep probe is needed to obtain minimally altered material.

Johnson, R. E.↗

The Oxidation Rate of SiC in High Pressure Water Vapor Environments

CVD SiC and sintered alpha-SiC samples were exposed at 1316 C in a high pressure burner rig at total pressures of 5.7, 15, and 25 atm for times up to 100h. Variations in sample emittance for the first nine hours of exposure were used to determine the thickness of the silica scale as a function of time. After accounting for volatility of silica in water vapor, the parabolic rate constants for Sic in water vapor pressures of 0.7, 1.8 and 3.1 atm were determined. The dependence of the parabolic rate constant on the water vapor pressure yielded a power law exponent of one. Silica growth on Sic is therefore limited by transport of molecular water vapor through the silica scale.

Opila, Elizabeth J.↗

Transparent, Conductive Coatings Developed for Arc-Proof Solar Arrays

Transparent, conductive thin-film coatings have many potential applications where a surface must be able to dissipate electrical charges without sacrificing its optical properties. Such applications include automotive and aircraft windows, heat mirrors, optoelectronic devices, gas sensors, and solar cell array surfaces for space applications. Many spacecraft missions require that solar cell array surfaces dissipate charges in order to avoid damage such as electronic upsets, formation of pinholes in the protective coatings on solar array blankets, and contamination due to deposition of sputtered products. In tests at the NASA Lewis Research Center, mixed thin-films of sputter-deposited indium tin oxide (ITO) and magnesium fluoride (MgF2) that could be tailored to the desired sheet resistivity, showed transmittance values of greater than 90 percent. The samples evaluated were composed of mixed, thin-film ITO/MgF2 coatings, with a nominal thickness of 650 angstroms, deposited onto glass substrates. Preliminary results indicated that these coatings were durable to vacuum ultraviolet radiation and atomic oxygen. These coatings show promise for use on solar array surfaces in polar low-Earth-orbit environments, where a sheet resistivity of less than 10(exp 8)/square is required, and in geosynchronous orbit environments, where a resistivity of less than 10(exp 9)/square is required.

Source record↗

Light Microscopy Module: An On-Orbit Microscope Planned for the Fluids and Combustion Facility on the International Space Station

The Light Microscopy Module (LMM) is planned as a fully remotely controllable on-orbit microscope subrack facility, allowing flexible scheduling and control of fluids and biology experiments within NASA Glenn Research Center's Fluids and Combustion Facility on the International Space Station. Within the Fluids and Combustion Facility, four fluids physics experiments will utilize an instrument built around a light microscope. These experiments are the Constrained Vapor Bubble experiment (Peter C. Wayner of Rensselaer Polytechnic Institute), the Physics of Hard Spheres Experiment-2 (Paul M. Chaikin of Princeton University), the Physics of Colloids in Space-2 experiment (David A. Weitz of Harvard University), and the Low Volume Fraction Colloidal Assembly experiment (Arjun G. Yodh of the University of Pennsylvania). The first experiment investigates heat conductance in microgravity as a function of liquid volume and heat flow rate to determine, in detail, the transport process characteristics in a curved liquid film. The other three experiments investigate various complementary aspects of the nucleation, growth, structure, and properties of colloidal crystals in microgravity and the effects of micromanipulation upon their properties. Key diagnostic capabilities for meeting the science requirements of the four experiments include video microscopy to observe sample features including basic structures and dynamics, interferometry to measure vapor bubble thin film thickness, laser tweezers for colloidal particle manipulation and patterning, confocal microscopy to provide enhanced three-dimensional visualization of colloidal structures, and spectrophotometry to measure colloidal crystal photonic properties.

Doherty, Michael P.↗