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At least 505 records · Page 28

Combined Falling Drop/Open Port Sampling Interface System for Automated Flow Injection Mass Spectrometry

The aim of this work was to demonstrate and to evaluate the analytical performance of a combined falling drop/open port sampling interface (OPSI) system as a simple noncontact, no-carryover, automated system for flow injection analysis with mass spectrometry. The falling sample drops were introduced into the OPSI using a widely available autosampler platform utilizing low cost disposable pipet tips and conventional disposable microtiter well plates. The volume of the drops that fell onto the OPSI was in the 7–15 μL range with an injected sample volume of several hundred nanoliters. Sample drop height, positioning of the internal capillary on the sampling end of the probe, and carrier solvent flow rate were optimized for maximum signal. Sample throughput, signal reproducibility, matrix effects, and quantitative analysis capability of the system were established using the drug molecule propranolol and its isotope labeled internal standard in water, unprocessed river water and two commercially available buffer matrices. A sample-to-sample throughput of ~45 s with a ~4.5 s base-to-base flow injection peak profile was obtained in these experiments. In addition, quantitation with minimally processed rat plasma samples was demonstrated with three different statin drugs (atorvastatin, rosuvastatin, and fluvastatin). Direct characterization capability of unprocessed samples was demonstrated by the analysis of neat vegetable oils. Employing the autosampler system for spatially resolved liquid extraction surface sampling exemplified by the analysis of propranolol and its hydroxypropranolol glucuronide phase II metabolites from a rat thin tissue section was also illustrated.

47 OTHER INSTRUMENTATION↗

Off-Equilibrium Reactivity of Boron-Enriched Metal Diboride Surfaces in Electroreduction Conditions

Boron-based materials, featuring B-dependent reactivity and diverse phases, are emerging as promising catalyst systems. However, the catalytic mechanism on many borides remains poorly understood due to complex surface reconstructions under reaction conditions. Here, we investigate the MoB 2 surface in conditions of hydrogen evolution reaction in acidic media, using grand canonical global optimization, grand canonical density functional theory, ab initio molecular dynamics, free energy surface sampling, and an analytical model for electrochemical barrier evaluation. We propose a boron-enrichment strategy to tune the surface reactivity of the hexagonal face of MoB 2 . We reveal the dynamic nature of the B-enriched surface under H coverage and kinetic trapping of the system in the metastable regime with an extensive examination of the deactivation pathways. The metastable center B site on B-enriched surfaces, featuring buckled-up configuration and a usual relaxation effect, is found to be highly active toward HER via the Volmer–Heyrovsky mechanism. In conclusion, this work demonstrates how off-equilibrium behaviors can arise from the interplay between adsorbate coverage and surface reconstruction on a seemingly simple surface, and we present a theoretical framework and computational workflows to address these behaviors, along with other realistic complexities, in kinetics simulations.

Adsorption↗

Instrument for spatially resolved, temperature-dependent electrochemical impedance spectroscopy of thin films under locally controlled atmosphere

We demonstrate an instrument for spatially resolved measurements (mapping) of electrochemical impedance under various temperatures and gas environments. Automated measurements are controlled by a custom LabVIEW program, which manages probe motion, sample motion, temperature ramps, and potentiostat functions. Sample and probe positioning is provided by stepper motors. Dry or hydrated atmospheres (air or nitrogen) are available. The configurable heater reaches temperatures up to 500 °C, although the temperature at the sample surface is moderated by the gas flow rate. The local gas environment is controlled by directing flow toward the sample via a glass enclosure that surrounds the gold wire probe. Software and hardware selection and design are discussed. Reproducibility and accuracy are quantified on a Ba(Zr,Y)O 3-δ proton-conducting electrolyte thin film synthesized by pulsed laser deposition. The mapping feature of the instrument is demonstrated on a compositionally graded array of electrocatalytically active Ba(Co,Fe,Zr,Y)O 3-δ thin film microelectrodes. The resulting data indicate that this method proficiently maps property trends in these materials, thus demonstrating the reliability and usefulness of this method for investigating electrochemically active thin films.

47 OTHER INSTRUMENTATION↗

X-ray quantification of oxygen groups on diamond surfaces for quantum applications

Abstract Identifying the surface chemistry of diamond materials is increasingly important for device applications, especially quantum sensors. Oxygen-related termination species are widely used because they are naturally abundant, chemically stable, and compatible with stable nitrogen vacancy centres near the diamond surface. Diamond surfaces host a mixture of oxygen-related species, and the precise chemistry and relative coverage of different species can lead to dramatically different electronic properties, with direct consequences for near-surface quantum sensors. However, it is challenging to unambiguously identify the different groups or quantify the relative surface coverage. Here we show that a combination of x-ray absorption and photoelectron spectroscopies can be used to quantitatively identify the coverage of carbonyl functional groups on the { 100 } diamond surface. Using this method we reveal an unexpectedly high fraction of carbonyl groups ( > 9%) on a wide range of sample surfaces. Furthermore, through a combination of ab initio calculations and spectroscopic studies of engineered surfaces, we reveal unexpected complexities in the x-ray spectroscopy of oxygen terminated diamond surfaces. Of particular note, we find the binding energies of carbonyl-related groups on diamond differs significantly from other organic systems, likely resulting in previous misestimation of carbonyl fractions on diamond surfaces.

36 MATERIALS SCIENCE↗

Measurement of Dielectric Multipactor Thresholds at 110 GHz

We report experimental measurements of the threshold for multipactor discharges on dielectric surfaces at 110 GHz. Multipactor was studied in two geometries: electric field polarized parallel to or perpendicular to the sample surface. Measured multipactor thresholds ranged from 15 to 34 MV /m, more than 10 times higher than those found at conventional microwave frequencies. Measured thresholds were compared with prior data at lower frequencies, showing agreement with theoretical predictions that thresholds increase linearly with frequency. Measurements of the rf power dissipated in the multipactor show low dissipation (≤ 1%) for the parallel electric field case, but very strong dissipation for the perpendicular case, also in agreement with theoretical predictions. In conclusion, the agreement between experiment and theory over a wide range of frequencies provides a strong basis for the understanding of dielectric multipactor discharges.

43 PARTICLE ACCELERATORS↗

Flexural strength of a conventionally processed and additively manufactured debased 94% alumina

Mechanical strength of a 94 wt% debased alumina was measured using ASTM-C1161 specimens fabricated via conventional and lithography-based ceramic manufacturing (LCM) methods. The effects of build orientation and a 1500°C wet hydrogen fire added to the LCM firing sequence on strength were evaluated. Additionally, a Weibull fit to the conventional flexural specimen data yielded 20 and 356 MPa for the modulus and characteristic strength, respectively. Weibull fits of the data from the LCM specimens yielded moduli between 7.5 and 11.3 and characteristics strengths between 333 and 339 MPa. A Weibull fit to data from LCM specimens subjected to the wet hydrogen fire yielded 14.2 and 376 MPa for the modulus and characteristic strength, respectively. The 95% confidence intervals for all Weibull parameters are reported. Average Archimedes bulk densities of LCM and conventional specimens were 3.732 and 3.730 g/cm 3 , respectively. Process dependent differences in surface morphology were observed in scanning electron microscope (SEM) images of specimen surfaces. SEM images of LCM specimen cross-sections showed alumina grain texture dependent on build direction, but no evidence of porosity concentrated in planes between printed layers. Fracture surfaces of LCM and conventionally processed specimens revealed hackle lines and mirror regions indicative of fracture initiation at the sample surface rather than the interior.

36 MATERIALS SCIENCE↗

Atmospheric-pressure Molecular Imaging of Biological Tissues and Biofilms by LAESI Mass Spectrometry

Ambient ionization methods in mass spectrometry allow analytical investigations to be performed directly on a tissue or biofilm under nativelike experimental conditions. Laser ablation electrospray ionization (LAESI) is one such development and is particularly well-suited for the investigation of water-containing specimens. LAESI utilizes a mid-infrared laser beam (2.94 μm wavelength) to excite the water molecules of the sample. When the ablation fluence threshold is exceeded, the sample material is expelled in the form of particulate matter and these projectiles travel to tens of millimeters above the sample surface. In LAESI, this ablation plume is intercepted by highly charged droplets to capture a fraction of the ejected sample material and convert its chemical constituents into gas-phase ions. A mass spectrometer equipped with an atmospheric-pressure ion source interface is employed to analyze and record the composition of the released ions originating from the probed area (pixel) of the sample. A systematic interrogation over an array of pixels opens a way for molecular imaging in the microprobe analysis mode. A unique aspect of LAESI mass spectrometric imaging is depth profiling that, in combination with lateral imaging, enables threedimensional (3D) molecular imaging. With current lateral and depth resolutions of ~100 μm and ~40 μm, respectively, LAESI mass spectrometric imaging helps to explore the molecular structure of biological tissues. Herein, we review the major elements of a LAESI system and provide guidelines for a successful imaging experiment.

59 BASIC BIOLOGICAL SCIENCES↗

The chemical activities of the Viking biology experiments and the arguments for the presence of superoxides, peroxides, gamma-Fe2O3 and carbon suboxide polymer in the Martian soil

The evolution of N2, Ar, O2, and CO2 from Martian soil as a function of humidity in the Gas Exchange Experiment are correlated with the mean level of water vapor in the Martian atmosphere. All but O2 are associated with desorption. The evolution of oxygen is consistent with the presence of alkaline earth and alkali metal superoxides; and their peroxides and the gamma-Fe2O3 in the soil can account for the generation of radioactive gas in the Labeled Release Experiment. The slower evolution of CO2 from both the Gas Exchange Experiment and the Labeled Release Experiment are associated with the direct oxidation of organics by gamma-Fe2O3. The Pyrolytic Release Experiment's second peak may be carbon suboxide as demonstrated by laboratory experiments. A necessary condition is that the polymer exists in the Martian soil. We ascribe the activity of the surface samples to the reaction of Martian particulates with an anhydrous CO2 atmosphere activated by uv and ionizing radiations. The surface particles are ultimately altered by exposure to small but significant amounts of water at the sites. From the working model, we have predicted the peculiar nature of the chemical entities and demonstrated that the model is justified by laboratory data. The final confirmation of this model will entail a return to Mars, but the nature and implications of this chemistry for the Martian surface is predicted to reveal even more about Mars with further simulations in the laboratory.

long duration↗

Comparative geochemistry of Apollo 16 surface soils and samples from cores 64002 and 60002 through 60007

New data are presented for the concentrations of 23 to 27 elements in nine Apollo 16 surface soil samples, two subsplits each of 12 splits of core 60002-7, and one subsplit each of 10 splits of drive tube 64002. The surface soils are generally similar to other surface soils collected at their respective stations. All ten 64002 samples are similar to each other and to the station 4 surface soils and distinctly different from soils at other stations. High iron concentrations previously reported for these same subsplits of 60002-7 result primarily from meteoritic metal. One sample from each core is contaminated by stainless steel. The recently proposed ferroan anorthositic norites are required to explain the soil compositions. A yet uncharacterized component with high concentrations of Na, Sr, and Eu is also needed.

Korotev, R. L.↗

The Petrology and Geochemistry of Feldspathic Granulitic Breccia NWA 3163: Implications for the Lunar Crust

Lunar meteorites are crucial to understand the Moon s geological history because, being samples of the lunar crust that have been ejected by random impact events, they potentially originate from areas outside the small regions of the lunar surface sampled by the Apollo and Luna missions. The Apollo and Luna sample sites are contained within the Procellarum KREEP Terrain (PKT, Jolliff et al., 2000), where KREEP refers to potassium, rare earth element, and phosphorus-rich lithologies. The KREEP-rich rocks in the PKT are thought to be derived from late-stage residual liquids after approx.95-99% crystallization of a lunar magma ocean (LMO). These are understood to represent late-stage liquids which were enriched in incompatible trace elements (ITE) relative to older rocks (Snyder et al., 1992). As a consequence, the PKT is a significant reservoir for Th and KREEP. However, the majority of the lunar surface is likely to be significantly more depleted in ITE (84%, Jolliff et al., 2000). Lunar meteorites that are low in KREEP and Th may thus sample regions distinct from the PKT and are therefore a valuable source of information regarding the composition of KREEP-poor lunar crust. Northwest Africa (NWA) 3163 is a thermally metamorphosed ferroan, feldspathic, granulitic breccia composed of igneous clasts with a bulk anorthositic, noritic bulk composition. It is relatively mafic (approx.5.8 wt.% FeO; approx.5 wt.% MgO) and has some of the lowest concentrations of ITEs (17ppm Ba) compared to the feldspathic lunar meteorite (FLM) and Apollo sample suites (Hudgins et al., 2011). Localized plagioclase melting and incipient melting of mafic minerals require localized peak shock pressures in excess of 45 GPa (Chen and El Goresy, 2000; Hiesinger and Head, 2006). NWA 3163, and paired samples NWA 4481 and 4883, have previously been interpreted to represent an annealed micro-breccia which was produced by burial metamorphism at depth in the ancient lunar crust (Fernandes et al., 2009). This is in contrast to the interpretation of Hudgins et al. (2009) where NWA 3163 was interpreted to have formed through contact metamorphism. To further constrain its origin, we examine the petrogenesis of NWA 3163 with a particular emphasis on in-situ measurement of trace elements within constituent minerals, Sm-Nd and Rb-Sr isotopic systematics on separated mineral fractions and petrogenetic modeling.

McLeod, C. L.↗

Radioactivites in returned lunar materials and in meteorites

The cosmic-ray, solar-flare, and solar-wind bombardments of lunar rocks and soils and meteorites were studied by measurements of tritium, carbon-14 and argon radioactivity. The radioactivity integrates the bombardment for a time period equal to several half-lines. H-3, Ar-37, Ar-39, C-14. For the interior samples of lunar rocks and for deep lunar soil samples, the amounts of the radioactivities were equal to those calculated for galactic cosmic-ray interactions. The top near-surface samples of lunar rocks and the shallow lunar soil samples show excess amounts of the radioactivities attributable to solar flares. Lunar soil fines contain a large amount of hydrogen due to implanted solar wind. Studies of the H-3 in lunar soils and in recovered Surveyor-3 materials gave an upper limit for the H-3/H ratio in the solar wind of 10 to the -11th power. Solar wind carbon is also implanted on lunar soil fines. Lunar soils collected on the surface contained a 0.14 component attributable to implanted solar wind C-14. The C-14/H ratio attributed to the solar wind from this C-14 excess is approximately 4 x 10 to the -11th power.

Fireman, E. L.↗

Control of the positional relationship between a sample collection instrument and a surface to be analyzed during a sampling procedure using a laser sensor

A system and method utilizes distance-measuring equipment including a laser sensor for controlling the collection instrument-to-surface distance during a sample collection process for use, for example, with mass spectrometric detection. The laser sensor is arranged in a fixed positional relationship with the collection instrument, and a signal is generated by way of the laser sensor which corresponds to the actual distance between the laser sensor and the surface. The actual distance between the laser sensor and the surface is compared to a target distance between the laser sensor and the surface when the collection instrument is arranged at a desired distance from the surface for sample collecting purposes, and adjustments are made, if necessary, so that the actual distance approaches the target distance.

47 OTHER INSTRUMENTATION↗

Combined Experimental and Modeling Study of the Interactions of Acid Gas with Common Spacecraft Surfaces for Fire Safety Applications

A fire in a spacecraft poses detrimental consequences and risks mission success in addition to crew safety. This is compounded during long-duration missions when the crew has limited options to recover from a fire. A common spacecraft fire concern is the smoldering of wire insulation, typically made from Polyvinyl chloride (PVC) or Polytetrafluoroethylene (PTFE). This creates acid gases such as Hydrogen Chloride (HCl), Hydrogen Fluoride (HF) and Hydrogen Cyanide (HCN). These poisonous gases are hazardous to the crew. They also interact with common surfaces within the spacecraft more than dominant combustion products such as CO2 and H2O. This makes them more difficult to track for potential fire detection techniques, or for postfire clean-up. It is imperative to be able to understand and predict the fate of these poisonous species in a microgravity environment in order to design a safe vehicle. HCl interacts with a number of materials inside a spacecraft. Primary among these materials is aluminum, which is abundantly used due to its strong and light weight nature. Aluminum has a natural oxide layer that protects it from corrosion but is typically treated to enhance this oxide layer. Among these treatments is a chromate conversion coating (CCC), which provides a thin enough protective oxide layer to still conduct electricity, and a traditional anodized material that has a thicker oxide layer that does not conduct electricity. Nomex is another common material found inside a spacecraft. It is a flame-resistant woven polymer that is related to nylon. This commercially available material is used for cargo storage bags and as a fire barrier. Physics-based models were developed to predict the uptake of HCl by these materials. The ultimate objective of these models is to predict the fate of HCl within the spacecraft so that sensors can be placed in meaningful locations in future missions based on the model predictions. To support these modeling efforts, experiments were performed in a cast acrylic test cell that measured the difference between the inlet and outlet concentration of HCl after inserting a sample rod of the test material. Different uptake capacities were realized for each type of sample tested. A computational fluid dynamics model (CFD) model of the reactor was then constructed that used a one-step global reaction rate with calibratable reaction (or kinetic) constants. These constants were calibrated to match the HCl uptake on the CCC aluminum samples, and the same kinetic constants were then tested for the stock and anodized aluminum samples. Model predictions matched the experimental data for the stock aluminum, and to a much lesser extent, the anodized aluminum. The model was additionally validated at different flow rates, sample surface areas, and inlet concentrations, and showed good agreement for all stock and CCC samples. The model did not accurately predict the HCl uptake in the anodized samples compared to the other two types of aluminum. Adjusting the kinetic constants and transport properties did little to improve the prediction. X-Ray Photoelectron Spectroscopy (XPS) was used to determine that the oxide layer thickness of anodized aluminum is approximately 5,000 nm, compared to 250 nm for CCC and 50 nm for stock. XPS also revealed presence of chlorine further down in the aluminum oxide layer in anodized samples than CCC and stock samples after the samples were saturated with HCl, indicating that accounting for diffusion of HCl into the oxide layer is important for accurate prediction of HCl uptake onto anodized aluminum. Consequently, a multi-scale model was developed and tested. First, a single pore inside the anodized aluminum oxide layer was modeled and is referred to as the pore-scale model. In this model, HCl diffused through the pore and reacted with the aluminum oxide pore wall to create aluminum chloride. The sample was then saturated when the mass transfer resistance through the growing aluminum chloride layer became too large for the HCl to reach the aluminum oxide wall and continue the reaction. This pore-scale model was coupled to the reactor-scale model using a concentration-dependent diffusion coefficient, resulting in much more accurate predictions (approximately half the sum square error of the aforementioned reactor-scale model that produced good agreement for stock and CCC) for a variety of operating conditions. The amount of water vapor or relative humidity (RH) in the flow during a reactor experiment was determined to influence HCl uptake. Experiments were performed to understand the interaction of gaseous HCl with aluminum surfaces in the presence of water vapor. The results show that increasing levels of RH increased the capacity of aluminum to adsorb HCl but decreased the capacity of Nomex to uptake HCl. A series of tests were performed on individual aluminum samples after they had been saturated with a fixed concentration of HCl in dry air conditions with the goal of determining how their HCl uptake capacity changes after various treatments with water relative to the original saturation tests. HCl-saturated aluminum samples subjected to a second dry air flow at the same HCl concentration as the original test had an uptake of 23.5% of the original sample with no treatment in between. Saturated aluminum samples subjected to an air flow with a RH of 90% in between tests had an uptake of 35.6% of the original. Saturated aluminum samples submerged in distilled water for 12 hours in between tests had an uptake of 82.2% of the original sample. Previously saturated aluminum tested with HCl and a 50% RH air flow resulted in similar uptake characteristics in multiple repeated tests. The experiments show the profound effect water vapor has on HCl uptake onto aluminum surfaces. In the samples subjected to water vapor or liquid water, capillary condensation and capillary diffusion alters the transport of HCl significantly. A model was proposed that developed a relationship between RH and the coefficient of HCl diffusion in aluminum chloride. This produced an “S-shaped” curve with diffusion coefficient as a function of RH, with 45% RH represented as the point where the diffusion coefficient is halfway between no water saturation and 100% water saturation in the aluminum chloride product layer. No difference in uptake characteristics for the experiment or model were realized between 50% and 62% RH. The results from the large-scale microgravity experiment, Saffire, are discussed as they pertain to the fate of HCl throughout a spacecraft. HCl was released, both as a standalone event, and in concurrence with the burning of a structured cloth. These events only produced a small response in the far field HCl sensor, while a PMMA burn that did not produce HCl had a significantly greater response. A ground-based large-scale facility was constructed to flow acid gas at the scale and configuration realized in the Saffire experiments. A CFD model of this duct was constructed to test kinetic parameters developed in this work at a larger scale and different geometric configuration and to predict the results of the large-scale facility. The models developed in this work were used to interpret the results of the microgravity tests and lead the discussion on what further experiments and models are needed in order to predict the fate of acid gas in a spacecraft environment. To summarize, the major contributions of this work are as follows: the capacity to uptake HCl, with and without the presence of water vapor, was measured for a variety of real spacecraft surfaces. Several different models (single reactor-scale, multiscale, spacecraft-scale) were developed and with the aid of modeling, the rate of uptake for those surfaces was also predicted and validated. The kinetic parameters determined from the small-scale reactor experiments and models were used to predict large-scale and microgravity tests. Conclusions from this research will be used in the design of spacecraft vehicles and large-scale microgravity fire safety experiments. The models built by this work will aid designers in sensor placement and could be used to predict acid gas transport from fires in partial gravity, as would be seen in Lunar and Martian habitats.

fire safety↗

Techniques for Down-Sampling a Measured Surface Height Map for Model Validation

This software allows one to down-sample a measured surface map for model validation, not only without introducing any re-sampling errors, but also eliminating the existing measurement noise and measurement errors. The software tool of the current two new techniques can be used in all optical model validation processes involving large space optical surfaces

Sidick, Erkin↗

Constant-Distance Mode Nanospray Desorption Electrospray Ionization Mass Spectrometry Imaging of Biological Samples with Complex Topography

A new approach for constant distance mode mass spectrometry imaging of biological samples using nanospray desorption electrospray ionization (nano-DESI MSI) was developed by integrating a shear-force probe with nano-DESI probe. The technical concept and basic instrumental setup as well as general operation of the system are described. Mechanical dampening of resonant oscillations due to the presence of shear forces between the probe and the sample surface enables constant-distance imaging mode via a computer controlled closed feedback loop. The capability of simultaneous chemical and topographic imaging of complex biological samples is demonstrated using living Bacillus Subtilis ATCC 49760 colonies on agar plates. The constant-distance mode nano-DESI MSI enabled imaging of many metabolites including non-ribosomal peptides (surfactin, plipastatin and iturin) and iron-bound heme on the surface of living bacterial colonies ranging in diameter from 10 mm to 13 mm with height variations of up to 0.8 mm above the agar plate. Co-registration of ion images to topographic images provided higher-contrast images. Constant-mode nano-DESI MSI is ideally suited for imaging biological samples of complex topography in their native state.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterizing physical, chemical, and magnetic properties at the nanoscale

Synchrotron light sources are extremely useful for the characterization of materials in many different research fields (including physics, chemistry, materials science, biology, medicine, geology, and cultural heritage). The evolution of technology, however, currently points toward the miniaturization of devices and molecular motors, as well as the creation (through atomic manipulation) of new materials. This brings an acute necessity for direct chemical imaging of materials, i.e., with the use of x-ray microscopy at the nanometer and atomic length scales.1, 2 Although a variety of new x-ray nanoprobes and x-ray microscopy techniques have been developed in recent years, the spatial resolution of direct chemical or magnetic contrast imaging techniques remains on the order of several nanometers. Invented in the 1980s, scanning tunneling microscopy (STM) allows a large range of materials to be viewed at the atomic level.3 STM also offers a finer degree of spatial resolution than almost any other image technique, but it is chemically ‘blind’ and thus cannot be used alone to directly identify chemical elements on a surface. For many years, researchers have attempted to solve this problem by combining STM with synchrotron x-ray excitations,4–7 and a new technique—known as synchrotron xray scanning tunneling microscopy (SX-STM)—has emerged. In this technique—which combines the chemical sensitivity of xrays with the high spatial resolution of STM—a monochromatic x-ray beam is used to illuminate a tip-sample junction, while the tip makes raster scans across the sample surface. A feedback system maintains a tip–sample separation that is typically less than 1nm. The goal is tomodulate the tunneling current through x-ray excitation and therewith obtain electronic and chemical contrast. It is difficult, however, to achieve real chemical contrast because of three serious issues. First, electrons excited by x-rays do not just tunnel into the tip, but can also be ejected from the sample and hit the sidewalls of the tip detector (which degrades the spatial resolution). Second, because photoejected electrons still provide a deceptive current signal in the far field, the STM feedback system can lift the tip out of the tunneling regime without being noticed. Last, themeasured tip current is always a convolution of the conventional tunnel current (which is related to the sample topography) and the x-ray-excited electrons (which carry the material’s chemical information).

36 MATERIALS SCIENCE↗

Chemical stability of highly (0001) textured Sm(CoCu){sub 5} thin films with a thin Ta capping layer

With the highest magnetocrystalline anisotropy constant (Ku) among practical magnetic materials, SmCo{sub 5} could be a very attractive candidate for future high areal density magnetic recording. However, its corrosion resistance is always a concern in recording media applications. In this paper, the chemical stability and microstructures of highly (0001) textured Sm(CoCu){sub 5} thin films with and without a 3 nm Ta capping layer were reported. For Sm(CoCu){sub 5} thin films without a capping layer, the coercivity decreases significantly (from 8kOe to 1kOe) within one month. Sm(CoCu){sub 5} thin films capped with a thin Ta layer (3 nm) behave differently. Even exposed to a laboratory environment (25 deg. C) over 3 years, the Ta-capped Sm(CoCu){sub 5} thin films are stable in terms of structural and magnetic properties, i.e., there were no changes in X-ray diffraction peaks and vibrating sample magnetometer hysteresis loops. Microstructure of Ta-capped Sm(CoCu){sub 5} thin films showed that Sm(CoCu){sub 5} formed a domelike particle assembly structure on a smooth Ru underlayer and were well covered by partially oxidized Ta capping layer, as shown by TEM cross-section micrographs. Accelerated corrosion treatment (130 deg. C, 95% relative humidity, 6 h) was performed on Ta-capped Sm(CoCu){sub 5} thin films. X-ray photoelectron spectroscopy (XPS) results showed that no Co was detected on the sample surface before the corrosion treatment, but strong XPS signals of CoOx and Co(OH)x were observed after treatment. Therefore, none of our Sm(CoCu){sub 5} thin films can pass the accelerated corrosion test. Hcp-phased CoPt-alloys are proposed as better capping materials for Sm(CoCu){sub 5} thin films in future high-density magnetic recording applications.

36 MATERIALS SCIENCE↗

ARTIFACT FORMATION DURING NEUTRALIZATION OF TANK 50 SAMPLES

Degradation products have been identified in the extracts of Tank 50 samples analyzed by semivolatile organic compound analysis (SVOA) using gas chromatography/mass spectrometry (GC/MS). These materials, identified as short chain alkyl alcohols, were formed by acidification during sample preparation. A number of questions were raised about the formation of these and other materials reported in Tank 50 surface samples, and this report serves to address these questions.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗