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At least 865 records · Page 48

Soil Analysis Micro-Mission Concepts Derived from the MSP 2001 Mars Environmental Compatibility Assessment (MECA)

The Mars Environmental Compatibility Assessment (MECA) will evaluate the Martian environment for soil and dust-related hazards to human exploration as part of the Mars Surveyor Program 2001 Lander. The integrated MECA payload contains a wet-chemistry laboratory, a microscopy station, an electrometer to characterize the electrostatic environment, and arrays of material patches to study abrasion and adhesion. Heritage will be all-important for low cost micro-missions, and adaptations of instruments developed for the Pathfinder, '98 and '01 Landers should be strong contenders for '03 flights. This talk has three objectives: (1) Familiarize the audience with MECA instrument capabilities; (2) present concepts for stand-alone and/or mobile versions of MECA instruments; and (3) broaden the context of the MECA instruments from human exploration to a comprehensive scientific survey of Mars. Due to time limitations, emphasis will be on the chemistry and microscopy experiments. Ion-selective electrodes and related sensors in MECA's wet-chemistry laboratory will evaluate total dissolved solids, redox potential, pH, and the concentration of many soluble ions and gases in wet Martian soil. These electrodes can detect potentially dangerous heavy-metal ions, emitted pathogenic gases, and the soil's corrosive potential, and experiments will include cyclic voltammetry and anodic stripping. For experiments beyond 2001, enhancements could allow multiple use of the cells (for mobile experiments) and reagent addition (for quantitative mineralogical and exobiological analysis). MECA's microscopy station combines optical and atomic-force microscopy (AFM) in an actively focused, controlled illumination environment to image particles from millimeters to nanometers in size. Careful selection of substrates allows controlled experiments in adhesion, abrasion, hardness, aggregation, magnetic and other properties. Special tools allow primitive manipulation (brushing and scraping) of samples. Soil particle properties including size, shape, color, hardness, adhesive potential (electrostatic and magnetic), will be determined using an array of sample receptacles and collection substrates. The simple, rugged atomic-force microscope will image in the submicron size range and has the capability of performing a particle-by-particle analysis of the dust and soil. Future implementations might enhance the optical microscopy with spectroscopy, or incorporate advanced AFM techniques for thermogravimetric and chemical analysis.

Hecht, M. H.↗

A covalent modification for graphene by adamantane groups through two-step chlorination-Grignard reactions

Chemical modification of graphene is a promising approach to manipulate its properties for its end applications. Herein we designed a two-step route through chlorination-Grignard reactions to covalently decorate the surface of graphene with adamantane groups. The chemically modified graphene was characterized by Raman spectroscopy, atomic force microscopy, and X-ray photoelectron spectroscopy. Chlorination of graphene occurred rapidly, and the substitution of chlorine atoms on chlorinated graphene by adamantane Grignard reagent afforded adamantane graphene in almost quantitative yield. Adamantane groups were found to be covalently bonded to the graphene carbons. The present two-step procedure may provide an effective and facile route for graphene modification with varieties of organic functional groups. - Graphical abstract: Adamantane groups covalently functionalized graphene is obtained by direct substitution of chlorinated graphene with bromoadamantane Grignard reagent.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Riley oxidation: A forgotten name reaction for synthesis of selenium nanoparticles

A simple wet chemical method, involving reaction of acetone with selenium dioxide, has been developed, to synthesize polyvinyl alcohol-stabilized selenium nanoparticles. The method is capable of producing nanoparticles in the size range of about 100-300 nm, under ambient conditions. The synthesized nanoparticles can be separated easily from the aqueous sols by a high-speed centrifuge, and can be re-dispersed in aqueous medium by a sonicator. The effect of concentrations of selenium dioxide, acetone and PVA on the size of the selenium nanoparticles has been studied. The size of the selenium nanoparticles has been found to increase with increase in the reaction time as well as the concentration of selenium dioxide, while it decreases with increase in the concentration of the stabilizer, PVA. The synthesized selenium nanoparticles have been characterized by UV-visible optical absorption spectroscopy, X-ray diffraction, energy dispersive X-ray analysis, differential scanning calorimetry, atomic force microscopy, scanning electron microscopy and transmission electron microscopy techniques.

36 MATERIALS SCIENCE↗

Asymmetrical In{sub 0.1}Ga{sub 0.9}As/Al{sub 0.3}Ga{sub 0.7}As quantum rings and their optical properties

In{sub 0.1}Ga{sub 0.9}As/Al{sub 0.3}Ga{sub 0.7}As quantum rings were fabricated by droplet epitaxy technique using molecular beam epitaxy (MBE). 7.5 ML In{sub 0.1}Ga{sub 0.9}As droplets are deposited on Al{sub 0.3}Ga{sub 0.7}As epitaxial layer at 350°C and 250°C. After that, they were crystallized under As{sub 4} pressure of 8×10{sup −6} torr at 250°C. The surface morphology of quantum rings is studied by atomic force microscopy. It is found that quantum rings are not symmetrical due to anisotropic behavior of In and Ga atom migration during crystallization process. The quantum ring density of the sample deposition at 350°C and 250°C are 1×10{sup 9} cm{sup −2} and 2.6×10{sup 9} cm{sup −2}, respectively. Consequently, the asymmetric quantum rings with deposition at 350°C give two photoluminescence (PL) peaks at 1.27 and 1.38 eV at 20K. However, the PL peak of quantum rings with deposition at 350°C is merged with GaAs peak due to the poor size distribution.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Nanoscale nuclei in phase change materials: Origin of different crystallization mechanisms of Ge{sub 2}Sb{sub 2}Te{sub 5} and AgInSbTe

Phase change memory devices are based on the rapid and reversible amorphous-to-crystalline transformations of phase change materials, such as Ge{sub 2}Sb{sub 2}Te{sub 5} and AgInSbTe. Since the maximum switching speed of these devices is typically limited by crystallization speed, understanding the crystallization process is of crucial importance. While Ge{sub 2}Sb{sub 2}Te{sub 5} and AgInSbTe show very different crystallization mechanisms from their melt-quenched states, the nanostructural origin of this difference has not been clearly demonstrated. Here, we show that an amorphous state includes different sizes and number of nanoscale nuclei, after thermal treatment such as melt-quenching or furnace annealing is performed. We employ fluctuation transmission electron microscopy to detect nanoscale nuclei embedded in amorphous materials, and use a pump-probe laser technique and atomic force microscopy to study the kinetics of nucleation and growth. We confirm that melt-quenched amorphous Ge{sub 2}Sb{sub 2}Te{sub 5} includes considerably larger and more quenched-in nuclei than its as-deposited state, while melt-quenched AgInSbTe does not, and explain this contrast by the different ratio between quenching time and nucleation time in these materials. In addition to providing insights to the crystallization process in these technologically important devices, this study presents experimental illustrations of temperature-dependence of nucleation rate and growth speed, which was predicted by theory of phase transformation but rarely demonstrated.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Analysis of the Thermal Stability of Very Thin Surface Layers of Corrosion Inhibitors by Time-of-Flight Secondary Ion Mass Spectrometry

The powerful nature of the secondary ion mass spectrometry (SIMS) technique was explored in order to analyse very thin surface layers that were self-assembled on steel material from acidic solution. These surface layers are adsorbed corrosion inhibitors. The SIMS technique proved useful to characterise the molecular structure and homogeneity of thin surface layers in the nanometre range of specific analytes on the metallic substrate. Using SIMS, the thermal stability of these layers was further investigated and the desorption energy at a certain temperature was determined, where special attention was devoted to the method’s static limit. In order to compare, and for certain cases emphasise, the benefits gained by using SIMS in such surface analysis compared with the X-ray photoelectron spectroscopy (XPS) method, the same samples were also analysed by means of the latter. XPS is usually considered to be the most powerful analytical tool in surface analysis studies, but, as shown herein, it has certain limitations compared to SIMS. Finally, the surface topography was investigated by employing atomic force microscopy (AFM) in order to carry out a comprehensive surface analysis. .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Assessing Pair Interaction Potentials of Nanoparticles on Liquid Interfaces

The pair interaction potentials of polymer-grafted silica nanoparticles (NPs) at liquid surfaces were confirmed by scanning electron microscopy, exploiting the nonvolatility of ionic liquids to stabilize the specimens against microscope vacuum. Even at near contact, individual, two-dimensionally well-dispersed NPs were resolved. The potential of mean force, reduced to the pair interaction potential for dilute NPs, was extracted with good accuracy from the radial distribution function, as both NP diameter and grafted polymer chain length were varied. Although NP polydispersity somewhat broadened the core repulsion, the pair potential well-approximated a hard sphere interaction, making these systems suitable for model studies of interfacially bound NPs. For short (5 kDa) poly(ethylene glycol) ligands, a weak (< k B T ) long-range attraction was discerned, and for ligands of identical length, pair potentials overlapped for NPs of different diameter; the attraction is predicted to arise from ligand-induced menisci. To understand better the interactions underlying the pair potential, NP surface-binding energies were measured by interfacial tensiometry, and NP contact angles were analyzed by atomic force microscopy and transmission electron microscopy.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

The MSP 2001 Mars Environmental Compatibility Assessment (MECA)

The Mars Environmental Compatibility Assessment (MECA) will evaluate the Martian environment for soil and dust-related hazards to human exploration as part of the Mars Surveyor Program 2001 Lander. Sponsored by the Human Exploration and Development of Space (HEDS) enterprise, MECA's goal is to evaluate potential geochemical and environmental hazards that may confront future Martian explorers, and to guide HEDS scientists in the development of high fidelity Mars soil simulants. The integrated MECA payload contains a wet-chemistry laboratory, a microscopy station, an electrometer to characterize the electrostatics of the soil and its environment, and arrays of material patches to study the abrasive and adhesive properties of soil grains. The instrument will acquire soil samples with a robotic arm equipped with a camera. MECA will examine surface and subsurface soil and dust in order to characterize particle size, shape, hardness, and also physical characteristics that may provide clues to mineralogy. MECA will characterize soil/water mixtures with respect to pH, redox potential, total dissolved ions, and trace toxins. MECA will determine the nature of electrostatic charging associated with excavation of soil, and the influence of ionizing radiation on material properties. It will also observe natural dust accumulation on engineering materials. To accomplish these objectives, MECA is allocated a mass of 10 kg within an enclosure of 35 x 25 x 15 cm. The Wet Chemistry Laboratory (WCL) consists of four identical cells that will accept samples from surface and subsurface regions accessible to the Lander's robotic arm, mix them with water, and perform extensive analysis of the solution. Ion-selective electrodes and related sensors will evaluate total dissolved solids, redox potential, pH, and the concentration of many soluble ions and gases in wet Martian soil. These electrodes can detect potentially dangerous heavy-metal ions, emitted pathogenic gases, and the soil's corrosive potential. Experiments will include cyclic voltammetry and anodic stripping voltammetry. Complementary to the Viking experiments, the chemical laboratory will characterize the water-soil solution rather than emitted gases. Nonetheless, through analysis of dissolved gases it will be able to replicate many of the Viking observations related to oxidants. MECA's microscopy station combines optical and atomic-force microscopy (AFM) in an actively focused, controlled illumination environment to image particles from millimeters to nanometers in size. Careful selection of substrates allows controlled experiments in adhesion, abrasion, hardness, aggregation, magnetic and other properties. Special tools allow primitive manipulation (brushing and scraping) of samples. Soil particle properties including size, shape, color, hardness, adhesive potential (electrostatic and magnetic), will be determined using an array of sample receptacles and collection substrates. The simple, rugged atomic-force microscope will image in the submicron size range and has the capability of performing a particle-by-particle analysis of the dust and soil. On Earth, the earliest forms of life are preserved as microfossils. The atomic-force microscope will have the required resolution to image down to the scale of terrestrial microfossils and beyond. Mounted on the end of the robot arm, MECA's electrometer actually consists of four types of sensors: an electric field meter, several triboelectricity monitors, an ion gauge, and a thermometer. Tempered only by ultraviolet-light-induced ions and a low-voltage breakdown threshold, the dry, cold, dusty martian environment presents an imposing electrostatic hazard to both robots and humans. The field meter will measure the ambient field on nearby objects while the triboelectric sensors, using identical circuitry, will measure the charge accumulated on test substances as they are dragged through the soil by the arm. The ion chamber, open to the environment, will sense both charged dust and free ions in the air. Over and above the potential threat to electronics, the electrostatic environment holds one of the keys to transport of dust and, consequently, Martian meteorology. Viewed with the robot arm camera, the abrasion and adhesion plates are strategically placed to allow direct observation of the interaction between materials and soils on a macroscopic scale. Materials of graded hardness are placed directly under the robot arm scoop to sense wear and soil hardness. A second array, placed on the lander deck, is deployed after the dust plume of landing has settled. It can be manipulated in a primitive fashion by the arm, first having dirt deposited on it from the scoop and subsequently shaken clean. A third array will passively collect dust from the atmosphere. In addition to objectives related to human exploration, the MECA data set will be rich in information relevant to basic geology, paleoclimate, and exobiology issues. To understand both contemporaneous and ancient processes on Mars, the mineralogy, petrology, and reactivity of Martian surface materials should be constrained. The MECA experiment will shed light on these quantities through its combination of chemistry and microscopy. MECA will be capable of measuring the composition of ancient surface water environments, observing microscopic evidence of geological (and biological?) processes, inferring soil and dust transport, comminution and weathering mechanisms, and characterizing soil horizons that might be encountered during excavation.

Hecht, M. H.↗

The mechanism of low-k SiOCH film modification by oxygen atoms

The interaction of oxygen atoms with three types of plasma enhanced chemical vapor deposition low-k SiOCH films is studied. The samples were treated by O atoms in the far plasma afterglow conditions in a special experimental system designed for this study. The experimental system allowed avoiding the effect of ions and vacuum ultraviolet (VUV) photons on surface reactions and controlling the oxygen atom concentration over the samples. Fourier-transform infrared spectroscopy, x-ray fluorescence, and atomic force microscopy techniques were used to analyze the changes occurring in low-k films. Monte Carlo model for O atom interaction with low-k material that includes penetration, recombination, and reactions with methyl groups was developed. It is shown that the surface recombination on the pore wall surface determines the profile and penetration depth of O atoms into the films. The reaction of O atoms with methyl groups has lower probability and therefore proceeds in the background mode.

36 MATERIALS SCIENCE↗

175 MeV Au{sup +13} ion irradiation induced structural and morphological modifications in zinc oxide thin films

Thin films of ZnO were deposited, on Si substrates, using the RF-sputtering technique and irradiated by the 175 MeV Au{sup +13} beams. The structural changes were investigated by x-ray diffraction (XRD) measurements. The particle size found to increase with the increasing ion fluence up to 1 Multiplication-Sign 10{sup 12} ion/cm{sup 2}. At highest irradiation fluence of 5 Multiplication-Sign 10{sup 12} ion/cm{sup 2} the average particle size decreases. The Raman spectroscopy measurements were performed to understand the local phonon mode of the samples. The surface morphology of the as-deposited and irradiated thin films is measured by the Atomic Force Microscopy (AFM).

36 MATERIALS SCIENCE↗

Study of quasi-two- and three-dimensional ordered porous structures by means of small-angle X-ray scattering in the grazing incidence geometry

The structure of surface layers of thin metal inverse opals has been studied first by the grazing-incidence small-angle X-ray scattering technique. Contributions of the form factor and structure factor to the small-angle diffraction pattern have been separated using a numerical model of the scattering process. The complementary use of the small-angle X-ray scattering and grazing-incidence small-angle X-ray scattering techniques has provided independent information about the bulk and surface properties of the samples and allowed a type of defect in the investigated structures to be determined. The measurement results have been verified by atomic force microscopy.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Growth modes of thin films of ligand-free metal clusters

Size-selected Mo{sub n}{sup −}, W{sub n}{sup −}, and Fe{sub n}{sup −} cluster anions are deposited on a weakly interacting substrate (highly oriented pyrolytic graphite) and studied ex-situ using atomic force microscopy. Depending on size, three growth modes can be distinguished. Very small clusters consisting of less than 10–30 atoms behave similar to atoms and coalesce into 3-dimensional bulk-like islands. Medium sized clusters consisting of hundreds of atoms do not coalesce and follow a Stanski-Krastanov growth pattern. At low coverage, an almost perfect monolayer is formed. This is a new finding different from all previous studies on deposited metal clusters. For clusters with several thousands of atoms, the growth pattern again changes. At low coverage, the substrate is dotted with individual clusters, while at high coverage, the surface becomes extremely rough.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

TUNING OF SIZE AND SHAPE OF AU-PT NANOCATALYST FOR DIRECT METHANOL FUEL CELLS

In this paper, we report the precise control of the size, shape and surface morphology of Au-Pt nanocatalysts (cubes, blocks, octahedrons and dogbones) synthesized via a seed-mediated approach. Gold 'seeds' of different aspect ratios (1 to 4.2), grown by a silver-assisted approach, were used as templates for high-yield production of novel Au-Pt nanocatalysts at a low temperature (40 C). Characterization by electron microscopy (SEM, TEM, HRTEM), energy dispersive X-ray analysis (EDX), UV-Vis spectroscopy, zeta-potential (surface charge), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma mass spectrometry (ICP-MS) were used to better understand their physico-chemical properties, preferred reactivities and underlying nanoparticle growth mechanism. A rotating disk electrode was used to evaluate the Au-Pt nanocatalysts electrochemical performance in the oxygen reduction reaction (ORR) and the methanol oxidation reaction (MOR) of direct methanol fuel cells. The results indicate the Au-Pt dogbones are partially and in some cases completely unaffected by methanol poisoning during the evaluation of the ORR. The ORR performance of the octahedron particles in the absence of MeOH is superior to that of the Au-Pt dogbones and Pt-black, however its performance is affected by the presence of MeOH.

10 SYNTHETIC FUELS↗

Small-displacement measurements using high-order Hermite-Gauss modes

We present a scheme for small-displacement measurements using high-order Hermite-Gauss modes and balanced homodyne detection. We demonstrate its use with experimental results of displacement measurements using fundamental transverse mode TEM{sub 00} and first order transverse mode TEM{sub 10} as signal modes. The results show a factor of 1.41 improvement in measurement precision with the TEM{sub 10} mode compared with that with the TEM{sub 00} mode. This scheme has potential applications in precision metrology, atomic force microscopy, and optical imaging.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Discovery of Nb hydride precipitates in superconducting qubits

We report the first evidence of the formation of niobium hydrides within niobium films on silicon substrates in superconducting qubits fabricated at Rigetti Computing. We combine complementary techniques including room and cryogenic temperature atomic scale high-resolution and scanning transmission electron microscopy (HR-TEM and STEM), atomic force microscopy (AFM), and the time-of-flight secondary ion mass spectroscopy (TOF-SIMS) to reveal the existence of the niobium hydride precipitates directly in the Rigetti chip areas. Electron diffraction and high-resolution transmission electron microscopy (HR-TEM) analyses are performed at room and cryogenic temperatures (~106 K) on superconducting qubit niobium film areas, and reveal the formation of three types of Nb hydride domains with different crystalline orientations and atomic structures. There is also variation in their size and morphology from small (~5 nm) irregular shape domains within the Nb grains to large (~10-100 nm) Nb grains fully converted to niobium hydride. As niobium hydrides are non-superconducting and can easily change in size and location upon different cooldowns to cryogenic temperatures, our findings highlight a new previously unknown source of decoherence in superconducting qubits, contributing to both quasiparticle and two-level system (TLS) losses, and offering a potential explanation for qubit performance changes upon cooldowns. A pathway to mitigate the formation of the Nb hydrides for superconducting qubit applications is also discussed.

Lee, Jaeyel↗

Thermal Annealing Effect on Structure and Properties of Tungsten Surface Irradiated with High Fluence and Low Energy Alpha-Particles

The paper presents research into the surface morphology, helium cluster formation and mechanical properties of high-purity tungsten after the high fluence and low-energy helium ion implantation and subsequent annealing. Investigations are based on scanning electron and atomic force microscopy observations and thermal desorption measurements. Because of the local stresses appearing within the energy loss straggling of helium ions, atoms migrate at distances significantly increasing the ion projective range, and create mobile coalescence of helium atoms and immobile helium-vacancy clusters. The latter form helium bubbles in the energy loss straggling which cause the surface blistering. Local stresses induced by helium coalescence and helium-vacancy clusters beyond the energy loss straggling result in the material strengthening or hardness increase. Subsequent 600°С annealing provides the size growth of blisters on the metal surface irradiated with helium ions and high helium desorption due to the migration of mobile coalescence of helium atoms. With the increasing annealing temperature from 600 to 1000°С, the layer corresponding to the projective range of helium ions fully fractures due to the interstitial helium atoms releasing from immobile helium-vacancy clusters. After 1000°С annealing, the tungsten hardness returns to its initial value.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Temperature dependent dual hydrogen sensor response of Pd nanoparticle decorated Al doped ZnO surfaces

Sputter deposited Al doped ZnO (AZO) thin films exhibit a dual hydrogen sensing response in the temperature range 40 °C–150 °C after surface modifications with palladium nanoparticles. The unmodified AZO films showed no response in hydrogen in the temperature range 40 °C–150 °C. The operational temperature windows on the low and high temperature sides have been estimated by isolating the semiconductor-to-metal transition temperature zone of the sensor device. The gas response pattern was modeled by considering various adsorption isotherms, which revealed the dominance of heterogeneous adsorption characteristics. The Arrhenius adsorption barrier showed dual variation with change in hydrogen gas concentration on either side of the semiconductor-to-metal transition. A detailed analysis of the hydrogen gas response pattern by considering the changes in nano palladium due to hydrogen adsorption, and semiconductor-to-metal transition of nanocrystalline Al doped ZnO layer due to temperature, along with material characterization studies by glancing incidence X-ray diffraction, atomic force microscopy, and transmission electron microscopy, are presented.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Tin diselenide quantum-sized island films

Island films based on the intermediate phases forming in Ge-Se and Sn-Se systems are prepared by the incongruent evaporation of film structures of a Sn{sub 1-x}Se{sub x} composition. The surface morphology of these structures is studied by atomic force microscopy (AFM). The effect of growth conditions on the size distribution of islands is established.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗