Search NASA⌕ Search

SEARCH · Search NASA

Results for “Surface sampling probe”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 631 records · Page 35
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Small-angle X-ray and neutron scattering

Small-angle scattering (SAS) is a technique that is able to probe the structural organization of matter and quantify its response to changes in external conditions. X-ray and neutron scattering profiles measured from bulk materials or materials deposited at surfaces arise from nanostructural inhomogeneities of electron or nuclear density. Furthermore, the analysis of SAS data from coherent scattering events provides information about the length scale distributions of material components. Samples for SAS studies may be prepared in situ or under near-native conditions and the measurements performed at various temperatures, pressures, flows, shears or stresses, and in a time-resolved fashion. In this Primer, we provide an overview of SAS, summarizing the types of instrument used, approaches for data collection and calibration, available data analysis methods, structural information that can be obtained using the method, and data depositories, standards and formats. Recent applications of SAS in structural biology and the soft-matter and hard-matter sciences are also discussed.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2020

Development of a Platform at the Matter in Extreme Conditions End Station for Characterization of Matter Heated by Intense Laser-Accelerated Protons

High intensity short-pulse lasers have made possible the generation of energetic proton beams, unlocking numerous applications in high energy density science. One such application is uniform and isochoric heating of materials to the warm dense matter (WDM) state. We have developed a new experimental platform to simultaneously create and probe warm dense matter at the Matter in Extreme Conditions (MEC) end station at the Linac Coherent Light Source (LCLS). The short pulse optical laser (delivering up to 1 J in 45 fs) and the ultra-bright LCLS x-ray laser with tunable frequency respectively deliver high power required to heat materials to WDM and precision-timed high-resolution x-rays to probe them. The laser-accelerated proton beam driven from a flat 1.5 μm Cu foil was first measured then directed to a secondary sample of Al or polypropylene, typically 300-400 μm away. The time evolution of the sample electron temperature was measured using streaked optical pyrometry, where we observed a peak temperature of 0.9 0.15 eV on the rear surface of an Al sample heated by the proton beam. Here, the simulations using the hybrid-PIC code LSP and the rad-hydro code HELIOS show that a measured proton beam can heat Al to approximately 4 eV and polypropylene to 1 eV if instead focused by a hemispherical Cu target. Through additional LSP simulations, we anticipate creating hotter warm dense matter states (20 eV) by increasing the laser energy to 10 J and keeping the other laser parameters fixed.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
NASA NTRS1989

Spatially resolved organic analysis of the Allende meteorite

The distribution of polycyclic aromatic hydrocarbons (PAHs) in the Allende meteorite has been probed with two-step laser desorption/laser multiphoton ionization mass spectrometry. This method allows direct in situ analysis with a spatial resolution of 1 sq mm or better of selected organic molecules. Spectra from freshly fractured interior surfaces of the meteorite show that PAH concentrations are locally high compared to the average concentrations found by wet chemical analysis of pulverized samples. The data suggest that the PAHs are primarily associated with the fine-grained matrix, where the organic polymer occurs. In addition, highly substituted PAH skeletons were observed. Interiors of individual chondrules were devoid of PAHs at the detection limit (about 0.05 ppm).

Zenobi, Renato↗
NASA NTRS2014

Remote Recession Sensing of Ablative Heat Shield Materials

Tests were performed to demonstrate the feasibility of a new method of measuring surface recession of a material sample during arc-jet testing in the NASA Ames mARC subscale developmental facility. The measurement principle was inspired through tracer elements such as Ca and Na which were seen in the spectra taken during the airborne observation campaign of the Stardust re-entry and which could be clearly observed standing out against the emission spectra emitted by postshock layer and glowing surface of the re-entry capsule. The measurement principle involves seeding of the heat shield materials at a defined depth with tracer elements which show strong and characteristic emission lines in the post shock plasma. Once the material recession reaches the seeding depth, these elements get into the hot plasma and show up in the emission spectra. The methodology was successfully demonstrated during arc-jet testing of phenolic impregnated carbonablator (PICA) material which was seeded in depth with a mixture of NaCl and MgCl in powder form. In the emission spectroscopy data, the emission lines of Mg and Na showed up about 1.5 seconds after probe insertion into the arc-jet plasma and vanished after another 2.5 seconds when recessionhad consumed the seeding material. From these data, a recession rate of about 1 mm/s is estimated.The heat flux during the test was measured to be 2575 W/sq cm on a hemispherical heat flux probewhich corresponds to a heat flux of 1036 W/sq cm on the rectangular test articles. An estimate for a lower limit of the surface temperature of 2800K during the test was obtained by fitting Planck radiation to the continuum spectra emitted by the PICA sample. Typical recession rates of PICA during testing in the large arc-jet facilities at similar test conditions are reported to be on the order of 0.05 to 0.1 cm/s which agrees well with the recession rates of 0.05-0.06 cm/s estimated from the emission spectroscopy data. Further tests under better controlled conditions are suggested to quantify this measurement method. Through a different choice of seeding materials with lower melting point, an extension of the measurement principle to monitor char depth seems feasible but was not yet demonstrated. Possible applications besides ground testing are recession and possibly char depth measurements during real re-entry. Detection through emission spectroscopy could be accomplished through ground based or airborne observation as performed during the Stardust and Hayabusa re-entries, or through on-board spectrometers. A suitable mission would be the re-entryof the OSIRIS-REX mission planned for late 2023. The measured data are presented and interpreted, the results and details of future applications are discussed.

instrumentation↗
DOE OSTI2018

Revealing the beneficial role of K in grain interiors, grain boundaries, and at the buffer interface for highly efficient CuInSe 2 solar cells

K incorporation within grain boundaries, grain interiors, and interfaces has been studied within CuInSe 2 solar cells to better understand the beneficial or detrimental role of K distribution among these regions in chalcopyrite–based solar cells. Solar cells have been fabricated with intentional K introduction into specific regions of the device including the CuInSe 2 /CdS interface (CuInSe 2 /KInSe 2 /CdS) and the grain interiors (Cu 0.93 K 0.07 InSe 2 /CdS). A control CuInSe 2 /CdS device was also studied to separate effects of K originating from the soda–lime glass substrate from those of intentionally introduced K. The experiment was designed to understand K effects in Cu(In,Ga)Se 2 solar cells while mitigating complications from multiple elements in the 3 + site. The distribution of all elements within these samples has been directly observed with sub–nm resolution via atom probe tomography. In addition, electron beam–induced current measurements have been performed to correlate the atom probe tomography compositional profiles to the nanoscale carrier collection properties. The experiments show that a large decrease in the Cu/In ratio at the CdS interface can be achieved by forming KInSe 2 at the absorber surface, which drastically improves the device efficiency. The results presented here show a direct link between K concentration, Cu depletion, and In accumulation, such that the Cu/In ratio significantly reduces with K incorporation. In conclusion, the findings help clarify the mechanism behind K–induced efficiency enhancement.

14 SOLAR ENERGY↗
DOE OSTI2014

Integration of atomic layer deposited high-k dielectrics on GaSb via hydrogen plasma exposure

In this letter we report the efficacy of a hydrogen plasma pretreatment for integrating atomic layer deposited (ALD) high-k dielectric stacks with device-quality p-type GaSb(001) epitaxial layers. Molecular beam eptiaxy-grown GaSb surfaces were subjected to a 30 minute H{sub 2}/Ar plasma treatment and subsequently removed to air. High-k HfO{sub 2} and Al{sub 2}O{sub 3}/HfO{sub 2} bilayer insulating films were then deposited via ALD and samples were processed into standard metal-oxide-semiconductor (MOS) capacitors. The quality of the semiconductor/dielectric interface was probed by current-voltage and variable-frequency admittance measurements. Measurement results indicate that the H{sub 2}-plamsa pretreatment leads to a low density of interface states nearly independent of the deposited dielectric material, suggesting that pre-deposition H{sub 2}-plasma exposure, coupled with ALD of high-k dielectrics, may provide an effective means for achieving high-quality GaSb MOS structures for advanced Sb-based digital and analog electronics.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microstructural Changes and Chemical Analysis of Fission Products in Irradiated Uranium-7 wt.% Molybdenum Metallic Fuel Using Atom Probe Tomography

Understanding the microstructural and phase changes occurring during irradiation and their impact on metallic fuel behavior is integral to research and development of nuclear fuel programs. This paper reports systematic analysis of as-fabricated and irradiated low-enriched U-Mo (uranium-molybdenum metal alloy) fuel using atom probe tomography (APT). This study is carried out on U-7 wt.% Mo fuel particles coated with a ZrN layer contained within an Al matrix during irradiation. The dispersion fuel plates from which the fuel samples were extracted are irradiated at Belgian Nuclear Research Centre (SCK CEN) with burn-up of 52% and 66% in the framework of the SELENIUM (Surface Engineering of Low ENrIched Uranium-Molybdenum) project. The APT studies on U-Mo particles from as-fabricated fuel plates enriched to 19.8% revealed predominantly γ-phase U-Mo, along with a network of the cell boundary decorated with α-U, γ’-U2Mo, and UC precipitates along the grain boundaries. The corresponding APT characterization of irradiated fuel samples showed formation of fission gas bubbles enriched with solid fission products. The intermediate burnup sample showed a uniform distribution of the typical bubble superlattice with a radius of 2 nm arranged in a regular lattice, while the high burnup sample showed a non-uniform distribution of bubbles in grain-refined regions. There was no evidence of remnant α-U, γ’-U2Mo, and UC phases in the irradiated U-7 wt.% Mo samples.

Bachhav, Mukesh↗
DOE OSTI2017

Material property analytical relations for the case of an AFM probe tapping a viscoelastic surface containing multiple characteristic times

We explore the contact problem of a flat-end indenter penetrating intermittently a generalized viscoelastic surface, containing multiple characteristic times. This problem is especially relevant for nanoprobing of viscoelastic surfaces with the highly popular tapping-mode AFM imaging technique. By focusing on the material perspective and employing a rigorous rheological approach, we deliver analytical closed-form solutions that provide physical insight into the viscoelastic sources of repulsive forces, tip-sample dissipation and virial of the interaction. We also offer a systematic comparison to the well-established standard harmonic excitation, which is the case relevant for dynamic mechanical analysis (DMA) and for AFM techniques where tip–sample sinusoidal interaction is permanent. This comparison highlights the substantial complexity added by the intermittent-contact nature of the interaction, which precludes the derivation of straightforward equations as is the case for the well-known harmonic excitations. The derivations offered have been thoroughly validated through numerical simulations. Despite the complexities inherent to the intermittent-con-tact nature of the technique, the analytical findings highlight the potential feasibility of extracting meaningful viscoelastic properties with this imaging method.

36 MATERIALS SCIENCE↗
DOE OSTI2015

PROBING STELLAR ACCRETION WITH MID-INFRARED HYDROGEN LINES

In this paper we investigate the origin of the mid-infrared (IR) hydrogen recombination lines for a sample of 114 disks in different evolutionary stages (full, transitional, and debris disks) collected from the Spitzer archive. We focus on the two brighter H I lines observed in the Spitzer spectra, the H I (7-6) at 12.37 μm and the H I (9-7) at 11.32 μm. We detect the H I (7-6) line in 46 objects, and the H I (9-7) in 11. We compare these lines with the other most common gas line detected in Spitzer spectra, the [Ne II] at 12.81 μm. We argue that it is unlikely that the H I emission originates from the photoevaporating upper surface layers of the disk, as has been found for the [Ne II] lines toward low-accreting stars. Using the H I (9-7)/H I (7-6) line ratios we find these gas lines are likely probing gas with hydrogen column densities of 10{sup 10}-10{sup 11} cm{sup –3}. The subsample of objects surrounded by full and transitional disks show a positive correlation between the accretion luminosity and the H I line luminosity. These two results suggest that the observed mid-IR H I lines trace gas accreting onto the star in the same way as other hydrogen recombination lines at shorter wavelengths. A pure chromospheric origin of these lines can be excluded for the vast majority of full and transitional disks. We report for the first time the detection of the H I (7-6) line in eight young (<20 Myr) debris disks. A pure chromospheric origin cannot be ruled out in these objects. If the H I (7-6) line traces accretion in these older systems, as in the case of full and transitional disks, the strength of the emission implies accretion rates lower than 10{sup –10} M {sub ☉} yr{sup –1}. We discuss some advantages of extending accretion indicators to longer wavelengths, and the next steps required pinning down the origin of mid-IR hydrogen lines.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS1978

Electron emission from nickel-alloy surfaces in cesium vapor

The cesiated electron emission was measured for three candidate electrodes for use as collectors in thermionic converters. Nickel, Inconel 600 and Hastelloy were tested with a 412 K cesium reservoir. Peak emission from the alloys was found to be comparable to that from pure nickel. Both the Inconel and the Hastelloy samples had work functions of 1.64 eV at peak emission. The minimum work functions were estimated to be 1.37 eV at a probe temperature of 750 K for Inconel and 1.40 eV for Hastelloy at 665 K. The bare work function for both alloys is estimated to be approximately the same as for pure nickel, 4.8 eV.

Manda, M.↗
NASA NTRSDate not supplied

Ultraviolet/Visible Reflectance Spectra of Returned Samples of (162173) Ryugu Unexposed to Earth’s Atmosphere

Following the successful return of JAXA’s Hayabusa2 sample capsule, the material from asteroid (162173) Ryugu retrieved from the spacecraft retrieval container has been the subject of multi-pronged analyses [e.g., 1]. We undertook an effort to acquire reflectance spectra covering 200- to- 1100 nm of particles from Ryugu. This region probes the near-ultraviolet (NUV) to acquire reflectance spectra that cover the 250-nm Fresnel peak that can result from increased graphitization (reduced H content) of carbon-bearing materials. Laboratory tests show that increased graphitization could result from the effects of increased temperature, an effect of space weathering of materials closer to the Sun. Some ground-based reflectance spectra and space-based photometry of Ryugu show that reflectance is increasing with decreasing wavelength, suggesting the beginning of a UV upturn [2]. We sought evidence for space weathering (graphitization) of the Ryugu material at NUV wavelengths, by acquiring reflectance spectra of surface samples.

F Vilas↗
DOE OSTI2025

Subnanometer Thick Native sp 2 Carbon on Oxidized Diamond Surfaces

Oxygen-terminated diamond has a wide breadth of applications, which include stabilizing near-surface color centers, semiconductor devices, and biological sensors. Despite the vast literature on characterizing functionalization groups on diamond, the chemical composition of the shallowest portion of the surface (<1 nm) is challenging to probe with conventional techniques like XPS and FTIR. In this work, we demonstrate the use of angleresolved XPS to probe the first ten nanometers of both oxygen and hydrogen terminated (100) single-crystalline diamond grown via chemical vapor deposition (CVD). With the use of consistent peakfitting methods, the peak identities and relative peak binding energies were identified for sp 2 carbon, ether, hydroxyl, carbonyl, and C−H groups for both of these diamond surface terminations. For the oxygen-terminated sample, we also quantified the thickness of the sp 2 carbon layer situated on top of the bulk sp 3 diamond bonded carbon to be 0.3 ± 0.1 nm, based on the analysis of the Auger electron spectra and D-parameter calculations. These results indicate that the majority of the oxygen is bonded to the sp 2 carbon layer on the diamond, and not directly to the sp 3 diamond bonded carbon.

Carbon↗
DOE OSTI2024

Irreversible Catalyst Deactivation Mechanisms of PdO/γ-Al 2 O 3 Catalysts for Lean Methane Oxidation

PdO/γ-Al 2 O 3 catalysts suffer from gradual and irreversible catalyst deactivation under lean CH 4 oxidation conditions, especially in a wet feed. Here, time-resolved CO chemisorption DRIFTS measurements are conducted systematically on a series of PdO/γ-Al 2 O 3 catalysts to probe the surface reactivity of PdO nanoparticles after various in situ pretreatments. At 80 °C, CO barely adsorbs on fully oxidized PdO surfaces but interacts with coordinatively unsaturated Pd sites, causing gradual reduction of the PdO surfaces. This results in the formation of characteristic IR bands on various metallic Pd 0 sites. By monitoring and comparing the formation kinetics of these IR bands on samples before and after CH 4 oxidation, we theorize that the irreversible catalyst deactivation during CH 4 oxidation is caused by PdO surface reconstruction, in which coordinatively unsaturated Pd sites gradually become fully coordinated by oxygen. Effectively, the surface reconstruction leads to the formation of a passivation layer on the PdO nanoparticles, which hinders their ability in activating CH 4 , and hence the subsequent oxidation reaction. Temperature-programmed reduction with CO as the reductant (CO-TPR) reveals that the passivation layer formed during CH 4 oxidation is significant enough to increase the reduction temperature of PdO nanoparticles of the 3.0% PdO/γ-Al 2 O 3 samples, although such an effect is less obvious for the 0.4% PdO/γ-Al 2 O 3 samples. On the other hand, it is also discovered that the passivation layer is not completely inert. Under certain reaction conditions, with some being relatively mild, such as low-temperature CO oxidation in a net lean atmosphere and in the presence of H 2 O, the passivation layer can undergo structure change which results in regeneration or even activation of CH 4 oxidation activity of an already deactivated catalyst. Additionally, it is discovered that the fully coordinated Pd–O surface is a metastable phase under CH 4 oxidation conditions. In the presence of H 2 O and at ambient temperatures, surfaces with coordinatively unsaturated Pd sites are thermodynamically more favorable.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Effective Strategy for Improving Electrocatalyst Durability by Adhesive Immobilization of Catalyst Nanoparticles on Graphitic Carbon Supports

We have found that Ta-based additive films in our catalyst system act as adhesives, which improves electrocatalyst durability by immobilizing the catalyst Pt NPs on the graphitic Vulcan carbon support. Furthermore, we suggest that this can be a general design principle in producing higher-durability electrocatalysts on graphitic supports. By electrochemically probing the contributing roles of the tantalum oxide (Ta 2 O 5 ) and the polyphosphate (PPA) components in separate samples, we show that these combine to produce the observed improvement in activity and durability of our best catalyst, the tantalum polyphosphate (TaOPO 4 )-treated sample. To control variables for a valid electrochemical comparison, such as dissimilar catalyst particle size distributions and variations in surface coverage, four new catalyst samples closely matched in every way were prepared: (1) Pt/VC, (2) Pt/[PPA/VC], (3) Pt/[Ta 2 O 5 /VC], and (4) Pt[TaOPO 4 /VC]. We present HR-TEM/HAADF-STEM, EDS elemental mapping, PXRD, XPS, and electrochemical activity and durability evidence, showing that the TaOPO4 and Ta2O5 additives act as adhesives, effectively tethering the NPs to the VC graphitic support surface. Pt/[Ta 2 O 5 /VC] exhibited 3× better durability as compared with the Pt/VC control because of better catalyst nanoparticle immobilization by the Ta 2 O 5 adhesive. Pt[TaOPO 4 /VC] is the overall best performer, exhibiting both a high MA of 0.82 A mg Pt –1, the highest ORR MA after heat treatment, as well as 1.75× greater durability over the Pt/VC control.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Surface Terminations of LaAlO 3 Perovskite Nanoparticles as Viewed by Solid-State Nuclear Magnetic Resonance

Nanocrystal surfaces generally undergo reconstructions that differentiate them from the bulk structures, often in nontrivial ways. Understanding these terminations is critical across diverse fields, from heterogeneous catalysis to the formation of topological states and the synthesis of semiconductor nanomaterials. Determining surface structures is currently an interdisciplinary task, most often involving high-resolution electron microscopy and surface electron diffraction. These methods, however, do not provide a global view of the ensemble of structures present in a sample. Here, we show how surface-sensitive solid-state nuclear magnetic resonance (SSNMR) spectroscopy methods can bridge this gap. In this context, we investigated the surface structure of lanthanum aluminate (LaAlO 3 ) perovskite nanoparticles. Four distinct surface terminations have previously been observed for this material, but their relative abundances were unknown. Using an array of double- and triple-resonance SSNMR methods probing the relative proximities of surface 1 H, 27 Al, 17 O, and 139 La nuclei, we conclude the surface to be majority terminated (80%) by AlO x with substantial (20%) LaO x terminated regions.

Materials↗
NASA NTRS1975

Ion-probe studies of artificially implanted ions in lunar samples

The ion microprobe at the Johnson Space Center was used to study depth profiles of artificially implanted ions in lunar samples. Five polished sections of typical mare basalts (12040 and 12018) were irradiated with nine different elements at two energies and the resulting concentrations were measured as a function of depth in the minerals plagioclase, pyroxene, and ilmenite. These preliminary simulation experiments were undertaken to determine whether the ion probe can be used to measure solar-wind-implanted elements on the surface of lunar rock crystals and soil grains and to study mechanisms for the redistribution. The results obtained so far demonstrate that depth profiles can indeed be measured with the ion probe. From estimated exposure times of mature soil grains and selected vug crystals, it appears possible (if difficult) to detect several solar-wind-implanted elements.

Zinner, E.↗
DOE OSTI2012

Improvement of the identification of multiwall carbon nanotubes carpet thermal conductivity by pulsed photothermal method

Thermal properties in multiwall carbon nanotubes carpets and micro-devices are investigated using a nanosecond photothermal method. Gradually, the identification model and experimental protocol are performed to increase the method accuracy for the thermal conductivity determination. In the experimental protocol, a nanosecond UV monopulse laser beam is used to heat the surface of a multilayer (600 nm of Ti/20 {mu}m of carbon nanotube carpet) sample. In the 1D identification model with two layers and a thermal contact resistance, the effect of the laser excitation temporal shape is taken into account. In this study, this first approach allows to improve the accuracy of apparent thermal conductivity measurements of multiwall carbon nanotubes carpet. The carbon nanotubes carpet apparent thermal conductivity value went from being to 180 {+-} 5 W Multiplication-Sign m{sup -1} Multiplication-Sign K{sup -1}. In the second approach, two laser beams are coupled in order to increase the interaction time duration from 27 ns to 60 ns. It becomes possible to probe different depths in the carpet. The obtained value (180 W Multiplication-Sign m{sup -1} Multiplication-Sign K{sup -1}) confirms the pulsed photothermal method consistency for porous samples. Finally, assuming that the carbon nanotubes are parallel and without any defects, the equivalent intrinsic thermal conductivity of a single carbon nanotube is estimated to be around 3600 W Multiplication-Sign m{sup -1} Multiplication-Sign K{sup -1}.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2011

Scaling and disorder analysis of local I–V curves from ferroelectric thin films of lead zirconate titanate

In this paper, differential analysis of current–voltage characteristics, obtained on the surface of epitaxial films of ferroelectric lead zirconate titanate (Pb(Zr 0.2 Ti 0.8 )O 3 ) using scanning probe microscopy, was combined with spatially resolved mapping of variations in local conductance to differentiate between candidate mechanisms of local electronic transport and the origin of disorder. Within the assumed approximations, electron transport was inferred to be determined by two mechanisms depending on the magnitude of applied bias, with the low-bias range dominated by the trap-assisted Fowler–Nordheim tunneling through the interface and the high-bias range limited by the hopping conduction through the bulk. Phenomenological analysis of the I–V curves has further revealed that the transition between the low- and high-bias regimes is manifested both in the strength of variations within the I–V curves sampled across the surface, as well as the spatial distribution of conductance. Finally, spatial variations were concluded to originate primarily from the heterogeneity of the interfacial electronic barrier height with an additional small contribution from random changes in the tip–contact geometry.

36 MATERIALS SCIENCE↗