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At least 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Versatile technique for assessing thickness of 2D layered materials by XPS

X-ray photoelectron spectroscopy (XPS) has been utilized as a versatile method for thickness characterization of various two-dimensional (2D) films. Accurate thickness can be measured simultaneously while acquiring XPS data for chemical characterization of 2D films having thickness up to approximately 10 nm. For validating the developed technique, thicknesses of few-layer graphene (FLG), MoS 2 and amorphous boron nitride (a-BN) layer, produced by microwave plasma chemical vapor deposition (MPCVD), plasma enhanced chemical vapor deposition (PECVD), and pulsed laser deposition (PLD) respectively, were accurately measured. The intensity ratio between photoemission peaks recorded for the films (C 1s, Mo 3d, B 1s) and the substrates (Cu 2p, Al 2p, Si 2p) is the primary input parameter for thickness calculation, in addition to the atomic densities of the substrate and the film, and the corresponding electron attenuation length (EAL). The XPS data was used with a proposed model for thickness calculations, which was verified by cross-sectional transmission electron microscope (TEM) measurement of thickness for all the films. The XPS method determines thickness values averaged over an analysis area which is orders of magnitude larger than the typical area in cross-sectional TEM imaging, hence provides an advanced approach for thickness measurement over large areas of 2D materials. The study confirms that the versatile XPS method allows rapid and reliable assessment of the 2D material thickness and this method can facilitate in tailoring growth conditions for producing very thin 2D materials effectively over a large area. Furthermore, the XPS measurement for a typical 2D material is non-destructive and does not require special sample preparation. Furthermore, after XPS analysis, exactly the same sample can undergo further processing or utilization.

2D film thickness↗
NASA NTRS1986

Input impedance of a probe-fed circular microstrip antenna with thick substrate

A method of computing the input impedance for the probe fed circular microstrip antenna with thick dielectric substrate is presented. Utilizing the framework of the cavity model, the fields under the microstrip patch are expanded in a set of modes satisfying the boundary conditions on the eccentrically located probe, as well as on the cavity magnetic wall. A mode-matching technique is used to solve for the electric field at the junction between the cavity and the coaxial feed cable. The reflection coefficient of the transverse electromagnetic (TEM) mode incident in the coaxial cable is determined, from which the input impedance of the antenna is computed. Measured data are presented to verify the theoretical calculations. Results of the computation of various losses for the circular printed antenna as a function of substrate thickness are also included.

Davidovitz, M.↗
DOE OSTI2018

Automated Labeling of Electron Microscopy Images Using Deep Learning

© 2018 IEEE. Searching for scientific data requires metadata providing a relevant context. Today, generating metadata is a time and labor intensive manual process that is often neglected, and important datasets are not accessible through search. We investigate the use of machine learning to generalize metadata from a subset of labeled data, thus increasing the availability of meaningful metadata for search. Specifically, we consider electron microscopy images collected at the National Center for Electron Microscopy (NCEM) at the Lawrence Berkeley National Laboratory (LBNL) and use deep learning to discern characteristics from a small subset of labeled images and transfer labels to the entire image corpus. Relatively small training set sizes and a minimum resolution of 512\times 512 pixels required by the application domain pose unique challenges. We overcome these challenges by using a simple yet powerful convolutional network architecture that limits the number of free parameters to lower the required amount of computational power and reduce the risk of overfitting. We achieve a classification accuracy of approximately 80% in discerning between images recorded in two operating modes of the electron microscope-transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). We use transfer learning-i.e., re-using the pre-trained convolution layers from the TEM vs. STEM classification problem-to generalize labels and achieve an accuracy of approximately 70 % despite current experiments being limited to small training data sets. We present these predictions as suggestions to domain scientists through a web-based tool to accelerate the labeling process with the goal of further validating our approach and improving the accuracy of automatically created labels.

Weber, Gunther H↗
DOE OSTI2017

Investigation of the Interaction between Nafion Ionomer and Surface Functionalized Carbon Black Using Both Ultrasmall Angle X-ray Scattering and Cryo-TEM

In making a catalyst ink, the interaction between Nafion ionomer and catalyst support are the key factors that directly affect both ionic conductivity and electronic conductivity of the catalyst layer in a membrane electrode assembly (MEA). One of the major aims of this investigation is to understand the behavior of the catalyst support, Vulcan XC-72 (XC-72) aggregates, in the existence of the Nafion ionomer in a catalyst ink to fill the knowledge gap of the interaction of these components. The dispersion of catalyst ink not only depends on the solvent, but also depends on the interaction of Nafion and carbon particles in the ink. The interaction of Nafion ionomer particles and XC-72 catalyst aggregates in liquid media was studied using ultra small angle x-ray scattering (USAXS) and cryogenic TEM techniques. Carbon black XC-72) and functionalized carbon black systems were introduced to study the interaction behaviors. A multiple curve fitting was used to extract the particle size and size distribution from scattering data. The results suggest that the particle size and size distribution of each system changed significantly in Nafion + XC-72 system, Nafion + NH2-XC72 system, and Nafion + SO3H-XC-72 system, which indicates that an interaction among these components (i.e. ionomer particles and XC-72 aggregates) exists. The cryogenic TEM, which allows for the observation the size of particles in a liquid, was used to validate the scattering results and shows excellent agreement.

Catalyst Ink↗
DOE OSTI2016

Development of zinc oxide nanoparticle by sonochemical method and study of their physical and optical properties

With the miniaturization of crystal size, the fraction of under-coordinated surface atoms becomes dominant, and hence, materials in the nano-regime behave very differently from the similar material in a bulk. Zinc oxide (ZnO), particularly, exhibits extraordinary properties such as a wide direct band gap (3.37 eV), large excitation binding energy (60 meV), low refractive index (1.9), stability to intense ultraviolet (UV) illumination, resistance to high-energy irradiation, and lower toxicity as compared to other semiconductors. This very property makes Zinc Oxide a potential candidate in many application fields, particularly as a prominent semiconductor. Zinc Oxide plays a significant role in many technological advances with its application in semiconductor mediated photocatalytic processes and sensor, solar cells and others. In present study, Zinc Oxide (ZnO) has been synthesized using three different precursors by sonochemical method. Zinc Acetate Dihydrate, Zinc Nitrate Hexahydrate and Zinc Sulphate Heptahydrate used as a precursor for the synthesis process. The synthesized ZnO nanoparticle has been found under the range of ∼50 nm. Zinc oxide nanoparticles were characterized using different characterizing tools. The as-synthesized ZnO was characterized by Fourier Transform-Infrared Spectroscopy (FT-IR) for the determination of functional group; Scanning Electron Microscopy equipped with Energy Dispersive Spectroscopy (SEM-EDS) for Morphology and elemental detection respectively, Transmission Electron Microscopy for Particle size distribution and morphology and X-Ray Diffraction (XRD) for the confirmation of crystal structure of the nanomaterial. The optical properties of the ZnO were examined by UV-VIS spectroscopy equipped with Diffuse Reflectance spectroscopy (DRS) confirmed the optical band gap of ZnO-3 around 3.23 eV resembles with the band gap of bulk ZnO (3.37eV). The TEM micrograph of the as-synthesized material showed perfectly spherical shaped nanoparticle under the size range of 50nm. The XRD data showed that the ZnO-3 which was synthesized using Zinc Nitrate Hexahydrate as precursor showed the hexagonal wurtzite crystal structure. The XRD data obtained were compared with the JCPDS standard data. The precursor Zinc Nitrate Hexahydrate (ZnO-3) showed the good yield, monodispersity and size of nanoparticle under the range of 50 nm. The ZnO nanoparticles synthesize using different precursor was found effective in order of ZnO-3, followed by ZnO-1 & ZnO-2. The Synthesized ZnO has wider application in environmental remediation and clean-up as a potential nano-catalyst.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Synthesis and magnetic properties of nickel nanoparticles

Monodisperse nickel nanoparticles (Ni-NPs) were synthesized via a thermal decomposition process. The NPs were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). They were spherical with mean diameter of 4 nm. Zero field cooled (ZFC) and field cooled (FC) magnetization versus temperature data displayed interesting magnetic interactions. ZFC showed a peak at 4.49 K, indicating the super paramagnetic behavior. Magnetic anisotropic constant was estimated to be 4.62×10{sup 5} erg/cm{sup 3} and coercive field was 168 Oe at 3 K.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
NASA NTRS1994

The nature of agglutinitic glass in the fine-size fraction of lunar soil 10084

Agglutinitic glass contains much of the reduced Fe in lunar soils, and it contributes to the modification of reflectance spectra from lunar soils. Previous work has shown that agglutinitic glass can be compositionally heterogeneous, but the scale of these heterogeneities is not well known. In addition, few data are available on the characteristics of the inclusions in agglutinitic glass. Here we report on our preliminary transmission electron microscope (TEM) examination of agglutinitic glass fragments from the Apollo 11 soil 10084.

Keller, Lindsay P.↗
NASA NTRS2013

Allochthonous Addition of Meteoritic Organics to the Lunar Regolith

Preparation of lunar samples 74220,861 was discussed in detail in [3, 4]. Our analysis sequence was as follows: optical microscopy, UV fluorescence imaging, -Raman, FESEM-EDX imaging and mapping, FETEMEDX imaging and mapping of a Focused Ion Beam (FIB) extracted section, and NanoSIMs analysis. We observed fluffytextured C-rich regions of interest (ROI) on three different volcanic glass beads. Each ROI was several m2 in size and fluoresced when exposed to UV. Using FESEM/EDX, the largest ROI measured ~36 m and was located on an edge of a plateau located on the uppermost surface of the bead. The ROI was covered on one edge by a siliceous filament emanating from the plateau surface indicating it was attached to the bead while on the Moon. EDX mapping of the ROI shows it is composed primarily of heterogeneously distributed C. Embedded with the carbonaceous phase are localized concentrations of Si, Fe, Al and Ti indicating the presence of glass and/or minerals grains. -Raman showed strong D- and G-bands and their associated second order bands; intensity and location of these bands indicates the carbonaceous matter is structurally disorganized. A TEM thin section was extracted from the surface of a glass bead using FIB microscopy. High resolution TEM imaging and selected area electron diffraction demonstrate the carbonaceous layer to be amorphous; it lacked any long or short range order characteristic of micro- or nanocrystalline graphite. Additionally TEM imaging also revealed the presence of submicron mineral grains, typically < 50 nm in size, dispersed within the carbonaceous layer. NanoSIMs data will be presented and discussed at the meeting. Given the noted similarities between the carbonaceous matter present on 74220 glass beads and meteoritic kerogen, we suggest the allochthonous addition of meteoritic organics as the most probable source for the C-rich ROIs.

Thomas-Keprta, K. L.↗
DOE OSTI2015

In Situ TEM Study of Reversible and Irreversible Electroforming in Pt/Ti:NiO/Pt Heterostructures

Experimental verification of the microscopic origin of resistance switching in metal/oxide/metal heterostructures is needed for applications in non-volatile memory and neuromorphic computing. Numerous reports suggest that resistance switching in NiO is caused by local reduction of the oxide layer into nanoscale conducting filaments, but few reports have shown experimental evidence correlating electroforming with site-specific changes in composition. We have investigated the mechanisms of reversible and irreversible electroforming in 250–500 nm wide pillars patterned from a single Ta/Ti/Pt/Ti-doped NiO/Pt/Ta heterostructure and have shown that these can coexist within a single sample. We performed in situ transmission electron microscopy (TEM) electroform- ing and switching on each pillar to correlate the local electron transport behavior with microstructure and composition in each pillar. DFT calculations fitted to electron energy loss spectroscopy data showed that the Ti-doped NiO layer is partially reduced after reversible electroforming, with the formation of oxygen vacancies ordered into lines in the <110> direction. However, under the same probing conditions, adjacent pillars show irreversible electroforming caused by electromigration of metallic Ta to form a single bridge across the oxide layer. We propose that the different electroforming behaviors are related to microstructural variations across the sample and may lead to switching variability.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2023

Advances in imaging, scattering, spectroscopy, and machine learning-aided approaches for multiscale characterization of cementitious systems

Recent progress in methods used in the multiscale characterization of cementitious systems is reviewed, focusing on advances in imaging, scattering, and spectroscopy. The review includes relevant applications and developments in machine learning and other data analytics approaches to enhance characterization. Developments in imaging using light and electron microscopy as well as x-ray (i.e., from synchrotron) methods are summarized. Updates include scanning electron microscopy (SEM), transmission electron microscopy (TEM), tomography, and holography. A critical overview of spectroscopy (e.g., MAS NMR, Raman) and scattering (e.g., neutron, x-ray, synchrotron x-ray) methods is provided, and the intersection of these with imaging is developed (e.g., Raman imaging). Additionally, the paper summarizes recent developments in and implementations of state-of-the-art machine-learning algorithms and data analytics methods for automated, systematic, and/or quantitative analyses of image data sets. The review considers but is not limited to the application of these methods for investigating the hydration and microstructure development of cement phases, low-carbon-footprint cements (e.g., limestone calcined clay cements, LC3), environmental interactions (e.g., ASR) and model systems. Finally, the present work provides a critical presentation of advances in characterization methods that link together the composition and multiscale structure of cementitious materials.

42 ENGINEERING↗
DOE OSTI2014

Iron oxide hydroxide nanoflower assisted removal of arsenic from water

Graphical abstract: Non-magnetic polycrystalline iron oxide hydroxide nanoparticle with flower like morphology is found to play as an effective adsorbent media to remove As(III) from 300 μg L{sup −1} to less than 10 μg L{sup −1} from drinking water over wide range of pH. TEM image clearly reveals that the nanoparticle looks flower like morphology with average particle size less than 20 nm. The maximum sorption capacity of the sorbent is found to be 475 μg g{sup −1} for arsenic at room temperature and the data fitted to different isotherm models indicate the heterogeneity of the adsorbent surface. The material can be regenerated up to 70% using dilute hydrochloric acid and it would be utilized for de-arsenification purposes. - Highlights: • The work includes synthesis of iron oxide hydroxide nanoflower and its applicability for the removal of arsenic from water. • The nanoparticle was characterized using modern instrumental methods like FESEM, TEM, BET, XRD, etc. • The maximum sorption capacity of the sorbent is found to be 475 μg g{sup −1} for arsenic at room temperature. • The sorption is multilayered on the heterogeneous surface of the nano adsorbent. • The mechanism of arsenic removal of IOH nanoflower follows both adsorption and ion-exchange. - Abstract: Non-magnetic polycrystalline iron oxide hydroxide nanoparticle with flower like morphology is found to play as an effective adsorbent media to remove As(III) from 300 μg L{sup −1} to less than 10 μg L{sup −1} from drinking water over wide range of pH. The nanoparticle was characterized by X-ray powder diffraction analysis (XRD), BET surface area, FTIR, FESEM and TEM images. TEM image clearly reveals flower like morphology with average particle size less than 20 nm. The nanoflower morphology is also supported by FESEM images. The maximum sorption capacity of the sorbent is found to be 475 μg g{sup −1} for arsenic and the data fitted to different isotherm models indicate the heterogeneity of the adsorbent surface. Study on adsorption kinetics shows that adsorption of arsenic onto iron oxide hydroxide nanoflower follows pseudo-second order kinetic. The material can be regenerated up to 70% using dilute hydrochloric acid and it would be utilized for de-arsenification purposes.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructural Characterization of Irradiated U0.7ZrH1.6 Using Ultrasonic Techniques

In recent years, there has been an increased level of effort to understand the changes in microstructure that occur due to irradiation of nuclear fuel. The primary driver for this increased effort is the potential for designing new fuels that are safer and more reliable, in turn enabling new and improved reactor technologies. Much of the data on microstructural change in irradiated fuels is generated through a host of post irradiation examination techniques such as optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) to determine grain structure, porosity, crack geometry, etc. in irradiated fuels. Such “traditional” examination techniques were recently used to characterize a novel new fuel consisting of U0.17ZrH1.6 pellets bonded to zircaloy-2 cladded with lead-bismuth eutectic before and after irradiation. However, alternative methods such as ultrasonic inspection can provide an opportunity for nondestructively assessing microstructure in both in-pile and post-irradiation examinations. In this paper, we briefly describe initial results of ultrasonic examination of the U0.17ZrH1.6 pellets (unirradiated and irradiated), in a post-irradiation examination study. Data indicate some correlation with microstructural changes due to irradiation; however, it is not clear what the specific microstructural changes are that are influencing the ultrasonic measurements. Interestingly, specimens with nominally identical burnup show differences in ultrasonic signatures, indicating apparent microstructural differences between these specimens. A summary of the experimental study, preliminary data and findings are presented in this short paper. Additional details of the analysis will be included in the presentation.

Microstructure evaluation↗
DOE OSTI2023

Photocatalytic degradation of orange II dye via high pore volume polymorph zirconium-doped titania under visible light irradiation

A series of mixed-phase Zr-doped TiO 2 was utilized for the photocatalytic degradation of orange II dye. These materials were synthesized through a sol–gel technique by varying the amounts of zirconium in the photocatalysts. These materials were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray fluorescence (XRF), Raman spectroscopy, thermogravimetry analysis (TGA), and X-ray photoelectron spectroscopy (XPS) among others. XRF and XPS data showed that the elemental composition of the photocatalysts consists of zirconium, titanium, and oxygen. In addition, XRD and Raman spectroscopy confirmed the existence of anatase and rutile phases of TiO 2 . The TGA analyses showed that the undoped TiO 2 was the most stable, with no significant weight loss during the heating range. Furthermore, the materials can effectively degrade orange II dye solution up to 7 cycles through asymmetric cleavage of the azo bond.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Central exclusive production at RHIC

The present status and future plans of the physics program of Central Exclusive Production (CEP) at RHIC are described. The measurements are based on the detection of the forward protons from the Double Pomeron Exchange (DPE) process in the Roman Pot system and of the recoil system of charged particles from the DPE process measured in the STAR experiment’s Time Projection Chamber (TPC). The data described here were taken using polarized proton-proton collisions at ps = 200 GeV. The preliminary spectra of two pion and four pion invariant mass reconstructed by STAR TPC in central region of pseudo-rapidity | | < 1, are presented. Near future plans to take data with the current system at center-of-mass energy ps = 200 GeV and plans to upgrade the forward proton tagging sys- tem are presented. Also a possible addition of the Roman Pots to the sPHENIX detector is discussed.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2014

Impact of fluorine based reactive chemistry on structure and properties of high moment magnetic material

The impact of the fluorine-based reactive ion etch (RIE) process on the structural, electrical, and magnetic properties of NiFe and CoNiFe-plated materials was investigated. Several techniques, including X-ray fluorescence, 4-point-probe, BH looper, transmission electron microscopy (TEM), and electron energy loss spectroscopy (EELS), were utilized to characterize both bulk film properties such as thickness, average composition, Rs, ρ, Bs, Ms, and surface magnetic “dead” layers' properties such as thickness and element concentration. Experimental data showed that the majority of Rs and Bs changes of these bulk films were due to thickness reduction during exposure to the RIE process. ρ and Ms change after taking thickness reduction into account were negligible. The composition of the bulk films, which were not sensitive to surface magnetic dead layers with nano-meter scale, showed minimum change as well. It was found by TEM and EELS analysis that although both before and after RIE there were magnetic dead layers on the top surface of these materials, the thickness and element concentration of the layers were quite different. Prior to RIE, dead layer was actually native oxidation layers (about 2 nm thick), while after RIE dead layer consisted of two sub-layers that were about 6 nm thick in total. Sub-layer on the top was native oxidation layer, while the bottom layer was RIE “damaged” layer with very high fluorine concentration. Two in-situ RIE approaches were also proposed and tested to remove such damaged sub-layers.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Effect of the both texture and electrical properties of activated carbon on the CO{sub 2} adsorption capacity

Highlights: • A series of activated carbon pellet without binder was prepared by chemical activation. • Carbon dioxide storage isotherm at 30 °C and up to 25 bars was measured for the microporous carbon. • Adsorption enthalpies have been correlated with the carbon dioxide uptake. • Pyrolysis temperature effect on the electrical conductivity of the samples. • Impact of the both texture and electrical properties on CO{sub 2} adsorption capacity have been deducted - Abstract: A series of activated carbon pellets (ACP) based on olive stones were studied for CO{sub 2} storage application. The surface area, pore volume, and pore diameter were evaluated from the analysis of N{sub 2} adsorption isotherm data. The characterization of carbon materials was performed by scanning electron microscopy (SEM), the powder X-ray diffraction (PXRD) and transmission electron microscopy (TEM). The adsorption enthalpies were obtained by microcalorimetry. The effect of pyrolysis temperature on textural, electrical conductivity and gas adsorption capacities of the ACP were investigated by adsorbing CO{sub 2} at 303 K in the pressure range of 0–2.3 MPa. In fact the electrical conductivity is strongly affected by the microporosity of the samples and the size of the micropore. It increases when the pore size decreases which affect the CO{sub 2} adsorption. Also with increases temperature the free electrons concentration on the surface increases which affect the interaction of the adsorbed gas molecules.

36 MATERIALS SCIENCE↗