In situ synthesis of semiconducting single-walled carbon nanotubes by modified arc discharging method

NASA Astrophysics Data System (ADS)

Zhao, Tingkai; Ji, Xianglin; Jin, Wenbo; Yang, Wenbo; Zhao, Xing; Dang, Alei; Li, Hao; Li, Tiehu

2017-02-01

Semiconducting single-walled carbon nanotubes (s-SWCNTs) were in situ synthesized by a temperature-controlled arc discharging furnace with DC electric field using Co-Ni alloy powder as catalyst in helium gas. The microstructures of s-SWCNTs were characterized using high-resolution transmission electron microscopy, electron diffraction, and Raman spectrometry apparatus. The experimental results indicated that the best voltage value in DC electric field is 54 V, and the environmental temperature of the reaction chamber is 600 °C. The mean diameter of s-SWCNTs was estimated about 1.3 nm. The chiral vector ( n, m) of s-SWCNTs was calculated to be (10, 10) type according to the electron diffraction patterns.

One step synthesis of porous graphene by laser ablation: A new and facile approach

NASA Astrophysics Data System (ADS)

Kazemizadeh, Fatemeh; Malekfar, Rasoul

2018-02-01

Porous graphene (PG) was obtained using one step laser process. Synthesis was carried out by laser ablation of nickel-graphite target under ultra-high flow of argon gas. The field emission scanning electron microscopy (FE-SEM) results showed the formation of a porous structure and the transmission electron microscopy (TEM) revealed that the porosity of PGs increase under intense laser irradiation. Structural characterization study using Raman spectroscopy, X-ray powder diffraction (XRD) and selected area electron diffraction (SAED) technique showed that the obtained PGs display high crystalline structure in the form of few layer rhombohedral graphitic arrangement that can be interpreted as the phase prior to the formation of other carbon nanostructures.

Science Notes.

ERIC Educational Resources Information Center

Piearce, Trevor; And Others

1988-01-01

Provides explanations of 15 experiments, laboratory activities, demonstrations, and lessons for use in instruction. Includes information on Daphnia, wild garlic, crystals, gas chromatographs, bleaches, alcohols, reactivity series, chemistry formula, electronic keyboards and waveforms, interference and diffraction gravity, Moire fringe patterns,…

Molecular structure and conformational preferences of 1-bromo-1-silacyclohexane, CH2(CH2CH2)2SiH-Br, as studies by gas-phase electron diffraction and quantum chemistry

NASA Astrophysics Data System (ADS)

Belyakov, A. V.; Baskakov, A. A.; Naraev, V. N.; Rykov, A. N.; Oberhammer, H.; Arnason, I.; Wallevik, S. O.

2012-10-01

The molecular structure of axial and equatorial conformer of the 1-bromo-1-silacyclohexane molecule, CH2(CH2CH2)2SiH-Br, as well as thermodynamic equilibrium between these species are investigated by means of gas-phase electron diffraction and quantum chemistry on the MP2(full)/SDB-AUG-cc-PVTZ level of theory. It is revealed that according to electron diffraction data, the compound exists in the gasphase as a mixture of conformers possessing the chair conformation of the six-membered ring and C s symmetry and differing in the axial and equatorial position of the Si-Br bond (ax. = 80(5) mol %, eq. = 20(7) mol %) at 352 K, that corresponds to the value of A = ( G {ax/○} - G {eq/○}) = -0.82(32) kcal/mol. It is found that observed data agree well with theoretical ones. Using Natural Bond Orbital (NBO) analysis it is revealed that axial conformer of 1-bromo-1-silacyclohexane molecule is an example of the stabilization of the form that is unfavorable from the point of view of steric effects and effects of conjugations. It is concluded that stabilization is achieved due to electrostatic interactions.

Fabrication, characterization and gas sensing studies of PPy/MWCNT/SLS nanocomposite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tiwari, D. C., E-mail: dctiwari2001@yahoo.com; Atri, Priyanka, E-mail: dctiwari2001@yahoo.com; Sharma, R.

2014-04-24

Multiwall carbon nanotubes (MWCNT) coated with polypyrrole nanocomposite was prepared by in-situ chemical oxidative polymerization method in the presence of surfactant (SLS). The scanning electron microscope (SEM) pictures indicate the core shell structure of PPy/MWCNT/SLS nanocomposite. Nature of the prepared material was investigated by X-ray diffraction spectroscopy. This nanocomposite shows the excellent gas sensing behaviour for ammonia gas at 150 ppm and 300 ppm levels.

In-Depth View of the Structure and Growth of SnO2 Nanowires and Nanobrushes.

PubMed

Stuckert, Erin P; Geiss, Roy H; Miller, Christopher J; Fisher, Ellen R

2016-08-31

Strategic application of an array of complementary imaging and diffraction techniques is critical to determine accurate structural information on nanomaterials, especially when also seeking to elucidate structure-property relationships and their effects on gas sensors. In this work, SnO2 nanowires and nanobrushes grown via chemical vapor deposition (CVD) displayed the same tetragonal SnO2 structure as revealed via powder X-ray diffraction bulk crystallinity data. Additional characterization using a range of electron microscopy imaging and diffraction techniques, however, revealed important structure and morphology distinctions between the nanomaterials. Tailoring scanning transmission electron microscopy (STEM) modes combined with transmission electron backscatter diffraction (t-EBSD) techniques afforded a more detailed view of the SnO2 nanostructures. Indeed, upon deeper analysis of individual wires and brushes, we discovered that, despite a similar bulk structure, wires and brushes grew with different crystal faces and lattice spacings. Had we not utilized multiple STEM diffraction modes in conjunction with t-EBSD, differences in orientation related to bristle density would have been overlooked. Thus, it is only through a methodical combination of several structural analysis techniques that precise structural information can be reliably obtained.

Extracting conformational structure information of benzene molecules via laser-induced electron diffraction

DOE PAGES

Ito, Yuta; Wang, Chuncheng; Le, Anh-Thu; ...

2016-05-01

Here, we have measured the angular distributions of high energy photoelectrons of benzene molecules generated by intense infrared femtosecond laser pulses. These electrons arise from the elastic collisions between the benzene ions with the previously tunnel-ionized electrons that have been driven back by the laser field. Theory shows that laser-free elastic differential cross sections (DCSs) can be extracted from these photoelectrons, and the DCS can be used to retrieve the bond lengths of gas-phase molecules similar to the conventional electron diffraction method. From our experimental results, we have obtained the C-C and C-H bond lengths of benzene with a spatialmore » resolution of about 10 pm. Our results demonstrate that laser induced electron diffraction (LIED) experiments can be carried out with the present-day ultrafast intense lasers already. Looking ahead, with aligned or oriented molecules, more complete spatial information of the molecule can be obtained from LIED, and applying LIED to probe photo-excited molecules, a “molecular movie” of the dynamic system may be created with sub-A°ngstrom spatial and few-ten femtosecond temporal resolutions.« less

Chemical vapor deposition growth

NASA Technical Reports Server (NTRS)

Ruth, R. P.; Manasevit, H. M.; Kenty, J. L.; Moudy, L. A.; Simpson, W. I.; Yang, J. J.

1976-01-01

A chemical vapor deposition (CVD) reactor system with a vertical deposition chamber was used for the growth of Si films on glass, glass-ceramic, and polycrystalline ceramic substrates. Silicon vapor was produced by pyrolysis of SiH4 in a H2 or He carrier gas. Preliminary deposition experiments with two of the available glasses were not encouraging. Moderately encouraging results, however, were obtained with fired polycrystalline alumina substrates, which were used for Si deposition at temperatures above 1,000 C. The surfaces of both the substrates and the films were characterized by X-ray diffraction, reflection electron diffraction, scanning electron microscopy optical microscopy, and surface profilometric techniques. Several experiments were conducted to establish baseline performance data for the reactor system, including temperature distributions on the sample pedestal, effects of carrier gas flow rate on temperature and film thickness, and Si film growth rate as a function of temperature.

Facile synthesis of α-Fe{sub 2}O{sub 3} nanoparticles for high-performance CO gas sensor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cuong, Nguyen Duc, E-mail: nguyenduccuong@hueuni.edu.vn; Faculty of Hospitality and Tourism, Hue University, 22 Lam Hoang, Vy Da Ward, Hue City; Khieu, Dinh Quang

2015-08-15

Highlights: • We have demonstrated a facile method to prepare Fe{sub 2}O{sub 3} nanoparticles. • The gas sensing properties of α-Fe{sub 2}O{sub 3} have been invested. • The results show potential application of α-Fe{sub 2}O{sub 3} NPs for CO sensors in environmental monitoring. - Abstract: Iron oxide nanoparticles (NPs) were prepared via a simple hydrothermal method for high performance CO gas sensor. The synthesized α-Fe{sub 2}O{sub 3} NPs were characterized by X-ray diffraction, nitrogen adsorption/desorption isotherm, scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED). The SEM, TEM results revealedmore » that obtained α-Fe{sub 2}O{sub 3} particles had a peanut-like geometry with hemispherical ends. The response of the α-Fe{sub 2}O{sub 3} NPs based sensor to carbon monoxide (CO) and various concentrations of other gases were measured at different temperatures. It found that the sensor based on the peanut-like α-Fe{sub 2}O{sub 3} NPs exhibited high response, fast response–recovery, and good selectivity to CO at 300 °C. The experimental results clearly demonstrated the potential application of α-Fe{sub 2}O{sub 3} NPs as a good sensing material in the fabrication of CO sensor.« less

Determination of the molecular structure of tetrakis(trimethylsilyl)hydrazine, N 2(SiMe 3) 4, in the gas phase by electron diffraction

NASA Astrophysics Data System (ADS)

Brain, Paul T.; Irving, Iain A.; Rankin, David W. H.; Robertson, Heather E.; Leung, Wing-Por; Bühl, Michael

1997-09-01

The gas-phase molecular structure of tetrakis(trimethylsily)hydrazine, N 2(SiMe 3) 4, in the gas phase has been determined by electron diffraction. The skeleton consists of two planar NSi 2 fragments which are not coplanar, but twisted 86.9(38)° relative to one another. This conformation, combined with the arrangements of the trimethylsilyl groups, gives the molecule overall D2 symmetry, and ensures that there are no major steric interactions between the groups. Ab initio calculations at the {SCF}/{6-31 G∗ } level confirm that D2 symmetry is favoured. The bond lengths ( ra) of 143.3(16) pm for NN. 175.9(5) pm for SiN and 187.5(2) pm for SiC, and the SiNSi and CSiC angles of 124.1(15)° and 108.8(7) respectively, also indicate that this is not a severely strained molecule, although the SiN distance is quite long, being comparable to that observed in N(SiMe 3) 3.

Dimethylalkoxygallane incorporating a donor-functionalised alkoxide: the monomeric gas-phase structure.

PubMed

Knapp, Caroline E; Carmalt, Claire J; McMillan, Paul F; Wann, Derek A; Robertson, Heather E; Rankin, David W H

2008-12-28

The structure of the vapour produced upon heating the dimethylalkoxygallane [Me(2)GaOCH(2)CH(2)NMe(2)](2) has been studied by gas-phase electron diffraction and ab initio molecular orbital calculations; only the monomeric form [Me(2)GaOCH(2)CH(2)NMe(2)] is observed in the vapour, with the nitrogen atom forming a dative bond with the metal centre.

MeV electron acceleration at 1kHz with <10 mJ laser pulses

NASA Astrophysics Data System (ADS)

Salehi, Fatholah; Goers, Andy; Hine, George; Feder, Linus; Kuk, Donghoon; Kim, Ki-Yong; Milchberg, Howard

2016-10-01

We demonstrate laser driven acceleration of electrons at 1 kHz repetition rate with pC charge above 1MeV per shot using < 10 mJ pulse energies focused on a near-critical density He or H2 gas jet. Using the H2 gas jet, electron acceleration to 0.5 MeV in 10 fC bunches was observed with laser pulse energy as low as 1.3mJ . Using a near-critical density gas jet sets the critical power required for relativistic self-focusing low enough for mJ scale laser pulses to self- focus and drive strong wakefields. Experiments and particle-in-cell simulations show that optimal drive pulse duration and chirp for maximum electron bunch charge and energy depends on the target gas species. High repetition rate, high charge, and short duration electron bunches driven by very modest pulse energies constitutes an ideal portable electron source for applications such as ultrafast electron diffraction experiments and high rep. rate γ-ray production. This work is supported by the US Department of Energy, the National Science Foundation, and the Air Force Office of Scientific Research.

Femtosecond X-ray diffraction from an aerosolized beam of protein nanocrystals

DOE PAGES

Awel, Salah; Kirian, Richard A.; Wiedorn, Max O.; ...

2018-02-01

High-resolution Bragg diffraction from aerosolized single granulovirus nanocrystals using an X-ray free-electron laser is demonstrated. The outer dimensions of the in-vacuum aerosol injector components are identical to conventional liquid-microjet nozzles used in serial diffraction experiments, which allows the injector to be utilized with standard mountings. As compared with liquid-jet injection, the X-ray scattering background is reduced by several orders of magnitude by the use of helium carrier gas rather than liquid. Such reduction is required for diffraction measurements of small macromolecular nanocrystals and single particles. High particle speeds are achieved, making the approach suitable for use at upcoming high-repetition-rate facilities.

Diffractive imaging of a rotational wavepacket in nitrogen molecules with femtosecond megaelectronvolt electron pulses

DOE PAGES

Yang, Jie; Guehr, Markus; Vecchione, Theodore; ...

2016-04-05

Imaging changes in molecular geometries on their natural femtosecond timescale with sub-Angström spatial precision is one of the critical challenges in the chemical sciences, as the nuclear geometry changes determine the molecular reactivity. For photoexcited molecules, the nuclear dynamics determine the photoenergy conversion path and efficiency. Here we report a gas-phase electron diffraction experiment using megaelectronvolt (MeV) electrons, where we captured the rotational wavepacket dynamics of nonadiabatically laser-aligned nitrogen molecules. We achieved a combination of 100 fs root-mean-squared temporal resolution and sub-Angstrom (0.76 Å) spatial resolution that makes it possible to resolve the position of the nuclei within the molecule.more » In addition, the diffraction patterns reveal the angular distribution of the molecules, which changes from prolate (aligned) to oblate (anti-aligned) in 300 fs. Lastly, our results demonstrate a significant and promising step towards making atomically resolved movies of molecular reactions.« less

Spatially resolved texture and microstructure evolution of additively manufactured and gas gun deformed 304L stainless steel investigated by neutron diffraction and electron backscatter diffraction

DOE PAGES

Takajo, Shigehiro; Brown, Donald William; Clausen, Bjorn; ...

2018-04-30

In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufacturing. The projectile was compressively deformed using a Taylor Anvil Gas Gun, leading to a huge strain gradient along the axis of the deformed cylinder. Spatially resolved neutron diffraction measurements on the HIgh Pressure Preferred Orientation time-of-flight diffractometer (HIPPO) and Spectrometer for Materials Research at Temperature and Stress diffractometer (SMARTS) beamlines at the Los Alamos Neutron Science CEnter (LANSCE) with Rietveld and single-peak analysis were used to quantitatively evaluate the volume fractions of the α, γ, and ε phases as well as residualmore » strain and texture. The texture of the γ phase is consistent with uniaxial compression, while the α texture can be explained by the Kurdjumov–Sachs relationship from the γ texture after deformation. This indicates that the material first deformed in the γ phase and subsequently transformed at larger strains. The ε phase was only found in volumes close to the undeformed material with a texture connected to the γ texture by the Shoji–Nishiyama orientation relationship. This allows us to conclude that the ε phase occurs as an intermediate phase at lower strain, and is superseded by the α phase when strain increases further. We found a proportionality between the root-mean-squared microstrain of the γ phase, dominated by the dislocation density, with the α volume fraction, consistent with strain-induced martensite α formation. In conclusion, knowledge of the sample volume with the ε phase from the neutron diffraction analysis allowed us to identify the ε phase by electron back scatter diffraction analysis, complementing the neutron diffraction analysis with characterization on the grain level.« less

Spatially resolved texture and microstructure evolution of additively manufactured and gas gun deformed 304L stainless steel investigated by neutron diffraction and electron backscatter diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takajo, Shigehiro; Brown, Donald William; Clausen, Bjorn

In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufacturing. The projectile was compressively deformed using a Taylor Anvil Gas Gun, leading to a huge strain gradient along the axis of the deformed cylinder. Spatially resolved neutron diffraction measurements on the HIgh Pressure Preferred Orientation time-of-flight diffractometer (HIPPO) and Spectrometer for Materials Research at Temperature and Stress diffractometer (SMARTS) beamlines at the Los Alamos Neutron Science CEnter (LANSCE) with Rietveld and single-peak analysis were used to quantitatively evaluate the volume fractions of the α, γ, and ε phases as well as residualmore » strain and texture. The texture of the γ phase is consistent with uniaxial compression, while the α texture can be explained by the Kurdjumov–Sachs relationship from the γ texture after deformation. This indicates that the material first deformed in the γ phase and subsequently transformed at larger strains. The ε phase was only found in volumes close to the undeformed material with a texture connected to the γ texture by the Shoji–Nishiyama orientation relationship. This allows us to conclude that the ε phase occurs as an intermediate phase at lower strain, and is superseded by the α phase when strain increases further. We found a proportionality between the root-mean-squared microstrain of the γ phase, dominated by the dislocation density, with the α volume fraction, consistent with strain-induced martensite α formation. In conclusion, knowledge of the sample volume with the ε phase from the neutron diffraction analysis allowed us to identify the ε phase by electron back scatter diffraction analysis, complementing the neutron diffraction analysis with characterization on the grain level.« less

Monitoring nonadiabatic avoided crossing dynamics in molecules by ultrafast X-ray diffraction

DOE PAGES

Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2017-05-26

We examine time-resolved X-ray diffraction from molecules in the gas phase which undergo nonadiabatic avoided-crossing dynamics involving strongly coupled electrons and nuclei. Several contributions to the signal are identified, representing (in decreasing strength) elastic scattering, contributions of the electronic coherences created by nonadiabatic couplings in the avoided crossing regime, and inelastic scattering. The former probes the charge density and delivers direct information on the evolving molecular geometry. The latter two contributions are weaker and carry spatial information through the transition charge densities (off-diagonal elements of the charge-density operator). Furthermore, simulations are presented for the nonadiabatic harpooning process in the excitedmore » state of sodium fluoride.« less

1-Methoxy-1-silacyclohexane: Synthesis, molecular structure and conformational behavior by gas electron diffraction, Raman spectroscopy and quantum chemical calculations

NASA Astrophysics Data System (ADS)

Shlykov, Sergey A.; Puchkov, Boris V.; Arnason, Ingvar; Wallevik, Sunna Ó.; Giricheva, Nina I.; Girichev, Georgiy V.; Zhabanov, Yuriy A.

2018-02-01

The synthesis and results of gas electron diffraction (GED), temperature-dependent Raman spectroscopy, along with detailed quantum chemical (QC) study of 1-methoxy-1-silacyclohexane 1 are reported. Within the series of the QC results, DFT(B3LYP, PBE0, M06, M062X), and MP2, the conformational preference predictions are rather contradictive. From the both GED and Raman experimental methods applied, the vapour and liquid phases of 1 were found to exist as a mixture of two conformers, gauche-axial and gauche-equatorial, with almost equal contributions, while the trans-forms are much less stable. In addition, theoretical calculations on the cyclohexane analog, methoxycyclohexane 2, are performed in order to compare with the conformational properties of 1. The latter is predicted not to diminish the axial/equatorial ratio, as contrasted to the expectations at switching the point of the substituent attachment from Si to C.

Tungsten-Doped TiO2 Nanolayers with Improved CO2 Gas Sensing Properties for Environmental Applications

NASA Astrophysics Data System (ADS)

Saberi, Maliheh; Ashkarran, Ali Akbar

Tungsten-doped TiO2 gas sensors were successfully synthesized using sol-gel process and spin coating technique. The fabricated sensor was characterized by field emission scanning electron microscopy (FE-SEM), ultraviolet visible (UV-Vis) spectroscopy, transmission electron microscopy (TEM), X-Ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Gas sensing properties of pristine and tungsten-doped TiO2 nanolayers (NLs) were probed by detection of CO2 gas. A series of experiments were conducted in order to find the optimum operating temperature of the prepared sensors and also the optimum value of tungsten concentration in TiO2 matrix. It was found that introducing tungsten into the TiO2 matrix enhanced the gas sensing performance. The maximum response was found to be (1.37) for 0.001g tungsten-doped TiO2 NLs at 200∘C as an optimum operating temperature.

High-Resolution Infrared and Electron-Diffraction Studies of Trimethylenecyclopropane ([3]-Radialene)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wright, Corey; Holmes, Joshua; Nibler, Joseph W.

2013-05-16

Combined high-resolution spectroscopic, electron-diffraction, and quantum theoretical methods are particularly advantageous for small molecules of high symmetry and can yield accurate structures that reveal subtle effects of electron delocalization on molecular bonds. The smallest of the radialene compounds, trimethylenecyclopropane, [3]-radialene, has been synthesized and examined in the gas phase by these methods. The first high-resolution infrared spectra have been obtained for this molecule of D3h symmetry, leading to an accurate B0 rotational constant value of 0.1378629(8) cm-1, within 0.5% of the value obtained from electronic structure calculations (density functional theory (DFT) B3LYP/cc-pVTZ). This result is employed in an analysis ofmore » electron-diffraction data to obtain the rz bond lengths (in Å): C-H = 1.072 (17), C-C = 1.437 (4), and C=C = 1.330 (4). The analysis does not lead to an accurate value of the HCH angle; however, from comparisons of theoretical and experimental angles for similar compounds, the theoretical prediction of 117.5° is believed to be reliable to within 2°. The effect of electron delocalization in radialene is to reduce the single C-C bond length by 0.07 Å compared to that in cyclopropane.« less

Molecular geometry of vanadium dichloride and vanadium trichloride: a gas-phase electron diffraction and computational study.

PubMed

Varga, Zoltán; Vest, Brian; Schwerdtfeger, Peter; Hargittai, Magdolna

2010-03-15

The molecular geometries of VCl2 and VCl3 have been determined by computations and gas-phase electron diffraction (ED). The ED study is a reinvestigation of the previously published analysis for VCl2. The structure of the vanadium dichloride dimer has also been calculated. According to our joint ED and computational study, the evaporation of a solid sample of VCl2 resulted in about 66% vanadium trichloride and 34% vanadium dichloride in the vapor. Vanadium dichloride is unambiguously linear in its 4Sigma(g)+ ground electronic state. For VCl3, all computations yielded a Jahn-Teller-distorted ground-state structure of C(2v) symmetry. However, it lies merely less than 3 kJ/mol lower than the 3E'' state (D(3h) symmetry). Due to the dynamic nature of the Jahn-Teller effect in this case, rigorous distinction cannot be made between the planar models of either D(3h) symmetry or C(2v) symmetry for the equilibrium structure of VCl3. Furthermore, the presence of several low-lying excited electronic states of VCl3 is expected in the high-temperature vapor. To our knowledge, this is the first experimental and computational study of the VCl3 molecule.

Structure and conformation of 1,4-difluorobutane as determined by gas-phase electron diffraction, and by molecular mechanics and ab initio calculations

NASA Astrophysics Data System (ADS)

Krosley, Kevin; Hagen, Kolbjørn; Hedberg, Kenneth

1995-06-01

Gas-phase electron diffraction data at 23°C together with molecular mechanics (MM3) and ab initio (HF/6-31G∗, gaussian 86) calculations have been used to determine the structure and conformations of 1,4-difluorobutane. The object was to ascertain whether effects similar to the gauche effect in 1,2-difluoroethane, which serves to stabilize the gauche form with the fluorine atoms in close proximity, could also operate in 1,4-difluorobutane. It was found both theoretically and experimentally that the proportion of those conformers having close fluorine atoms was small, implying the absence of effects similar to the gauche effect. The conformational composition estimated from the theoretical calculations is in good agreement with the experimental data. The experimental electron diffraction results constrained by assumptions drawn from the theoretical calculations, ED/MM3 [ED/ab initio], for the principal distances ( {r g}/{Å}) and angles ( {∠ α}/{deg}) with estimated 2σ uncertainties are as follows: r(CH) = 1.105(3) [1.106(3)], r(CF) = 1.398(2) [1.398(2)], r(C 1C 2) = 1.513(2) [1.516(2)], r(C 2C 3) = 1.537(2) [1.532(2)], ∠FCC = 110.9(3) [111.1(3)], ∠CCC = 112.9(4) [112.9(4)], and ∠HCH = 100(3) [100(3)].

Effect of annealing on Curie temperature and phase transition in La{sub 0.55}Sr{sub 0.08}Mn{sub 0.37}O{sub 3} epitaxial films grown on SrTiO{sub 3} (100) substrates by reactive radio frequency magnetron sputtering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ichinose, T.

2016-08-15

Mn-poor LaSrMnO{sub 3} (LSMO) epitaxial films were grown on SrTiO{sub 3} (100) substrates by radio frequency magnetron sputtering in an argon and oxygen gas mix, and then the samples were annealed in air at various temperatures (T{sub a}). 2 theta-chi X-ray diffraction mapping, nano-beam diffraction analysis through transmission electron microscopy, and electron back scatter diffraction through scanning electron microscopy revealed that the crystal symmetry of the LSMO films changed from monoclinic/orthorhombic to rhombohedral on annealing in air. Curie temperature (T{sub C}) of the LSMO films was found to increase with increasing T{sub a}, and become higher than the room temperaturemore » at T{sub a} ≥ 861 °C, indicating that the cause of these changes was the filling of oxygen and the transition of the crystal symmetry into rhombohedral. - Highlights: •Mn-poor LSMO changed from monoclinic/orthorhombic to rhombohedral by oxygen supply. •Mn-poor LSMO was increased T{sub C} by changed crystal symmetry, and it showed T{sub C} above RT. •Annealed in air effectively supplied O{sub 2} more than O{sub 2} gas during sputtering •EBSD is useful to evaluate crystal symmetry of complex oxide film from the substrate.« less

In-situ TEM on (de)hydrogenation of Pd at 0.5-4.5 bar hydrogen pressure and 20-400°C.

PubMed

Yokosawa, Tadahiro; Alan, Tuncay; Pandraud, Gregory; Dam, Bernard; Zandbergen, Henny

2012-01-01

We have developed a nanoreactor, sample holder and gas system for in-situ transmission electron microscopy (TEM) of hydrogen storage materials up to at least 4.5 bar. The MEMS-based nanoreactor has a microheater, two electron-transparent windows and a gas inlet and outlet. The holder contains various O-rings to have leak-tight connections with the nanoreactor. The system was tested with the (de)hydrogenation of Pd at pressures up to 4.5 bar. The Pd film consisted of islands being 15 nm thick and 50-500 nm wide. In electron diffraction mode we observed reproducibly a crystal lattice expansion and shrinkage owing to hydrogenation and dehydrogenation, respectively. In selected-area electron diffraction and bright/dark-field modes the (de)hydrogenation of individual Pd particles was followed. Some Pd islands are consistently hydrogenated faster than others. When thermally cycled, thermal hysteresis of about 10-16°C between hydrogen absorption and desorption was observed for hydrogen pressures of 0.5-4.5 bar. Experiments at 0.8 bar and 3.2 bar showed that the (de)hydrogenation temperature is not affected by the electron beam. This result shows that this is a fast method to investigate hydrogen storage materials with information at the nanometer scale. Copyright © 2011 Elsevier B.V. All rights reserved.

Vapor phase diamond growth technology

NASA Technical Reports Server (NTRS)

Angus, J. C.

1981-01-01

Ion beam deposition chambers used for carbon film generation were designed and constructed. Features of the developed equipment include: (1) carbon ion energies down to approx. 50 eV; (2) in suit surface monitoring with HEED; (3) provision for flooding the surface with ultraviolet radiation; (4) infrared laser heating of substrate; (5) residual gas monitoring; (6) provision for several source gases, including diborane for doping studies; and (7) growth from either hydrocarbon source gases or from carbon/argon arc sources. Various analytical techniques for characterization of from carbon/argon arc sources. Various analytical techniques for characterization of the ion deposited carbon films used to establish the nature of the chemical bonding and crystallographic structure of the films are discussed. These include: H2204/HN03 etch; resistance measurements; hardness tests; Fourier transform infrared spectroscopy; scanning auger microscopy; electron spectroscopy for chemical analysis; electron diffraction and energy dispersive X-ray analysis; electron energy loss spectroscopy; density measurements; secondary ion mass spectroscopy; high energy electron diffraction; and electron spin resonance. Results of the tests are summarized.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens.

PubMed

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10(-2) Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens

NASA Astrophysics Data System (ADS)

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10-2 Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Influence of nitrogen in the shielding gas on corrosion resistance of duplex stainless steel welds

NASA Astrophysics Data System (ADS)

Bhatt, R. B.; Kamat, H. S.; Ghosal, S. K.; de, P. K.

1999-10-01

The influence of nitrogen in shielding gas on the corrosion resistance of welds of a duplex stainless steel (grade U-50), obtained by gas tungsten arc (GTA) with filler wire, autogenous GTA (bead-on-plate), electron beam welding (EBW), and microplasma techniques, has been evaluated in chloride solutions at 30 °C. Pitting attack has been observed in GTA, electron beam welding, and microplasma welds when welding has been carried out using pure argon as the shielding gas. Gas tungsten arc welding with 5 to 10% nitrogen and 90 to 95% argon, as the shielding gas, has been found to result in an improved pitting corrosion resistance of the weldments of this steel. However, the resistance to pitting of autogenous welds (bead-on-plate) obtained in pure argon as the shielding gas has been observed to remain unaffected. Microscopic examination, electron probe microanalysis (EPMA), and x-ray diffraction studies have revealed that the presence of nitrogen in the shielding gas in the GTA welds not only modifies the microstructure and the austenite to ferrite ratio but also results in a nearly uniform distribution of the various alloying elements, for example, chromium, nickel, and molybdenum among the constitutent phases, which are responsible for improved resistance to pitting corrosion.

Influence of nitrogen in the shielding gas on corrosion resistance of duplex stainless steel welds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bhatt, R.B.; Kamat, H.S.; Ghosal, S.K.

1999-10-01

The influence of nitrogen in shielding gas on the corrosion resistance of welds of a duplex stainless steel (grade U-50), obtained by gas tungsten arc (GTA) with filler wire, autogenous GTA (bead-on-plate), electron beam welding (EBW), and microplasma techniques, has been evaluated in chloride solutions at 30 C. Pitting attack has been observed in GTA, electron beam welding, and microplasma welds when welding has been carried out using pure argon as the shielding gas. Gas tungsten arc welding with 5 to 10% nitrogen and 90 to 95% argon, as the shielding gas, has been found to result in an improvedmore » pitting corrosion resistance of the weldments of this steel. However, the resistance of pitting of autogenous welds (bead-on-plate) obtained in pure argon as the shielding gas has been observed to remain unaffected. Microscopic examination, electron probe microanalysis (EPMA), and x-ray diffraction studies have revealed that the presence of nitrogen in the shielding gas in the GTA welds not only modifies the microstructure and the austenite to ferrite ratio but also results in a nearly uniform distribution of the various alloying elements, for example, chromium, nickel, and molybdenum among the constituent phases, which are responsible for improved resistance to pitting corrosion.« less

Search for life on Mars: Evaluation of techniques

NASA Technical Reports Server (NTRS)

Schwartz, D. E.; Mancinelli, R. L.; White, M. R.

1995-01-01

An important question for exobiology is, did life evolve on Mars? To answer this question, experiments must be conducted on the martian surface. Given current mission constraints on mass, power, and volume, these experiments can only be performed using proposed analytical techniques such as: electron microscopy, X-ray fluorescence, X-ray diffraction, a-proton backscatter, g-ray spectrometry, differential thermal analysis, differential scanning calorimetry, pyrolysis gas chromatography, mass spectrometry, and specific element detectors. Using prepared test samples consisting of 1% organic matter (bovine serum albumin) in palagonite and a mixture of palagonite, clays, iron oxides, and evaporites, it was determined that a combination of X-ray diffraction and differential thermal analysis coupled with gas chromatography provides the best insight into the chemistry, mineralogy, and geological history of the samples.

Search for life on Mars: evaluation of techniques.

PubMed

Schwartz, D E; Mancinelli, R L; White, M R

1995-03-01

An important question for exobiology is, did life evolve on Mars? To answer this question, experiments must be conducted on the martian surface. Given current mission constraints on mass, power, and volume, these experiments can only be performed using proposed analytical techniques such as: electron microscopy, X-ray fluorescence, X-ray diffraction, alpha-proton backscatter, gamma-ray spectrometry, differential thermal analysis, differential scanning calorimetry, pyrolysis gas chromatography, mass spectrometry, and specific element detectors. Using prepared test samples consisting of 1% organic matter (bovine serum albumin) in palagonite and a mixture of palagonite, clays, iron oxides, and evaporites, it was determined that a combination of X-ray diffraction and differential thermal analysis coupled with gas chromatography provides the best insight into the chemistry, mineralogy, and geological history of the samples.

Structural characterization and gas reactions of small metal particles by high resolution in-situ TEM (Transmission Electron Microscopy) and TED (Transmission Electron Diffraction)

NASA Technical Reports Server (NTRS)

Heinemann, K.

1987-01-01

The detection and size analysis of small metal particles supported on amorphous substrates becomes increasingly difficult when the particle size approaches that of the phase contrast background structures of the support. An approach of digital image analysis, involving Fourier transformation of the original image, filtering, and image reconstruction was studied with respect to the likelihood of unambiguously detecting particles of less than 1 nm diameter on amorphous substrates from a single electron micrograph.

ZnO nanomaterials based surface acoustic wave ethanol gas sensor.

PubMed

Wu, Y; Li, X; Liu, J H; He, Y N; Yu, L M; Liu, W H

2012-08-01

ZnO nanomaterials based surface acoustic wave (SAW) gas sensor has been investigated in ethanol environment at room temperature. The ZnO nanomaterials have been prepared through thermal evaporation of high-purity zinc powder. The as-prepared ZnO nanomaterials have been characterized with scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray Diffraction (XRD) techniques. The results indicate that the obtained ZnO nanomaterials, including many types of nanostructures such as nanobelts, nanorods, nanowires as well as nanosheets, are wurtzite with hexagonal structure and well-crystallized. The SAW sensor coated with the nanostructured ZnO materials has been tested in ethanol gas of various concentrations at room temperature. A network analyzer is used to monitor the change of the insertion loss of the SAW sensor when exposed to ethanol gas. The insertion loss of the SAW sensor varies significantly with the change of ethanol concentration. The experimental results manifest that the ZnO nanomaterials based SAW ethanol gas sensor exhibits excellent sensitivity and good short-term reproducibility at room temperature.

Synthesis of porous SnO2 nanocubes via selective leaching and enhanced gas-sensing properties

NASA Astrophysics Data System (ADS)

Li, Yining; Wei, Qi; Song, Peng; Wang, Qi

2016-01-01

Porous micro-/nanostructures are of great interest in many current and emerging areas of technology. In this paper, porous SnO2 nanocubes have been successfully fabricated via a selective leaching strategy using CoSn(OH)6 as precursor. The structure and morphology of as-prepared samples were investigated by several techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric and differential scanning calorimeter analysis (TG⿿DSC), transmission electron microscopy (TEM) and N2 adsorption⿿desorption analyses. On the basis of those characterizations, the mechanism for the formation of porous SnO2 nanocubes has been proposed. Owing to the well-defined and uniform porous structures, porous SnO2 nanocubes possessing more adsorbent amount of analytic gas and accelerate the transmission speed so as to enhance the gas-sensing properties. Gas sensing investigation showed that the sensor based on porous SnO2 nanocubes exhibited high response, short response⿿recovery times and good selectivity to ethanol gas.

Relationship between H2 sorption properties and aqueous corrosion mechanisms in A2Ni7 hydride forming alloys (A = Y, Gd or Sm)

NASA Astrophysics Data System (ADS)

Charbonnier, Véronique; Monnier, Judith; Zhang, Junxian; Paul-Boncour, Valérie; Joiret, Suzanne; Puga, Beatriz; Goubault, Lionel; Bernard, Patrick; Latroche, Michel

2016-09-01

Intermetallic compounds A2B7 (A = rare earth, B = transition metal) are of interest for Ni-MH batteries. Indeed they are able to absorb hydrogen reversibly and exhibit good specific capacity in electrochemical route. To understand the effect of rare earth on properties of interest such as thermodynamic, cycling stability and corrosion, we synthesized and studied three compounds: Y2Ni7, Gd2Ni7 and Sm2Ni7. Using Sieverts' method, we plot P-c-isotherms up to 10 MPa and study hydride stability upon solid-gas cycling. Electrochemical cycling was also performed, as well as calendar and cycling corrosion study. Corrosion products were characterized by means of X-ray diffraction, electron diffraction, Raman micro-spectroscopy and scanning and transmission electron microscopies. Magnetic measurements were also performed to calculate corrosion rates. A corrosion mechanism, based on the nature of corrosion products, is proposed. By combining results from solid-gas cycling, electrochemical cycling and corrosion study, we attribute the loss in capacity either to corrosion or loss of crystallinity.

Isolation and reversible dimerization of a selenium-selenium three-electron σ-bond.

PubMed

Zhang, Senwang; Wang, Xingyong; Su, Yuanting; Qiu, Yunfan; Zhang, Zaichao; Wang, Xinping

2014-06-11

Three-electron σ-bonding that was proposed by Linus Pauling in 1931 has been recognized as important in intermediates encountered in many areas. A number of three-electron bonding systems have been spectroscopically investigated in the gas phase, solution and solid matrix. However, X-ray diffraction studies have only been possible on simple noble gas dimer Xe∴Xe and cyclic framework-constrained N∴N radical cations. Here, we show that a diselena species modified with a naphthalene scaffold can undergo one-electron oxidation using a large and weakly coordinating anion, to afford a room-temperature-stable radical cation containing a Se∴Se three-electron σ-bond. When a small anion is used, a reversible dimerization with phase and marked colour changes is observed: radical cation in solution (blue) but diamagnetic dimer in the solid state (brown). These findings suggest that more examples of three-electron σ-bonds may be stabilized and isolated by using naphthalene scaffolds together with large and weakly coordinating anions.

Highly Sensitive and Selective Hydrogen Gas Sensor Using the Mesoporous SnO₂ Modified Layers.

PubMed

Xue, Niuzi; Zhang, Qinyi; Zhang, Shunping; Zong, Pan; Yang, Feng

2017-10-14

It is important to improve the sensitivities and selectivities of metal oxide semiconductor (MOS) gas sensors when they are used to monitor the state of hydrogen in aerospace industry and electronic field. In this paper, the ordered mesoporous SnO₂ (m-SnO₂) powders were prepared by sol-gel method, and the morphology and structure were characterized by X-ray diffraction analysis (XRD), transmission electron microscope (TEM) and Brunauer-Emmett-Teller (BET). The gas sensors were fabricated using m-SnO₂ as the modified layers on the surface of commercial SnO₂ (c-SnO₂) by screen printing technology, and tested for gas sensing towards ethanol, benzene and hydrogen with operating temperatures ranging from 200 °C to 400 °C. Higher sensitivity was achieved by using the modified m-SnO₂ layers on the c-SnO₂ gas sensor, and it was found that the S(c/m2) sensor exhibited the highest response (Ra/Rg = 22.2) to 1000 ppm hydrogen at 400 °C. In this paper, the mechanism of the sensitivity and selectivity improvement of the gas sensors is also discussed.

Crystal growth of carbonate apatite using a CaCO3 flux.

PubMed

Suetsugu, Y; Tanaka, J

1999-09-01

Single crystals of carbonate apatite were grown using a CaCO3 flux under an Ar gas pressure of 55 MPa. The crystals obtained were observed by scanning electron microscopy, optical microscopy and X-ray diffraction. Electron probe microanalyses and thermal analyses were performed. CO3 ions in planar triangle form replaced both OH sites and PO4 tetrahedral sites in the apatite structure: in particular, the OH sites were perfectly substituted by CO3 ions using this method.

Diffraction of a plane wave on two-dimensional conductive structures and a surface wave

NASA Astrophysics Data System (ADS)

Davidovich, Mikhael V.

2018-04-01

We consider the structures type of two-dimensional electron gas in the form of a thin conductive, in particular, graphene films described by tensor conductivity, which are isolated or located on the dielectric layers. The dispersion equation for hybrid modes, as well as scattering parameters. We show that free wave (eigenwaves) problem follow from the problem of diffraction when linking the amplitude of the current of the linear equations are unsolvable, i.e., the determinant of this system is zero. As a particular case the dispersion equation follow from the conditions of matching (with zero reflection coefficient).

Gas Sensing Properties of ZnO-SnO2 Nanostructures.

PubMed

Chen, Weigen; Li, Qianzhu; Xu, Lingna; Zeng, Wen

2015-02-01

One-dimensional (1D) semiconductor metal oxide nanostructures have attracted increasing attention in electrochemistry, optics, magnetic, and gas sensing fields for the good properties. N-type low dimensional semiconducting oxides such as SnO2 and ZnO have been known for the detection of inflammable or toxic gases. In this paper, we fabricated the ZnO-SnO2 and SnO2 nanoparticles by hydrothermal synthesis. Microstructure characterization was performed using X-ray diffraction (XRD) and surface morphologies for both the pristine and doped samples were observed using field emission scanning electron microscope (FESEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). Then we made thin film gas sensor to study the gas sensing properties of ZnO-SnO2 and SnO2 gas sensor to H2 and CO. A systematic comparison study reveals an enhanced gas sensing performance for the sensor made of SnO2 and ZnO toward H2 and CO over that of the commonly applied undecorated SnO2 nanoparticles. The improved gas sensing properties are attributed to the size of grains and pronounced electron transfer between the compound nanostructures and the absorbed oxygen species as well as to the heterojunctions of the ZnO nanoparticles to the SnO2 nanoparticles, which provide additional reaction rooms. The results represent an advance of compound nanostructures in further enhancing the functionality of gas sensors, and this facile method could be applicable to many sensing materials, offering a new avenue and direction to detect gases of interest based on composite tin oxide nanoparticles.

Highly Sensitive NiO Nanoparticle based Chlorine Gas Sensor

NASA Astrophysics Data System (ADS)

Arif, Mohd.; Sanger, Amit; Singh, Arun

2018-03-01

We have synthesized a chemiresistive sensor for chlorine (Cl2) gas in the range of 2-200 ppm based on nickel oxide (NiO) nanoparticles obtained by wet chemical synthesis. The nanoparticles were characterized by x-ray diffraction (XRD) analysis, field-emission scanning electron microscopy (FE-SEM), thermogravimetric analysis (TGA), transmission electron microscopy (TEM), Fourier-transform infrared (FTIR) spectroscopy, Raman spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy, and photoluminescence (PL) spectroscopy. XRD spectra of the sensing layer revealed the cubic phase of NiO nanoparticles. The NiO nanoparticle size was calculated to be ˜ 21 nm using a Williamson-Hall plot. The bandgap of the NiO nanoparticles was found to be 3.13 eV using Tauc plots of the absorbance curve. Fast response time (12 s) and optimum recovery time (˜ 27 s) were observed for 10 ppm Cl2 gas at moderate temperature of 200°C. These results demonstrate the potential application of NiO nanoparticles for fabrication of highly sensitive and selective sensors for Cl2 gas.

Carbon Nanotubes, Nanocrystal Forms, and Complex Nanoparticle Aggregates in common fuel-gas combustion sources and the ambient air

NASA Astrophysics Data System (ADS)

Murr, L. E.; Bang, J. J.; Esquivel, E. V.; Guerrero, P. A.; Lopez, D. A.

2004-06-01

Aggregated multiwall carbon nanotubes (with diameters ranging from ˜3 to 30nm) and related carbon nanocrystal forms ranging in size from 0.4 to 2 μm (average diameter) have been collected in the combustion streams for methane/air, natural gas/air, and propane gas/air flames using a thermal precipitator. Individual particle aggregates were collected on carbon/formvar-coated 3mm nickel grids and examined in a transmission electron microscope, utilizing bright-field imaging, selected-area electron diffraction analysis, and energy-dispersive X-ray spectrometry techniques. The natural gas and propane gas sources were domestic (kitchen) stoves, and similar particle aggregates collected in the outdoor air were correspondingly identified as carbon nanocrystal aggregates and sometimes more complex aggregates of silica nanocrystals intermixed with the carbon nanotubes and other carbon nanocrystals. Finally, and in light of the potential for methane-series gas burning as major sources of carbon nanocrystal aggregates in both the indoor and outdoor air, data for natural gas consumption and corresponding asthma deaths and incidence are examined with a degree of speculation regarding any significance in the correlations.

Thermal alteration of young kerogen in relation to petroleum genesis

NASA Technical Reports Server (NTRS)

Ishiwatari, R.; Ishiwatari, M.; Kaplan, I. R.; Rohrback, B. G.

1976-01-01

Kerogen, humic acid, and lipid material were separated from a young marine sediment and heated in sealed tubes in a nitrogen atmosphere at 150 and 410 C. Gaseous and liquid products generated during heating, and also the residual organic material, were characterized by gas-liquid chromatography, elemental analysis, infrared and electron spin resonance spectroscopy, and X-ray diffraction.

Microstructures of GaN1-xPx layers grown on (0001) GaN substrates by gas source molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Seong, Tae-Yeon; Bae, In-Tae; Choi, Chel-Jong; Noh, D. Y.; Zhao, Y.; Tu, C. W.

1999-03-01

Transmission electron microscope (TEM), transmission electron diffraction (TED), and synchrotron x-ray diffraction (XRD) studies have been performed to investigate microstructural behavior of gas source molecular beam epitaxial GaN1-xPx layers grown on (0001) GaN/sapphire at temperatures (Tg) in the range 500-760 °C. TEM, TED, and XRD results indicate that the samples grown at Tg⩽600 °C undergo phase separation resulting in a mixture of GaN-rich and GaP-rich GaNP with zinc-blende structure. However, the samples grown at Tg⩾730 °C are found to be binary zinc-blende GaN(P) single crystalline materials. As for the 500 °C layer, the two phases are randomly oriented and distributed, whereas the 600 °C layer consists of phases that are elongated and inclined by 60°-70° clockwise from the [0001]α-GaN direction. The samples grown at Tg⩾730 °C are found to consist of two types of microdomains, namely, GaN(P)I and GaN(P)II; the former having twin relation to the latter.

Gas-sensing performances of Cd-doped ZnO nanoparticles synthesized by a surfactant-mediated method for n-butanol gas

NASA Astrophysics Data System (ADS)

Zhao, Rongjun; Li, Kejin; Wang, Zhezhe; Xing, Xinxin; Wang, Yude

2018-01-01

Zinc oxide nanoparticles with the different Cd doping contents were prepared by with a surfactant-mediated method in this paper. The effects of Cd doping on the gas sensing properties of the ZnO nanoparticles were studied. The morphology and microstructure of as-prepared samples were characterized by X-ray diffraction (XRD); scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution TEM (HRTEM), respectively. The results reveal that all the products are the high crystalline hexagonal wurtzite ZnO crystal structure. The gas-sensing characteristics of the Cd doped ZnO nanoparticles for volatile organic compounds (VOCs) were investigated. At its optimal operation temperature of 300 °C, the sensing properties of the Cd doped ZnO nanoparticles for n-butanol gas exhibit a high-performance gas sensing performances including high gas response, good selectivity, response/recovery time, and repeatability as well as stability. Especially, its response reaches 130 for 100 ppm n-butanol of ZnO nanoparticles with 2.5% Cd doping. Those values demonstrate the potential of using as-prepared Cd doped ZnO nanoparticles for n-butanol gas detection, making them to be promising candidates for practical detectors to n-butanol gas. Apart from these, the mechanism related to the advanced properties was also investigated and presented.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ito, Yuta; Wang, Chuncheng; Le, Anh-Thu

Here, we have measured the angular distributions of high energy photoelectrons of benzene molecules generated by intense infrared femtosecond laser pulses. These electrons arise from the elastic collisions between the benzene ions with the previously tunnel-ionized electrons that have been driven back by the laser field. Theory shows that laser-free elastic differential cross sections (DCSs) can be extracted from these photoelectrons, and the DCS can be used to retrieve the bond lengths of gas-phase molecules similar to the conventional electron diffraction method. From our experimental results, we have obtained the C-C and C-H bond lengths of benzene with a spatialmore » resolution of about 10 pm. Our results demonstrate that laser induced electron diffraction (LIED) experiments can be carried out with the present-day ultrafast intense lasers already. Looking ahead, with aligned or oriented molecules, more complete spatial information of the molecule can be obtained from LIED, and applying LIED to probe photo-excited molecules, a “molecular movie” of the dynamic system may be created with sub-A°ngstrom spatial and few-ten femtosecond temporal resolutions.« less

Porous Si nanowires for highly selective room-temperature NO2 gas sensing

NASA Astrophysics Data System (ADS)

Kwon, Yong Jung; Mirzaei, Ali; Gil Na, Han; Kang, Sung Yong; Choi, Myung Sik; Bang, Jae Hoon; Oum, Wansik; Kim, Sang Sub; Kim, Hyoun Woo

2018-07-01

We report the room-temperature sensing characteristics of Si nanowires (NWs) fabricated from p-Si wafers by a metal-assisted chemical etching method, which is a facile and low-cost method. X-ray diffraction was used to the the study crystallinity and phase formation of Si NWs, and product morphology was examined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). After confirmation of Si NW formation via the SEM and TEM micrographs, sensing tests were carried out at room temperature, and it was found that the Si NW sensor prepared from Si wafers with a resistivity of 0.001–0.003 Ω.cm had the highest response to NO2 gas (Rg/Ra = 1.86 for 50 ppm NO2), with a fast response (15 s) and recovery (30 s) time. Furthermore, the sensor responses to SO2, toluene, benzene, H2, and ethanol were nearly negligible, demonstrating the excellent selectivity to NO2 gas. The gas-sensing mechanism is discussed in detail. The present sensor can operate at room temperature, and is compatible with the microelectronic fabrication process, demonstrating its promise for next-generation Si-based electronics fused with functional chemical sensors.

Gas Sensors Based on Tin Oxide Nanoparticles Synthesized from a Mini-Arc Plasma Source

DOE PAGES

Lu, Ganhua; Huebner, Kyle L.; Ocola, Leonidas E.; ...

2006-01-01

Minimore » aturized gas sensors or electronic noses to rapidly detect and differentiate trace amount of chemical agents are extremely attractive. In this paper, we report on the fabrication and characterization of a functional tin oxide nanoparticle gas sensor. Tin oxide nanoparticles are first synthesized using a convenient and low-cost mini-arc plasma source. The nanoparticle size distribution is measured online using a scanning electrical mobility spectrometer (SEMS). The product nanoparticles are analyzed ex-situ by high resolution transmission electron microscopy (HRTEM) for morphology and defects, energy dispersive X-ray (EDX) spectroscopy for elemental composition, electron diffraction for crystal structure, and X-ray photoelectron spectroscopy (XPS) for surface composition. Nonagglomerated rutile tin oxide ( SnO 2 ) nanoparticles as small as a few nm have been produced. Larger particles bear a core-shell structure with a metallic core and an oxide shell. The nanoparticles are then assembled onto an e-beam lithographically patterned interdigitated electrode using electrostatic force to fabricate the gas sensor. The nanoparticle sensor exhibits a fast response and a good sensitivity when exposed to 100 ppm ethanol vapor in air.« less

Porous Si nanowires for highly selective room-temperature NO2 gas sensing.

PubMed

Kwon, Yong Jung; Mirzaei, Ali; Na, Han Gil; Kang, Sung Yong; Choi, Myung Sik; Bang, Jae Hoon; Oum, Wansik; Kim, Sang Sub; Kim, Hyoun Woo

2018-07-20

We report the room-temperature sensing characteristics of Si nanowires (NWs) fabricated from p-Si wafers by a metal-assisted chemical etching method, which is a facile and low-cost method. X-ray diffraction was used to the the study crystallinity and phase formation of Si NWs, and product morphology was examined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). After confirmation of Si NW formation via the SEM and TEM micrographs, sensing tests were carried out at room temperature, and it was found that the Si NW sensor prepared from Si wafers with a resistivity of 0.001-0.003 Ω.cm had the highest response to NO 2 gas (R g /R a  = 1.86 for 50 ppm NO 2 ), with a fast response (15 s) and recovery (30 s) time. Furthermore, the sensor responses to SO 2 , toluene, benzene, H 2 , and ethanol were nearly negligible, demonstrating the excellent selectivity to NO 2 gas. The gas-sensing mechanism is discussed in detail. The present sensor can operate at room temperature, and is compatible with the microelectronic fabrication process, demonstrating its promise for next-generation Si-based electronics fused with functional chemical sensors.

Successful Cleaning and Study of Contamination of Si(001) in Ultrahigh Vacuum

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gheorghe, N. G.; Lungu, G. A.; Husanu, M. A.

2011-10-03

This paper presents the very first surface physics experiment performed in ultrahigh vacuum (UHV) in Romania, using a new molecular beam epitaxy (MBE) installation. Cleaning of a Si(001) wafer was achieved by using a very simple technique: sequences of annealing at 900-1000 deg. C in ultrahigh vacuum: low 10{sup -8} mbar, with a base pressure of 1.5x10{sup -10} mbar. The preparation procedure is quite reproducible and allows repeated cleaning of the Si(001) after contamination in ultrahigh vacuum. The Si(001) single crystal surface is characterized by low energy electron diffraction (LEED), reflection high energy electron diffraction (RHEED), and Auger electron spectroscopymore » (AES). The latter technique is utilized in order to investigate the sample contamination by the residual gas in the UHV chamber, as determined by a residual gas analyzer (RGA). Unambiguous assignment of oxidized and unoxidized silicon is provided; also, an important feature is that the LVV Auger peak at 90-92 eV cannot be solely attributed to clean Si (i.e. Si surrounded only by Si), but also to silicon atoms bounded with carbon. Even with a sum of partial pressures of oxygen and carbon containing molecules in the range of 5x10{sup -10} mbar, the sample is contaminated very quickly, having a (1/e) lifetime of about 76 minutes.« less

Low-pressure clathrate-hydrate formation in amorphous astrophysical ice analogs

NASA Technical Reports Server (NTRS)

Blake, D. F.; Allamandola, L. J.; Sandford, S.; Hudgins, D.; Freund, F.

1991-01-01

In modeling cometary ice, the properties of clathrate hydrates were used to explain anomalous gas release at large radial distances from the Sun, and the retention of particular gas inventories at elevated temperatures. Clathrates may also have been important early in solar system history. However, there has never been a reasonable mechanism proposed for clathrate formation under the low pressures typical of these environments. For the first time, it was shown that clathrate hydrates can be formed by warming and annealing amorphous mixed molecular ices at low pressures. The complex microstructures which occur as a result of clathrate formation from the solid state may provide an explanation for a variety of unexplained phenomena. The vacuum and imaging systems of an Hitachi H-500H Analytical Electron Microscope was modified to study mixed molecular ices at temperatures between 12 and 373 K. The resulting ices are characterized by low-electron dose Transmission Electron Microscopy (TEM) and Selected Area Electron Diffraction (SAED). The implications of these results for the mechanical and gas release properties of comets are discussed. Laboratory IR data from similar ices are presented which suggest the possibility of remotely observing and identifying clathrates in astrophysical objects.

Highly Sensitive and Selective Hydrogen Gas Sensor Using the Mesoporous SnO2 Modified Layers

PubMed Central

Xue, Niuzi; Zhang, Qinyi; Zhang, Shunping; Zong, Pan; Yang, Feng

2017-01-01

It is important to improve the sensitivities and selectivities of metal oxide semiconductor (MOS) gas sensors when they are used to monitor the state of hydrogen in aerospace industry and electronic field. In this paper, the ordered mesoporous SnO2 (m-SnO2) powders were prepared by sol-gel method, and the morphology and structure were characterized by X-ray diffraction analysis (XRD), transmission electron microscope (TEM) and Brunauer–Emmett–Teller (BET). The gas sensors were fabricated using m-SnO2 as the modified layers on the surface of commercial SnO2 (c-SnO2) by screen printing technology, and tested for gas sensing towards ethanol, benzene and hydrogen with operating temperatures ranging from 200 °C to 400 °C. Higher sensitivity was achieved by using the modified m-SnO2 layers on the c-SnO2 gas sensor, and it was found that the S(c/m2) sensor exhibited the highest response (Ra/Rg = 22.2) to 1000 ppm hydrogen at 400 °C. In this paper, the mechanism of the sensitivity and selectivity improvement of the gas sensors is also discussed. PMID:29036898

a Facile Synthesis of Fully Porous Tazo Composite and its Remarkable Gas Sensitive Performance

NASA Astrophysics Data System (ADS)

Liang, Dongdong; Liu, Shimin; Wang, Zhinuo; Guo, Yu; Jiang, Weiwei; Liu, Chaoqian; Ding, Wanyu; Wang, Hualin; Wang, Nan; Zhang, Zhihua

The composite of a nanocrystalline SnO2 thick film deposited on an Al-doped ZnO ceramic substrate was firstly proposed. This study also provided a simple, fast and cost effective method to prepare SnO2 thick film and Al-doped ZnO ceramic as well as the final composite. The crystal structure, morphology, composition, pore size distribution and gas sensitivity of the composite were investigated by means of X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, Barrett-Joyner-Halenda analysis and gas sensitive measurement system. Results indicated that the composite was fully porous consisted of SnO2, ZnO and ZnAl2O4 crystal phases. The macrosized pores generated in the composite could enhance the gas infiltration into the sensing layers effectively. In this way, combining a high gas-transporting-capability and a nanocrystalline SnO2 thick film, the composite showed very impressive performance. The gas sensitivity of the composite was high enough for ethanol vapor with different concentrations, which was comparable to other kinds of reported SnO2 gas sensors, while showing two straight lines with a turning point at 1000ppm. Finally, the gas sensitive mechanism was proposed based on the microstructure and composition of the composite.

Structure determination of molecules in an alignment laser field by femtosecond photoelectron diffraction using an X-ray free-electron laser

PubMed Central

Minemoto, Shinichirou; Teramoto, Takahiro; Akagi, Hiroshi; Fujikawa, Takashi; Majima, Takuya; Nakajima, Kyo; Niki, Kaori; Owada, Shigeki; Sakai, Hirofumi; Togashi, Tadashi; Tono, Kensuke; Tsuru, Shota; Wada, Ken; Yabashi, Makina; Yoshida, Shintaro; Yagishita, Akira

2016-01-01

We have successfully determined the internuclear distance of I2 molecules in an alignment laser field by applying our molecular structure determination methodology to an I 2p X-ray photoelectron diffraction profile observed with femtosecond X-ray free electron laser pulses. Using this methodology, we have found that the internuclear distance of the sample I2 molecules in an alignment Nd:YAG laser field of 6 × 1011 W/cm2 is elongated by from 0.18 to 0.30 Å “in average” relatively to the equilibrium internuclear distance of 2.666 Å. Thus, the present experiment constitutes a critical step towards the goal of femtosecond imaging of chemical reactions and opens a new direction for the study of ultrafast chemical reaction in the gas phase. PMID:27934891

Imaging CF3I conical intersection and photodissociation dynamics by ultrafast electron diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Jie

Conical intersections play a critical role in excited state dynamics of polyatomic molecules, as they govern the reaction pathways of many nonadiabatic processes. However, ultrafast probes have lacked sufficient spatial resolution to image wavepacket trajectories through these intersections directly. Here we present the simultaneous experimental characterization of one-photon and two-photon excitation channels in isolated CF3I molecules using ultrafast gas phase electron diffraction. In the two-photon channel, we have mapped out the real space trajectories of a coherent nuclear wavepacket, which bifurcates onto two potential energy surfaces when passing through a conical intersection. In the one-photon channel, we have resolved excitationmore » of both the umbrella and the breathing vibrational modes in the CF3 fragment in multiple nuclear dimensions. These findings benchmark and validate ab-initio nonadiabatic dynamics calculations.« less

Acetone Sensing Properties of a Gas Sensor Composed of Carbon Nanotubes Doped With Iron Oxide Nanopowder

PubMed Central

Tan, Qiulin; Fang, Jiahua; Liu, Wenyi; Xiong, Jijun; Zhang, Wendong

2015-01-01

Iron oxide (Fe2O3) nanopowder was prepared by a precipitation method and then mixed with different proportions of carbon nanotubes. The composite materials were characterized by X-ray powder diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy. A fabricated heater-type gas sensor was compared with a pure Fe2O3 gas sensor under the influence of acetone. The effects of the amount of doping, the sintering temperature, and the operating temperature on the response of the sensor and the response recovery time were analyzed. Experiments show that doping of carbon nanotubes with iron oxide effectively improves the response of the resulting gas sensors to acetone gas. It also reduces the operating temperature and shortens the response recovery time of the sensor. The response of the sensor in an acetone gas concentration of 80 ppm was enhanced, with good repeatability. PMID:26569253

Acetone Sensing Properties of a Gas Sensor Composed of Carbon Nanotubes Doped With Iron Oxide Nanopowder.

PubMed

Tan, Qiulin; Fang, Jiahua; Liu, Wenyi; Xiong, Jijun; Zhang, Wendong

2015-11-11

Iron oxide (Fe₂O₃) nanopowder was prepared by a precipitation method and then mixed with different proportions of carbon nanotubes. The composite materials were characterized by X-ray powder diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy. A fabricated heater-type gas sensor was compared with a pure Fe₂O₃ gas sensor under the influence of acetone. The effects of the amount of doping, the sintering temperature, and the operating temperature on the response of the sensor and the response recovery time were analyzed. Experiments show that doping of carbon nanotubes with iron oxide effectively improves the response of the resulting gas sensors to acetone gas. It also reduces the operating temperature and shortens the response recovery time of the sensor. The response of the sensor in an acetone gas concentration of 80 ppm was enhanced, with good repeatability.

One-Dimensional Photonic Crystal Superprisms

NASA Technical Reports Server (NTRS)

Ting, David

2005-01-01

Theoretical calculations indicate that it should be possible for one-dimensional (1D) photonic crystals (see figure) to exhibit giant dispersions known as the superprism effect. Previously, three-dimensional (3D) photonic crystal superprisms have demonstrated strong wavelength dispersion - about 500 times that of conventional prisms and diffraction gratings. Unlike diffraction gratings, superprisms do not exhibit zero-order transmission or higher-order diffraction, thereby eliminating cross-talk problems. However, the fabrication of these 3D photonic crystals requires complex electron-beam substrate patterning and multilayer thin-film sputtering processes. The proposed 1D superprism is much simpler in structural complexity and, therefore, easier to design and fabricate. Like their 3D counterparts, the 1D superprisms can exhibit giant dispersions over small spectral bands that can be tailored by judicious structure design and tuned by varying incident beam direction. Potential applications include miniature gas-sensing devices.

Enhancement of photoluminescence intensity of GaAs with cubic GaS chemical vapor deposited using a structurally designed single-source precursor

NASA Technical Reports Server (NTRS)

Macinnes, Andrew N.; Power, Michael B.; Barron, Andrew R.; Jenkins, Phillip P.; Hepp, Aloysius F.

1993-01-01

A two order-of-magnitude enhancement of photoluminescence intensity relative to untreated GaAs has been observed for GaAs surfaces coated with chemical vapor-deposited GaS. The increase in photoluminescence intensity can be viewed as an effective reduction in surface recombination velocity and/or band bending. The gallium cluster /(t-Bu)GaS/4 was used as a single-source precursor for the deposition of GaS thin films. The cubane core of the structurally characterized precursor is retained in the deposited film producing a cubic phase. Furthermore, a near-epitaxial growth is observed for the GaS passivating layer. Films were characterized by transmission electron microscopy, X-ray powder diffraction, and X-ray photoelectron and Rutherford backscattering spectroscopies.

Photoluminescence intensity enhancement of GaAs by vapor-deposited GaS - A rational approach to surface passivation

NASA Technical Reports Server (NTRS)

Jenkins, Phillip P.; Hepp, Aloysius F.; Power, Michael B.; Macinnes, Andrew N.; Barron, Andrew R.

1993-01-01

A two order-of-magnitude enhancement of photoluminescence intensity relative to untreated GaAs has been observed for GaAs surfaces coated with chemical vapor-deposited GaS. The increase in photoluminescence intensity can be viewed as an effective reduction in surface recombination velocity and/or band bending. The gallium cluster (/t-Bu/GaS)4 was used as a single-source precursor for the deposition of GaS thin films. The cubane core of the structurally-characterized precursor is retained in the deposited film producing a cubic phase. Furthermore, a near-epitaxial growth is observed for the GaS passivating layer. Films were characterized by transmission electron microscopy, X-ray powder diffraction, and X-ray photoelectron and Rutherford backscattering spectroscopies.

A simple large-scale synthesis of mesoporous In2O3 for gas sensing applications

NASA Astrophysics Data System (ADS)

Zhang, Su; Song, Peng; Yan, Huihui; Yang, Zhongxi; Wang, Qi

2016-08-01

In this paper, large-scale mesoporous In2O3 nanostructures were synthesized by a facile Lewis acid catalytic the furfural alcohol resin (FAR) template route for the high-yield. Their morphology and structure were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal and thermogravimetry analysis (DSC-TG) and the Brunauer-Emmett-Teller (BET) approach. The as-obtained mesoporous In2O3 nanostructures possess excellent mesoporous and network structure, which increases the contact area with the gases, it is conducive for adsorption-desorption of gas on the surface of In2O3. The In2O3 particles and pores were both about 15 nm and very uniform. In gas-sensing measurements with target gases, the gas sensor based on mesoporous In2O3 nanostructures showed a good response, short response-recovery time, good selectivity and stability to ethanol. These properties are due to the large specific surface area of mesoporous structure. This synthetic method could use as a new design concept for functional mesoporous nanomaterials and for mass production.

A Comparative Study of Chemically and Biologically Synthesized MgO Nanomaterial for Liquefied Petroleum Gas Detection

NASA Astrophysics Data System (ADS)

Thirupathi, Rampelly; Solleti, Goutham; Sreekanth, Tirumala; Sadasivuni, Kishor Kumar; Venkateswara Rao, Kalagadda

2018-03-01

The exceptional chemical and physical properties of nanostructured materials are extremely suitable for designing new and enhanced sensing devices, particularly gas sensors and biosensors. The present work describes the synthesis of magnesium oxide (MgO) nanoparticles through two methods: a green synthesis using aloe vera plant extract and a chemical method using a glycine-based solution combustion route. In a single step, the extracted organic molecules from aloe vera plants were used to reduce metal ions by the green method. MgO nanoparticles were coated onto the interdigital electrode using the drop-drying method. The dynamic gas-sensing characteristics were measured for liquefied petroleum gas (LPG) at different concentrations and various temperatures. The MgO nanoparticles were characterized by using x-ray diffraction, field emission scanning electron microscopy, and high-resolution transmission electron microscopy to determine the size and structure of the particles. The product's functional properties were analyzed by Fourier transform-infrared spectroscopy and UV-visible spectroscopy. We found that the LPG sensing behavior of biologically synthesized MgO registers excellent sensitivity at various operating temperatures.

A Comparative Study of Chemically and Biologically Synthesized MgO Nanomaterial for Liquefied Petroleum Gas Detection

NASA Astrophysics Data System (ADS)

Thirupathi, Rampelly; Solleti, Goutham; Sreekanth, Tirumala; Sadasivuni, Kishor Kumar; Venkateswara Rao, Kalagadda

2018-07-01

The exceptional chemical and physical properties of nanostructured materials are extremely suitable for designing new and enhanced sensing devices, particularly gas sensors and biosensors. The present work describes the synthesis of magnesium oxide (MgO) nanoparticles through two methods: a green synthesis using aloe vera plant extract and a chemical method using a glycine-based solution combustion route. In a single step, the extracted organic molecules from aloe vera plants were used to reduce metal ions by the green method. MgO nanoparticles were coated onto the interdigital electrode using the drop-drying method. The dynamic gas-sensing characteristics were measured for liquefied petroleum gas (LPG) at different concentrations and various temperatures. The MgO nanoparticles were characterized by using x-ray diffraction, field emission scanning electron microscopy, and high-resolution transmission electron microscopy to determine the size and structure of the particles. The product's functional properties were analyzed by Fourier transform-infrared spectroscopy and UV-visible spectroscopy. We found that the LPG sensing behavior of biologically synthesized MgO registers excellent sensitivity at various operating temperatures.

A highly sensitive room temperature H2S gas sensor based on SnO2 multi-tube arrays bio-templated from insect bristles.

PubMed

Tian, Junlong; Pan, Feng; Xue, Ruiyang; Zhang, Wang; Fang, Xiaotian; Liu, Qinglei; Wang, Yuhua; Zhang, Zhijian; Zhang, Di

2015-05-07

A tin oxide multi-tube array (SMTA) with a parallel effect was fabricated through a simple and promising method combining chemosynthesis and biomimetic techniques; a biomimetic template was derived from the bristles on the wings of the Alpine Black Swallowtail butterfly (Papilio maackii). SnO2 tubes are hollow and porous structures with micro-pores regularly distributed on the wall. The morphology, the delicate microstructure and the crystal structure of this SMTA were characterized by super resolution digital microscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The SMTA exhibits a high sensitivity to H2S gas at room temperature. It also exhibits a short response/recovery time, with an average value of 14/30 s at 5 ppm. In particular, heating is not required for the SMTA in the gas sensitivity measurement process. On the basis of these results, SMTA is proposed as a suitable new material for the design and fabrication of room-temperature H2S gas sensors.

Nanostructured tin oxide films: Physical synthesis, characterization, and gas sensing properties.

PubMed

Ingole, S M; Navale, S T; Navale, Y H; Bandgar, D K; Stadler, F J; Mane, R S; Ramgir, N S; Gupta, S K; Aswal, D K; Patil, V B

2017-05-01

Nanostructured tin oxide (SnO 2 ) films are synthesized using physical method i.e. thermal evaporation and are further characterized with X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, and atomic force microscopy measurement techniques for confirming its structure and morphology. The chemiresistive properties of SnO 2 films are studied towards different oxidizing and reducing gases where these films have demonstrated considerable selectivity towards oxidizing nitrogen dioxide (NO 2 ) gas with a maximum response of 403% to 100ppm @200°C, and fast response and recovery times of 4s and 210s, respectively, than other test gases. In addition, SnO 2 films are enabling to detect as low as 1ppm NO 2 gas concentration @200°C with 23% response enhancement. Chemiresistive performances of SnO 2 films are carried out in the range of 1-100ppm and reported. Finally, plausible adsorption and desorption reaction mechanism of NO 2 gas molecules with SnO 2 film surface has been thoroughly discussed by means of an impedance spectroscopy analysis. Copyright © 2017 Elsevier Inc. All rights reserved.

Multi-applicative tetragonal TiO2/SnO2 nanocomposites for photocatalysis and gas sensing

NASA Astrophysics Data System (ADS)

Patil, S. M.; Dhodamani, A. G.; Vanalakar, S. A.; Deshmukh, S. P.; Delekar, S. D.

2018-04-01

TiO2-based mixed metal oxide heteronanostructures have multiple applications in photocatalysis and gas sensing because of their charge transport properties. In this study, we prepared tetragonal TiO2/SnO2 nanocomposites (NCs) with different weight percentages using a simple wet impregnation method. The physicochemical properties of the NCs were investigated using X-ray diffraction, Fourier transform-infrared spectroscopy, ultraviolet-visible spectroscopy, field-emission scanning electron microscopy, energy dispersive X-ray spectroscopy, transmission electron microscopy, and Brunauer-Emmett-Teller surface area analysis. The results showed that the surface area of the NCs increased significantly and the anatase TiO2 was sensitized after the addition of a small amount of cassiterite SnO2 NPs. We systematically studied the as-prepared NCs during the photocatalytic degradation of Congo Red dye under visible light irradiation (λ > 420 nm) and NH3 gas sensing, which demonstrated the efficient photocatalytic performance and the superior sensing response of the catalyst with a weight composition of 25% SnO2 in TiO2 (4:1) compared with the other NCs or the bare individual nanoparticles. The improved photocatalytic and gas sensing performance of the TiO2/SnO2 (4:1) NCs may be attributed to the increased active surface area, the increased adsorption of the dye and target gas molecules, as well as efficient electron-hole charge separation and transfer.

In situ etching WO{sub 3} nanoplates: Hydrothermal synthesis, photoluminescence and gas sensor properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Su, Xintai, E-mail: suxintai827@163.com; Li, Yani; Jian, Jikang

2010-12-15

A novel hydrothermal process using p-nitrobenzoic acid as structure-directing agent has been employed to synthesize plate-shaped WO{sub 3} nanostructures containing holes. The p-nitrobenzoic acid plays a critical role in the synthesis of such novel WO{sub 3} nanoplates. The morphology, structure and optical property of the WO{sub 3} nanoplates have been characterized by transmission electron microcopy (TEM), scanning electron microcopy (SEM), X-ray diffraction (XRD) and photoluminescence (PL). The lateral size of the nanoplates is 500-1000 nm, and the thickness is about 80 nm. The formation mechanism of WO{sub 3} nanoplates is discussed briefly. The gas sensitivity of WO{sub 3} nanoplates wasmore » studied to ethanol and acetone at different operation temperatures and concentrations. Furthermore, the WO{sub 3} nanoplate-based gas sensor exhibits high sensitivity for ethanol and acetone as well as quick response and recovery time at low temperature.« less

Studies on the sensing behaviour of nanocrystalline CuGa(2)O(4) towards hydrogen, liquefied petroleum gas and ammonia.

PubMed

Biswas, Soumya Kanti; Sarkar, Arpita; Pathak, Amita; Pramanik, Panchanan

2010-06-15

In the present article, the gas sensing behaviour of nanocrystalline CuGa(2)O(4) towards H(2), liquefied petroleum gas (LPG) and NH(3) has been reported for the first time. Nanocrystalline powders of CuGa(2)O(4) having average particle sizes in the range of 30-60nm have been prepared through thermal decomposition of an aqueous precursor solution comprising copper nitrate, gallium nitrate and triethanol amine (TEA), followed by calcination at 750 degrees C for 2h. The synthesized nanocrystalline CuGa(2)O(4) powders have been characterised through X-ray diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM) study, energy dispersive X-ray (EDX) analysis and BET (Brunauer-Emmett-Teller) surface area measurement. The synthesized CuGa(2)O(4) having spinel structure with specific surface area of 40m(2)/g exhibits maximum sensitivity towards H(2), LPG, and NH(3) at 350 degrees C.

Why is the antipodal effect in closo-1-SB9H9 so large? A possible explanation based on the geometry from the concerted use of gas electron diffraction and computational methods.

PubMed

Hnyk, Drahomír; Wann, Derek A; Holub, Josef; Samdal, Svein; Rankin, David W H

2011-06-07

The molecular structure of 1-thia-closo-decaborane(9), 1-SB(9)H(9), has been determined by the concerted use of gas electron diffraction and quantum-chemical calculations. Assuming C(4v) symmetry, the cage structure was distorted from a symmetrically bicapped square antiprism (D(4d) symmetry) mainly through substantial expansion of the tetragonal belt of boron atoms adjacent to sulfur. The S-B and (B-B)(mean) distances are well determined with r(h1) = 193.86(14) and 182.14(8) pm, respectively. Geometrical parameters calculated using the MP2(full)/6-311++G** method and at levels reported earlier [MP2(full)/6-311G**, B3LYP/6-311G** and B3LYP/cc-pVQZ], as well as calculated vibrational amplitudes and (11)B NMR chemical shifts, are in good agreement with the experimental findings. In particular, the so-called antipodal chemical shift of apical B(10) (71.8 ppm) is reproduced well by the GIAO-MP2 calculations and its large magnitude is schematically accounted for, as is the analogous antipodal chemical shift of B(12) in the twelve-vertex closo-1-SB(11)H(11).

Freeze drying-assisted synthesis of Pt@reduced graphene oxide nanocomposites as excellent hydrogen sensor

NASA Astrophysics Data System (ADS)

Lu, Xiaojing; Song, Xinjie; Gu, Cuiping; Ren, Haibo; Sun, Yufeng; Huang, Jiarui

2018-05-01

Quick and efficient detection of low concentrations of hydrogen remains a challenge because of the stability of hydrogen. A sensor based on reduced oxide graphene functionalized with Pt nanoparticles is successfully fabricated using a freeze-drying method followed by heat treatment. The structure and morphology of the Pt@rGO nanocomposites are well analyzed by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy. The as-prepared Pt@rGO nanocomposites show excellent hydrogen gas sensing properties at a low working temperature of 50 °C. The sensitivity toward 0.5% hydrogen is 8%. The response and recovery times of the sensor exposed to 0.5% hydrogen are 63 and 104 s, respectively. The gas-sensing mechanism of Pt@rGO sensor is also discussed.

Nanostructured Tungsten Oxide Composite for High-Performance Gas Sensors

PubMed Central

Feng-Chen, Siyuan; Aldalbahi, Ali; Feng, Peter Xianping

2015-01-01

We report the results of composite tungsten oxide nanowires-based gas sensors. The morphologic surface, crystallographic structures, and chemical compositions of the obtained nanowires have been investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman scattering, respectively. The experimental measurements reveal that each wire consists of crystalline nanoparticles with an average diameter of less than 250 nm. By using the synthesized nanowires, highly sensitive prototypic gas sensors have been designed and fabricated. The dependence of the sensitivity of tungsten oxide nanowires to the methane and hydrogen gases as a function of time has been obtained. Various sensing parameters such as sensitivity, response time, stability, and repeatability were investigated in order to reveal the sensing ability. PMID:26512670

Hierarchical porous ZnO microflowers with ultra-high ethanol gas-sensing at low concentration

NASA Astrophysics Data System (ADS)

Song, Liming; Yue, He; Li, Haiying; Liu, Li; Li, Yu; Du, Liting; Duan, Haojie; Klyui, N. I.

2018-05-01

Hierarchical porous and non-porous ZnO microflowers have been successfully fabricated by hydrothermal method. Their crystal structure, morphology and gas-sensing properties were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and chemical gas sensing intelligent analysis system (CGS). Compared with hierarchical non-porous ZnO microflowers, hierarchical porous ZnO microflowers exhibited ultra-high sensitivity with 50 ppm ethanol at 260 °C and the response is 110, which is 1.8 times higher than that of non-porous ZnO microflowers. Moreover, the lowest concentration limit of hierarchical porous ZnO microflowers (non-porous ZnO microflowers) to ethanol is 0.1 (1) ppm, the response value is 1.6 (1).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pawar, C. S., E-mail: charudutta-p@yahoo.com; Gujar, M. P.; Mathe, V. L.

Nano crystalline Nickel Zinc ferrite (Ni{sub 0.25}Zn{sub 0.75}Fe{sub 2}O{sub 4}) thin films were synthesized by Sol Gel method for gas response. The phase and microstructure of the obtained Ni{sub 0.25}Zn{sub 0.75}Fe{sub 2}O{sub 4} thin films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM). The nanostructured Ni{sub 0.25}Zn{sub 0.75}Fe{sub 2}O{sub 4} thin film shows single spinel phase. Magnetic study was obtained with the help of VSM. The effects of working temperature on the gas response were studied. The results reveal that the Ni{sub 0.25}Zn{sub 0.75}Fe{sub 2}O{sub 4} thin film gas sensor shows good selectivity to chlorine gas at roommore » temperature. The sensor shows highest sensitivity (∼50%) at room temperature, indicating its application in detecting chlorine gas at room temperature in the future.« less

Application of ZnO Nanoparticle as Sulphide Gas Sensor Using UV/VIS/NIR-Spectrophotometer

NASA Astrophysics Data System (ADS)

Juliasih, N.; Buchari; Noviandri, I.

2017-04-01

The nanoparticle of metal oxides has great unique characteristics that applicable to the wide industrial as sensors and catalysts for reducing environmental pollution. Sulphide gas monitors and detectors are required for assessing safety aspects, due to its toxicity level. A thin film of ZnO as the sulphide gas sensor was synthesised by the simple method of chemical liquid deposition with variation of annealing temperature from 200 ºC to 500 ºC, and characterised by Scanning Electron Microscope (SEM), X-Ray Diffraction (XRD), and UV/VIS/NIR-Spectrophotometer. Characterization studies showed nanoparticle size from the range 62 - 92 nm of diameters. The application this ZnO thin film to sulfide gas, detected by UV/VIS/NIR Spectrophotometer with diffuse reflectance, showed specific chemical reaction by the shifting of maximum % Reflectance peak. The gas sensing using this method is applicable at room.

Controllable fabrication of copper phthalocyanine nanostructure crystals.

PubMed

Liu, Fangmei; Sun, Jia; Xiao, Si; Huang, Wenglong; Tao, Shaohua; Zhang, Yi; Gao, Yongli; Yang, Junliang

2015-06-05

Copper phthalocyanine (CuPc) nanostructure crystals, including nanoflower, nanoribbon, and nanowire, were controllably fabricated by temperature gradient physical vapor deposition (TG-PVD) through controlling the growth parameters. In a controllable growth system with carrier gas N2, nanoflower, nanoribbon, and nanowire crystals were formed in a high-temperature zone, medium-temperature zone, and low-temperature zone, respectively. They were proved to be β-phase, coexist of α-phase and β-phase, and α-phase respectively based on x-ray diffraction results. Furthermore, ultralong CuPc nanowires up to several millimeters could be fabricated by TG-PVD without carrier gas, and they were well-aligned to form large-area CuPc nanowire crystal arrays by the Langmuir-Blodgett method. The nanostructure crystals showed unusual optical absorption spectra from the ultraviolet-visible to near-infrared range, which was explained by the diffraction and scattering caused by the wavelength-sized nanostructures. These CuPc nanostructure crystals show potential applications in organic electronic and optoelectronic devices.

Gas-phase surface esterification of cellulose microfibrils and whiskers.

PubMed

Berlioz, Sophie; Molina-Boisseau, Sonia; Nishiyama, Yoshiharu; Heux, Laurent

2009-08-10

A new and highly efficient synthetic method has been developed for the surface esterification of model cellulosic substrates of high crystallinity and accessibility, namely, freeze-dried tunicin whiskers and bacterial cellulose microfibrils dried by the critical point method. The reaction, which is based on the gas-phase action of palmitoyl chloride, was monitored by solid-state CP-MAS (13)C NMR. It was found that the grafting density not only depended on the experimental conditions, but also on the nature and conditioning of the cellulose samples. The structural and morphological modifications of the substrates at various degrees of grafting were revealed by scanning electron microscopy and X-ray diffraction analysis. These characterizations indicated that the esterification proceeded from the surface of the substrate to their crystalline core. Hence, for moderate degree of substitution, the surface was fully grafted whereas the cellulose core remained unmodified and the original fibrous morphology maintained. An almost total esterification could be achieved under certain conditions, leading to highly substituted cellulose esters, presenting characteristic X-ray diffraction patterns.

Characterization of pure Ni ultrafine/nanoparticles synthesized by electromagnetic levitational gas condensation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khodaei, Azin, E-mail: Azin.Khodaei@gmail.com; Hasannasab, Malihe; Amousoltani, Narges

2016-02-15

Highlights: • Ni ultrafine/nanoparticles were produced using the single-step ELGC method. • Ar and He–20%Ar gas mixtures were used as the condensing gas under 1 atm. • Effects of gas type and flow rate on particle size distribution were investigated. • The nanoparticles showed both high saturation magnetization and low coercivity. - Abstract: In this work, Ni ultrafine/nanoparticles were directly produced using the one-step, relatively large-scale electromagnetic levitational gas condensation method. In this process, Ni vapors ascending from the levitated droplet were condensed by Ar and He–20%Ar gas mixtures under atmospheric pressure. Effects of type and flow rate of themore » condensing gas on the size, size distribution and crystallinity of Ni particles were investigated. The particles were characterized by scanning electron microscopy, X-ray diffraction and vibrating sample magnetometer (VSM). The process parameters for the synthesis of the crystalline Ni ultrafine/nanoparticles were determined.« less

Review of model sensor studies on Pd/SnO2(110) surfaces

NASA Technical Reports Server (NTRS)

Fryberger, Teresa B.; Semancik, Steve

1990-01-01

Studies performed at the National Institute of Standards and Technology on the model gas sensor system, Pd/SnO2(110), are reviewed. Adsorption and interfacial effects play a primary role in the gas sensing process, as they do in catalysis. For this reason, researchers have used a variety of surface sensitive techniques in the research, including x ray and ultraviolet photoelectron spectroscopies (XPS and UPS), low energy electron diffraction (LEED), and ion scattering spectroscopy (ISS). By combining these complementary techniques with in situ gas response (conductance) measurements, researchers were able to correlate directly sensor activity with the composition and structure of the Pd/SnO2 interface. Although the intent of this work is to develop an understanding of gas sensing mechanisms, its relevance to Pt/SnO2 catalytic systems is obvious.

Synthesis, Characterization, and Gas-Sensing Properties of Mesoporous Nanocrystalline Sn(x)Ti(1-x)O2.

PubMed

Zhong, Cheng; Lin, Zhidong; Guo, Fei; Wang, Xuehua

2015-06-01

A nanocomposite mesoporous material composed by SnO2 and TiO2 with the size of -5-9 nm were prepared via a facile wet-chemical approach combining with an annealing process. The microstructure of obtained Sn(x)Ti(1-x)O2 powders were characterized by X-ray diffraction, X-ray Photo-electronic Spectroscopy, scanning electron microscope, transmission electron microscope and nitrogen adsorption-desorption experiment. The gas sensing performances to several gases of the mesoporous material were studied. The sensors of Sn(x)Ti(1-x)O2 (ST10, with 9.1% Ti) exhibited very high responses to volatile organic compounds at 160 degrees C. The order of the responses to volatile gases based on ST10 was ethanol > formaldehyde > acetone > toluene > benzene > methane. Sensor based on ST10 displays a highest sensitivity to hydrogen at 200 degrees C. Sensor responses to H2 at 200 degrees C have been measured and analyzed in a wide concentration range from 5 to 2000 ppm. The solid solution Sn(x)Ti(1-x)O2 can be served as a potential gas-sensing material for a broad range of future sensor applications.

Solvent free tin oxide nanoparticle for gas sensing application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ranjan, Pranay, E-mail: pranjan@iitp.ac.in; Thakur, Ajay D.; Centre for Energy and Environment, Indian Institute of Technology Patna, Patliputra, Patna 800013 India

2016-05-06

A new modified technique of synthesizing tin oxide nanoparticles with crystallite size of 2 nm to 6 nm has been developed. Surface area of the nanoparticle has been increased as we approached towards the Debye length. Such a techniques for approaching the Debye length is expected to bring remarkable changes in the properties of resistive based gas sensors. The technique used here is less toxic, economical and has high yield. Phase purity, size, shape and composition has been investigated using x-ray diffraction, micro Raman, scanning electron microscopy and energy dispersive x ray spectroscopy. While surface area has been calculated through Brunaur-Emmett-Teller (BET).

Microwave assisted combustion synthesis of nanocrystalline CoFe2O4 for LPG sensing

NASA Astrophysics Data System (ADS)

Chaudhari, Prashant; Acharya, S. A.; Darunkar, S. S.; Gaikwad, V. M.

2015-08-01

A microwave-assisted citrate precursor method has been utilized for synthesis of nanocrystalline powders of CoFe2O4. The process takes only a few minutes to obtain as-synthesized CoFe2O4. Structural properties of the synthesized material were investigated by X-ray diffraction; scanning electron microscopy, Thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy. The gas sensing properties of thick film of CoFe2O4 prepared by screen printing towards Liquid Petroleum Gas (LPG) revealed that CoFe2O4 thick films are sensitive and shows maximum sensitivity at 350°C for 2500 ppm of LPG.

Nanometres-resolution Kikuchi patterns from materials science specimens with transmission electron forward scatter diffraction in the scanning electron microscope.

PubMed

Brodusch, N; Demers, H; Gauvin, R

2013-04-01

A charge-coupled device camera of an electron backscattered diffraction system in a scanning electron microscope was positioned below a thin specimen and transmission Kikuchi patterns were collected. Contrary to electron backscattered diffraction, transmission electron forward scatter diffraction provides phase identification and orientation mapping at the nanoscale. The minimum Pd particle size for which a Kikuchi diffraction pattern was detected and indexed reliably was 5.6 nm. An orientation mapping resolution of 5 nm was measured at 30 kV. The resolution obtained with transmission electron forward scatter diffraction was of the same order of magnitude than that reported in electron nanodiffraction in the transmission electron microscope. An energy dispersive spectrometer X-ray map and a transmission electron forward scatter diffraction orientation map were acquired simultaneously. The high-resolution chemical, phase and orientation maps provided at once information on the chemical form, orientation and coherency of precipitates in an aluminium-lithium 2099 alloy. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Electron Diffraction Using Transmission Electron Microscopy

PubMed Central

Bendersky, Leonid A.; Gayle, Frank W.

2001-01-01

Electron diffraction via the transmission electron microscope is a powerful method for characterizing the structure of materials, including perfect crystals and defect structures. The advantages of electron diffraction over other methods, e.g., x-ray or neutron, arise from the extremely short wavelength (≈2 pm), the strong atomic scattering, and the ability to examine tiny volumes of matter (≈10 nm3). The NIST Materials Science and Engineering Laboratory has a history of discovery and characterization of new structures through electron diffraction, alone or in combination with other diffraction methods. This paper provides a survey of some of this work enabled through electron microscopy. PMID:27500060

Magnesium Nanoparticles for Hydrogen Storage: Structure, Kinetics and Thermodynamics

NASA Astrophysics Data System (ADS)

Pasquini, L.; Brighi, M.; Montone, A.; Vittori Antisari, M.; Dam, B.; Palmisano, V.; Bonetti, E.

2012-08-01

Magnesium nanoparticles coated by a native oxide shell and decorated by palladium clusters were synthesized by the inert gas condensation technique. The kinetics and thermodynamics of hydrogen sorption were investigated by Sieverts measurements at high temperature and by optical hydrogenography close to ambient temperature. The structure and morphology of the nanoparticles were studied by electron microscopy and X-ray diffraction both in the as-prepared state and after hydrogen sorption cycles.

MBE growth and processing of III/V-nitride semiconductor thin film structures: Growth of gallium indium arsenic nitride and nano-machining with focused ion beam and electron beam

NASA Astrophysics Data System (ADS)

Park, Yeonjoon

The advanced semiconductor material InGaAsN was grown with nitrogen plasma assisted Molecular Beam Epitaxy (MBE). The InGaAsN layers were characterized with High Resolution X-ray Diffraction (HRXDF), Atomic Fore Microscope (AFM), X-ray Photoemission Spectroscopy (XPS) and Photo-Luminescence (PL). The reduction of the band gap energy was observed with the incorporation of nitrogen and the lattice matched condition to the GaAs substrate was achieved with the additional incorporation of indium. A detailed investigation was made for the growth mode changes from planar layer-by-layer growth to 3D faceted growth with a higher concentration of nitrogen. A new X-ray diffraction analysis was developed and applied to the MBE growth on GaAs(111)B, which is one of the facet planes of InGaAsN. As an effort to enhance the processing tools for advanced semiconductor materials, gas assisted Focused Ion Beam (FIB) vertical milling was performed on GaN. The FIB processed area shows an atomically flat surface, which is good enough for the fabrication of Double Bragg Reflector (DBR) mirrors for the Blue GaN Vertical Cavity Surface Emitting Laser (VCSEL) Diodes. An in-situ electron beam system was developed to combine the enhanced lithographic processing capability with the atomic layer growth capability by MBE. The electron beam system has a compensation capability against substrate vibration and thermal drift. In-situ electron beam lithography was performed with the low pressure assisting gas. The advanced processing and characterization methods developed in this thesis will assist the development of superior semiconductor materials for the future.

Hydrogen Gas Sensing Characteristics of Nanostructured NiO Thin Films Synthesized by SILAR Method

NASA Astrophysics Data System (ADS)

Karaduman, Irmak; Çorlu, Tugba; Yıldırım, M. Ali; Ateş, Aytunç; Acar, Selim

2017-07-01

Nanostructured NiO thin films have been synthesized by a facile, low-cost successive ionic layer adsorption and reaction (SILAR) method, and the effects of the film thickness on their hydrogen gas sensing properties investigated. The samples were characterized by scanning electron microscopy (SEM), x-ray diffraction (XRD) analysis, and energy-dispersive x-ray analysis. The XRD results revealed that the crystallinity improved with increasing thickness, exhibiting polycrystalline structure. SEM studies showed that all the films covered the glass substrate well. According to optical absorption measurements, the optical bandgap decreased with increasing film thickness. The gas sensing properties of the nanostructured NiO thin films were studied as a function of operating temperature and gas concentration. The samples showed good sensing performance of H2 gas with high response. The maximum response was 75% at operating temperature of 200°C for hydrogen gas concentration of 40 ppm. These results demonstrate that nanostructured NiO thin films synthesized by the SILAR method have potential for application in hydrogen detection.

Algan/Gan Hemt By Magnetron Sputtering System

NASA Astrophysics Data System (ADS)

Garcia Perez, Roman

In this thesis, the growth of the semiconductor materials AlGaN and GaN is achieved by magnetron sputtering for the fabrication of High Electron Mobility Transistors (HEMTs). The study of the deposited nitrides is conducted by spectroscopy, diffraction, and submicron scale microscope methods. The preparation of the materials is performed using different parameters in terms of power, pressure, temperature, gas, and time. Silicon (Si) and Sapphire (Al2O3) wafers are used as substrates. The chemical composition and surface topography of the samples are analyzed to calculate the materials atomic percentages and to observe the devices surface. The instruments used for the semiconductors characterization are X-ray Photoelectron Spectroscopy (XPS), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and Atomic Force Microscope (AFM). The project focused its attention on the reduction of impurities during the deposition, the controlled thicknesses of the thin-films, the atomic configuration of the alloy AlxGa1-xN, and the uniformity of the surfaces.

Synthesis of boron nitride nanostructures from catalyst of iron compounds via thermal chemical vapor deposition technique

NASA Astrophysics Data System (ADS)

da Silva, Wellington M.; Ribeiro, Hélio; Ferreira, Tiago H.; Ladeira, Luiz O.; Sousa, Edésia M. B.

2017-05-01

For the first time, patterned growth of boron nitride nanostructures (BNNs) is achieved by thermal chemical vapor deposition (TCVD) technique at 1150 °C using a mixture of FeS/Fe2O3 catalyst supported in alumina nanostructured, boron amorphous and ammonia (NH3) as reagent gas. This innovative catalyst was synthesized in our laboratory and systematically characterized. The materials were characterized by X-ray diffraction (XRD), Raman spectroscopy, Fourier-transform infrared spectroscopy (FTIR), Thermogravimetric analysis (TGA), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The X-ray diffraction profile of the synthesized catalyst indicates the coexistence of three different crystal structures showing the presence of a cubic structure of iron oxide and iron sulfide besides the gamma alumina (γ) phase. The results show that boron nitride bamboo-like nanotubes (BNNTs) and hexagonal boron nitride (h-BN) nanosheets were successfully synthesized. Furthermore, the important contribution of this work is the manufacture of BNNs from FeS/Fe2O3 mixture.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shete, Meera; Kumar, Prashant; Bachman, Jonathan E.

High aspect-ratio nanosheets of metal-organic frameworks (MOFs) hold promise for use as selective flakes in gas separation membranes. However, simple and scalable methods for the synthesis of MOF nanosheets have thus far remained elusive. Here, we describe the direct synthesis of Cu(BDC) (BDC2-= 1,4-benzenedicarboxylate) nanosheets with an average lateral size of 2.5 mu m and a thickness of 25 nm from a well-mixed solution. Characterization of the nanosheets by powder and thin film X-ray diffraction, electron microscopy, and electron diffraction reveals pronounced structural disorder that may affect their pore structure. Incorporation of the Cu (BDC) nanosheets into a Matrimid polymermore » matrix results in mixed matrix membranes (MMMs) that exhibit a 70% increase in the CO2/CH4 selectivity compared with that of Matrimid. Analysis of new and previously reported permeation data for Cu(BDC) MMMs using a mathematical model for selective flake composites indicates that further performance improvements could be achieved with the selection of different polymers for use in the continuous phase.« less

P-type sub-tungsten-oxide based urchin-like nanostructure for superior room temperature alcohol sensor

NASA Astrophysics Data System (ADS)

Yao, Yao; Yin, Mingli; Yan, Junqing; Liu, Shengzhong (Frank)

2018-05-01

Nanowires assembled sub-WO3 urchin-like nanostructures have been fabricated via a solvothermal method. The detailed structure and morphology features were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The results reveal that the individual nanowires are grown along the [0 0 1] direction, and assembled together to form an urchin-like nanostructure. Sensing performance of the sub-WO3 was investigated toward alcohol vapor. At room temperature, the sensor devices based on the WO3-x exhibit significantly higher sensitivity comparing to that of the stoichiometric WO3. The superior sensing performance of this WO3-x sensor is ascribed to the large specific surface area and abundant oxygen vacancies. The obvious enhancement of the gas sensing property can be very useful for the future design and development of room temperature gas sensors for other volatile organic compounds.

CTAB assisted synthesis of tungsten oxide nanoplates as an efficient low temperature NOX sensor

NASA Astrophysics Data System (ADS)

Mehta, Swati S.; Tamboli, Mohaseen S.; Mulla, Imtiaz S.; Suryavanshi, Sharad S.

2018-02-01

Tungsten oxide nanoplates with porous morphology were effectively prepared by acidification using CTAB (HexadeCetyltrimethyl ammonium bromide) as a surfactant. For characterization, the synthesized materials were subjected to X-Ray powder diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), UV-Visible spectroscopy (UV-Vis) and surface area (BET) measurements. The morphology and size of the particles were controlled by solution acidity. The BET results confirmed that the materials are well crystallized and mesoporous in nature. The nanocrystalline powder was used to prepare thick films by screen printing on alumina substrate for the investigation of gas sensing properties. The gas response measurements revealed that the samples acidified using 10 M H2SO4 exhibits highest response of 91% towards NOX at optimum temperature of 200 °C for 100 ppm, and it also exhibits 35% response at room temperature.

Synthesis, magnetic and ethanol gas sensing properties of semiconducting magnetite nanoparticles

NASA Astrophysics Data System (ADS)

Al-Ghamdi, Ahmed A.; Al-Hazmi, Faten; Al-Tuwirqi, R. M.; Alnowaiser, F.; Al-Hartomy, Omar A.; El-Tantawy, Farid; Yakuphanoglu, F.

2013-05-01

The superparamagnetic magnetite (Fe3O4) nanoparticles with an average size of 7 nm were synthesized using a rapid and facile microwave hydrothermal technique. The structure of the magnetite nanoparticles was characterized by X-ray diffraction (X-ray), field effect scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). The prepared Fe3O4 was shown to have a cubic phase of pure magnetite. Magnetization hysteresis loop shows that the synthesized magnetite exhibits no hysteretic features with a superparamagnetic behavior. The ethanol gas sensing properties of the synthesized magnetite were investigated, and it was found that the responsibility time is less than 10 s with good reproducibility for ethanol sensor. Accordingly, it is evaluated that the magnetite nanoparticles can be effectively used as a solid state ethanol sensor in industrial commercial product applications.

Synthesis and characterization of Ti-Si-C-N films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shtansky, D.V.; Levashov, E.A.; Sheveiko, A.N.

1999-09-01

This study represents one of the first attempts to deposit multicomponent (more than three components) thin films by magnetron sputtering of multiphase composite targets (three phases or even more). Films of Ti-Si-C-N were synthesized through dc magnetron sputtering of xTiC + yTi{sub 3}SiC{sub 2} + zA composite targets (A was TiSi{sub 2}, SiC, or a mixture of these phases) in an argon atmosphere or in a gaseous mixture of argon and nitrogen. The as-deposited films were characterized using Auger electron spectroscopy, X-ray diffraction, transmission electron microscopy using selected area electron diffraction and high-resolution techniques, and microhardness. It was shown thatmore » the substrate temperature and the nitrogen concentration in the reactive gas had a strong influence on the structure and the composition of the as-deposited films. Polycrystalline grains contained a high density of dislocations and exhibited a curved appearance of the lattice fringes that is probably due to the presence of the long-range stress fields. The measurements of the lattice parameters using the selected area electron diffraction pattern (SA EDP) method indicated, with a high probability, that the polycrystalline grains consist of clusters of atoms with varying compositions. The grain boundaries in the nanocrystalline Ti-Si-C-N films had both ordered and disordered regions, although some regions close to the interface exhibited neither a fully crystalline nor a homogeneously amorphous structure. The contribution of compressive stress as determined by an increase in the fcc lattice parameter is also discussed.« less

Liquefied petroleum gas sensor based on manganese (III) oxide and zinc manganese (III) oxide nanoparticles

NASA Astrophysics Data System (ADS)

Sharma, Shiva; Chauhan, Pratima; Husain, Shahid

2018-01-01

In this paper, {{{Mn}}}2{{{O}}}3 and {{{ZnMn}}}2{{{O}}}4 nanoparticles (NPs) are successfully synthesized using chemical co-precipitation method at room temperature and further annealed at 450 °C. The structure, crystallite size, morphology, specific surface area (SSA) and band gap energy have been determined by x-ray diffraction, transmission electron microscopy, Brunauer-Emmett-Teller surface area analysis, scanning electron microscopy (SEM-EDS) and UV-visible spectrophotometer. The sensor films of the {{{Mn}}}2{{{O}}}3 NPs and {{{ZnMn}}}2{{{O}}}4 NPs have been fabricated onto glass substrate using spin coater system separately. These sensor films are investigated for different concentrations (200-1200 ppm) of liquefied petroleum gas (LPG) at different operating temperatures ranging from 100 °C to 400 °C. A comparative study of gas sensing properties shows that spinel {{{ZnMn}}}2{{{O}}}4 sensor film exhibit excellent response (≈ 80 % ) towards 1000 ppm LPG at 300 °C in comparison to {{{Mn}}}2{{{O}}}3 sensor films. The enhancement in the gas sensing characteristics of {{{ZnMn}}}2{{{O}}}4 sensor film is attributed to the reduced crystallite size, greater SSA, and modification in structure as well as morphology.

Formation of the ZnFe2O4 phase in an electric arc furnace off-gas treatment system.

PubMed

Suetens, T; Guo, M; Van Acker, K; Blanpain, B

2015-04-28

To better understand the phenomena of ZnFe2O4 spinel formation in electric arc furnace dust, the dust was characterized with particle size analysis, X-ray fluorescence (XRF), electron backscatter diffraction (EBSD), and electron probe micro-analysis (EPMA). Different ZnFe2O4 formation reaction extents were observed for iron oxide particles with different particle sizes. ZnO particles were present as both individual particles and aggregated on the surface of larger particles. Also, the slag particles found in the off-gas were shown not to react with the zinc vapor. After confirming the presence of a ZnFe2O4 formation reaction, the thermodynamic feasibility of in-process separation - a new electric arc furnace dust treatment technology - was reevaluated. The large air intake and the presence of iron oxide particles in the off-gas were included into the thermodynamic calculations. The formation of the stable ZnFe2O4 spinel phase was shown to be thermodynamically favorable in current electric arc furnace off-gas ducts conditions even before reaching the post combustion chamber. Copyright © 2015 Elsevier B.V. All rights reserved.

Calcination Method Synthesis of SnO2/g-C3N4 Composites for a High-Performance Ethanol Gas Sensing Application

PubMed Central

Cao, Jianliang; Qin, Cong; Wang, Yan; Zhang, Bo; Gong, Yuxiao; Zhang, Huoli; Sun, Guang; Bala, Hari; Zhang, Zhanying

2017-01-01

The SnO2/g-C3N4 composites were synthesized via a facile calcination method by using SnCl4·5H2O and urea as the precursor. The structure and morphology of the as-synthesized composites were characterized by the techniques of X-ray diffraction (XRD), the field-emission scanning electron microscopy and transmission electron microscopy (SEM and TEM), energy dispersive spectrometry (EDS), thermal gravity and differential thermal analysis (TG-DTA), and N2-sorption. The analysis results indicated that the as-synthesized samples possess the two dimensional structure. Additionally, the SnO2 nanoparticles were highly dispersed on the surface of the g-C3N4nanosheets. The gas-sensing performance of the as-synthesized composites for different gases was tested. Moreover, the composite with 7 wt % g-C3N4 content (SnO2/g-C3N4-7) SnO2/g-C3N4-7 exhibits an admirable gas-sensing property to ethanol, which possesses a higher response and better selectivity than that of the pure SnO2-based sensor. The high surface area of the SnO2/g-C3N4 composite and the good electronic characteristics of the two dimensional graphitic carbon nitride are in favor of the elevated gas-sensing property. PMID:28468245

Characteristics of layered tin disulfide deposited by atomic layer deposition with H2S annealing

NASA Astrophysics Data System (ADS)

Lee, Seungjin; Shin, Seokyoon; Ham, Giyul; Lee, Juhyun; Choi, Hyeongsu; Park, Hyunwoo; Jeon, Hyeongtag

2017-04-01

Tin disulfide (SnS2) has attracted much attention as a two-dimensional (2D) material. A high-quality, low-temperature process for producing 2D materials is required for future electronic devices. Here, we investigate tin disulfide (SnS2) layers deposited via atomic layer deposition (ALD) using tetrakis(dimethylamino)tin (TDMASn) as a Sn precursor and H2S gas as a sulfur source at low temperature (150° C). The crystallinity of SnS2 was improved by H2S gas annealing. We carried out H2S gas annealing at various conditions (250° C, 300° C, 350° C, and using a three-step method). Angle-resolved X-ray photoelectron spectroscopy (ARXPS) results revealed the valence state corresponding to Sn4+ and S2- in the SnS2 annealed with H2S gas. The SnS2 annealed with H2S gas had a hexagonal structure, as measured via X-ray diffraction (XRD) and the clearly out-of-plane (A1g) mode in Raman spectroscopy. The crystallinity of SnS2 was improved after H2S annealing and was confirmed using the XRD full-width at half-maximum (FWHM). In addition, high-resolution transmission electron microscopy (HR-TEM) images indicated a clear layered structure.

Crystal structure and composition of BAlN thin films: Effect of boron concentration in the gas flow

NASA Astrophysics Data System (ADS)

Wang, Shuo; Li, Xiaohang; Fischer, Alec M.; Detchprohm, Theeradetch; Dupuis, Russell D.; Ponce, Fernando A.

2017-10-01

We have investigated the microstructure of BxAl1-xN films grown by flow-modulated epitaxy at 1010 °C, with B/(B + Al) gas-flow ratios ranging from 0.06 to 0.18. The boron content obtained from X-ray diffraction (XRD) patterns ranges from x = 0.02 to 0.09. On the other hand, boron content deduced from the aluminum signal in the Rutherford backscattering spectra (RBS) ranges from x = 0.06 to 0.16, closely following the gas-flow ratios. Transmission electron microscopy indicates the sole presence of a wurtzite crystal structure in the BAlN films, and a tendency towards columnar growth for B/(B + Al) gas-flow ratios below 0.12. For higher ratios, the BAlN films exhibit a tendency towards twin formation and finer microstructure. Electron energy loss spectroscopy has been used to profile spatial variations in the composition of the films. The RBS data suggest that the incorporation of B is highly efficient for our growth method, while the XRD data indicate that the epitaxial growth may be limited by a solubility limit in the crystal phase at about 9%, for the range of B/(B + Al) gas-flow ratios that we have studied, which is significantly higher than previously thought.

Highly sensitive nanostructure SnO2 based gas sensor for environmental pollutants

NASA Astrophysics Data System (ADS)

Korgaokar, Sushil; Moradiya, Meet; Prajapati, Om; Thakkar, Pranav; Pala, Jay; Savaliya, Chirag; Parikh, Sachin; Markna, J. H.

2017-05-01

A major quantity of pollutants are produced from industries and vehicles in the form of gas. New approaches are needed to solve well-known environmental pollutants like CO, CO2, NO2, SOx. Therefore detection with effective gas sensors is a vital part of pollution prevention efforts. There is a need to develop fast, rapid, cost-effective, highly sensitive, low power, and non-intrusive rugged sensors that can be easily installed. In the present study, nanostructured SnO2 used as a sensitive material in the devices and synthesized using hydrothermal process. The detailed development of the fabrication of SnO2 nanostructures gas sensor is described, which shows the remarkable change in the sensing properties with varying particle size. Additionally, we have used X-ray diffraction, scanning electron microscopy (SEM) for characterization and carefully examined the relative parameters like response magnitude (sensitivity) and selectivity of SnO2 nano structures with different particle size.

Iron single crystal growth from a lithium-rich melt

NASA Astrophysics Data System (ADS)

Fix, M.; Schumann, H.; Jantz, S. G.; Breitner, F. A.; Leineweber, A.; Jesche, A.

2018-03-01

α -Fe single crystals of rhombic dodecahedral habit were grown from a Li84N12Fe∼3 melt. Crystals of several millimeter along a side form at temperatures around T ≈ 800 ° C. Upon further cooling the growth competes with the formation of Fe-doped Li3N. The b.c.c. structure and good sample quality of α -Fe single crystals were confirmed by X-ray and electron diffraction as well as magnetization measurements and chemical analysis. A nitrogen concentration of 90 ppm was detected by means of carrier gas hot extraction. Scanning electron microscopy did not reveal any sign of iron nitride precipitates.

Energy-resolved coherent diffraction from laser-driven electronic motion in atoms

NASA Astrophysics Data System (ADS)

Shao, Hua-Chieh; Starace, Anthony F.

2017-10-01

We investigate theoretically the use of energy-resolved ultrafast electron diffraction to image laser-driven electronic motion in atoms. A chirped laser pulse is used to transfer the valence electron of the lithium atom from the ground state to the first excited state. During this process, the electronic motion is imaged by 100-fs and 1-fs electron pulses in energy-resolved diffraction measurements. Simulations show that the angle-resolved spectra reveal the time evolution of the energy content and symmetry of the electronic state. The time-dependent diffraction patterns are further interpreted in terms of the momentum transfer. For the case of incident 1-fs electron pulses, the rapid 2 s -2 p quantum beat motion of the target electron is imaged as a time-dependent asymmetric oscillation of the diffraction pattern.

Ammonia gas sensing behavior of tanninsulfonic acid doped polyaniline-TiO₂ composite.

PubMed

Bairi, Venu Gopal; Bourdo, Shawn E; Sacre, Nicolas; Nair, Dev; Berry, Brian C; Biris, Alexandru S; Viswanathan, Tito

2015-10-16

A highly active tannin doped polyaniline-TiO₂ composite ammonia gas sensor was developed and the mechanism behind the gas sensing activity was reported for the first time. A tanninsulfonic acid doped polyaniline (TANIPANI)-titanium dioxide nanocomposite was synthesized by an in situ polymerization of aniline in the presence of tanninsulfonic acid and titanium dioxide nanoparticles. X-ray diffraction and thermogravimetric analysis were utilized to determine the incorporation of TiO₂ in TANIPANI matrix. UV-Visible and infrared spectroscopy studies provided information about the electronic interactions among tannin, polyaniline, and TiO₂. Scanning electron microscopy (SEM) along with energy dispersive X-ray spectroscopy (EDS) and atomic force microscopy (AFM) surface analysis techniques were used to investigate the metal oxide dispersions inside polyaniline matrix. Gas sensors were prepared by spin coating solutions of TANIPANI-TiO₂ and TANIPANI composites onto glass slides. Sensors were tested at three different concentrations (20 ppm, 40 ppm, and 60 ppm) of ammonia gas at ambient temperature conditions by measuring the changes in surface resistivity of the films with respect to time. Ammonia gas sensing plots are presented showing the response values, response times and recovery times. The TANIPANI-TiO₂ composite exhibited better response and shorter recovery times when compared to TANIPANI control and other polyaniline composites that have been reported in the literature. For the first time a proposed mechanism of gas sensing basing on the polaron band localization and its effects on the gas sensing behavior of polyaniline are reported.

Ultrafast electron diffraction with megahertz MeV electron pulses from a superconducting radio-frequency photoinjector

DOE Office of Scientific and Technical Information (OSTI.GOV)

Feng, L. W.; Lin, L.; Huang, S. L.

We report ultrafast relativistic electron diffraction operating at the megahertz repetition rate where the electron beam is produced in a superconducting radio-frequency (rf) photoinjector. We show that the beam quality is sufficiently high to provide clear diffraction patterns from gold and aluminium samples. With the number of electrons, several orders of magnitude higher than that from a normal conducting photocathode rf gun, such high repetition rate ultrafast MeV electron diffraction may open up many new opportunities in ultrafast science.

Synthesis, characterization and liquefied petroleum gas (LPG) sensing properties of WO3 nano-particles

NASA Astrophysics Data System (ADS)

Singh, Subhash; Majumder, S. B.

2018-05-01

Metal oxide sensors, such as ZnO, SnO2, and WO3 etc. have been utilized for several decades for low-costd etection of combustible and toxic gases. In the present work tungsten oxide (WO3) nanoparticles have been prepared by using an economic wet chemical synthesis route. To understand the phase formation behavior of the synthesized powders, X-ray diffraction analysis has been performed. The microstructure evolution of the synthesized powders was characterized by field-emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM). The calcined phase pure WO3 nanoparticles are investigated in terms of LPG gas sensing properties. The gas sensing measurements has been done in two different mode of operation (namely static and dynamic measurements). The degree of oxygen deficiency in the WO3 sensor also affected the sensor properties and the optimum oxygen content of WO3 was necessary to get high sensitivity for LPG. The WO3 sensor shows the excellent sensor properties for LPG at the operating temperature of 250°C.

Long-baseline optical intensity interferometry. Laboratory demonstration of diffraction-limited imaging

NASA Astrophysics Data System (ADS)

Dravins, Dainis; Lagadec, Tiphaine; Nuñez, Paul D.

2015-08-01

Context. A long-held vision has been to realize diffraction-limited optical aperture synthesis over kilometer baselines. This will enable imaging of stellar surfaces and their environments, and reveal interacting gas flows in binary systems. An opportunity is now opening up with the large telescope arrays primarily erected for measuring Cherenkov light in air induced by gamma rays. With suitable software, such telescopes could be electronically connected and also used for intensity interferometry. Second-order spatial coherence of light is obtained by cross correlating intensity fluctuations measured in different pairs of telescopes. With no optical links between them, the error budget is set by the electronic time resolution of a few nanoseconds. Corresponding light-travel distances are approximately one meter, making the method practically immune to atmospheric turbulence or optical imperfections, permitting both very long baselines and observing at short optical wavelengths. Aims: Previous theoretical modeling has shown that full images should be possible to retrieve from observations with such telescope arrays. This project aims at verifying diffraction-limited imaging experimentally with groups of detached and independent optical telescopes. Methods: In a large optics laboratory, artificial stars (single and double, round and elliptic) were observed by an array of small telescopes. Using high-speed photon-counting solid-state detectors and real-time electronics, intensity fluctuations were cross-correlated over up to 180 baselines between pairs of telescopes, producing coherence maps across the interferometric Fourier-transform plane. Results: These interferometric measurements were used to extract parameters about the simulated stars, and to reconstruct their two-dimensional images. As far as we are aware, these are the first diffraction-limited images obtained from an optical array only linked by electronic software, with no optical connections between the telescopes. Conclusions: These experiments serve to verify the concepts for long-baseline aperture synthesis in the optical, somewhat analogous to radio interferometry.

A measurement of electron-wall interactions using transmission diffraction from nanofabricated gratings

NASA Astrophysics Data System (ADS)

Barwick, Brett; Gronniger, Glen; Yuan, Lu; Liou, Sy-Hwang; Batelaan, Herman

2006-10-01

Electron diffraction from metal coated freestanding nanofabricated gratings is presented, with a quantitative path integral analysis of the electron-grating interactions. Electron diffraction out to the 20th order was observed indicating the high quality of our nanofabricated gratings. The electron beam is collimated to its diffraction limit with ion-milled material slits. Our path integral analysis is first tested against single slit electron diffraction, and then further expanded with the same theoretical approach to describe grating diffraction. Rotation of the grating with respect to the incident electron beam varies the effective distance between the electron and grating bars. This allows the measurement of the image charge potential between the electron and the grating bars. Image charge potentials that were about 15% of the value for that of a pure electron-metal wall interaction were found. We varied the electron energy from 50to900eV. The interaction time is of the order of typical metal image charge response times and in principle allows the investigation of image charge formation. In addition to the image charge interaction there is a dephasing process reducing the transverse coherence length of the electron wave. The dephasing process causes broadening of the diffraction peaks and is consistent with a model that ascribes the dephasing process to microscopic contact potentials. Surface structures with length scales of about 200nm observed with a scanning tunneling microscope, and dephasing interaction strength typical of contact potentials of 0.35eV support this claim. Such a dephasing model motivated the investigation of different metallic coatings, in particular Ni, Ti, Al, and different thickness Au-Pd coatings. Improved quality of diffraction patterns was found for Ni. This coating made electron diffraction possible at energies as low as 50eV. This energy was limited by our electron gun design. These results are particularly relevant for the use of these gratings as coherent beam splitters in low energy electron interferometry.

Molybdenum Oxide Nitrides of the Mo2(O,N,□)5 Type: On the Way to Mo2O5.

PubMed

Weber, Dominik; Huber, Manop; Gorelik, Tatiana E; Abakumov, Artem M; Becker, Nils; Niehaus, Oliver; Schwickert, Christian; Culver, Sean P; Boysen, Hans; Senyshyn, Anatoliy; Pöttgen, Rainer; Dronskowski, Richard; Ressler, Thorsten; Kolb, Ute; Lerch, Martin

2017-08-07

Blue-colored molybdenum oxide nitrides of the Mo 2 (O,N,□) 5 type were synthesized by direct nitridation of commercially available molybdenum trioxide with a mixture of gaseous ammonia and oxygen. Chemical composition, crystal structure, and stability of the obtained and hitherto unknown compounds are studied extensively. The average oxidation state of +5 for molybdenum is proven by Mo K near-edge X-ray absorption spectroscopy; the magnetic behavior is in agreement with compounds exhibiting Mo V O 6 units. The new materials are stable up to ∼773 K in an inert gas atmosphere. At higher temperatures, decomposition is observed. X-ray and neutron powder diffraction, electron diffraction, and high-resolution transmission electron microscopy reveal the structure to be related to VNb 9 O 24.9 -type phases, however, with severe disorder hampering full structure determination. Still, the results demonstrate the possibility of a future synthesis of the potential binary oxide Mo 2 O 5 . On the basis of these findings, a tentative suggestion on the crystal structure of the potential compound Mo 2 O 5 , backed by electronic-structure and phonon calculations from first principles, is given.

Digital electron diffraction – seeing the whole picture

PubMed Central

Beanland, Richard; Thomas, Paul J.; Woodward, David I.; Thomas, Pamela A.; Roemer, Rudolf A.

2013-01-01

The advantages of convergent-beam electron diffraction for symmetry determination at the scale of a few nm are well known. In practice, the approach is often limited due to the restriction on the angular range of the electron beam imposed by the small Bragg angle for high-energy electron diffraction, i.e. a large convergence angle of the incident beam results in overlapping information in the diffraction pattern. Techniques have been generally available since the 1980s which overcome this restriction for individual diffracted beams, by making a compromise between illuminated area and beam convergence. Here a simple technique is described which overcomes all of these problems using computer control, giving electron diffraction data over a large angular range for many diffracted beams from the volume given by a focused electron beam (typically a few nm or less). The increase in the amount of information significantly improves the ease of interpretation and widens the applicability of the technique, particularly for thin materials or those with larger lattice parameters. PMID:23778099

Synthesis of zinc ultrafine powders via the Guen–Miller flow-levitation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jigatch, A. N., E-mail: jan@chph.ras.ru; Leipunskii, I. O.; Kuskov, M. L.

2015-12-15

Zinc ultrafine powders (UFPs) with the average particle size of 0.175 to 1.24 μm are synthesized via the flow-levitation method. The peculiarities of the formation of zinc UFPs are considered with respect to the carrier gas properties (heat capacity, thermal conductivity, and diffusion coefficient), as well as the gas flow parameters (pressure and flow rate). The obtained zinc particles are studied via scanning electron microscopy and X-ray diffraction. The factors determining the crystal structure of zinc particles and their size distribution are discussed as well. The data on oxidation of zinc stored in unsealed containers under normal conditions are alsomore » presented.« less

ZnO nanoparticles based fiber optic gas sensor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Narasimman, S.; Sivacoumar, R.; Alex, Z. C.

In this work, ZnO nanoparticles were synthesized by simple aqueous chemical route method. The synthesized ZnO nanoparticles were characterized by X-ray diffraction and scanning electron microscope. The sensitivity of the nanoparticles was studied for different gases like acetone, ammonia and ethanol in terms of variation in spectral light intensity. The XRD and SEM analysis confirms the formation of hexagonal wurtzite structure with the grain size of 11.2 nm. The small cladding region of the optical fiber was replaced with the synthesized nanoparticles. The light spectrum was recorded for different gas concentrations. The synthesized nanoparticles showed high sensitivity towards ammonia in lowmore » ppm level and acetone in high ppm level.« less

Preparation and characterization of Ag-doped In2O3 nanoparticles gas sensor

NASA Astrophysics Data System (ADS)

Anand, Kanica; Kaur, Jasmeet; Singh, Ravi Chand; Thangaraj, Rengasamy

2017-08-01

Pure and Ag-doped In2O3 nanoparticles are synthesized by the co-precipitation method and are characterized by X-ray diffraction, transmission electron microscopy and photoluminescence spectroscopy. Gas sensing properties of the sensors has been investigated towards methanol, ethanol, acetone and LPG at different operating temperatures. It is found that the sensor response magnitude of the 3% Ag-doped In2O3 nanoparticles sensors is higher to 50 ppm of ethanol at 300 °C, to acetone at 350 °C and to LPG at 400 °C. This is mainly attributed to the large number of oxygen vacancies and defects in doped sensors as corroborated by the photoluminescence studies.

Novel Gas Sensor Based on ZnO Nanorod Circular Arrays for C2H5OH Gas Detection.

PubMed

Jianjiao, Zhang; Hongyan, Yue; Erjun, Guo; Shaolin, Zhang; Liping, Wang; Chunyu, Zhang; Xin, Gao; Jing, Chang; Hong, Zhang

2015-03-01

Novel side-heating gas sensor based on ZnO nanorod circular arrays was firstly fabricated by hydrothermal treatment assisted with a kind of simple dip-coating technique. The structure and morphologies of ZnO nanorods were characterized by X-ray diffraction (XRD), Scanning Electron Microscope (SEM), respectively. XRD result indicates that the obtained ZnO nanorods have good crystalline with the hexagonal wurtzite structure. SEM result indicates that ZnO nanorod arrays are vertically growth on the surface of ceramic tube of side-heating sensor with controlled diameter and length, narrow size distribution and high orientation. The gas sensing properties of ZnO nanorod circular arrays are also evaluated. Comparative to the sensor based on scattered ZnO nanorods responding to 25 ppm H2, CO, C6H5CH3 and C2H5OH gas, respectively, the sensing values of high orientation gas sensor are generally increased by 5%. This novel sensor has good application promising for the fabrication of cost effective and high performance gas sensors.

Si substrates texturing and vapor-solid-solid Si nanowhiskers growth using pure hydrogen as source gas

NASA Astrophysics Data System (ADS)

Nordmark, H.; Nagayoshi, H.; Matsumoto, N.; Nishimura, S.; Terashima, K.; Marioara, C. D.; Walmsley, J. C.; Holmestad, R.; Ulyashin, A.

2009-02-01

Scanning and transmission electron microscopies have been used to study silicon substrate texturing and whisker growth on Si substrates using pure hydrogen source gas in a tungsten hot filament reactor. Substrate texturing, in the nanometer to micrometer range of mono- and as-cut multicrystalline silicon, was observed after deposition of WSi2 particles that acted as a mask for subsequent hydrogen radical etching. Simultaneous Si whisker growth was observed for long residence time of the source gas and low H2 flow rate with high pressure. The whiskers formed via vapor-solid-solid growth, in which the deposited WSi2 particles acted as catalysts for a subsequent metal-induced layer exchange process well below the eutectic temperature. In this process, SiHx species, formed by substrate etching by the H radicals, diffuse through the metal particles. This leads to growth of crystalline Si whiskers via metal-induced solid-phase crystallization. Transmission electron microscopy, electron diffraction, and x-ray energy dispersive spectroscopy were used to study the WSi2 particles and the structure of the Si substrates in detail. It has been established that the whiskers are partly crystalline and partly amorphous, consisting of pure Si with WSi2 particles on their tips as well as sometimes being incorporated into their structure.

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

Relativistic electron diffraction at the UCLA Pegasus photoinjector laboratory.

PubMed

Musumeci, P; Moody, J T; Scoby, C M

2008-10-01

Electron diffraction holds the promise to yield real-time resolution of atomic motion in an easily accessible environment like a university laboratory at a fraction of the cost of fourth-generation X-ray sources. Currently the limit in time-resolution for conventional electron diffraction is set by how short an electron pulse can be made. A very promising solution to maintain the highest possible beam intensity without excessive pulse broadening from space charge effects is to increase the electron energy to the MeV level where relativistic effects significantly reduce the space charge forces. Rf photoinjectors can in principle deliver up to 10(7)-10(8) electrons packed in bunches of approximately 100-fs length, allowing an unprecedented time resolution and enabling the study of irreversible phenomena by single-shot diffraction patterns. The use of rf photoinjectors as sources for ultrafast electron diffraction has been recently at the center of various theoretical and experimental studies. The UCLA Pegasus laboratory, commissioned in early 2007 as an advanced photoinjector facility, is the only operating system in the country, which has recently demonstrated electron diffraction using a relativistic beam from an rf photoinjector. Due to the use of a state-of-the-art ultrashort photoinjector driver laser system, the beam has been measured to be sub-100-fs long, at least a factor of 5 better than what measured in previous relativistic electron diffraction setups. Moreover, diffraction patterns from various metal targets (titanium and aluminum) have been obtained using the Pegasus beam. One of the main laboratory goals in the near future is to fully develop the rf photoinjector-based ultrafast electron diffraction technique with particular attention to the optimization of the working point of the photoinjector in a low-charge ultrashort pulse regime, and to the development of suitable beam diagnostics.

Synthesis, characterization and experimental investigation of Cu-BTC as CO2 adsorbent from flue gas.

PubMed

Xie, Jiangkun; Yan, Naiqiang; Qu, Zan; Yang, Shijian

2012-01-01

Porous Cu-BTC material was synthesized by the solvothermal method. Powder X-ray diffraction (PXRD) was used to test the phase purity of the synthesized material and investigate its structural stability under the influence of flue gas components. The thermal stability of the material was determined through thermal gravimetric (TG) analysis. Scanning electron microscopy (SEM) was employed to study the microstructure of the material. Cu-BTC was demonstrated not only to have high CO2 adsorption capacity but also good selectivity of CO2 over N2 by means of packed bed tests. The adsorption capacity of Cu-BTC for CO2 was about 69 mL/g at 22 degrees C. The influence of the main flue gas components on the CO2 capacity of the material were discussed as well.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Groenen, Rik; Smit, Jasper; Orsel, Kasper

The oxidation of species in the plasma plume during pulsed laser deposition controls both the stoichiometry as well as the growth kinetics of the deposited SrTiO{sub 3} thin films, instead of the commonly assumed mass distribution in the plasma plume and the kinetic energy of the arriving species. It was observed by X-ray diffraction that SrTiO{sub 3} stoichiometry depends on the composition of the background gas during deposition, where in a relative small pressure range between 10{sup −2} mbars and 10{sup −1} mbars oxygen partial pressure, the resulting film becomes fully stoichiometric. Furthermore, upon increasing the oxygen (partial) pressure, themore » growth mode changes from 3D island growth to a 2D layer-by-layer growth mode as observed by reflection high energy electron diffraction.« less

Hydrogen sorption in Pd-decorated Mg-MgO core-shell nanoparticles

NASA Astrophysics Data System (ADS)

Callini, E.; Pasquini, L.; Piscopiello, E.; Montone, A.; Antisari, M. Vittori; Bonetti, E.

2009-06-01

Mg nanoparticles with metal-oxide core-shell morphology were synthesized by inert-gas condensation and decorated by in situ Pd deposition. Transmission electron microscopy and x-ray diffraction underline the formation of a noncontinuous layer with Pd clusters on top of the MgO shell. Even in the presence of a thick MgO interlayer, a modest (2 at. %) Pd decoration deeply enhances the hydrogen sorption properties: previously inert nanoparticles exhibit metal-hydride transformation with fast kinetics and gravimetric capacity above 5 wt %.

Properties of planar structures based on Policluster films of diamond and AlN

NASA Astrophysics Data System (ADS)

Belyanin, A. F.; Luchnikov, A. P.; Nalimov, S. A.; Bagdasarian, A. S.

2018-01-01

AlN films doped with zinc were grown on Si substrates by RF magnetron reactive sputtering of a compound target. Policluster films of diamond doped with boron were formed on layered Si/AlN substrates from the gas phase hydrogen and methane, activated arc discharge. By electron microscopy, X-ray diffraction and Raman spectroscopy the composition and structure of synthetic policluster films of diamond and AlN films were studied. Photovoltaic devices based on the AlN/PFD layered structure are presented.

Nanomodulated electron beams via electron diffraction and emittance exchange for coherent x-ray generation

NASA Astrophysics Data System (ADS)

Nanni, E. A.; Graves, W. S.; Moncton, D. E.

2018-01-01

We present a new method for generation of relativistic electron beams with current modulation on the nanometer scale and below. The current modulation is produced by diffracting relativistic electrons in single crystal Si, accelerating the diffracted beam and imaging the crystal structure, then transferring the image into the temporal dimension via emittance exchange. The modulation period can be tuned by adjusting electron optics after diffraction. This tunable longitudinal modulation can have a period as short as a few angstroms, enabling production of coherent hard x-rays from a source based on inverse Compton scattering with total accelerator length of approximately ten meters. Electron beam simulations from cathode emission through diffraction, acceleration, and image formation with variable magnification are presented along with estimates of the coherent x-ray output properties.

Synthesis of octahedral like Cu-BTC derivatives derived from MOF calcined under different atmosphere for application in CO oxidation

NASA Astrophysics Data System (ADS)

Yang, Yiqiong; Dong, Han; Wang, Yin; He, Chi; Wang, Yuxin; Zhang, Xiaodong

2018-02-01

A series of octahedral structure Cu-BTC derivatives were successfully achieved through direct calcination of copper based metal organic framework Cu-BTC under different atmosphere (CO reaction gas, oxidizing gas O2, reducing gas H2, inert gas Ar). The Cu-BTC derivatives were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), laser Raman spectroscopy (LRS), N2 adsorption-desorption isotherm, element analysis, H2-temperature program reduction (H2-TPR) and X-ray photoelectron spectroscopic (XPS). It is found that Cu-BTC derivative derived from MOF calcined under reaction gas/O2 (Cu-BTC-CO/Cu-BTC-O) only retain Cu2O and CuO species. In addition, a weak Cu-BTC structure and Cu particles were observed on Cu-BTC derivative derived from MOF calcined under H2 (Cu-BTC-H). Obviously differently, Cu-BTC derivative derived from MOF calcined under Ar (Cu-BTC-Ar) still retains good MOF structure. The catalytic performance for CO oxidation over Cu-BTC derivatives was studied. It was found that Cu-BTC-CO showed a smaller specific surface area (8.0 m2/g), but presented an excellent catalytic performance, long-term stability and cycling stability with a complete CO conversion temperature (T100) of 140 °C, which was ascribed to the higher Cu2O/CuO ratio, good low temperature reduction behavior and a high quantity of surface active oxygen species.

Ultrafast electron microscopy in materials science, biology, and chemistry

NASA Astrophysics Data System (ADS)

King, Wayne E.; Campbell, Geoffrey H.; Frank, Alan; Reed, Bryan; Schmerge, John F.; Siwick, Bradley J.; Stuart, Brent C.; Weber, Peter M.

2005-06-01

The use of pump-probe experiments to study complex transient events has been an area of significant interest in materials science, biology, and chemistry. While the emphasis has been on laser pump with laser probe and laser pump with x-ray probe experiments, there is a significant and growing interest in using electrons as probes. Early experiments used electrons for gas-phase diffraction of photostimulated chemical reactions. More recently, scientists are beginning to explore phenomena in the solid state such as phase transformations, twinning, solid-state chemical reactions, radiation damage, and shock propagation. This review focuses on the emerging area of ultrafast electron microscopy (UEM), which comprises ultrafast electron diffraction (UED) and dynamic transmission electron microscopy (DTEM). The topics that are treated include the following: (1) The physics of electrons as an ultrafast probe. This encompasses the propagation dynamics of the electrons (space-charge effect, Child's law, Boersch effect) and extends to relativistic effects. (2) The anatomy of UED and DTEM instruments. This includes discussions of the photoactivated electron gun (also known as photogun or photoelectron gun) at conventional energies (60-200 keV) and extends to MeV beams generated by rf guns. Another critical aspect of the systems is the electron detector. Charge-coupled device cameras and microchannel-plate-based cameras are compared and contrasted. The effect of various physical phenomena on detective quantum efficiency is discussed. (3) Practical aspects of operation. This includes determination of time zero, measurement of pulse-length, and strategies for pulse compression. (4) Current and potential applications in materials science, biology, and chemistry. UEM has the potential to make a significant impact in future science and technology. Understanding of reaction pathways of complex transient phenomena in materials science, biology, and chemistry will provide fundamental knowledge for discovery-class science.

Energy-weighted dynamical scattering simulations of electron diffraction modalities in the scanning electron microscope.

PubMed

Pascal, Elena; Singh, Saransh; Callahan, Patrick G; Hourahine, Ben; Trager-Cowan, Carol; Graef, Marc De

2018-04-01

Transmission Kikuchi diffraction (TKD) has been gaining momentum as a high resolution alternative to electron back-scattered diffraction (EBSD), adding to the existing electron diffraction modalities in the scanning electron microscope (SEM). The image simulation of any of these measurement techniques requires an energy dependent diffraction model for which, in turn, knowledge of electron energies and diffraction distances distributions is required. We identify the sample-detector geometry and the effect of inelastic events on the diffracting electron beam as the important factors to be considered when predicting these distributions. However, tractable models taking into account inelastic scattering explicitly are lacking. In this study, we expand the Monte Carlo (MC) energy-weighting dynamical simulations models used for EBSD [1] and ECP [2] to the TKD case. We show that the foil thickness in TKD can be used as a means of energy filtering and compare band sharpness in the different modalities. The current model is shown to correctly predict TKD patterns and, through the dictionary indexing approach, to produce higher quality indexed TKD maps than conventional Hough transform approach, especially close to grain boundaries. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Femtosecond time-resolved MeV electron diffraction

DOE PAGES

Zhu, Pengfei; Zhu, Y.; Hidaka, Y.; ...

2015-06-02

We report the experimental demonstration of femtosecond electron diffraction using high-brightness MeV electron beams. High-quality, single-shot electron diffraction patterns for both polycrystalline aluminum and single-crystal 1T-TaS 2 are obtained utilizing a 5 fC (~3 × 10 4 electrons) pulse of electrons at 2.8 MeV. The high quality of the electron diffraction patterns confirms that electron beam has a normalized emittance of ~50 nm rad. The transverse and longitudinal coherence length is ~11 and ~2.5 nm, respectively. The timing jitter between the pump laser and probe electron beam was found to be ~100 fs (rms). The temporal resolution is demonstrated bymore » observing the evolution of Bragg and superlattice peaks of 1T-TaS 2 following an 800 nm optical pump and was found to be 130 fs. Lastly, our results demonstrate the advantages of MeV electrons, including large elastic differential scattering cross-section and access to high-order reflections, and the feasibility of ultimately realizing below 10 fs time-resolved electron diffraction.« less

Electron diffraction covering a wide angular range from Bragg diffraction to small-angle diffraction.

PubMed

Nakajima, Hiroshi; Kotani, Atsuhiro; Harada, Ken; Mori, Shigeo

2018-04-09

We construct an electron optical system to investigate Bragg diffraction (the crystal lattice plane, 10-2 to 10-3 rad) with the objective lens turned off by adjusting the current in the intermediate lenses. A crossover was located on the selected-area aperture plane. Thus, the dark-field imaging can be performed by using a selected-area aperture to select Bragg diffraction spots. The camera length can be controlled in the range of 0.8-4 m without exciting the objective lens. Furthermore, we can observe the magnetic-field dependence of electron diffraction using the objective lens under weak excitation conditions. The diffraction mode for Bragg diffraction can be easily switched to a small-angle electron diffraction mode having a camera length of more than 100 m. We propose this experimental method to acquire electron diffraction patterns that depict an extensive angular range from 10-2 to 10-7 rad. This method is applied to analyze the magnetic microstructures in three distinct magnetic materials, i.e. a uniaxial magnetic structure of BaFe10.35Sc1.6Mg0.05O19, a martensite of a Ni-Mn-Ga alloy, and a helical magnetic structure of Ba0.5Sr1.5Zn2Fe12O22.

Hybrid Modes in Long Wavelength Free Electron Lasers

DTIC Science & Technology

2010-12-01

response, including the time for reviewing instruction, searching existing data sources, gathering and maintaining the data needed, and completing and...diffraction along one axis, allowing free space diffraction along the other axis. We continue the analysis of the relativistic electron beam, co-propagating...control diffraction along one axis, allowing free space diffraction along the other axis. We continue the analysis of the relativistic electron beam, co

Structure analysis of the single-domain Si(111)4 × 1-In surface by μ-probe Auger electron diffraction and μ-probe reflection high energy electron diffraction

NASA Astrophysics Data System (ADS)

Nakamura, N.; Anno, K.; Kono, S.

1991-10-01

A single-domain Si(111)4 × 1-In surface has been studied by μ-probe reflection high-energy electron diffraction (RHEED) to elucidate the symmetry of the 4 × 1 surface. Azimuthal diffraction patterns of In MNN Auger electron have been obtained by a μ-probe Auger electron diffraction (AED) apparatus from the single-domain Si(111)4 × 1-In surface. On the basis of information from scanning tunneling microscopy [J. Microsc. 152 (1988) 727] and under the assumption that the 4 × 1 surface is composed of In-overlayers, the μ-probe AED patterns were kinematically analyzed to reach a concrete model of indium arrangement.

Synthesis and study of the synthetic hydroxyapatite doped with aluminum

NASA Astrophysics Data System (ADS)

Goldberg, M.; Smirnov, V.; Antonova, O.; Konovalov, A.; Fomina, A.; Komlev, V. S.; Barinov, S.; Rodionov, A.; Gafurov, M.; Orlinskii, S.

2018-05-01

Powders of synthetic hydroxyapatite doped with aluminium (Al) ions in concentrations 0 and 20 mol. % were synthesized by the precipitation method from the nitrate solutions and investigated by atomic emission spectrometry with inductively coupled plasma (AES-ICP), X-ray diffraction (XRD), scanning electron microscopy (SEM), gas absorption and conventional electron paramagnetic resonance (EPR). It is shown that for the chosen synthesis route an introduction of Al provokes formation of highly anisotropic phase, leads to the decrease in the crystallinity while no significant changes in the EPR spectra of the radiation-induced defects is observed. The results could be used for understanding the structural transformations with Al doping of the mineralized materials for geological and biomedical applications.

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

DOE PAGES

Fan, D.; Huang, J. W.; Zeng, X. L.; ...

2016-05-23

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.« less

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fan, D.; Huang, J. W.; Zeng, X. L.

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.« less

Ammonia Gas Sensing Behavior of Tanninsulfonic Acid Doped Polyaniline-TiO2 Composite

PubMed Central

Bairi, Venu Gopal; Bourdo, Shawn E.; Sacre, Nicolas; Nair, Dev; Berry, Brian C.; Biris, Alexandru S.; Viswanathan, Tito

2015-01-01

A highly active tannin doped polyaniline-TiO2 composite ammonia gas sensor was developed and the mechanism behind the gas sensing activity was reported for the first time. A tanninsulfonic acid doped polyaniline (TANIPANI)-titanium dioxide nanocomposite was synthesized by an in situ polymerization of aniline in the presence of tanninsulfonic acid and titanium dioxide nanoparticles. X-ray diffraction and thermogravimetric analysis were utilized to determine the incorporation of TiO2 in TANIPANI matrix. UV-Visible and infrared spectroscopy studies provided information about the electronic interactions among tannin, polyaniline, and TiO2. Scanning electron microscopy (SEM) along with energy dispersive X-ray spectroscopy (EDS) and atomic force microscopy (AFM) surface analysis techniques were used to investigate the metal oxide dispersions inside polyaniline matrix. Gas sensors were prepared by spin coating solutions of TANIPANI-TiO2 and TANIPANI composites onto glass slides. Sensors were tested at three different concentrations (20 ppm, 40 ppm, and 60 ppm) of ammonia gas at ambient temperature conditions by measuring the changes in surface resistivity of the films with respect to time. Ammonia gas sensing plots are presented showing the response values, response times and recovery times. The TANIPANI-TiO2 composite exhibited better response and shorter recovery times when compared to TANIPANI control and other polyaniline composites that have been reported in the literature. For the first time a proposed mechanism of gas sensing basing on the polaron band localization and its effects on the gas sensing behavior of polyaniline are reported. PMID:26501291

Pt-decorated GaN nanowires with significant improvement in H2 gas-sensing performance at room temperature.

PubMed

Abdullah, Q N; Yam, F K; Hassan, Z; Bououdina, M

2015-12-15

Superior sensitivity towards H2 gas was successfully achieved with Pt-decorated GaN nanowires (NWs) gas sensor. GaN NWs were fabricated via chemical vapor deposition (CVD) route. Morphology (field emission scanning electron microscopy and transmission electron microscopy) and crystal structure (high resolution X-ray diffraction) characterizations of the as-synthesized nanostructures demonstrated the formation of GaN NWs having a wurtzite structure, zigzaged shape and an average diameter of 30-166nm. The Pt-decorated GaN NWs sensor shows a high response of 250-2650% upon exposure to H2 gas concentration from 7 to 1000ppm respectively at room temperature (RT), and then increases to about 650-4100% when increasing the operating temperature up to 75°C. The gas-sensing measurements indicated that the Pt-decorated GaN NWs based sensor exhibited efficient detection of H2 at low concentration with excellent sensitivity, repeatability, and free hysteresis phenomena over a period of time of 100min. The large surface-to-volume ratio of GaN NWs and the catalytic activity of Pt metal are the most influential factors leading to the enhancement of H2 gas-sensing performances through the improvement of the interaction between the target molecules (H2) and the sensing NWs surface. The attractive low-cost, low power consumption and high-performance of the resultant decorated GaN NWs gas sensor assure their uppermost potential for H2 gas sensor working at low operating temperature. Copyright © 2015 Elsevier Inc. All rights reserved.

Nanomodulated electron beams via electron diffraction and emittance exchange for coherent x-ray generation

DOE PAGES

Nanni, E. A.; Graves, W. S.; Moncton, D. E.

2018-01-19

We present a new method for generation of relativistic electron beams with current modulation on the nanometer scale and below. The current modulation is produced by diffracting relativistic electrons in single crystal Si, accelerating the diffracted beam and imaging the crystal structure, then transferring the image into the temporal dimension via emittance exchange. The modulation period can be tuned by adjusting electron optics after diffraction. This tunable longitudinal modulation can have a period as short as a few angstroms, enabling production of coherent hard x-rays from a source based on inverse Compton scattering with total accelerator length of approximately tenmore » meters. Electron beam simulations from cathode emission through diffraction, acceleration, and image formation with variable magnification are presented along with estimates of the coherent x-ray output properties.« less

Nanomodulated electron beams via electron diffraction and emittance exchange for coherent x-ray generation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nanni, E. A.; Graves, W. S.; Moncton, D. E.

We present a new method for generation of relativistic electron beams with current modulation on the nanometer scale and below. The current modulation is produced by diffracting relativistic electrons in single crystal Si, accelerating the diffracted beam and imaging the crystal structure, then transferring the image into the temporal dimension via emittance exchange. The modulation period can be tuned by adjusting electron optics after diffraction. This tunable longitudinal modulation can have a period as short as a few angstroms, enabling production of coherent hard x-rays from a source based on inverse Compton scattering with total accelerator length of approximately tenmore » meters. Electron beam simulations from cathode emission through diffraction, acceleration, and image formation with variable magnification are presented along with estimates of the coherent x-ray output properties.« less

Synthesis and characterization of InNbO₄ nanopowder for gas sensors.

PubMed

Balamurugan, C; Vijayakumar, E; Subramania, A

2012-01-15

Indium niobate (InNbO(4)) nanopowder was prepared by a comparatively low temperature niobium citrate complex process. The prepared InNbO(4) was characterized by thermal analysis, X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy, diffuse reflectance spectroscopy (DRS), and impedance studies. It revealed that the well crystalline monoclinic InNbO(4) nanopowder was obtained at the calcination temperature of 600°C. The average particle diameter was 22nm. The optical band gap was found to be 2.66eV. The temperature dependent conductivity obeyed Arrhenius relation. The activation energy of the conductivity process was calculated to be 0.43eV. The gas sensing behaviour of the prepared InNbO(4) was studied by measuring the change in resistance of the sensor material as a function of various concentrations of the test gases such as liquid petroleum gas (LPG), ammonia (NH(3)) and ethanol (C(2)H(5)OH) at their optimized operating temperature. InNbO(4) had a better sensitivity to LPG (0.97) and NH(3) (0.70) gas than ethanol (0.46). The sensor responses of InNbO(4) as a function of gas concentrations and with recovery time were also studied in detail. Copyright © 2011 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Haishuang; Krysiak, Yaşar; Hoffmann, Kristin

The crystal structure and disorder phenomena of Al{sub 4}B{sub 2}O{sub 9}, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al{sub 4}B{sub 2}O{sub 9}, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO{sub 6} octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along themore » b axis are observed. Analysis of the modulation pattern implies a mean superstructure (AAB) with a threefold b axis, where B corresponds to an A layer shifted by ½a and ½c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns. - Graphical abstract: Crystal structure and disorder phenomena of B-rich Al{sub 4}B{sub 2}O{sub 9} studied by automated electron diffraction tomography (ADT) and described by diffraction simulation using DISCUS. - Highlights: • Ab-initio structure solution by electron diffraction from single nanocrystals. • Detected modulation corresponding mainly to three-fold superstructure. • Diffuse diffraction streaks caused by stacking faults in disordered crystals. • Observed streaks explained by simulated electron diffraction patterns.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eaton, Craig; Brahlek, Matthew; Engel-Herbert, Roman, E-mail: rue2@psu.edu

The authors report the growth of stoichiometric SrVO{sub 3} thin films on (LaAlO{sub 3}){sub 0.3}(Sr{sub 2}AlTaO{sub 6}){sub 0.7} (001) substrates using hybrid molecular beam epitaxy. This growth approach employs a conventional effusion cell to supply elemental A-site Sr and the metalorganic precursor vanadium oxytriisopropoxide (VTIP) to supply vanadium. Oxygen is supplied in its molecular form through a gas inlet. An optimal VTIP:Sr flux ratio has been identified using reflection high-energy electron-diffraction, x-ray diffraction, atomic force microscopy, and scanning transmission electron microscopy, demonstrating stoichiometric SrVO{sub 3} films with atomically flat surface morphology. Away from the optimal VTIP:Sr flux, characteristic changes inmore » the crystalline structure and surface morphology of the films were found, enabling identification of the type of nonstoichiometry. For optimal VTIP:Sr flux ratios, high quality SrVO{sub 3} thin films were obtained with smallest deviation of the lattice parameter from the ideal value and with atomically smooth surfaces, indicative of the good cation stoichiometry achieved by this growth technique.« less

Solar physical vapor deposition preparation and microstructural characterization of TiO2 based nanophases for dye-sensitized solar cell applications.

PubMed

Negrea, Denis; Ducu, Catalin; Moga, Sorin; Malinovschi, Viorel; Monty, Claude J A; Vasile, Bogdan; Dorobantu, Dorel; Enachescu, Marian

2012-11-01

Titanium dioxide exists in three crystalline phases: anatase, rutile and brookite. Although rutile is thermodynamically more stable, anatase is considered as the most favorable phase for photocatalysis and solar energy conversion. Recent studies have shown a significant improvement of light harvesting and overall solar conversion efficiency of anatase nanoparticles in dye-sensitized solar cells (DSSCs) when using a mixture of anatase and rutile phases (10-15% rutile). TiO2 nanopowders have been prepared by a solar physical vapor deposition process (SPVD). This method has been developed in Odeillo-Font Romeu France using "heliotron" solar reactors working under concentrated sunlight in 2 kW solar furnaces. By controlling reactor's atmosphere type (air/argon) and gas pressure, several types of anatase/rutile nanophases have been obtained with slightly different microstructural properties and morphological characteristics. X-ray diffraction analyses (XRD) were performed on precursor and on the SPVD obtained nanopowders. Information concerning their phase composition and coherence diffraction domain (crystallites size and strain) was obtained. Nanopowders morphology has been studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM).

Properties of Nitrogen-Doped Zinc Telluride Films for Back Contact to Cadmium Telluride Photovoltaics

NASA Astrophysics Data System (ADS)

Shimpi, Tushar M.; Drayton, Jennifer; Swanson, Drew E.; Sampath, Walajabad S.

2017-08-01

Zinc telluride (ZnTe) films have been deposited onto uncoated glass superstrates by reactive radiofrequency (RF) sputtering with different amounts of nitrogen introduced into the process gas, and the structural and electronic transport properties of the resulting nitrogen-doped ZnTe (ZnTe:N) films characterized. Based on transmission and x-ray diffraction measurements, it was observed that the crystalline quality of the ZnTe:N films decreased with increasing nitrogen in the deposition process. The bulk carrier concentration of the ZnTe:N films determined from Hall-effect measurements showed a slight decrease at 4% nitrogen flow rate. The effect of ZnTe:N films as back contact to cadmium telluride (CdTe) solar cells was also investigated. ZnTe:N films were deposited before or after CdCl2 passivation on CdTe/CdS samples. Small-area devices were characterized for their electronic properties. Glancing-angle x-ray diffraction measurements and energy-dispersive spectroscopy analysis confirmed substantial loss of zinc from the samples where CdCl2 passivation was carried out after ZnTe:N film deposition.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mirzaei, B.; Silva, J. R. G.; Hayton, D.

We present an 8-beam local oscillator (LO) for the astronomically significant [OI] line at 4.7 THz. The beams are generated using a quantum cascade laser (QCL) in combination with a Fourier phase grating. The grating is fully characterized using a third order distributed feedback (DFB) QCL with a single mode emission at 4.7 THz as the input. The measured diffraction efficiency of 74.3% is in an excellent agreement with the calculated result of 75.4% using a 3D simulation. We show that the power distribution among the diffracted beams is uniform enough for pumping an array receiver. To validate the gratingmore » bandwidth, we apply a far-infrared (FIR) gas laser emission at 5.3 THz as the input and find a very similar performance in terms of efficiency, power distribution, and spatial configuration of the diffracted beams. Both results represent the highest operating frequencies of THz phase gratings reported in the literature. By injecting one of the eight diffracted 4.7 THz beams into a superconducting hot electron bolometer (HEB) mixer, we find that the coupled power, taking the optical loss into account, is in consistency with the QCL power value.« less

8-beam local oscillator array at 4.7 THz generated by a phase grating and a quantum cascade laser.

PubMed

Mirzaei, B; Silva, J R G; Hayton, D; Groppi, C; Kao, T Y; Hu, Q; Reno, J L; Gao, J R

2017-11-27

We present an 8-beam local oscillator (LO) for the astronomically significant [OI] line at 4.7 THz. The beams are generated using a quantum cascade laser (QCL) in combination with a Fourier phase grating. The grating is fully characterized using a third order distributed feedback (DFB) QCL with a single mode emission at 4.7 THz as the input. The measured diffraction efficiency of 74.3% is in an excellent agreement with the calculated result of 75.4% using a 3D simulation. We show that the power distribution among the diffracted beams is uniform enough for pumping an array receiver. To validate the grating bandwidth, we apply a far-infrared (FIR) gas laser emission at 5.3 THz as the input and find a very similar performance in terms of efficiency, power distribution, and spatial configuration of the diffracted beams. Both results represent the highest operating frequencies of THz phase gratings reported in the literature. By injecting one of the eight diffracted 4.7 THz beams into a superconducting hot electron bolometer (HEB) mixer, we find that the coupled power, taking the optical loss into account, is in consistency with the QCL power value.

Core Perylene Diimide Designs via Direct Bay- and ortho-(Poly)trifluoromethylation: Synthesis, Isolation, X-Ray Structures, Optical and Electronic Properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clikeman, Tyler T.; Bukovsky, Eric V.; Wang, Xue-Bin

2015-09-22

We developed an efficient solvent- and catalyst-free direct polytrifluoromethylation of solid perylene-3,4,9,10-tetracarboxylic dianhydride that produced a new family of (poly)perfluoroalkyl bay- and ortho-substituted PDIs with two different imide substituents. Direct hydrogen substitution with CN group led to the synthesis of a cyanated perfluoroalkyl PDI derivative for the first time. Absorption, steady-state and time-resolved emission, X-ray diffraction, electrochemical, and gas-phase electron affinity data allowed for systematic studies of substitution effects at bay, ortho, and imide positions in the new PDIs. Solid-state packing showed remarkable variations in the intermolecular interactions that are important for charge transport and photophysical properties. Moreover, analysis ofmore » the electrochemical data for 143 electron poor PDIs, including newly reported compounds, revealed some general trends and peculiar effects from substituting electron-withdrawing groups at all three positions.« less

Core Perylene Diimide Designs via Direct Bay and Ortho (Poly)trifluoromethylation: Synthesis, Isolation, X-ray Structures, Optical and Electronic Properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clikeman, Tyler T.; Bukovsky, Eric V.; Wang, Xue B.

2015-09-22

We developed an efficient solvent- and catalyst-free direct polytrifluoromethylation of solid perylene-3,4,9,10-tetracarboxylic dianhydride that produced a new family of (poly)perfluoroalkyl bay and ortho substituted PDIs with two different imide substituents. Direct hydrogen substitution with CN group led to the synthesis of a cyanated perfluoroalkyl PDI derivative for the first time. Absorption, steady-state and time-resolved emission, X-ray diffraction, electrochemical, and gas-phase electron affinity data allowed for systematic studies of substitution effects at bay, ortho, and imide positions in the new PDIs. Solid-state packing showed remarkable variations in the intermolecular interactions that are important for charge transport and photophysical properties. Analysis ofmore » the electrochemical data for 143 electron poor PDIs, including newly reported compounds, revealed some general trends and peculiar effects of electron withdrawing group substitution at all three positions.« less

Observations on the Role of Hydrogen in Facet Formation in Near-alpha Titanium (Preprint)

DTIC Science & Technology

2011-05-01

using quantitative tilt fractography and electron backscatter diffraction while facet topography was examined using ultra high resolution scanning...quantitative tilt fractography and electron backscatter diffraction while facet topography was examined using ultra high resolution scanning electron...tilt fractography / electron backscatter diffraction (EBSD) technique in which both the crystallographic orientation of the fractured grain and the

Total-scattering pair-distribution function of organic material from powder electron diffraction data.

PubMed

Gorelik, Tatiana E; Schmidt, Martin U; Kolb, Ute; Billinge, Simon J L

2015-04-01

This paper shows that pair-distribution function (PDF) analyses can be carried out on organic and organometallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction and nanodiffraction in transmission electron microscopy or nanodiffraction in scanning transmission electron microscopy modes. The methods were demonstrated on organometallic complexes (chlorinated and unchlorinated copper phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering data and avoiding beam damage of the sample are possible to resolve.

Simple fabrication process for 2D ZnO nanowalls and their potential application as a methane sensor.

PubMed

Chen, Tse-Pu; Chang, Sheng-Po; Hung, Fei-Yi; Chang, Shoou-Jinn; Hu, Zhan-Shuo; Chen, Kuan-Jen

2013-03-20

Two-dimensional (2D) ZnO nanowalls were prepared on a glass substrate by a low-temperature thermal evaporation method, in which the fabrication process did not use a metal catalyst or the pre-deposition of a ZnO seed layer on the substrate. The nanowalls were characterized for their surface morphology, and the structural and optical properties were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence (PL). The fabricated ZnO nanowalls have many advantages, such as low growth temperature and good crystal quality, while being fast, low cost, and easy to fabricate. Methane sensor measurements of the ZnO nanowalls show a high sensitivity to methane gas, and rapid response and recovery times. These unique characteristics are attributed to the high surface-to-volume ratio of the ZnO nanowalls. Thus, the ZnO nanowall methane sensor is a potential gas sensor candidate owing to its good performance.

A novel flexible room temperature ethanol gas sensor based on SnO2 doped poly-diallyldimethylammonium chloride.

PubMed

Zhan, Shuang; Li, Dongmei; Liang, Shengfa; Chen, Xin; Li, Xia

2013-04-02

A novel flexible room temperature ethanol gas sensor was fabricated and demonstrated in this paper. The polyimide (PI) substrate-based sensor was formed by depositing a mixture of SnO2 nanopowder and poly-diallyldimethylammonium chloride (PDDAC) on as-patterned interdigitated electrodes. PDDAC acted both as the binder, promoting the adhesion between SnO2 and the flexible PI substrate, and the dopant. We found that the response of SnO2-PDDAC sensor is significantly higher than that of SnO2 alone, indicating that the doping with PDDAC effectively improved the sensor performance. The SnO2-PDDAC sensor has a detection limit of 10 ppm at room temperature and shows good selectivity to ethanol, making it very suitable for monitoring drunken driving. The microstructures of the samples were examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscope (TEM) and Fourier transform infrared spectra (FT-IR), and the sensing mechanism is also discussed in detail.

Simple Fabrication Process for 2D ZnO Nanowalls and Their Potential Application as a Methane Sensor

PubMed Central

Chen, Tse-Pu; Chang, Sheng-Po; Hung, Fei-Yi; Chang, Shoou-Jinn; Hu, Zhan-Shuo; Chen, Kuan-Jen

2013-01-01

Two-dimensional (2D) ZnO nanowalls were prepared on a glass substrate by a low-temperature thermal evaporation method, in which the fabrication process did not use a metal catalyst or the pre-deposition of a ZnO seed layer on the substrate. The nanowalls were characterized for their surface morphology, and the structural and optical properties were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence (PL). The fabricated ZnO nanowalls have many advantages, such as low growth temperature and good crystal quality, while being fast, low cost, and easy to fabricate. Methane sensor measurements of the ZnO nanowalls show a high sensitivity to methane gas, and rapid response and recovery times. These unique characteristics are attributed to the high surface-to-volume ratio of the ZnO nanowalls. Thus, the ZnO nanowall methane sensor is a potential gas sensor candidate owing to its good performance. PMID:23519350

Investigation of the gas-phase structure and rotational barrier of trimethylsilyl trifluoromethanesulfonate and comparison with covalent sulfonates

NASA Astrophysics Data System (ADS)

Defonsi Lestard, María E.; Tuttolomondo, María E.; Varetti, Eduardo L.; Wann, Derek A.; Robertson, Heather E.; Rankin, David W. H.; Altabef, Aida Ben

2010-12-01

The molecular structure of trimethylsilyl trifluoromethanesulfonate, CF 3SO 2OSi(CH 3) 3, has been determined in the gas phase from electron-diffraction data supplemented by ab initio (MP2) and DFT calculations using 6-31G(d), 6-311++G(d,p) and 6-311G++(3df,3pd) basis sets. Both experimental and theoretical data indicate that only one gauche conformer is possible by rotating about the O-S bond. The anomeric effect is a fundamental stereoelectronic interaction and presents a profound influence on the electronic geometry. We have investigated the origin of the anomeric effect by means of NBO and AIM analysis. A natural bond orbital analysis showed that the lpπ[O bonded to Si)] → σ *[C-S] hyperconjugative interaction favors the gauche conformation. In addition, comparison of the structural and stereoelectronic properties of the title molecule with those of silyl trifluoromethanesulfonate and methyl trifluoromethanesulfonate has been carried out.

Oxidation-chlorination of binary Ni-Cr alloys in flowing Ar-O2-Cl2 gas mixtures at 1200 K

NASA Technical Reports Server (NTRS)

Mcnallan, M. J.; Lee, Y. Y.; Chang, Y. W.; Jacobson, N. S.; Doychak, J.

1991-01-01

Nickel-chromium alloys are resistant to oxidation because of the selective oxidation of chromium to form a protective Cr2O3 scale. In chlorine-containing environments, volatile corrosion products can also be formed. The mixed oxidation-chlorination of Ni-4.5Cr, Ni-13.8Cr, and Ni-26.5Cr (by weight) alloys in Ar-O2-Cl2 gas mixtures is investigated using thermogravimetric analysis and atmospheric-pressure-sampling mass spectrometry, followed by examination of the corrosion products using scanning electron microscopy and X-ray diffraction analysis. The overall kinetics of the corrosion are affected by the relative amounts of oxides and chlorides formed and the composition of the oxide corrosion products.

Investigation on the Enhanced Oxidation of Ferritic/Martensitic Steel P92 in Pure Steam

PubMed Central

Yuan, Juntao; Wu, Ximao; Wang, Wen; Zhu, Shenglong; Wang, Fuhui

2014-01-01

Oxidation of ferritic/martensitic steel P92 was investigated in pure oxygen and in pure steam at 600–800 °C by thermogravimetric analysis (TGA), optical microscopy (OM), scanning electron microscopy (SEM), and X-ray diffraction (XRD). The results showed that the oxidation of P92 was significantly enhanced and multilayer scale with an outer iron oxides layer formed in pure steam. At 700 °C, the gas switch markedly influenced the scaling kinetics and scale microstructure. It was supposed that the higher affinity of iron to steam would be attributed to the enhanced oxidation of P92 in pure steam, and the much easier transport of hydroxyl would account for the significant difference induced by gas switch. PMID:28788592

3D visualization of molecular structures in the MOGADOC database

NASA Astrophysics Data System (ADS)

Vogt, Natalja; Popov, Evgeny; Rudert, Rainer; Kramer, Rüdiger; Vogt, Jürgen

2010-08-01

The MOGADOC database (Molecular Gas-Phase Documentation) is a powerful tool to retrieve information about compounds which have been studied in the gas-phase by electron diffraction, microwave spectroscopy and molecular radio astronomy. Presently the database contains over 34,500 bibliographic references (from the beginning of each method) for about 10,000 inorganic, organic and organometallic compounds and structural data (bond lengths, bond angles, dihedral angles, etc.) for about 7800 compounds. Most of the implemented molecular structures are given in a three-dimensional (3D) presentation. To create or edit and visualize the 3D images of molecules, new tools (special editor and Java-based 3D applet) were developed. Molecular structures in internal coordinates were converted to those in Cartesian coordinates.

Synthesis of Zeolite-X from Bottom Ash for H2 Adsorption

NASA Astrophysics Data System (ADS)

Kurniawan, R. Y.; Romadiansyah, T. Q.; Tsamarah, A. D.; Widiastuti, N.

2018-01-01

Zeolite-X was synthesized from bottom ash power plant waste using fusion method on air atmosphere. The fused product dissolved in demineralized water and aluminate solution was added to adjust the SiO2/Al2O3 molar ratio gel prior hydrothermal process. The synthesis results were characterized using X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Fourier Transform Infrared (FTIR). The results showed that the zeolite-X has a high crystallinity with octahedral particle. The pure-form zeolite-X then was characterized and tested for H2 gas adsorption by gravimetric method to determine the H2 gas adsorption capacity of zeolite-X from bottom ash and it was compared to synthetic zeolite-X.

Enhancement of two dimensional electron gas concentrations due to Si{sub 3}N{sub 4} passivation on Al{sub 0.3}Ga{sub 0.7}N/GaN heterostructure: strain and interface capacitance analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dinara, Syed Mukulika, E-mail: smdinara.iit@gmail.com; Jana, Sanjay Kr.; Ghosh, Saptarsi

2015-04-15

Enhancement of two dimensional electron gas (2DEG) concentrations at Al{sub 0.3}Ga{sub 0.7}N/GaN hetero interface after a-Si{sub 3}N{sub 4} (SiN) passivation has been investigated from non-destructive High Resolution X-ray Diffraction (HRXRD) analysis, depletion depth and capacitance-voltage (C-V) profile measurement. The crystalline quality and strained in-plane lattice parameters of Al{sub 0.3}Ga{sub 0.7}N and GaN were evaluated from double axis (002) symmetric (ω-2θ) diffraction scan and double axis (105) asymmetric reciprocal space mapping (DA RSM) which revealed that the tensile strain of the Al{sub 0.3}Ga{sub 0.7}N layer increased by 15.6% after SiN passivation. In accordance with the predictions from theoretical solution of Schrödinger-Poisson’smore » equations, both electrochemical capacitance voltage (ECV) depletion depth profile and C-V characteristics analyses were performed which implied effective 9.5% increase in 2DEG carrier density after passivation. The enhancement of polarization charges results from increased tensile strain in the Al{sub 0.3}Ga{sub 0.7}N layer and also due to the decreased surface states at the interface of SiN/Al{sub 0.3}Ga{sub 0.7}N layer, effectively improving the carrier confinement at the interface.« less

rf streak camera based ultrafast relativistic electron diffraction.

PubMed

Musumeci, P; Moody, J T; Scoby, C M; Gutierrez, M S; Tran, T

2009-01-01

We theoretically and experimentally investigate the possibility of using a rf streak camera to time resolve in a single shot structural changes at the sub-100 fs time scale via relativistic electron diffraction. We experimentally tested this novel concept at the UCLA Pegasus rf photoinjector. Time-resolved diffraction patterns from thin Al foil are recorded. Averaging over 50 shots is required in order to get statistics sufficient to uncover a variation in time of the diffraction patterns. In the absence of an external pump laser, this is explained as due to the energy chirp on the beam out of the electron gun. With further improvements to the electron source, rf streak camera based ultrafast electron diffraction has the potential to yield truly single shot measurements of ultrafast processes.

Thermal evaporation and condensation synthesis of metallic Zn layered polyhedral microparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khan, Waheed S.; Cao, Chuanbao, E-mail: cbcao@bit.edu.cn; Usman, Zahid

2011-12-15

Highlights: Black-Right-Pointing-Pointer Zn polyhedral microparticles prepared by thermal evaporation and condensation route. Black-Right-Pointing-Pointer Vapour-solid process based growth model governs the formation of Zn microparticles. Black-Right-Pointing-Pointer A strong PL emission band is observed at 369 nm in UV region. Black-Right-Pointing-Pointer Radiative recombination of electrons in the s, p conduction band and the holes in the d bands causes this emission. -- Abstract: Metallic zinc layered polyhedral microparticles have been fabricated by thermal evaporation and condensation technique using zinc as precursor at 750 Degree-Sign C for 120 min and NH{sub 3} as a carrier gas. The zinc polyhedral microparticles with oblate sphericalmore » shape are observed to be 2-9 {mu}m in diameter along major axes and 1-7 {mu}m in thickness along minor axes. The structural, compositional and morphological characterizations were performed by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). A vapour-solid (VS) mechanism based growth model has been proposed for the formation of Zn microparticles. Room temperature photoluminescence (PL) emission spectrum of the product exhibited a strong emission band at 369 nm attributed to the radiative recombination of electrons in the s, p conduction band near Fermi surface and the holes in the d bands generated by the optical excitation.« less

Gas Sensing Properties of p-Co₃O₄/n-TiO₂ Nanotube Heterostructures.

PubMed

Alev, Onur; Kılıç, Alp; Çakırlar, Çiğdem; Büyükköse, Serkan; Öztürk, Zafer Ziya

2018-03-23

In this paper, we fabricated p-Co₃O₄/n-TiO₂ heterostructures and investigated their gas sensing properties. The structural and morphological characterization were performed by scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy analysis (XPS). The electrical properties of the heterostructure were studied within the temperature range from 293 K to 423 K. Changes in electrical properties and sensing behavior against reducing and oxidizing gases were attributed to the formation of p-n heterojunctions at the Co₃O₄ and TiO₂ interface. In comparison with sensing performed with pristine TiO₂ nanotubes (NTs), a significant improvement in H₂ sensing at 200 °C was observed, while the sensing response against NO₂ decreased for the heterostructures. Additionally, a response against toluene gas, in contrast to pristine TiO₂ NTs, appeared in the Co₃O₄/TiO₂ heterostructure samples.

A novel process for comprehensive utilization of vanadium slag

NASA Astrophysics Data System (ADS)

Liu, Li-ying; Du, Tao; Tan, Wen-jun; Zhang, Xin-pu; Yang, Fan

2016-02-01

Traditional processes for treating vanadium slag generate a huge volume of solid residue and a large amount of harmful gas, which cause serious environmental problems. In this study, a new process for the comprehensive utilization of vanadium slag was proposed, wherein zeolite A and a V2O5/TiO2 system were synthesized. The structural properties of the as-synthesized zeolite A and the V2O5/TiO2 system were characterized using various experimental techniques, including X-ray diffraction, X-ray fluorescence, scanning electron microscopy, and infrared spectroscopy. The results reveal that zeolite A and the V2O5/TiO2 system are successfully obtained with high purity. The results of gas adsorption measurements indicate that the prepared zeolite A exhibits high selectivity for CO2 over N2 and is a candidate material for CO2 capture from flue-gas streams.

Investigating NO2 gas sensing behavior of flower-like MoS2 and rGO based nano-composite

NASA Astrophysics Data System (ADS)

Kanaujiya, Neha; Anupam, Golimar, Kapil; Pandey, Prateek Chandra; Jyoti, Varma, G. D.

2018-05-01

In the present work, MoS2 nano-sheets with flower-like morphology have been synthesized by facile hydrothermal method. The nano-composite of MoS2 and reduced graphene oxide (rGO) nano-sheets has been synthesized to study the gas sensing behavior. The structural and morphological characteristics of the as prepared samples are investigated by X-ray diffraction (XRD) and Field emission scanning electron microscopy (FESEM) respectively. The gas sensing behavior of the as synthesized MoS2 and composite samples have been studied for different concentrations of NO2 at different temperatures. Improvement in sensing response of composite sample as compared to bare MoS2 sample has been observed. Percentage response of ˜ 23% has been observed at room temperature for 40ppm NO2. The detail correlation between gas sensing behavior and structural characteristics of the composite sample will be described and discussed in this paper.

Effect of argon ion activity on the properties of Y 2O 3 thin films deposited by low pressure PACVD

NASA Astrophysics Data System (ADS)

Barve, S. A.; Jagannath; Deo, M. N.; Kishore, R.; Biswas, A.; Gantayet, L. M.; Patil, D. S.

2010-10-01

Yttrium oxide thin films are deposited by microwave electron cyclotron resonance (ECR) plasma assisted metal organic chemical vapour deposition process using an indegeneously developed Y(thd) 3 {(2,2,6,6-tetramethyl-3,5-heptanedionate)yttrium} precursor. Depositions were carried out at two different argon gas flow rates keeping precursor and oxygen gas flow rate constant. The deposited coatings are characterized by X-ray photoelectron spectroscopy (XPS), glancing angle X-ray diffraction (GIXRD) and infrared spectroscopy. Optical properties of the films are studied by spectroscopic ellipsometry. Hardness and elastic modulus of the films are measured by load depth sensing nanoindentation technique. Stability of the film and its adhesion with the substrate is inferred from the nanoscratch test. It is shown here that, the change in the argon gas flow rates changes the ionization of the gas in the microwave ECR plasma and imposes a drastic change in the characteristics like composition, structure as well as mechanical properties of the deposited film.

Influence of Different Aluminum Sources on the NH3 Gas-Sensing Properties of ZnO Thin Films

NASA Astrophysics Data System (ADS)

Ozutok, Fatma; Karaduman, Irmak; Demiri, Sani; Acar, Selim

2018-02-01

Herein we report Al-doped ZnO films (AZO) deposited on the ZnO seed layer by chemical bath deposition method. Al powder, Al oxide and Al chloride were used as sources for the deposition process and investigated for their different effects on the NH3 gas-sensing performance. The morphological and microstructural properties were investigated by employing x-ray powder diffraction, scanning electron microscopy analysis and energy-dispersive x-ray spectroscopy. The characterization studies showed that the AZO thin films are crystalline and exhibit a hexagonal wurtzite structure. Ammonia (NH3) gas-sensing measurements of AZO films were performed at different concentration levels and different operation temperatures from 50°C to 210°C. The sample based on powder-Al source showed a higher response, selectivity and short response/recovery time than the remaining samples. The powder Al sample exhibited 33% response to 10-ppm ammonia gas at 190°C, confirming a strong dependence on the dopant source type.

Room-temperature H2S Gas Sensor Based on Au-doped ZnFe2O4 Yolk-shell Microspheres.

PubMed

Yan, Yin; Nizamidin, Patima; Turdi, Gulmira; Kari, Nuerguli; Yimit, Abliz

2017-01-01

Room-temperature type H 2 S sensing devices that use Au-doped ZnFe 2 O 4 yolk-shell microspheres as the active material have been fabricated using a solvothermal method as well as subsequent annealing and a chemical etching process. The samples are characterized using X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), field-emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS). The results demonstrate that the doping of Au does not change the spinel structure of the products, which were yolk-shell microspheres, while the particle size varied with the Au doping concentration. Also, the as-fabricated sensor device exhibited excellent selectivity toward H 2 S gas at the room temperature; the gas-sensing property of 2 wt% Au-doped ZnFe 2 O 4 microspheres was the best. The Au-doped ZnFe 2 O 4 yolk-shell microspheres can be promising as a sensing material for H 2 S gas detecting at room temperature.

Effect of solution plasma process with bubbling gas on physicochemical properties of chitosan.

PubMed

Ma, Fengming; Li, Pu; Zhang, Baiqing; Zhao, Xin; Fu, Qun; Wang, Zhenyu; Gu, Cailian

2017-05-01

In the present work, solution plasma process (SPP) with bubbling gas was used to prepare oligochitosan. The effect of SPP irradiation with bubbling gas on the degradation of chitosan was evaluated by the intrinsic viscosity reduction rate and the degradation kinetic. The formation of OH radical was studied. Changes of the physicochemical properties of chitosan were measured by scanning electron microscopy, X-ray diffraction, and thermogravimetric analysis, as well as ultraviolet-visible, Fourier-transform infrared, and 13 C nuclear magnetic resonance spectroscopy. The results indicated an obvious decrease in the intrinsic viscosity reduction rate after SPP irradiation with bubbling gas, and that the rate with bubbling was higher than that without. The main chemical structure of chitosan remained intact after irradiation, but changes in the morphology, crystallinity, and thermal stability of oligochitosan were observed. In particular, the crystallinity and thermal stability tended to decrease. The present study indicated that SPP can be effectively used for the degradation of chitosan. Copyright © 2017. Published by Elsevier B.V.

CuO-Decorated ZnO Hierarchical Nanostructures as Efficient and Established Sensing Materials for H2S Gas Sensors

PubMed Central

Vuong, Nguyen Minh; Chinh, Nguyen Duc; Huy, Bui The; Lee, Yong-Ill

2016-01-01

Highly sensitive hydrogen sulfide (H2S) gas sensors were developed from CuO-decorated ZnO semiconducting hierarchical nanostructures. The ZnO hierarchical nanostructure was fabricated by an electrospinning method following hydrothermal and heat treatment. CuO decoration of ZnO hierarchical structures was carried out by a wet method. The H2S gas-sensing properties were examined at different working temperatures using various quantities of CuO as the variable. CuO decoration of the ZnO hierarchical structure was observed to promote sensitivity for H2S gas higher than 30 times at low working temperature (200 °C) compared with that in the nondecorated hierarchical structure. The sensing mechanism of the hybrid sensor structure is also discussed. The morphology and characteristics of the samples were examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis absorption, photoluminescence (PL), and electrical measurements. PMID:27231026

A Phase Separation Route to Synthesize α-Fe2O3 Porous Nanofibers via Electrospinning for Ultrafast Ethanol Sensing

NASA Astrophysics Data System (ADS)

Dong, Shuwen; Yan, Shuang; Gao, Wenyuan; Liu, Guishan; Hao, Hongshun

2018-07-01

A facile and economic procedure was provided to synthesize α-Fe2O3 nanofibers. In this procedure, porous α-Fe2O3 nanofibers were obtained by a single-polymer/binary-solvent system, while solid α-Fe2O3 nanofibers were prepared by a single-polymer/single-solvent system. The crystal structure and morphology of both samples were characterized by x-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption/desorption isotherms. The formation mechanism of porous structure was based on solvent evaporation-induced phase separation by the use of mixed solvents with different volatility. Furthermore, ethanol-sensing performance of the porous α-Fe2O3 nanofibers was evaluated and compared with solid α-Fe2O3 nanofibers. Results from gas-sensing measurements reveal that porous α-Fe2O3 nanofibers exhibit higher sensitivity and slightly longer recovery time than solid α-Fe2O3 nanofibers. Over all, the gas sensor based on porous α-Fe2O3 nanofibers shows excellent ethanol-sensing capability with high sensitivity and ultrafast response/recovery behaviors, indicating its potential application as a real-time monitoring gas sensor.

Acetylene Gas-Sensing Properties of Layer-by-Layer Self-Assembled Ag-Decorated Tin Dioxide/Graphene Nanocomposite Film

PubMed Central

Jiang, Chuanxing; Yin, Nailiang; Yao, Yao; Shaymurat, Talgar; Zhou, Xiaoyan

2017-01-01

This paper demonstrates an acetylene gas sensor based on an Ag-decorated tin dioxide/reduced graphene oxide (Ag–SnO2/rGO) nanocomposite film, prepared by layer-by-layer (LbL) self-assembly technology. The as-prepared Ag–SnO2/rGO nanocomposite was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectrum. The acetylene sensing properties were investigated using different working temperatures and gas concentrations. An optimal temperature of 90 °C was determined, and the Ag–SnO2/rGO nanocomposite sensor exhibited excellent sensing behaviors towards acetylene, in terms of response, repeatability, stability and response/recovery characteristics, which were superior to the pure SnO2 and SnO2/rGO film sensors. The sensing mechanism of the Ag–SnO2/rGO sensor was attributed to the synergistic effect of the ternary nanomaterials, and the heterojunctions created at the interfaces between SnO2 and rGO. This work indicates that the Ag–SnO2/rGO nanocomposite is a good candidate for constructing a low-temperature acetylene sensor. PMID:28927021

A Phase Separation Route to Synthesize α-Fe2O3 Porous Nanofibers via Electrospinning for Ultrafast Ethanol Sensing

NASA Astrophysics Data System (ADS)

Dong, Shuwen; Yan, Shuang; Gao, Wenyuan; Liu, Guishan; Hao, Hongshun

2018-04-01

A facile and economic procedure was provided to synthesize α-Fe2O3 nanofibers. In this procedure, porous α-Fe2O3 nanofibers were obtained by a single-polymer/binary-solvent system, while solid α-Fe2O3 nanofibers were prepared by a single-polymer/single-solvent system. The crystal structure and morphology of both samples were characterized by x-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption/desorption isotherms. The formation mechanism of porous structure was based on solvent evaporation-induced phase separation by the use of mixed solvents with different volatility. Furthermore, ethanol-sensing performance of the porous α-Fe2O3 nanofibers was evaluated and compared with solid α-Fe2O3 nanofibers. Results from gas-sensing measurements reveal that porous α-Fe2O3 nanofibers exhibit higher sensitivity and slightly longer recovery time than solid α-Fe2O3 nanofibers. Over all, the gas sensor based on porous α-Fe2O3 nanofibers shows excellent ethanol-sensing capability with high sensitivity and ultrafast response/recovery behaviors, indicating its potential application as a real-time monitoring gas sensor.

Fabrication of hierarchical flower-like porous ZnO nanostructures from layered ZnC2O4·3Zn(OH)2 and gas sensing properties

NASA Astrophysics Data System (ADS)

Cui, Jiashan; Sun, Jianbo; Liu, Xin; Li, Jinwei; Ma, Xinzhi; Chen, Tingting

2014-07-01

ZnO materials with porous and hierarchical flower-like structure were synthesized through mild hydrothermal and simple calcination approach, in which the flower-like layered zinc oxalate hydroxide (ZnC2O4·3Zn(OH)2) precursor was first synthesized and then calcined at 600 °C. The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopic (TEM), Brunauer-Emmett-Teller (BET) and thermogravimetric (TG) analysis. We proposed the possible growth mechanism of the material via studying the time evolution experiment results. In the process of reaction, oxalic acid as a structure-directing agent hydrolyzed and then formed primarily sheets-like intermediate ZnC2O4·2H2O. Hexamethylenetetramine (HMT) as surfactant, with directional adsorption, leads to the formation of layered zinc oxalate hydroxide precursor. Furthermore, the gas sensitivity also can be characterized, whose results indicated that the synthesized materials had a preferable selectivity to ethanol gas. The fast response rate and reversible performance can be attributed to the produced greater specific surface area produced, which was caused by the porous and hierarchical flower-like structure.

N-Sulfinylimine compounds, R-NSO: a chemistry family with strong temperament

NASA Astrophysics Data System (ADS)

Romano, R. M.; Della Védova, C. O.

2000-04-01

In this review, an update on the structural properties and theoretical studies of N-sulfinylimine compounds (R-NSO) is reported. They were deduced using several experimental techniques: gas-electron diffraction (GED), X-ray diffraction, 17O NMR, ultraviolet-visible absorption spectroscopy (UV-Vis), FTIR (including matrix studies of molecular randomisation) and Raman (including pre-resonant Raman spectra). Data are compared with those obtained by theoretical calculations. With these tools, excited state geometry using the time-dependent theory was calculated for these kinds of compounds. The existence of pre-resonant Raman effect was reported recently for R-NSO compounds. The configuration of R-NSO compounds was checked for this series confirming the existence of only one syn configuration. This finding is corroborated by theoretical calculations. The method of preparation is also summarised.

A chemical reduction approach to the synthesis of copper nanoparticles

NASA Astrophysics Data System (ADS)

Khan, Ayesha; Rashid, Audil; Younas, Rafia; Chong, Ren

2016-11-01

Development of improved methods for the synthesis of copper nanoparticles is of high priority for the advancement of material science and technology. Herein, starch-protected zero-valent copper (Cu) nanoparticles have been successfully synthesized by a novel facile route. The method is based on the chemical reduction in aqueous copper salt using ascorbic acid as reducing agent at low temperature (80 °C). X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray spectroscopy measurements were taken to investigate the size, structure and composition of synthesized Cu nanocrystals, respectively. Average crystallite size of Cu nanocrystals calculated from the major diffraction peaks using the Scherrer formula is about 28.73 nm. It is expected that the outcomes of the study take us a step closer toward designing rational strategies for the synthesis of nascent Cu nanoparticles without inert gas protection.

The Heisenberg Uncertainty Principle Demonstrated with An Electron Diffraction Experiment

ERIC Educational Resources Information Center

Matteucci, Giorgio; Ferrari, Loris; Migliori, Andrea

2010-01-01

An experiment analogous to the classical diffraction of light from a circular aperture has been realized with electrons. The results are used to introduce undergraduate students to the wave behaviour of electrons. The diffraction fringes produced by the circular aperture are compared to those predicted by quantum mechanics and are exploited to…

High quality single shot ultrafast MeV electron diffraction from a photocathode radio-frequency gun

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fu, Feichao; Liu, Shengguang; Zhu, Pengfei

2014-08-15

A compact ultrafast electron diffractometer, consisting of an s-band 1.6 cell photocathode radio-frequency gun, a multi-function changeable sample chamber, and a sensitive relativistic electron detector, was built at Shanghai Jiao Tong University. High-quality single-shot transmission electron diffraction patterns have been recorded by scattering 2.5 MeV electrons off single crystalline gold and polycrystalline aluminum samples. The high quality diffraction pattern indicates an excellent spatial resolution, with the ratio of the diffraction ring radius over the ring rms width beyond 10. The electron pulse width is estimated to be about 300 fs. The high temporal and spatial resolution may open new opportunities inmore » various areas of sciences.« less

High quality single shot ultrafast MeV electron diffraction from a photocathode radio-frequency gun.

PubMed

Fu, Feichao; Liu, Shengguang; Zhu, Pengfei; Xiang, Dao; Zhang, Jie; Cao, Jianming

2014-08-01

A compact ultrafast electron diffractometer, consisting of an s-band 1.6 cell photocathode radio-frequency gun, a multi-function changeable sample chamber, and a sensitive relativistic electron detector, was built at Shanghai Jiao Tong University. High-quality single-shot transmission electron diffraction patterns have been recorded by scattering 2.5 MeV electrons off single crystalline gold and polycrystalline aluminum samples. The high quality diffraction pattern indicates an excellent spatial resolution, with the ratio of the diffraction ring radius over the ring rms width beyond 10. The electron pulse width is estimated to be about 300 fs. The high temporal and spatial resolution may open new opportunities in various areas of sciences.

Total-scattering pair-distribution function of organic material from powder electron diffraction data

DOE PAGES

Gorelik, Tatiana E.; Billinge, Simon J. L.; Schmidt, Martin U.; ...

2015-04-01

This paper shows for the first time that pair-distribution function analyses can be carried out on organic and organo-metallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction (SAED) and nanodiffraction in transmission electron microscopy (TEM) or nanodiffraction in scanning transmission electron microscopy (STEM) modes. The methods were demonstrated on organo-metallic complexes (chlorinated and unchlorinated copper-phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering datamore » and avoiding beam-damage of the sample are possible to resolve.« less

Dissociation behavior of methane--ethane mixed gas hydrate coexisting structures I and II.

PubMed

Kida, Masato; Jin, Yusuke; Takahashi, Nobuo; Nagao, Jiro; Narita, Hideo

2010-09-09

Dissociation behavior of methane-ethane mixed gas hydrate coexisting structures I and II at constant temperatures less than 223 K was studied with use of powder X-ray diffraction and solid-state (13)C NMR techniques. The diffraction patterns at temperatures less than 203 K showed both structures I and II simultaneously convert to Ih during the dissociation, but the diffraction pattern at temperatures greater than 208 K showed different dissociation behavior between structures I and II. Although the diffraction peaks from structure II decreased during measurement at constant temperatures greater than 208 K, those from structure I increased at the initial step of dissociation and then disappeared. This anomalous behavior of the methane-ethane mixed gas hydrate coexisting structures I and II was examined by using the (13)C NMR technique. The (13)C NMR spectra revealed that the anomalous behavior results from the formation of ethane-rich structure I. The structure I hydrate formation was associated with the dissociation rate of the initial methane-ethane mixed gas hydrate.

Ultrafast electron diffraction optimized for studying structural dynamics in thin films and monolayers

PubMed Central

Badali, D. S.; Gengler, R. Y. N.; Miller, R. J. D.

2016-01-01

A compact electron source specifically designed for time-resolved diffraction studies of free-standing thin films and monolayers is presented here. The sensitivity to thin samples is achieved by extending the established technique of ultrafast electron diffraction to the “medium” energy regime (1–10 kV). An extremely compact design, in combination with low bunch charges, allows for high quality diffraction in a lensless geometry. The measured and simulated characteristics of the experimental system reveal sub-picosecond temporal resolution, while demonstrating the ability to produce high quality diffraction patterns from atomically thin samples. PMID:27226978

Dark-field imaging based on post-processed electron backscatter diffraction patterns of bulk crystalline materials in a scanning electron microscope.

PubMed

Brodusch, Nicolas; Demers, Hendrix; Gauvin, Raynald

2015-01-01

Dark-field (DF) images were acquired in the scanning electron microscope with an offline procedure based on electron backscatter diffraction (EBSD) patterns (EBSPs). These EBSD-DF images were generated by selecting a particular reflection on the electron backscatter diffraction pattern and by reporting the intensity of one or several pixels around this point at each pixel of the EBSD-DF image. Unlike previous studies, the diffraction information of the sample is the basis of the final image contrast with a pixel scale resolution at the EBSP providing DF imaging in the scanning electron microscope. The offline facility of this technique permits the selection of any diffraction condition available in the diffraction pattern and displaying the corresponding image. The high number of diffraction-based images available allows a better monitoring of deformation structures compared to electron channeling contrast imaging (ECCI) which is generally limited to a few images of the same area. This technique was applied to steel and iron specimens and showed its high capability in describing more rigorously the deformation structures around micro-hardness indents. Due to the offline relation between the reference EBSP and the EBSD-DF images, this new technique will undoubtedly greatly improve our knowledge of deformation mechanism and help to improve our understanding of the ECCI contrast mechanisms. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fan, D.; Luo, S. N., E-mail: sluo@pims.ac.cn; Key Laboratory of Advanced Technologies of Materials, Ministry of Education, Southwest Jiaotong University, Chengdu, Sichuan 610031

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; fracture is dominated by splitting cracks followed by wing cracks, and diffraction peaks are broadened likely due to mosaic spread. Our results demonstrate the potential of such multiscale measurements for studying high strain-rate phenomena at dynamic extremes.« less

Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy.

PubMed

Zhu, Yihan; Ciston, Jim; Zheng, Bin; Miao, Xiaohe; Czarnik, Cory; Pan, Yichang; Sougrat, Rachid; Lai, Zhiping; Hsiung, Chia-En; Yao, Kexin; Pinnau, Ingo; Pan, Ming; Han, Yu

2017-05-01

Metal-organic frameworks (MOFs) are crystalline porous materials with designable topology, porosity and functionality, having promising applications in gas storage and separation, ion conduction and catalysis. It is challenging to observe MOFs with transmission electron microscopy (TEM) due to the extreme instability of MOFs upon electron beam irradiation. Here, we use a direct-detection electron-counting camera to acquire TEM images of the MOF ZIF-8 with an ultralow dose of 4.1 electrons per square ångström to retain the structural integrity. The obtained image involves structural information transferred up to 2.1 Å, allowing the resolution of individual atomic columns of Zn and organic linkers in the framework. Furthermore, TEM reveals important local structural features of ZIF-8 crystals that cannot be identified by diffraction techniques, including armchair-type surface terminations and coherent interfaces between assembled crystals. These observations allow us to understand how ZIF-8 crystals self-assemble and the subsequent influence of interfacial cavities on mass transport of guest molecules.

Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy

NASA Astrophysics Data System (ADS)

Zhu, Yihan; Ciston, Jim; Zheng, Bin; Miao, Xiaohe; Czarnik, Cory; Pan, Yichang; Sougrat, Rachid; Lai, Zhiping; Hsiung, Chia-En; Yao, Kexin; Pinnau, Ingo; Pan, Ming; Han, Yu

2017-05-01

Metal-organic frameworks (MOFs) are crystalline porous materials with designable topology, porosity and functionality, having promising applications in gas storage and separation, ion conduction and catalysis. It is challenging to observe MOFs with transmission electron microscopy (TEM) due to the extreme instability of MOFs upon electron beam irradiation. Here, we use a direct-detection electron-counting camera to acquire TEM images of the MOF ZIF-8 with an ultralow dose of 4.1 electrons per square ångström to retain the structural integrity. The obtained image involves structural information transferred up to 2.1 Å, allowing the resolution of individual atomic columns of Zn and organic linkers in the framework. Furthermore, TEM reveals important local structural features of ZIF-8 crystals that cannot be identified by diffraction techniques, including armchair-type surface terminations and coherent interfaces between assembled crystals. These observations allow us to understand how ZIF-8 crystals self-assemble and the subsequent influence of interfacial cavities on mass transport of guest molecules.

Carbynes - Carriers of primordial noble gases in meteorites

NASA Technical Reports Server (NTRS)

Whittaker, A. G.; Watts, E. J.; Lewis, R. S.; Anders, E.

1980-01-01

Five carbynes (triply bonded allotropes of carbon) have been found by electron diffraction in the Allende and Murchison carbonaceous chondrites: carbon VI, VIII, X, XI, and (tentatively) XII. From the isotopic composition of the associated noble-gas components, it appears that the carbynes in Allende (C3V chondrite) are local condensates from the solar nebula, whereas at least two carbynes in Murchison (C2 chondrite) are of exotic, presolar origin. They may be dust grains that condensed in stellar envelopes and trapped isotropically anomalous matter from stellar nucleosynthesis.

A Medipix quantum area detector allows rotation electron diffraction data collection from submicrometre three-dimensional protein crystals

PubMed Central

Nederlof, Igor; van Genderen, Eric; Li, Yao-Wang; Abrahams, Jan Pieter

2013-01-01

When protein crystals are submicrometre-sized, X-ray radiation damage precludes conventional diffraction data collection. For crystals that are of the order of 100 nm in size, at best only single-shot diffraction patterns can be collected and rotation data collection has not been possible, irrespective of the diffraction technique used. Here, it is shown that at a very low electron dose (at most 0.1 e− Å−2), a Medipix2 quantum area detector is sufficiently sensitive to allow the collection of a 30-frame rotation series of 200 keV electron-diffraction data from a single ∼100 nm thick protein crystal. A highly parallel 200 keV electron beam (λ = 0.025 Å) allowed observation of the curvature of the Ewald sphere at low resolution, indicating a combined mosaic spread/beam divergence of at most 0.4°. This result shows that volumes of crystal with low mosaicity can be pinpointed in electron diffraction. It is also shown that strategies and data-analysis software (MOSFLM and SCALA) from X-ray protein crystallography can be used in principle for analysing electron-diffraction data from three-dimensional nanocrystals of proteins. PMID:23793148

Fabrication and characterisation of ligand-functionalised ultrapure monodispersed metal nanoparticle nanoassemblies employing advanced gas deposition technique

NASA Astrophysics Data System (ADS)

Geremariam Welearegay, Tesfalem; Cindemir, Umut; Österlund, Lars; Ionescu, Radu

2018-02-01

Here, we report for the first time the fabrication of ligand-functionalised ultrapure monodispersed metal nanoparticles (Au, Cu, and Pt) from their pure metal precursors using the advanced gas deposition technique. The experimental conditions during nanoparticle formation were adjusted in order to obtain ultrafine isolated nanoparticles on different substrates. The morphology and surface analysis of the as-deposited metal nanoparticles were investigated using scanning electron microscopy, x-ray diffraction and Fourier transform infra-red spectroscopy, which demonstrated the formation of highly ordered pure crystalline nanoparticles with a relatively uniform size distribution of ∼10 nm (Au), ∼4 nm (Cu) and ∼3 nm (Pt), respectively. A broad range of organic ligands containing thiol or amine functional groups were attached to the nanoparticles to form continuous networks of nanoparticle-ligand nanoassemblies, which were characterised by scanning electron microscopy and x-ray photoelectron spectroscopy. The electrical resistance of the functional nanoassemblies deposited in the gap spacing of two microfabricated parallel Au electrodes patterned on silicon substrates ranged between tens of kΩ and tens of MΩ, which is suitable for use in many applications including (bio)chemical sensors, surface-enhanced Raman spectroscopy and molecular electronic rectifiers.

Influence of microstructure and elemental partitioning on pitting corrosion resistance of duplex stainless steel welding joints

NASA Astrophysics Data System (ADS)

Zhang, Zhiqiang; Jing, Hongyang; Xu, Lianyong; Han, Yongdian; Zhao, Lei; Zhang, Jianli

2017-02-01

The influences of microstructure and elemental partitioning on pitting corrosion resistance of duplex stainless steel joints welded by gas tungsten arc welding (GTAW) and flux-cored arc welding (FCAW) with different shielding gas compositions were studied by optical microscopy, electron backscatter diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, electron probe microanalysis, and potentiostatic and potentiodynamic polarization methods The adding 2% N2 in shielding gas facilitated primary austenite formation in GTAW weld metal (WM) and suppressed Cr2N precipitation in GTAW weld root. In the HAZ, the banded microstructure disappeared while the coarse ferrite grains maintained same orientation as the banded ferrite in the BM. In the WM, the ferrite had one single orientation throughout a grain, whereas several families of austenite appeared. The austenite both in BM and WM enriched in Ni and nitro`gen, while Cr and Mo were concentrated in the ferrite and thus no element showed clear dendritic distribution in the WM (ER2209 and E2209T1). In addition, the secondary austenite had higher Ni content but lower Cr and Mo content than the primary austenite. The N2-supplemented shielding gas promoted nitrogen solid-solution in the primary and secondary austenite. Furthermore, the secondary austenite had relatively lower pitting resistance equivalent number (PREN) than the ferrite and primary austenite, thereby resulting in its preferential corrosion. The Cr2N precipitation led to relatively poor resistance to pitting corrosion in three HAZs and pure Ar shielding GTAW weld root. The N2-supplemented shielding gas improved pitting corrosion resistance of GTAW joint by increasing PREN of secondary austenite and suppressing Cr2N precipitation. In addition, the FCAW WM had much poorer resistance to pitting corrosion than the GTAW WM due to many O-Ti-Si-Mn inclusions. In the BM, since the austenite with lower PREN compared to the ferrite, the pitting corrosion occurred at the ferrite and austenite interface or within the austenite.

Facile synthesis of Cu/Cu{sub x}O nanoarchitectures with adjustable phase composition for effective NO{sub x} gas sensor at room temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Lixue; Li, Li; Yang, Ying

2013-10-15

Graphical abstract: The Cu/Cu{sub x}O nanoarchitectures with 30–70 nm hollow nanospheres reduced by 3 mmol NaBH{sub 4} exhibits excellent gas-sensing property to low-concentration NO{sub x} gas at room temperature. - Highlights: • The Cu/Cu{sub x}O nanoarchitectures with hollow nanospheres are successfully synthesized. • The method is used for preparing the with Cu/Cu{sub x}O adjustable phase composition. • The C3 sample exhibites excellent gas-sensing propertie to NO{sub x} at room temperation. • The Cu/Cu{sub x}O nanoarchitectures have significant for application of gas sensor. - Abstract: The Cu/Cu{sub x}O nanoarchitectures with 30–70 nm hollow nanospheres are successfully synthesized by a facile wetmore » chemical method. The synthesized products have been studied by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermo gravimetric-differential scanning calorimetry (TG-DSC) analysis. The Cu/Cu{sub x}O sensors based on the nanoarchitectures are used to detect the NO{sub x} at room temperature. The results demonstrate that the obtained Cu/Cu{sub x}O nanoarchitectures reduced by 3 mmol NaBH{sub 4} exhibits excellent gas-sensing properties: low detection limit of 0.97 ppm, relatively high sensitivity, short response time, broad linear range and high selectivity. The reasons for gas-sensing activity enhancement on Cu/Cu{sub x}O nanoarchitectures are discussed. The Cu/Cu{sub x}O nanocrystalline with the hierarchical pores structure and tunable compositions have significant for application of gas sensor.« less

Three-dimensional electron diffraction of plant light-harvesting complex

PubMed Central

Wang, Da Neng; Kühlbrandt, Werner

1992-01-01

Electron diffraction patterns of two-dimensional crystals of light-harvesting chlorophyll a/b-protein complex (LHC-II) from photosynthetic membranes of pea chloroplasts, tilted at different angles up to 60°, were collected to 3.2 Å resolution at -125°C. The reflection intensities were merged into a three-dimensional data set. The Friedel R-factor and the merging R-factor were 21.8 and 27.6%, respectively. Specimen flatness and crystal size were critical for recording electron diffraction patterns from crystals at high tilts. The principal sources of experimental error were attributed to limitations of the number of unit cells contributing to an electron diffraction pattern, and to the critical electron dose. The distribution of strong diffraction spots indicated that the three-dimensional structure of LHC-II is less regular than that of other known membrane proteins and is not dominated by a particular feature of secondary structure. ImagesFIGURE 1FIGURE 2 PMID:19431817

Imaging electronic motions by ultrafast electron diffraction

NASA Astrophysics Data System (ADS)

Shao, Hua-Chieh; Starace, Anthony F.

2017-08-01

Recently ultrafast electron diffraction and microscopy have reached unprecedented temporal resolution, and transient structures with atomic precision have been observed in various reactions. It is anticipated that these extraordinary advances will soon allow direct observation of electronic motions during chemical reactions. We therefore performed a series of theoretical investigations and simulations to investigate the imaging of electronic motions in atoms and molecules by ultrafast electron diffraction. Three prototypical electronic motions were considered for hydrogen atoms. For the case of a breathing mode, the electron density expands and contracts periodically, and we show that the time-resolved scattering intensities reflect such changes of the charge radius. For the case of a wiggling mode, the electron oscillates from one side of the nucleus to the other, and we show that the diffraction images exhibit asymmetric angular distributions. The last case is a hybrid mode that involves both breathing and wiggling motions. Owing to the demonstrated ability of ultrafast electrons to image these motions, we have proposed to image a coherent population transfer in lithium atoms using currently available femtosecond electron pulses. A frequency-swept laser pulse adiabatically drives the valence electron of a lithium atom from the 2s to 2p orbitals, and a time-delayed electron pulse maps such motion. Our simulations show that the diffraction images reflect this motion both in the scattering intensities and the angular distributions.

Room-temperature CO Thermoelectric Gas Sensor based on Au/Co3O4 Catalyst Tablet.

PubMed

Sun, L; Luan, W L; Wang, T C; Su, W X; Zhang, L X

2017-02-17

A carbon monoxide (CO) thermoelectric (TE) gas sensor was fabricated by affixing a Au/Co 3 O 4 catalyst tablet on a TE film layer. The Au/Co 3 O 4 catalyst tablet was prepared by a co-precipitation and tablet compression method and its possible catalytic mechanism was discussed by means of x-ray diffraction, field emission scanning electron microscopy, high resolution transmission electron microscopy, x-ray photoelectron spectroscopy, temperature-programmed reduction of hydrogen, Fourier transform infrared spectroscopy and Brunauer-Emmett-Teller analysis. The optimal catalyst, with a Au content of 10 wt%, was obtained at a calcination temperature between 200 and 300 °C. The small size of the Au nanoparticles, high specific surface, the existence of Co 3+ and water-derived species contributed to  high catalytic activity. Based on the optimal Au/Co 3 O 4 catalyst tablet, the CO TE gas sensor worked at room temperature and showed a response voltage signal (ΔV) of 23 mV, high selectivity among hydrogen and methane, high stability, and a fast response time of 106 s for 30 000 ppm CO/air. In addition, a CO concentration in the range of 5000-30 000 ppm could obviously be detected and exhibited a linear relationship with ΔV. The CO TE gas sensor provides a promising option for the detection of CO gas at room temperature.

Incident-beam effects in electron-stimulated Auger-electron diffraction

NASA Astrophysics Data System (ADS)

Gao, Y.; Cao, Jianming

1991-04-01

We have examined incident-beam effects in electron-stimulated Auger-electron diffraction (AED) on a cleaved GaAs(110) surface. The results indicate that incident-beam diffraction is significant in an AED experiment, and that the dissipative nature of the incident beam in contributing to the Auger process must be accounted for. We have developed a qualitative model that describes the trend of the polar-angle dependence of the Auger intensity for both the incident and exit beams. In calculating the diffraction features, we used a zeroth-order approximation to simulate the dissipation of the incident beam, which is found to adequately describe the experimental data.

Role of precursor crystal structure on electrochemical performance of carbide-derived carbon electrodes

NASA Astrophysics Data System (ADS)

Palazzo, Benjamin; Norris, Zach; Taylor, Greg; Yu, Lei; Lofland, Samuel; Hettinger, Jeffrey

2015-03-01

Binary carbides with hexagonal and cubic crystal structures have been synthesized by reactive magnetron sputtering of vanadium and other transition metals in acetylene or methane gas mixed with argon. The binary carbides are converted to carbide-derived carbon (CDC) films using chlorine gas in a post-deposition process in an external vacuum reaction furnace. Residual chlorine has been removed using an annealing step in a hydrogen atmosphere. The CDC materials have been characterized by x-ray diffraction, x-ray fluorescence, and scanning electron microscopy. The performance of the CDC materials in electrochemical device applications has been measured with the hexagonal phase precursor demonstrating a significantly higher specific capacitance in comparison to that of the cubic phase. We report these results and pore-size distributions of these and similar materials.

Characterization of 17-4PH stainless steel powders produced by supersonic gas atomization

NASA Astrophysics Data System (ADS)

Zhao, Xin-Ming; Xu, Jun; Zhu, Xue-Xin; Zhang, Shao-Ming; Zhao, Wen-Dong; Yuan, Guo-Liang

2012-01-01

17-4PH stainless steel powders were prepared using a supersonic nozzle in a close-coupled gas atomization system. The characteristics of powder particles were carried out by means of a laser particle size analyzer, scanning electron microscopy (SEM), and the X-ray diffraction (XRD) technique. The results show that the mass median particle diameter is about 19.15 μm. Three main types of surface microstructures are observed in the powders: well-developed dendrite, cellular, and cellular dendrite structure. The XRD measurements show that, as the particle size decreases, the amount of fcc phase gradually decreases and that of bcc phase increases. The cooling rate is inversely related to the particle size, i.e., it decreases with an increase in particle size.

Enhanced gas sensing correlated with structural and optical properties of Cs-loaded SnO2 nanofilms

NASA Astrophysics Data System (ADS)

Elia Raine, P. J.; Arun George, P.; Balasundaram, O. N.; Varghese, T.

2016-09-01

The Cs-loaded SnO2 thin films were prepared by the spray pyrolysis technique and were characterized by X-ray diffraction, scanning electron microscopy, ultraviolet-visible spectroscopy, impedance spectroscopy and conductometric method. Investigations based on the structural, optical and electrical properties confirm an enhanced gas sensing potential of cesium-loaded tin oxide films. It is found that the tin oxide thin film doped with 4% Cs with a mean grain size of 20 nm at a deposition temperature of 350 ° C show a maximum sensor response of 97.5% for LPG consistently. It is also observed that the sensor response of Cs-doped SnO2 thin films depends on the dopant concentration and the deposition temperature of the film.

Exploring coherent electron excitation and migration dynamics by electron diffraction with ultrashort X-ray pulses.

PubMed

Yuan, Kai-Jun; Bandrauk, André D

2017-10-04

Exploring ultrafast charge migration is of great importance in biological and chemical reactions. We present a scheme to monitor attosecond charge migration in molecules by electron diffraction with spatial and temporal resolutions from ab initio numerical simulations. An ultraviolet pulse creates a coherent superposition of electronic states, after which a time-delayed attosecond X-ray pulse is used to ionize the molecule. It is found that diffraction patterns in the X-ray photoelectron spectra show an asymmetric structure, which is dependent on the time delay between the pump-probe pulses, encoding the information of molecular orbital symmetry and chemical bonding. We describe these phenomena by developing an electronic time-dependent ultrafast molecular photoionization model of a coherent superposition state. The periodical distortion of electron diffraction patterns illustrates the evolution of the electronic coherence, providing a tool for attosecond imaging of ultrafast molecular reaction processes.

Gas Sensor Based on 3-D WO₃ Inverse Opal: Design and Applications.

PubMed

Xing, Ruiqing; Du, Yang; Zhao, Xiaonan; Zhang, Xiu

2017-03-29

A three-dimensional inverse opal (3DIO) WO₃ architecture has been synthesized via a simple sacrificial template method. Morphology features of the 3DIO were characterized by scanning electron microscope (SEM) and its structure was characterized by X-ray diffraction (XRD). The shrinking ratio of the PMMA spheres was ~28.2% through measuring the distribution of the PMMA spheres and 3DIO WO₃ center-to-center distance between the spheres and macropores, respectively. Beyond that, the 3DIO gas sensing properties were investigated systematically and the sensing mechanism of 3DIO WO₃ was proposed. The results indicated that the response of the 3DIO sensor possessed excellent sensitivity to acetone gas, especially at trace levels. The 3DIO gas sensor response was ~7 to 5 ppm of acetone and could detect acetone low to 0.2 ppm effectively, which was in close proximity to the theoretical low detection limit of 0.14 ppm when R a /R g ≥ 1.2 was used as the criterion for reliable gas sensing. All in all, the obvious satisfaction of the gas-sensing properties was ascribed to the structure of the 3DIO, and the sensor could be a promising novel device in the future.

Highly improved ethanol gas-sensing performance of mesoporous nickel oxides nanowires with the stannum donor doping.

PubMed

Wei, Junqi; Li, Xiaoqing; Han, Yanbing; Xu, Jingcai; Jin, Hongxiao; Jin, Dingfeng; Peng, Xiaoling; Hong, Bo; Li, Jing; Yang, Yanting; Ge, Hongliang; Wang, Xinqing

2018-06-15

Mesoporous nickel oxides (NiO) and stannum(Sn)-doped NiO nanowires (NWs) were synthesized by using SBA-15 templates with the nanocasting method. X-ray diffraction, transmission electron microscope, energy dispersive spectrometry, nitrogen adsorption/desorption isotherm and UV-vis spectrum were used to characterize the phase structure, components and microstructure of the as-prepared samples. The gas-sensing analysis indicated that the Sn-doping could greatly improve the ethanol sensitivity for mesoporous NiO NWs. With the increasing Sn content, the ethanol sensitivity increased from 2.16 for NiO NWs up to the maximum of 15.60 for Ni 0.962 Sn 0.038 O 1.038 , and then decreased to 12.24 for Ni 0.946 Sn 0.054 O 1.054 to 100 ppm ethanol gas at 340 °C. The high surface area from the Sn-doping improved the adsorption of oxygen on the surface of NiO NWs, resulting in the smaller surface resistance in air. Furthermore, owing to the recombination of the holes in hole-accumulation lay with the electrons from the donor impurity level and the increasing the body defects for Sn-doping, the total resistance in ethanol gas enhanced greatly. It was concluded that the sensitivity of Sn-doped NiO NWs based sensor could be greatly improved by the higher surface area and high-valence donor substitution from Sn-doping.

Synthesis of basalt fiber@Zn1-xMgxO core/shell nanostructures for selective photoreduction of CO2 to CO

NASA Astrophysics Data System (ADS)

Kwak, Byeong Sub; Kim, Kang Min; Park, Sun-Min; Kang, Misook

2017-06-01

This study focused on the development of a catalyst for converting carbon dioxide, the main cause of global warming, into a beneficial energy source. Core@shell structured particles, BF@ZnO and BF@Zn1-xMgxO, are synthesized in order to selectively obtain CO gas from the photoreduction of CO2. A modified sol-gel process is used to synthesize the core@shell structures with a three-dimensional microstructure, which are subsequently characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDAX), ultraviolet (UV)-vis absorption, photoluminescence (PL), and photocurrent density analysis. The CO2 adsorption abilities of the core@shell particles are estimated through CO2-temperature programmed desorption (TPD). The core@shell structured BF@Zn1-xMgxO particles including the Mg ingredient significantly increased the adsorption of CO2 gas at the microfiber/nanoparticle interface. Both the BF@ZnO and BF@Zn1-xMgxO particles selectively reduce the carbon dioxide to carbon monoxide, with almost no other reduced products being observed. These results are attributed to the effective adsorption of CO2 gas and inhibited recombination of the photogenerated electron-hole pairs. BF@Zn0.75Mg0.25O exhibited superior photocatalytic behavior and selectively produced 5.0 μmolgcat-1 L-1 of CO gas after 8 h of reaction.

Highly improved ethanol gas-sensing performance of mesoporous nickel oxides nanowires with the stannum donor doping

NASA Astrophysics Data System (ADS)

Wei, Junqi; Li, Xiaoqing; Han, Yanbing; Xu, Jingcai; Jin, Hongxiao; Jin, Dingfeng; Peng, Xiaoling; Hong, Bo; Li, Jing; Yang, Yanting; Ge, Hongliang; Wang, Xinqing

2018-06-01

Mesoporous nickel oxides (NiO) and stannum(Sn)-doped NiO nanowires (NWs) were synthesized by using SBA-15 templates with the nanocasting method. X-ray diffraction, transmission electron microscope, energy dispersive spectrometry, nitrogen adsorption/desorption isotherm and UV–vis spectrum were used to characterize the phase structure, components and microstructure of the as-prepared samples. The gas-sensing analysis indicated that the Sn-doping could greatly improve the ethanol sensitivity for mesoporous NiO NWs. With the increasing Sn content, the ethanol sensitivity increased from 2.16 for NiO NWs up to the maximum of 15.60 for Ni0.962Sn0.038O1.038, and then decreased to 12.24 for Ni0.946Sn0.054O1.054 to 100 ppm ethanol gas at 340 °C. The high surface area from the Sn-doping improved the adsorption of oxygen on the surface of NiO NWs, resulting in the smaller surface resistance in air. Furthermore, owing to the recombination of the holes in hole-accumulation lay with the electrons from the donor impurity level and the increasing the body defects for Sn-doping, the total resistance in ethanol gas enhanced greatly. It was concluded that the sensitivity of Sn-doped NiO NWs based sensor could be greatly improved by the higher surface area and high-valence donor substitution from Sn-doping.

Electron coherent diffraction tomography of a nanocrystal

NASA Astrophysics Data System (ADS)

Dronyak, Roman; Liang, Keng S.; Tsai, Jin-Sheng; Stetsko, Yuri P.; Lee, Ting-Kuo; Chen, Fu-Rong

2010-05-01

Coherent diffractive imaging (CDI) with electron or x-ray sources is a promising technique for investigating the structure of nanoparticles down to the atomic scale. In electron CDI, a two-dimensional reconstruction is demonstrated using highly coherent illumination from a field-emission gun as a source of electrons. In a three-dimensional (3D) electron CDI, we experimentally determine the morphology of a single MgO nanocrystal using the Bragg diffraction geometry. An iterative algorithm is applied to invert the 3D diffraction pattern about a (200) reflection of the nanoparticle measured at an angular range of 1.8°. The results reveal a 3D image of the sample at ˜8 nm resolution, and agree with a simulation. Our work demonstrates an alternative approach to obtain the 3D structure of nanocrystals with an electron microscope.

Time-resolved x-ray imaging of a laser-induced nanoplasma and its neutral residuals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fluckiger, L.; Rupp, D.; Adolph, M.

The evolution of individual, large gas-phase xenon clusters, turned into a nanoplasma by a high power infrared laser pulse, is tracked from femtoseconds up to nanoseconds after laser excitation via coherent diffractive imaging, using ultra-short soft x-ray free electron laser pulses. A decline of scattering signal at high detection angles with increasing time delay indicates a softening of the cluster surface. Here we demonstrate, for the first time a representative speckle pattern of a new stage of cluster expansion for xenon clusters after a nanosecond irradiation. The analysis of the measured average speckle size and the envelope of the intensitymore » distribution reveals a mean cluster size and length scale of internal density fluctuations. Furthermore, the measured diffraction patterns were reproduced by scattering simulations which assumed that the cluster expands with pronounced internal density fluctuations hundreds of picoseconds after excitation.« less

Time-resolved x-ray imaging of a laser-induced nanoplasma and its neutral residuals

DOE PAGES

Fluckiger, L.; Rupp, D.; Adolph, M.; ...

2016-04-13

The evolution of individual, large gas-phase xenon clusters, turned into a nanoplasma by a high power infrared laser pulse, is tracked from femtoseconds up to nanoseconds after laser excitation via coherent diffractive imaging, using ultra-short soft x-ray free electron laser pulses. A decline of scattering signal at high detection angles with increasing time delay indicates a softening of the cluster surface. Here we demonstrate, for the first time a representative speckle pattern of a new stage of cluster expansion for xenon clusters after a nanosecond irradiation. The analysis of the measured average speckle size and the envelope of the intensitymore » distribution reveals a mean cluster size and length scale of internal density fluctuations. Furthermore, the measured diffraction patterns were reproduced by scattering simulations which assumed that the cluster expands with pronounced internal density fluctuations hundreds of picoseconds after excitation.« less

Rotational Spectra of Halogenated Ethers Used as Volatile Anaesthetics

NASA Astrophysics Data System (ADS)

Vega-Toribio, Alicia; Lesarri, Alberto; Suenram, Richard D.; Grabow, Jens-Uwe

2009-06-01

Following previous microwave investigations by Suenram et al., we will report on the rotational spectrum of several halogenated ethers used as volatile anaesthetics, including sevoflurane ((CF_3)_2CH-O-CH_2F), isoflurane (CF_3CHCl-O-CHF_2), enflurane (CHFClCF_2-O-CHF_2) and methoxyflurane (CHCl_2CF_2-O-CH_3). This study has been conducted in the 6-18 GHz centimetre-wave region using Balle-Flygare-type FT-microwave spectroscopy. The results will include the analysis of the rotational spectra of minor species in natural abundance (^{13}C and ^{18}O in some cases), structural calculations and auxiliary ab initio modelling. The conformational and structural conclusions will be compared with previous gas-phase electron diffraction and solid-state X-ray diffraction analysis. R. D. Suenram, D. J. Brugh, F. J. Lovas and C. Chu, 51st OSU Int. Symp. On Mol. Spectrosc., Columbus, OH, 1999, RB07

Carbonate-based zeolitic imidazolate framework for highly selective CO2 capture.

PubMed

Basnayake, Sajani A; Su, Jie; Zou, Xiadong; Balkus, Kenneth J

2015-02-16

In this study, we report the formation of a new crystal structure, ZIF-CO3-1, which results from the reaction of Zn(2+), 2-methylimidazole, and carbonate. ZIF-CO3-1 can be synthesized solvothermally in N,N-dimethylformamide (DMF)/water (H2O) or by utilizing of CO2 gas at various temperatures in DMF/H2O or H2O. This reaction selectively consumes CO2 because CO2 is incorporated in the ZIF as carbonate. CO2 can be quantitatively released by acidifying the ZIF. Powder X-ray diffraction, single-crystal X-ray diffraction, FTIR spectroscopy, scanning electron microscopy, elemental analysis, and thermogravimetric analysis were used to characterize the ZIF structure. ZIF-CO3-1 (chemical formula C9H10N4O3Zn2), crystallizes in the orthorhombic crystal system with noncentrosymmetric space group Pba2.

In-situ monitoring by reflective high energy electron diffraction during pulsed laser deposition

NASA Astrophysics Data System (ADS)

Blank, Dave H. A.; Rijnders, Guus J. H. M.; Koster, Gertjan; Rogalla, Horst

1999-01-01

Pulsed laser deposition (PLD) has developed during the past decade from a fast but limited preparation tool towards a competitive thin film deposition technique. One of the advantages above other techniques is the possibility of growth at relative high background pressure. There is a large freedom in choosing which kind of gas. Moreover, in a number of applications, the gaseous species in the background pressure are part of the elements to be grown, e.g., oxygen in the case of high Tc superconductors. However, the advantage of relative high pressures leads to restrictions of using standard diagnostics and monitoring of the film growth, e.g., reflective high energy electron diffraction (RHEED). Here, a PLD chamber including an in-situ RHEED system is presented, which makes it possible to monitor and study the growth at standard PLD parameters. Using a two-stages differential pumped, magnetically shielded, extension tube mounted at the electron gun side and a special designed phosphor screen including CCD camera, real time monitoring by observation of RHEED oscillations could be established at pressures up to 50 Pa. In this paper the latest results on applying this technique on SrTiO 3 and YBa 2Cu 3O 7 will be presented. Additional to the usual diagnostics performed with RHEED, another phenomena can be observed. The pulsed way of deposition, characteristic for PLD, leads to relaxations in the intensity of the diffracted pattern due to the mobility of the deposited material. These relaxation times give extra information about relaxation, crystallization, and nucleation of the deposited material. The presented technique leads to a better understanding of the growth during pulsed laser deposition and, because of the possibility to monitor the growth, will make PLD competitive with other deposition techniques.

Suppressing Ghost Diffraction in E-Beam-Written Gratings

NASA Technical Reports Server (NTRS)

Wilson, Daniel; Backlund, Johan

2009-01-01

A modified scheme for electron-beam (E-beam) writing used in the fabrication of convex or concave diffraction gratings makes it possible to suppress the ghost diffraction heretofore exhibited by such gratings. Ghost diffraction is a spurious component of diffraction caused by a spurious component of grating periodicity as described below. The ghost diffraction orders appear between the main diffraction orders and are typically more intense than is the diffuse scattering from the grating. At such high intensity, ghost diffraction is the dominant source of degradation of grating performance. The pattern of a convex or concave grating is established by electron-beam writing in a resist material coating a substrate that has the desired convex or concave shape. Unfortunately, as a result of the characteristics of electrostatic deflectors used to control the electron beam, it is possible to expose only a small field - typically between 0.5 and 1.0 mm wide - at a given fixed position of the electron gun relative to the substrate. To make a grating larger than the field size, it is necessary to move the substrate to make it possible to write fields centered at different positions, so that the larger area is synthesized by "stitching" the exposed fields.

8-beam local oscillator array at 47 THz generated by a phase grating and a quantum cascade laser

DOE PAGES

Mirzaei, B.; Silva, J. R. G.; Hayton, D.; ...

2017-11-13

We present an 8-beam local oscillator (LO) for the astronomically significant [OI] line at 4.7 THz. The beams are generated using a quantum cascade laser (QCL) in combination with a Fourier phase grating. The grating is fully characterized using a third order distributed feedback (DFB) QCL with a single mode emission at 4.7 THz as the input. The measured diffraction efficiency of 74.3% is in an excellent agreement with the calculated result of 75.4% using a 3D simulation. We show that the power distribution among the diffracted beams is uniform enough for pumping an array receiver. To validate the gratingmore » bandwidth, we apply a far-infrared (FIR) gas laser emission at 5.3 THz as the input and find a very similar performance in terms of efficiency, power distribution, and spatial configuration of the diffracted beams. Both results represent the highest operating frequencies of THz phase gratings reported in the literature. By injecting one of the eight diffracted 4.7 THz beams into a superconducting hot electron bolometer (HEB) mixer, we find that the coupled power, taking the optical loss into account, is in consistency with the QCL power value.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hayashida, Misa; Malac, Marek; Egerton, Ray F.

Electron tomography is a method whereby a three-dimensional reconstruction of a nanoscale object is obtained from a series of projected images measured in a transmission electron microscope. We developed an electron-diffraction method to measure the tilt and azimuth angles, with Kikuchi lines used to align a series of diffraction patterns obtained with each image of the tilt series. Since it is based on electron diffraction, the method is not affected by sample drift and is not sensitive to sample thickness, whereas tilt angle measurement and alignment using fiducial-marker methods are affected by both sample drift and thickness. The accuracy ofmore » the diffraction method benefits reconstructions with a large number of voxels, where both high spatial resolution and a large field of view are desired. The diffraction method allows both the tilt and azimuth angle to be measured, while fiducial marker methods typically treat the tilt and azimuth angle as an unknown parameter. The diffraction method can be also used to estimate the accuracy of the fiducial marker method, and the sample-stage accuracy. A nano-dot fiducial marker measurement differs from a diffraction measurement by no more than ±1°.« less

Molecular structure and conformations of para-methylbenzene sulfonamide and ortho-methylbenzene sulfonamide: gas electron diffraction and quantum chemical calculations study.

PubMed

Petrov, Vjacheslav M; Girichev, Georgiy V; Oberhammer, Heinz; Petrova, Valentina N; Giricheva, Nina I; Bardina, Anna V; Ivanov, Sergey N

2008-04-03

The molecular structure and conformational properties of para-methylbenzene sulfonamide (4-MBSA) and ortho-methylbenzene sulfonamide (2-MBSA) have been studied by gas electron diffraction (GED) and quantum chemical methods (B3LYP/6-311+G** and MP2/6-31G**). Quantum chemical calculations predict the existence of two conformers for 4-MBSA with the S-N bond perpendicular to the benzene plane and the NH2 group either eclipsing or staggering the S-O bonds of the SO2 group. Both conformers possess CS symmetry. The eclipsed form is predicted to be favored by DeltaE = 0.63 kcal/mol (B3LYP) or 1.00 kcal/mol (MP2). According to the calculations, the S-N bond in 2-MBSA can possess planar direction opposite the methyl group (phi(C2C1SN) = 180 degrees ) or nonplanar direction (phi(C2C1SN) approximately 60 degrees ). In both cases, the NH2 group can adopt eclipsed or staggered orientation, resulting in a total of four stable conformers. The nonplanar eclipsed conformer (C1 symmetry) and the planar eclipsed form (CS symmetry) are predicted to be favored. According to the GED analysis, the saturated vapor over solid 4-MBSA at T = 151(3) degrees C consists as mixture of the eclipsed (78(19) %) and staggered (22(19) %) forms. The saturated vapor over solid 2-MBSA at T = 157(3) degrees C consists as a mixture of the nonplanar eclipsed (69(11) %) and planar eclipsed (31(11) %) forms.

Spall Response of Additive Manufactured Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Brown, Andrew; Gregg, Adam; Escobedo, Jp; Hazell, Paul; East, Daniel; Quadir, Zakaria

2017-06-01

Additive manufactured (AM) Ti-6Al-4V was produced via electron beam melting (EBM) and laser melting deposition (LMD) techniques. The dynamic response of AM varieties of common aerospace and infrastructure metals are yet to be fully characterized and compared to their traditionally processed counterparts. Spall damage is one of the primary failure modes in metals subjected to shock loading from high velocity impact. Both EBM and LMD Ti-6Al-4V were shock loaded via flyer-target plate impact using a single-stage light gas gun. Target plates were subjected to pressures just above the spall strength of the material (3-5 GPa) to investigate the early onset of damage nucleation as a function of processing technique and shock orientation with respect to the AM-build direction. Post-mortem characterization of the spall damage and surrounding microstructure was performed using a combination of optical microscopy, scanning electron microscopy, and electron backscatter diffraction.

Dynamic diffraction effects and coherent breathing oscillations in ultrafast electron diffraction in layered 1T-TaSeTe

PubMed Central

Wei, Linlin; Sun, Shuaishuai; Guo, Cong; Li, Zhongwen; Sun, Kai; Liu, Yu; Lu, Wenjian; Sun, Yuping; Tian, Huanfang; Yang, Huaixin; Li, Jianqi

2017-01-01

Anisotropic lattice movements due to the difference between intralayer and interlayer bonding are observed in the layered transition-metal dichalcogenide 1T-TaSeTe following femtosecond laser pulse excitation. Our ultrafast electron diffraction investigations using 4D-transmission electron microscopy (4D-TEM) clearly reveal that the intensity of Bragg reflection spots often changes remarkably due to the dynamic diffraction effects and anisotropic lattice movement. Importantly, the temporal diffracted intensity from a specific crystallographic plane depends on the deviation parameter s, which is commonly used in the theoretical study of diffraction intensity. Herein, we report on lattice thermalization and structural oscillations in layered 1T-TaSeTe, analyzed by dynamic diffraction theory. Ultrafast alterations of satellite spots arising from the charge density wave in the present system are also briefly discussed. PMID:28470025

Coherent diffraction imaging analysis of shape-controlled nanoparticles with focused hard X-ray free-electron laser pulses.

PubMed

Takahashi, Yukio; Suzuki, Akihiro; Zettsu, Nobuyuki; Oroguchi, Tomotaka; Takayama, Yuki; Sekiguchi, Yuki; Kobayashi, Amane; Yamamoto, Masaki; Nakasako, Masayoshi

2013-01-01

We report the first demonstration of the coherent diffraction imaging analysis of nanoparticles using focused hard X-ray free-electron laser pulses, allowing us to analyze the size distribution of particles as well as the electron density projection of individual particles. We measured 1000 single-shot coherent X-ray diffraction patterns of shape-controlled Ag nanocubes and Au/Ag nanoboxes and estimated the edge length from the speckle size of the coherent diffraction patterns. We then reconstructed the two-dimensional electron density projection with sub-10 nm resolution from selected coherent diffraction patterns. This method enables the simultaneous analysis of the size distribution of synthesized nanoparticles and the structures of particles at nanoscale resolution to address correlations between individual structures of components and the statistical properties in heterogeneous systems such as nanoparticles and cells.

Time-resolved measurements with streaked diffraction patterns from electrons generated in laser plasma wakefield

NASA Astrophysics Data System (ADS)

He, Zhaohan; Nees, John; Hou, Bixue; Krushelnick, Karl; Thomas, Alec; Beaurepaire, Benoît; Malka, Victor; Faure, Jérôme

2013-10-01

Femtosecond bunches of electrons with relativistic to ultra-relativistic energies can be robustly produced in laser plasma wakefield accelerators (LWFA). Scaling the electron energy down to sub-relativistic and MeV level using a millijoule laser system will make such electron source a promising candidate for ultrafast electron diffraction (UED) applications due to the intrinsic short bunch duration and perfect synchronization with the optical pump. Recent results of electron diffraction from a single crystal gold foil, using LWFA electrons driven by 8-mJ, 35-fs laser pulses at 500 Hz, will be presented. The accelerated electrons were collimated with a solenoid magnetic lens. By applying a small-angle tilt to the magnetic lens, the diffraction pattern can be streaked such that the temporal evolution is separated spatially on the detector screen after propagation. The observable time window and achievable temporal resolution are studied in pump-probe measurements of photo-induced heating on the gold foil.

SnO2 Nanostructures: Effect of Processing Parameters on Their Structural and Functional Properties

NASA Astrophysics Data System (ADS)

Dontsova, Tetiana A.; Nagirnyak, Svitlana V.; Zhorov, Vladyslav V.; Yasiievych, Yuriy V.

2017-05-01

Zero- and 1D (one-dimensional) tin (IV) oxide nanostructures have been synthesized by thermal evaporation method, and a comparison of their morphology, crystal structure, sorption properties, specific surface area, as well as electrical characteristics has been performed. Synthesized SnO2 nanomaterials were studied by X-ray diffraction, scanning and transmission electron microscopy (SEM and TEM), N2 sorption/desorption technique, IR spectroscopy and, in addition, their current-voltage characteristics have also been measured. The single crystalline structures were obtained both in case of 0D (zero-dimensional) SnO2 powders and in case of 0D nanofibers, as confirmed by electron diffraction of TEM. It was found that SnO2 synthesis parameters significantly affect materials' properties by contributing to the difference in morphology, texture formation, changes in IR spectra of 1D structure as compared to 0D powders, increases in the specific surface area of nanofibers, and the alteration of current-voltage characteristics 0D and 1D SnO2 nanostructures. It was established that gas sensors utilizing of 1D nanofibers significantly outperform those based on 0D powders by providing higher specific surface area and ohmic I-V characteristics.

Synthesis and characterization of carbon-coated cobalt ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Bakhshi, Hamed; Shokuhfar, Ali; Vahdati, Nima

2016-09-01

Cobalt ferrite nanoparticles (CFNPs) were prepared via a reverse micelle method. The CFNPs were subsequently coated with carbon shells by means of thermal chemical vapor deposition (TCVD). In this process, acetylene gas (C2H2) was used as a carbon source and the coating was carried out for 1, 2, or 3 h at 750°C. The Ar/C2H2 ratio was 10:1. Heating during the TCVD process resulted in a NP core size that approached 30 nm; the thickness of the shell was less than 10 nm. The composition, structure, and morphology of the fabricated composites were characterized using X-ray diffraction, simultaneous thermal analysis, transmission electron microscopy, high-resolution transmission electron microscopy, and selected-area diffraction. A vibrating sample magnetometer was used to survey the samples' magnetic properties. The deposited carbon shell substantially affected the growth and magnetic properties of the CFNPs. Micro-Raman spectroscopy was used to study the carbon coating and revealed that the deposited carbon comprised graphite, multiwalled carbon nanotubes, and diamond- like carbon. With an increase in coating time, the intensity ratio between the amorphous and ordered peaks in the Raman spectra decreased, which indicated an increase in crystallite size.

High quality single shot diffraction patterns using ultrashort megaelectron volt electron beams from a radio frequency photoinjector.

PubMed

Musumeci, P; Moody, J T; Scoby, C M; Gutierrez, M S; Bender, H A; Wilcox, N S

2010-01-01

Single shot diffraction patterns using a 250-fs-long electron beam have been obtained at the UCLA Pegasus laboratory. High quality images with spatial resolution sufficient to distinguish closely spaced peaks in the Debye-Scherrer ring pattern have been recorded by scattering the 1.6 pC 3.5 MeV electron beam generated in the rf photoinjector off a 100-nm-thick Au foil. Dark current and high emittance particles are removed from the beam before sending it onto the diffraction target using a 1 mm diameter collimating hole. These results open the door to the study of irreversible phase transformations by single shot MeV electron diffraction.

Transferability of electronic structure of four energetic materials by using single crystal and high resolution X-ray diffraction experiments

NASA Astrophysics Data System (ADS)

Chen, Yu-Sheng

The electronic structures of four energetic materials, trinitrodiazapentalene (C6H3N5O6, TNDAP), beta-1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane (C4H8N8O8, beta-HMX), 1,3,3-trinitroazetidine (C3H4N4O6, TNAZ), and hexahydro-1,3,5-trinitro-1,3,5-s-triazine (C3H6N6O6, RDX), have been analyzed using Hansen-Coppens multipole refinements, using high resolution X-ray diffraction data collected at low temperature, as well as from theoretical calculated structure factors from the solid state phase using density functional theory (DFT), plus B3LYP level theory, and the 6-31G* basis set. However, when comparing both the deformation density and the electrostatic potentials from the theoretical results in TNDAP and TNAZ, they disagree with the experimental results. Therefore, those results have been deposited in appendices A4 and A6, for future reference. In HMX and RDX the theoretical results are in good agreement with experimental results. The physical properties derived from the electronic structure in these four energetic materials, such as multipole populations, the values of the electron density and its Laplacian of the electron density at the bond critical points, have also been calculated using "Atoms in Molecules" (AIM) theory both from the solid state phase calculation, and the experiment, as well as directly calculated from the free molecule in the gas phase. The electron density and the magnitude of its Laplacian from the gas phase are always larger than for the solid state phase calculation and the experiment. This may be due to the packing effect. The transferability of the experimental electronic structure of the NO 2 groups from HMX to TNDAP, TNAZ and RDX are also presented here. Even though the major populated multipoles are robust (small e.s.d.'s), these are few in number, compared with other lower populated multipoles for which the populations span a larger range. Since the deformation electron density distributions are reconstructed using linear combinations of the multipoles, it is necessary to give more degrees of freedom in the refinements. Therefore, those electron density distributions which have a wider range of the multipole populations should not be fixed in the refinements. Utilizing the same coordinate system setup in the multipole refinements of the functional groups, this system can be used as a starting point for solving the charge distribution of a larger system.

Molecular structure and conformational composition of 1,3-dihydroxyacetone studied by combined analysis of gas-phase electron diffraction data, rotational constants, and results of theoretical calculations. Ideal gas thermodynamic properties of 1,3-dihydroxyacetone.

PubMed

Dorofeeva, Olga V; Vogt, Natalja; Vogt, Jürgen; Popik, Mikhail V; Rykov, Anatolii N; Vilkov, Lev V

2007-07-19

The molecular structure of 1,3-dihydroxyacetone (DHA) has been studied by gas-phase electron diffraction (GED), combined analysis of GED and microwave (MW) data, ab initio, and density functional theory calculations. The equilibrium re structure of DHA was determined by a joint analysis of the GED data and rotational constants taken from the literature. The anharmonic vibrational corrections to the internuclear distances (re-ra) and to the rotational constants (B(i)e-B(i)0) needed for the estimation of the re structure were calculated from the B3LYP/cc-pVTZ cubic force field. It was found that the experimental data are well reproduced by assuming that DHA consists of a mixture of three conformers. The most stable conformer of C2v symmetry has two hydrogen bonds, whereas the next two lowest energy conformers (Cs and C1 symmetry) have one hydrogen bond and their abundance is about 30% in total. A combined analysis of GED and MW data led to the following equilibrium structural parameters (re) of the most abundant conformer of DHA (the uncertainties in parentheses are 3 times the standard deviations): r(C=O)=1.215(2) A, r(C-C)=1.516(2) A, r(C-O)=1.393(2) A, r(C-H)=1.096(4) A, r(O-H)=0.967(4) A, angleC-C=O=119.9(2) degrees, angleC-C-O=111.0(2) degrees, angleC-C-H=108.2(7) degrees, angleC-O-H=106.5(7) degrees. These structural parameters reproduce the experimental B(i)0 values within 0.05 MHz. The experimental structural parameters are in good agreement with those obtained from theoretical calculations. Ideal gas thermodynamic functions (S degrees (T), C degrees p(T), and H degrees (T)-H degrees (0)) of DHA were calculated on the basis of experimental and theoretical molecular parameters obtained in this work. The enthalpy of formation of DHA, -523+/-4 kJ/mol, was calculated by the atomization procedure using the G3X method.

High-resolution scanning precession electron diffraction: Alignment and spatial resolution.

PubMed

Barnard, Jonathan S; Johnstone, Duncan N; Midgley, Paul A

2017-03-01

Methods are presented for aligning the pivot point of a precessing electron probe in the scanning transmission electron microscope (STEM) and for assessing the spatial resolution in scanning precession electron diffraction (SPED) experiments. The alignment procedure is performed entirely in diffraction mode, minimising probe wander within the bright-field (BF) convergent beam electron diffraction (CBED) disk and is used to obtain high spatial resolution SPED maps. Through analysis of the power spectra of virtual bright-field images extracted from the SPED data, the precession-induced blur was measured as a function of precession angle. At low precession angles, SPED spatial resolution was limited by electronic noise in the scan coils; whereas at high precession angles SPED spatial resolution was limited by tilt-induced two-fold astigmatism caused by the positive spherical aberration of the probe-forming lens. Copyright © 2016 Elsevier B.V. All rights reserved.

Stretchable and Tunable Microtectonic ZnO-Based Sensors and Photonics.

PubMed

Gutruf, Philipp; Zeller, Eike; Walia, Sumeet; Nili, Hussein; Sriram, Sharath; Bhaskaran, Madhu

2015-09-16

The concept of realizing electronic applications on elastically stretchable "skins" that conform to irregularly shaped surfaces is revolutionizing fundamental research into mechanics and materials that can enable high performance stretchable devices. The ability to operate electronic devices under various mechanically stressed states can provide a set of unique functionalities that are beyond the capabilities of conventional rigid electronics. Here, a distinctive microtectonic effect enabled oxygen-deficient, nanopatterned zinc oxide (ZnO) thin films on an elastomeric substrate are introduced to realize large area, stretchable, transparent, and ultraportable sensors. The unique surface structures are exploited to create stretchable gas and ultraviolet light sensors, where the functional oxide itself is stretchable, both of which outperform their rigid counterparts under room temperature conditions. Nanoscale ZnO features are embedded in an elastomeric matrix function as tunable diffraction gratings, capable of sensing displacements with nanometre accuracy. These devices and the microtectonic oxide thin film approach show promise in enabling functional, transparent, and wearable electronics. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

CdO-based nanostructures as novel CO2 gas sensors

NASA Astrophysics Data System (ADS)

Krishnakumar, T.; Jayaprakash, R.; Prakash, T.; Sathyaraj, D.; Donato, N.; Licoccia, S.; Latino, M.; Stassi, A.; Neri, G.

2011-08-01

Crystalline Cd(OH)2/CdCO3 nanowires, having lengths in the range from 0.3 up to several microns and 5-30 nm in diameter, were synthesized by a microwave-assisted wet chemical route and used as a precursor to obtain CdO nanostructures after a suitable thermal treatment in air. The morphology and microstructure of the as-synthesized and annealed materials have been investigated by scanning electron microscopy, transmission electron microscopy, x-ray diffraction and thermogravimetry-differential scanning calorimetry. The change in morphology and electrical properties with temperature has revealed a wire-to-rod transformation along with a decreases of electrical resistance. Annealed samples were printed on a ceramic substrate with interdigitated contacts to fabricate resistive solid state sensors. Gas sensing properties were explored by monitoring CO2 in synthetic air in the concentration range 0.2-5 v/v% (2000-50 000 ppm). The effect of annealing temperature, working temperature and CO2 concentration on sensing properties (sensitivity, response/recovery time and stability) were investigated. The results obtained demonstrate that CdO-based thick films have good potential as novel CO2 sensors for practical applications.

A Novel Gas Sensor Based on MgSb2O6 Nanorods to Indicate Variations in Carbon Monoxide and Propane Concentrations

PubMed Central

Guillén-Bonilla, Héctor; Flores-Martínez, Martín; Rodríguez-Betancourtt, Verónica-María; Guillen-Bonilla, Alex; Reyes-Gómez, Juan; Gildo-Ortiz, Lorenzo; de la Luz Olvera Amador, María; Santoyo-Salazar, Jaime

2016-01-01

Bystromite (MgSb2O6) nanorods were prepared using a colloidal method in the presence of ethylenediamine, after a calcination step at 800 °C in static air. From X-ray powder diffraction analyses, a trirutile-type structure with lattice parameters a = 4.64 Å and c = 9.25 Å and space group P42/mnm was identified. Using scanning electron microscopy (SEM), microrods with sizes from 0.2 to 1.6 μm were observed. Transmission electron microscopy (TEM) analyses revealed that the nanorods had a length of ~86 nm and a diameter ~23.8 nm. The gas-sensing properties of these nanostructures were tested using pellets elaborated with powders of the MgSb2O6 oxide (calcined at 800 °C) at temperatures 23, 150, 200, 250 and 300 °C. The pellets were exposed to different concentrations of carbon monoxide (CO) and propane (C3H8) at these temperatures. The results showed that the MgSb2O6 nanorods possess excellent stability and high sensitivity in these atmospheres. PMID:26840318

A Novel Gas Sensor Based on MgSb2O6 Nanorods to Indicate Variations in Carbon Monoxide and Propane Concentrations.

PubMed

Guillén-Bonilla, Héctor; Flores-Martínez, Martín; Rodríguez-Betancourtt, Verónica-María; Guillen-Bonilla, Alex; Reyes-Gómez, Juan; Gildo-Ortiz, Lorenzo; de la Luz Olvera Amador, María; Santoyo-Salazar, Jaime

2016-01-30

Bystromite (MgSb2O6) nanorods were prepared using a colloidal method in the presence of ethylenediamine, after a calcination step at 800 °C in static air. From X-ray powder diffraction analyses, a trirutile-type structure with lattice parameters a = 4.64 Å and c = 9.25 Å and space group P4₂/mnm was identified. Using scanning electron microscopy (SEM), microrods with sizes from 0.2 to 1.6 μm were observed. Transmission electron microscopy (TEM) analyses revealed that the nanorods had a length of ~86 nm and a diameter ~23.8 nm. The gas-sensing properties of these nanostructures were tested using pellets elaborated with powders of the MgSb2O6 oxide (calcined at 800 °C) at temperatures 23, 150, 200, 250 and 300 °C. The pellets were exposed to different concentrations of carbon monoxide (CO) and propane (C3H8) at these temperatures. The results showed that the MgSb2O6 nanorods possess excellent stability and high sensitivity in these atmospheres.

Thickness and annealing effects on thermally evaporated InZnO thin films for gas sensors and blue, green and yellow emissive optical devices

NASA Astrophysics Data System (ADS)

Sugumaran, Sathish; Jamlos, Mohd Faizal; Ahmad, Mohd Noor; Bellan, Chandar Shekar; Sivaraj, Manoj

2016-08-01

Indium zinc oxide (InZnO) thin films with thicknesses of 100 nm and 200 nm were deposited on glass plate by thermal evaporation technique. Fourier transform infrared spectra showed a strong metal-oxide bond. X-ray diffraction patterns revealed amorphous nature for as-deposited film whereas polycrystalline structure for annealed films. Scanning electron microscope images showed a uniform distribution of spherical shape grains. Grain size was found to be higher for 200 nm film than 100 nm film. The presence of elements (In, Zn and O) was confirmed from energy dispersive X-ray analysis. Photoluminescence study of 200 nm film showed a blue, blue-green and blue-yellow emission whereas 100 nm film showed a broad green and green-yellow emissions. Both 100 nm and 200 nm films showed good oxygen sensitivity from room temperature to 400 °C. The observed optical and sensor results indicated that the prepared InZnO films are highly potential for room temperature gas sensor and blue, green and yellow emissive opto-electronic devices.

Semiconducting polymers for gas detection

NASA Technical Reports Server (NTRS)

Byrd, N. R.; Sheratte, M. B.

1975-01-01

Conjugated polyenes, and polyesters containing phthalocyanine in their backbone, were synthesized. These polymers were characterized by chemical analysis, thermogravimetric analysis, spectral analysis, and X-ray diffraction studies for crystallinity, as well as for their film-forming capability and gas/polymer interactions. Most of the polymers were relatively insensitive to water vapor up to 50 percent relative humidity, but the polyester/phthalocyanine (iron) polymer was relatively insensitive up to 100 percent RH. On the other hand, poly(p-dimethylaminophenylacetylene) was too conductive at 100 percent RH. Of the gases tested, the only ones that gave any evidence of interacting with the polymers were SO2, NOx, HCN and NH3. Poly(imidazole)/thiophene responded to each of these gases at all relative humidities, while the other polymers gave varying response, depending upon the RH. Thus, since most of these gases were electron-accepting, the electron-donating character of poly(imidazole)/thiophene substantiates the concept of electronegativity being the operating principle for interaction effects. Of the six polymers prepared, poly(imidazole)/thiophene first showed a very good response to smoldering cotton, but it later became nonresponsive; presumably due to oxidation effects.

A Microstructure Study on an AZ31 Magnesium Alloy Tube after Hot Metal Gas Forming Process

NASA Astrophysics Data System (ADS)

Liu, Yi; Wu, Xin

2007-06-01

An AZ31 magnesium alloy tube has been deformed by the hot metal gas forming (HMGF) technique. Microstructures before and after deformation have been investigated by using Electron Backscattered Diffraction (EBSD) and Electron Microscopy. Due to the inhomogeneous distribution by induction heating, there is a temperature gradient distribution along the tube axis. Accordingly, the deformation mechanism is also different. In the middle area of deformation zone where the temperature is ˜410 °C, almost no twinning has been found, whereas at the edge areas of deformation zone where the temperature is ˜200 °C, a high density of twins has been found. EBSD experiments show a weak (0001) fiber texture along the radial direction of the tube before and after deformation in the high-temperature zone. EBSD experiments on the low temperature deformation region were not successful due to the high stored energy. Schmid factor analysis on the EBSD data shows that, despite the (0001) fiber texture, there are still many grains favoring basal slip along both the axis direction and hoop direction.

Polyaniline-Cadmium Ferrite Nanostructured Composite for Room-Temperature Liquefied Petroleum Gas Sensing

NASA Astrophysics Data System (ADS)

Kotresh, S.; Ravikiran, Y. T.; Tiwari, S. K.; Vijaya Kumari, S. C.

2017-08-01

We introduce polyaniline-cadmium ferrite (PANI-CdFe2O4) nanostructured composite as a room-temperature-operable liquefied petroleum gas (LPG) sensor. The structure of PANI and the composite prepared by chemical polymerization was characterized by Fourier-transform infrared (FT-IR) spectroscopy, x-ray diffraction (XRD) analysis, and field-emission scanning electron microscopy. Comparative XRD and FT-IR analysis confirmed CdFe2O4 embedded in PANI matrix with mutual interfacial interaction. The nanostructure of the composite was confirmed by transmission electron microscopy. A simple LPG sensor operable at room temperature, exclusively based on spin-coated PANI-CdFe2O4 nanocomposite, was fabricated with maximum sensing response of 50.83% at 1000 ppm LPG. The response and recovery time of the sensor were 50 s and 110 s, respectively, and it was stable over a period of 1 month with slight degradation of 4%. The sensing mechanism is discussed on the basis of the p- n heterojunction barrier formed at the interface of PANI and CdFe2O4.

Evidence of environmental strains on charge injection in silole-based organic light-emitting diodes

NASA Astrophysics Data System (ADS)

Huby, N.; Hirsch, L.; Aubouy, L.; Gerbier, P.; van der Lee, A.; Amy, F.; Kahn, A.

2007-03-01

Using density functional theory (DFT) computations, we have demonstrated a substantial skeletal relaxation when the structure of 2,5-[bis-(4-anthracene-9-yl-phenyl]-1,1-dimethyl-3,4-diphenyl-silole (BAS) is optimized in the gas-phase comparing with the molecular structure determined from monocrystal x-ray diffraction. The origin of such a relaxation is explained by a strong environmental strains induced by the presence of anthracene entities. Moreover, the estimation of the frontier orbital levels showed that this structural relaxation affects mainly the LUMO that is lowered of 190meV in the gas phase. To check if these theoretical findings would be confirmed for thin films of BAS, we turned to ultraviolet photoemission spectroscopy and/or inverse photoemission spectroscopy and electro-optical measurements. Interestingly, the study of the current density or voltage and luminance or voltage characteristics of an ITO/PEDOT/BAS/Au device clearly demonstrated a very unusual temperature-dependent behavior. Using a thermally assisted tunnel transfer model, we found that this behavior likely originated from the variation of the electronic affinity of the silole derivative with the temperature. The thermal agitation relaxes the molecular strains in thin films as it is shown when passing from the crystalline to the gas phase. The relaxation of the intramolecular thus induces an increase of the electronic affinity and, as a consequence, the more efficient electron injection in organic light-emitting diodes.

Design of WO3-SnO2 core-shell nanofibers and their enhanced gas sensing performance based on different work function

NASA Astrophysics Data System (ADS)

Li, Feng; Gao, Xing; Wang, Rui; Zhang, Tong

2018-06-01

In this work, core-shell WO3-SnO2 (CS-WS) nanofibers (NFs) have been successfully synthesized via a coaxial electrospinning approach. The structure and morphology characteristics of the resultant products were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectra (XPS). To investigate the sensing mechanism of the CS-WS NFs, sensors based on SnO2 NFs, WO3 NFs, and SnO2-WO3 composite NFs were fabricated respectively, and their gas sensing properties were investigated by using CO, ethanol, toluene, acetone, and ammonia as the test gas. The results indicated that the CS-WS NFs exhibited a good response to ethanol (5.09 at 10 ppm) and short response/recovery time (18.5 s and 282 s) compared with the other test gases. The enhanced ethanol sensing properties of CS-WS NFs compared with those of SnO2 NFs were closely associated with the CS structure and its derivative effect due to the different work function of SnO2 and WO3. The approach proposed in this study may contribute to the realization of more sensitive metal oxide semiconductor (MOS) core-shell heterostructure sensors.

Morphology-modulation of SnO2 Hierarchical Architectures by Zn Doping for Glycol Gas Sensing and Photocatalytic Applications

NASA Astrophysics Data System (ADS)

Zhao, Qinqin; Ju, Dianxing; Deng, Xiaolong; Huang, Jinzhao; Cao, Bingqiang; Xu, Xijin

2015-01-01

The morphology of SnO2 nanospheres was transformed into ultrathin nanosheets assembled architectures after Zn doping by one-step hydrothermal route. The as-prepared samples were characterized in detail by various analytical techniques including scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and nitrogen adsorption-desorption technique. The Zn-doped SnO2 nanostructures proved to be the efficient gas sensing materials for a series of flammable and explosive gases detection, and photocatalysts for the degradation of methyl orange (MO) under UV irradiation. It was observed that both of the undoped and Zn-doped SnO2 after calcination exhibited tremendous gas sensing performance toward glycol. The response (S = Ra/Rg) of Zn-doped SnO2 can reach to 90 when the glycol concentration is 100 ppm, which is about 2 times and 3 times higher than that of undoped SnO2 sensor with and without calcinations, respectively. The result of photocatalytic activities demonstrated that MO dye was almost completely degraded (~92%) by Zn-doped SnO2 in 150 min, which is higher than that of others (MO without photocatalyst was 23%, undoped SnO2 without and with calcination were 55% and 75%, respectively).

Morphology-modulation of SnO2 Hierarchical Architectures by Zn Doping for Glycol Gas Sensing and Photocatalytic Applications

PubMed Central

Zhao, Qinqin; Ju, Dianxing; Deng, Xiaolong; Huang, Jinzhao; Cao, Bingqiang; Xu, Xijin

2015-01-01

The morphology of SnO2 nanospheres was transformed into ultrathin nanosheets assembled architectures after Zn doping by one-step hydrothermal route. The as-prepared samples were characterized in detail by various analytical techniques including scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and nitrogen adsorption-desorption technique. The Zn-doped SnO2 nanostructures proved to be the efficient gas sensing materials for a series of flammable and explosive gases detection, and photocatalysts for the degradation of methyl orange (MO) under UV irradiation. It was observed that both of the undoped and Zn-doped SnO2 after calcination exhibited tremendous gas sensing performance toward glycol. The response (S = Ra/Rg) of Zn-doped SnO2 can reach to 90 when the glycol concentration is 100 ppm, which is about 2 times and 3 times higher than that of undoped SnO2 sensor with and without calcinations, respectively. The result of photocatalytic activities demonstrated that MO dye was almost completely degraded (~92%) by Zn-doped SnO2 in 150 min, which is higher than that of others (MO without photocatalyst was 23%, undoped SnO2 without and with calcination were 55% and 75%, respectively). PMID:25597269

Detachment of CVD-grown graphene from single crystalline Ni films by a pure gas phase reaction

NASA Astrophysics Data System (ADS)

Zeller, Patrick; Henß, Ann-Kathrin; Weinl, Michael; Diehl, Leo; Keefer, Daniel; Lippmann, Judith; Schulz, Anne; Kraus, Jürgen; Schreck, Matthias; Wintterlin, Joost

2016-11-01

Despite great previous efforts there is still a high need for a simple, clean, and upscalable method for detaching epitaxial graphene from the metal support on which it was grown. We present a method based on a pure gas phase reaction that is free of solvents and polymer supports and avoids mechanical transfer steps. The graphene was grown on 150 nm thick, single crystalline Ni(111) films on Si(111) wafers with YSZ buffer layers. Its quality was monitored by using low energy electron diffraction and scanning tunneling microscopy. The gas phase etching uses a chemical transport reaction, the so-called Mond process, based on the formation of gaseous nickel tetracarbonyl in 1 bar of CO at 75 °C and by adding small amounts of sulfide catalysts. X-ray photoelectron spectroscopy, Raman spectroscopy and scanning electron microscopy were used to characterize the detached graphene. It was found that the method successfully removes the nickel from underneath the graphene layer, so that the graphene lies on the insulating oxide buffer layer. Small residual particles of nickel sulfide and cracks in the obtained graphene layer were identified. The defect concentrations were comparable to graphene samples obtained by wet chemical etching and by the bubbling transfer.

Coal emissions adverse human health effects associated with ultrafine/nano-particles role and resultant engineering controls.

PubMed

Oliveira, Marcos L S; Navarro, Orlando G; Crissien, Tito J; Tutikian, Bernardo F; da Boit, Kátia; Teixeira, Elba C; Cabello, Juan J; Agudelo-Castañeda, Dayana M; Silva, Luis F O

2017-10-01

There are multiple elements which enable coal geochemistry: (1) boiler and pollution control system design parameters, (2) temperature of flue gas at collection point, (3) feed coal and also other fuels like petroleum coke, tires and biomass geochemistry and (4) fuel feed particle size distribution homogeneity distribution, maintenance of pulverisers, etc. Even though there is a large number of hazardous element pollutants in the coal-processing industry, investigations on micrometer and nanometer-sized particles including their aqueous colloids formation reactions and their behaviour entering the environment are relatively few in numbers. X-ray diffraction (XRD), High Resolution-Transmission Electron microscopy (HR-TEM)/ (Energy Dispersive Spectroscopy) EDS/ (selected-area diffraction pattern) SAED, Field Emission-Scanning Electron Microscopy (FE-SEM)/EDS and granulometric distribution analysis were used as an integrated characterization techniques tool box to determine both geochemistry and nanomineralogy for coal fly ashes (CFAs) from Brazil´s largest coal power plant. Ultrafine/nano-particles size distribution from coal combustion emissions was estimated during the tests. In addition the iron and silicon content was determined as 54.6% of the total 390 different particles observed by electron bean, results aimed that these two particles represent major minerals in the environment particles normally. These data may help in future investigations to asses human health actions related with nano-particles. Copyright © 2017 Elsevier Inc. All rights reserved.

Evidence for the suppression of incident beam effects in Auger electron diffraction

NASA Astrophysics Data System (ADS)

Davoli, I.; Gunnella, R.; Bernardini, R.; De Crescenzi, M.

1998-01-01

Auger electron diffraction (AED) of the Cu(100) surface has been studied through the anisotropy of the elastic backdiffused beam electrons, the L 2,3M 4,5M 4,5 (LVV) and the M 2,3M 4,5M 4,5 (MVV) transitions in polar scan along the two main directions [001], [011] and in azimuth scan at normal emission. The intensity anisotropies of the low and high kinetic energy Auger lines are in antiphase to each other as in experiments in which these transitions are excited by X-ray photons. This behaviour has been exploited to single out the origin of the physical mechanisms accompanying the diffraction of the emitted electrons. Incident beam effects appear to be sizeable only when the collection of the AED spectra are made with an angle integrating electron analyser (cylindrical mirror analyser or low electron energy diffraction apparatus), but they appear negligible when electron collection is performed through a small solid-angle detector. The conclusions reached by our measurements are supported by good agreement with experimental and theoretical X-ray photoelectron diffraction data and demonstrate that, when the incident beam energy is sufficiently higher than the kinetic energy of the Auger electron detected, the influence of the incident beam on AED is negligible.

Structural and gasochromic properties of WO3 films prepared by reactive sputtering deposition

NASA Astrophysics Data System (ADS)

Yamamoto, S.; Hakoda, T.; Miyashita, A.; Yoshikawa, M.

2015-02-01

The effects of deposition temperature and film thickness on the structural and gasochromic properties of tungsten trioxide (WO3) films used for the optical detection of diluted cyclohexane gas have been investigated. The WO3 films were prepared on SiO2 substrates by magnetron sputtering, with the deposition temperature ranging from 300 to 550 °C in an Ar and O2 gas mixture. The films were characterized by scanning electron microscopy (SEM), x-ray diffraction (XRD), and Rutherford backscattering spectroscopy (RBS). The gasochromic properties of the WO3 films, coated with a catalytic Pt layer, were examined by exposing them to up to 5% cyclohexane in N2 gas. It was found that (001)-oriented monoclinic WO3 films, with a columnar structure, grew at deposition temperatures between 400 and 450 °C. Furthermore, (010)-oriented WO3 films were preferably formed at deposition temperatures higher than 500 °C. The gasochromic characterization of the Pt/WO3 films revealed that (001)-oriented WO3 films, with cauliflower-like surface morphology, were appropriate for the optical detection of cyclohexane gas.

Gamma ray irradiated AgFeO{sub 2} nanoparticles with enhanced gas sensor properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Xiuhua, E-mail: xhwang@mail.ahnu.edu.cn; Shi, Zhijie; Yao, Shangwu

2014-11-15

AgFeO{sub 2} nanoparticles were synthesized via a facile hydrothermal method and irradiated by various doses of gamma ray. The products were characterized with X-ray powder diffraction, UV–vis absorption spectrum and transmission electron microscope. The results revealed that the crystal structure, morphology and size of the samples remained unchanged after irradiation, while the intensity of UV–Vis spectra increased with irradiation dose increasing. In addition, gamma ray irradiation improved the performance of gas sensor based on the AgFeO{sub 2} nanoparticles including the optimum operating temperature and sensitivity, which might be ascribed to the generation of defects. - Graphical abstract: Gamma ray irradiationmore » improved the performance of gas sensor based on the AgFeO{sub 2} nanoparticles including sensitivity and optimum operating temperature, which might be ascribed to the generation of defects. - Highlights: • AgFeO{sub 2} nanoparticles were synthesized and irradiated with gamma ray. • AgFeO{sub 2} nanoparticles were employed to fabricate gas sensors to detect ethanol. • Gamma ray irradiation improved the sensitivity and optimum operating temperature.« less

Mesoporous activated carbon from corn stalk core for lithium ion batteries

NASA Astrophysics Data System (ADS)

Li, Yi; Li, Chun; Qi, Hui; Yu, Kaifeng; Liang, Ce

2018-04-01

A novel mesoporous activated carbon (AC) derived from corn stalk core is prepared via a facile and effective method which including the decomposition and carbonization of corn stalk core under an inert gas atmosphere and further activation process with KOH solution. The mesoporous activated carbon (AC) is characterized by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) measurements. These biomass waste derived from activated carbon is proved to be promising anode materials for high specific capacity lithium ion batteries. The activated carbon anode possesses excellent reversible capacity of 504 mAh g-1 after 100 cycles at 0.2C. Compared with the unactivated carbon (UAC), the electrochemical performance of activated carbon is significantly improved due to its mesoporous structure.

Atmospheric pressure chemical vapor deposition: an alternative route to large-scale MoS2 and WS2 inorganic fullerene-like nanostructures and nanoflowers.

PubMed

Li, Xiao-Lin; Ge, Jian-Ping; Li, Ya-Dong

2004-11-19

Large-scale MoS2 and WS2 inorganic fullerene-like (IF) nanostructures (onionlike nanoparticles, nanotubes) and elegant three-dimensional nanoflowers (NF) have been selectively prepared through an atmospheric pressure chemical vapor deposition (APCVD) process with the reaction of chlorides and sulfur. The morphologies were controlled by adjusting the deposition position, the deposition temperature, and the flux of the carrier gas. All of the nanostructures have been characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). A reaction mechanism is proposed based on the experimental results. The surface area of MoS2 IF nanoparticles and the field-emission effect of as-prepared WS2 nanoflowers is reported.

Sn 1-x VxOy thin films deposited by pulsed laser ablation for gas sensing devices

NASA Astrophysics Data System (ADS)

Duhalde, Stella; Vignolo, M. F.; Quintana, G.; Mercader, R.; Lamagna, Antonino

2000-02-01

Polycrystalline pure and V-doped SnO2 thin films have been prepare by pulsed laser deposition (PLD) on Si substrates, with a Si3Ni4 buffered layer. PLD technique, under proper conditions, has probed to produce nanocrystalline-structured materials, which are suitable for gas sensing. In this work we analyze the role of V doping in the structural properties and in the electrical conductivity of the films. The deposition temperature was fixed at 600 degrees C and the films were grown in oxygen atmosphere. The films resulted nanocrystalline with 50 to 120 nm average grain size connected by necks with high surface areas. The microstructural and electronic properties of all the films were analyzed using scanning-electron microscopy, x-ray diffraction and conversion electron Moessbauer spectroscopy. Electrical conductance in a dynamic regime in dry synthetic air has been evaluated as a function of temperature. Moessbauer spectra reveal the presence of 15 percent of Sn2+ in the 5at. percent V-doped films. At about 340 degrees C, a strong increase in the conductivity of the films occurs. Possible explanations are that thermal energy could excite electrons from the vanadium ions into the crystal's conduction band or promotes the diffusion of surface oxygen vacancies towards the bulk, increasing strongly the conductivity of the film.

Crystallography and Morphology of Niobium Carbide in As-Cast HP-Niobium Reformer Tubes

NASA Astrophysics Data System (ADS)

Buchanan, Karl G.; Kral, Milo V.

2012-06-01

The microstructures of two as-cast heats of niobium-modified HP stainless steels were characterized. Particular attention was paid to the interdendritic niobium-rich carbides formed during solidification of these alloys. At low magnifications, these precipitates are grouped in colonies of similar lamellae. Higher magnifications revealed that the lamellae actually obtain two distinct morphologies. The type I morphology exhibits broad planar interfaces with a smooth platelike shape. Type II lamellae have undulating interfaces and an overall reticulated shape. To provide further insight into the origin of these two different morphologies, the microstructure and crystallography of each have been studied in detail using high resolution scanning electron microscopy, transmission electron microscopy, various electron diffraction methods (electron backscatter diffraction (EBSD), selected area diffraction (SAD), and convergent beam electron diffraction (CBED)), and energy dispersive X-ray spectroscopy.

Excitation of phonons in medium-energy electron diffraction

NASA Astrophysics Data System (ADS)

Alvarez, M. A. Vicente; Ascolani, H.; Zampieri, G.

1996-03-01

The ``elastic'' backscattering of electrons from crystalline surfaces presents two regimes: a low-energy regime, in which the characteristic low-energy electron diffraction (LEED) pattern is observed, and a medium-energy regime, in which the diffraction pattern is similar to those observed in x-ray photoemission diffraction (XPD) and Auger electron diffraction (AED) experiments. We present a model for the electron scattering which, including the vibrational degrees of freedom of the crystal, contains both regimes and explains the passage from one regime to the other. Our model is based on a separation of the electron and atomic motions (adiabatic approximation) and on a cluster-type formulation of the multiple scattering of the electron. The inelastic scattering events (excitation and/or absorption of phonons) are treated as coherent processes and no break of the phase relation between the incident and the exit paths of the electron is assumed. The LEED and the medium-energy electron diffraction regimes appear naturally in this model as the limit cases of completely elastic scattering and of inelastic scattering with excitation and/or absorption of multiple phonons. Intensity patterns calculated with this model are in very good agreement with recent experiments of electron scattering on Cu(001) at low and medium energies. We show that there is a correspondence between the type of intensity pattern and the mean number of phonons excited and/or absorbed during the scattering: a LEED-like pattern is observed when this mean number is less than 2, LEED-like and XPD/AED-like features coexist when this number is 3-4, and a XPD/AED-like pattern is observed when this number is greater than 5-6.

Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

Chongad, L. S.; Sharma, A.; Banerjee, M.; Jain, A.

2016-10-01

Lead sulfide (PbS) nanoparticles were prepared by chemical precipitation method (CPM) with the assistance of H2S gas. The microstructure and morphology of the synthesized nanoparticles have been investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the PbS nanoparticles reveal formation of cubic phase. To investigate the quality of prepared nanoparticles, the particles size, lattice constant, strain, dislocation density etc. have been determined using XRD. TEM images reveal formation of cubic nanoparticles and the particle size determined from TEM images agree well with those from XRD.

Acquisition of an X-Ray Scattering System with Solid-Gas Reactor Chamber and Ultrafast Detection Capabilities for Research and Instruction in Science and Engineering

DTIC Science & Technology

2015-05-18

solar   cell  based  on  the  PEDOT:     PSS  hole  transport  layer  and  PCBM  electron  transport  layer...of  a   solar   cell                       10     X-­‐ray  diffraction  patterns  collected  in...the  UTEP  facility  on   hybrid  samples  of     CeO2/porous

Gas Sensitivity Study of Polypyrrole Decorated Graphene Oxide Thick Film

NASA Astrophysics Data System (ADS)

Patil, Pritam; Gaikwad, Ganesh; Patil, Devidas Ramrao; Naik, Jitendra

2016-04-01

Polypyrrole (PPy) and graphene oxide (GO) nanocomposites were prepared by in situ polymerization method. The synthesized nanocomposites were characterized for current-voltage characteristic, Fourier transform infrared spectroscopy, X-ray diffraction and field emission scanning electron microscopy, which gave the evidence of the strong interaction between PPy nanofibers and GO nanosheets. The PPy/GO nanocomposites were used for the sensing of H2S, LPG, CO2 and NH3 gases respectively at room temperature. It was observed that PPy/GO nanocomposites with different GO weight ratios (5, 10 and 20 %) had better selectivity and sensitivity towards NH3 at room temperature.

The effect of hydrogen on B4C coatings fabrication in inductively coupled plasma torch

NASA Astrophysics Data System (ADS)

Guo, Q. J.; Zhao, P.; Li, L.; Zhou, Q. J.; Ni, G. H.; Meng, Y. D.

2018-02-01

Boron carbide (B4C) coatings are prepared by an RF inductively coupled plasma (ICP) torch with different amounts of hydrogen introduced into the sheath gas. The effects of the added hydrogen on the characteristics of the plasma are diagnosed by optical emission spectroscopy and high speed photography. The effects on the melting of B4C particles in the plasma are studied by scanning electron microscopy (SEM). The microstructure of the B4C coatings was determined with SEM imaging and x-ray diffraction analysis. The results show that adding hydrogen to the sheath gas leads to plasma contraction, which results in higher gas temperature of plasma. It also enhances B4C particles spheroidizing and improves the compactness of B4C coatings. Plasma processing does not change the main phase of boron carbide. The obtained results on B4C coatings on Cu substrates allows for improving the B4C coatings fabrication process.

The indium oxide micro and nanopyramids: Morphology materializing and H2S sensing properties

NASA Astrophysics Data System (ADS)

Shariati, Mohsen

2015-07-01

Indium oxide (In2O3) pyramidal nano and microstructures were prepared by a thermal evaporation and condensation method. The preannealing step affected the nanostructures morphologies and their sensing capability. The nanosize structures have been fabricated in nucleated preorganized situation. By changing from prepared sites to undesired sites, the morphology was deteriorated. The synthesized In2O3 structures were characterized by field emission scanning electron microscopy (FESEM) and the X-ray diffraction (XRD) measurements. The FESEM images showed that nanostructures with 100-250 nm in size were fabricated. The XRD patterns indicated that most of the samples are crystalline. Then, the fabricated structures were investigated for H2S gas sensing. The nanocrystal pyramids were found to be sensitive to as low as 100 ppb of H2S gas at room temperature and microcrystal ones to 300 ppb. The nanopyramids demonstrated that they were very sensitive to gas presence and their response and recovery time were in a few seconds.

Nanostructured zinc oxide films synthesized by successive chemical solution deposition for gas sensor applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lupan, O.; Department of Physics, University of Central Florida, 4000 Central Florida Blvd., Orlando, FL 32816-2385; Chow, L.

2009-01-08

Nanostructured ZnO thin films have been deposited using a successive chemical solution deposition method. The structural, morphological, electrical and sensing properties of the films were studied for different concentrations of Al-dopant and were analyzed as a function of rapid photothermal processing temperatures. The films were investigated by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray photoelectron and micro-Raman spectroscopy. Electrical and gas sensitivity measurements were conducted as well. The average grain size is 240 and 224 A for undoped ZnO and Al-doped ZnO films, respectively. We demonstrate that rapid photothermal processing is an efficient method for improving themore » quality of nanostructured ZnO films. Nanostructured ZnO films doped with Al showed a higher sensitivity to carbon dioxide than undoped ZnO films. The correlations between material compositions, microstructures of the films and the properties of the gas sensors are discussed.« less

Gas-sensing behaviour of ZnO/diamond nanostructures.

PubMed

Davydova, Marina; Laposa, Alexandr; Smarhak, Jiri; Kromka, Alexander; Neykova, Neda; Nahlik, Josef; Kroutil, Jiri; Drahokoupil, Jan; Voves, Jan

2018-01-01

Microstructured single- and double-layered sensor devices based on p-type hydrogen-terminated nanocrystalline diamond (NCD) films and/or n-type ZnO nanorods (NRs) have been obtained via a facile microwave-plasma-enhanced chemical vapour deposition process or a hydrothermal growth procedure. The morphology and crystal structure of the synthesized materials was analysed with scanning electron microscopy, X-ray diffraction measurements and Raman spectroscopy. The gas sensing properties of the sensors based on i) NCD films, ii) ZnO nanorods, and iii) hybrid ZnO NRs/NCD structures were evaluated with respect to oxidizing (i.e., NO 2 , CO 2 ) and reducing (i.e., NH 3 ) gases at 150 °C. The hybrid ZnO NRs/NCD sensor showed a remarkably enhanced NO 2 response compared to the ZnO NRs sensor. Further, inspired by this special hybrid structure, the simulation of interaction between the gas molecules (NO 2 and CO 2 ) and hybrid ZnO NRs/NCD sensor was studied using DFT calculations.

Influence of reactive oxygen species during deposition of iron oxide films by high power impulse magnetron sputtering

NASA Astrophysics Data System (ADS)

Stranak, V.; Hubicka, Z.; Cada, M.; Bogdanowicz, R.; Wulff, H.; Helm, C. A.; Hippler, R.

2018-03-01

Iron oxide films were deposited using high power impulse magnetron sputtering (HiPIMS) of an iron cathode in an argon/oxygen gas mixture at different gas pressures (0.5 Pa, 1.5 Pa, and 5.0 Pa). The HiPIMS system was operated at a repetition frequency f  =  100 Hz with a duty cycle of 1%. A main goal is a comparison of film growth during conventional and electron cyclotron wave resonance-assisted HiPIMS. The deposition plasma was investigated by means of optical emission spectroscopy and energy-resolved mass spectrometry. Active oxygen species were detected and their kinetic energy was found to depend on the gas pressure. Deposited films were characterized by means of spectroscopic ellipsometry and grazing incidence x-ray diffraction. Optical properties and crystallinity of as-deposited films were found to depend on the deposition conditions. Deposition of hematite iron oxide films with the HiPIMS-ECWR discharge is attributed to the enhanced production of reactive oxygen species.

Diffraction effects and inelastic electron transport in angle-resolved microscopic imaging applications.

PubMed

Winkelmann, A; Nolze, G; Vespucci, S; Naresh-Kumar, G; Trager-Cowan, C; Vilalta-Clemente, A; Wilkinson, A J; Vos, M

2017-09-01

We analyse the signal formation process for scanning electron microscopic imaging applications on crystalline specimens. In accordance with previous investigations, we find nontrivial effects of incident beam diffraction on the backscattered electron distribution in energy and momentum. Specifically, incident beam diffraction causes angular changes of the backscattered electron distribution which we identify as the dominant mechanism underlying pseudocolour orientation imaging using multiple, angle-resolving detectors. Consequently, diffraction effects of the incident beam and their impact on the subsequent coherent and incoherent electron transport need to be taken into account for an in-depth theoretical modelling of the energy- and momentum distribution of electrons backscattered from crystalline sample regions. Our findings have implications for the level of theoretical detail that can be necessary for the interpretation of complex imaging modalities such as electron channelling contrast imaging (ECCI) of defects in crystals. If the solid angle of detection is limited to specific regions of the backscattered electron momentum distribution, the image contrast that is observed in ECCI and similar applications can be strongly affected by incident beam diffraction and topographic effects from the sample surface. As an application, we demonstrate characteristic changes in the resulting images if different properties of the backscattered electron distribution are used for the analysis of a GaN thin film sample containing dislocations. © 2017 The Authors. Journal of Microscopy published by JohnWiley & Sons Ltd on behalf of Royal Microscopical Society.

Carbon doped GaN buffer layer using propane for high electron mobility transistor applications: Growth and device results

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, X.; Nilsson, D.; Danielsson, Ö.

2015-12-28

The creation of a semi insulating (SI) buffer layer in AlGaN/GaN High Electron Mobility Transistor (HEMT) devices is crucial for preventing a current path beneath the two-dimensional electron gas (2DEG). In this investigation, we evaluate the use of a gaseous carbon gas precursor, propane, for creating a SI GaN buffer layer in a HEMT structure. The carbon doped profile, using propane gas, is a two stepped profile with a high carbon doping (1.5 × 10{sup 18 }cm{sup −3}) epitaxial layer closest to the substrate and a lower doped layer (3 × 10{sup 16 }cm{sup −3}) closest to the 2DEG channel. Secondary Ion Mass Spectrometry measurement showsmore » a uniform incorporation versus depth, and no memory effect from carbon doping can be seen. The high carbon doping (1.5 × 10{sup 18 }cm{sup −3}) does not influence the surface morphology, and a roughness root-mean-square value of 0.43 nm is obtained from Atomic Force Microscopy. High resolution X-ray diffraction measurements show very sharp peaks and no structural degradation can be seen related to the heavy carbon doped layer. HEMTs are fabricated and show an extremely low drain induced barrier lowering value of 0.1 mV/V, demonstrating an excellent buffer isolation. The carbon doped GaN buffer layer using propane gas is compared to samples using carbon from the trimethylgallium molecule, showing equally low leakage currents, demonstrating the capability of growing highly resistive buffer layers using a gaseous carbon source.« less

Gas hydrate characterization and grain-scale imaging of recovered cores from the Mount Elbert Gas Hydrate Stratigraphic Test Well, Alaska North Slope

USGS Publications Warehouse

Stern, Laura A.; Lorenson, T.D.; Pinkston, John C.

2011-01-01

Using cryogenic scanning electron microscopy (CSEM), powder X-ray diffraction, and gas chromatography methods, we investigated the physical states, grain characteristics, gas composition, and methane isotopic composition of two gas-hydrate-bearing sections of core recovered from the BPXA–DOE–USGS Mount Elbert Gas Hydrate Stratigraphic Test Well situated on the Alaska North Slope. The well was continuously cored from 606.5 m to 760.1 m depth, and sections investigated here were retrieved from 619.9 m and 661.0 m depth. X-ray analysis and imaging of the sediment phase in both sections shows it consists of a predominantly fine-grained and well-sorted quartz sand with lesser amounts of feldspar, muscovite, and minor clays. Cryogenic SEM shows the gas-hydrate phase forming primarily as a pore-filling material between the sediment grains at approximately 70–75% saturation, and more sporadically as thin veins typically several tens of microns in diameter. Pore throat diameters vary, but commonly range 20–120 microns. Gas chromatography analyses of the hydrate-forming gas show that it is comprised of mainly methane (>99.9%), indicating that the gas hydrate is structure I. Here we report on the distribution and articulation of the gas-hydrate phase within the cores, the grain morphology of the hydrate, the composition of the sediment host, and the composition of the hydrate-forming gas.

Gas hydrate characterization and grain-scale imaging of recovered cores from the Mount Elbert Gas Hydrate Stratigraphic Test Well, Alaska North Slope

USGS Publications Warehouse

Stern, L.A.; Lorenson, T.D.; Pinkston, J.C.

2011-01-01

Using cryogenic scanning electron microscopy (CSEM), powder X-ray diffraction, and gas chromatography methods, we investigated the physical states, grain characteristics, gas composition, and methane isotopic composition of two gas-hydrate-bearing sections of core recovered from the BPXA-DOE-USGS Mount Elbert Gas Hydrate Stratigraphic Test Well situated on the Alaska North Slope. The well was continuously cored from 606.5. m to 760.1. m depth, and sections investigated here were retrieved from 619.9. m and 661.0. m depth. X-ray analysis and imaging of the sediment phase in both sections shows it consists of a predominantly fine-grained and well-sorted quartz sand with lesser amounts of feldspar, muscovite, and minor clays. Cryogenic SEM shows the gas-hydrate phase forming primarily as a pore-filling material between the sediment grains at approximately 70-75% saturation, and more sporadically as thin veins typically several tens of microns in diameter. Pore throat diameters vary, but commonly range 20-120 microns. Gas chromatography analyses of the hydrate-forming gas show that it is comprised of mainly methane (>99.9%), indicating that the gas hydrate is structure I. Here we report on the distribution and articulation of the gas-hydrate phase within the cores, the grain morphology of the hydrate, the composition of the sediment host, and the composition of the hydrate-forming gas. ?? 2009.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-05-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the `diffraction before destruction' scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

PubMed Central

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-01-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the ‘diffraction before destruction’ scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles. PMID:24763651

Electron diffraction using ultrafast electron bunches from a laser-wakefield accelerator at kHz repetition rate

NASA Astrophysics Data System (ADS)

He, Z.-H.; Thomas, A. G. R.; Beaurepaire, B.; Nees, J. A.; Hou, B.; Malka, V.; Krushelnick, K.; Faure, J.

2013-02-01

We show that electron bunches in the 50-100 keV range can be produced from a laser wakefield accelerator using 10 mJ, 35 fs laser pulses operating at 0.5 kHz. It is shown that using a solenoid magnetic lens, the electron bunch distribution can be shaped. The resulting transverse and longitudinal coherence is suitable for producing diffraction images from a polycrystalline 10 nm aluminum foil. The high repetition rate, the stability of the electron source, and the fact that its uncorrelated bunch duration is below 100 fs make this approach promising for the development of sub-100 fs ultrafast electron diffraction experiments.

Diffraction and microscopy with attosecond electron pulse trains

NASA Astrophysics Data System (ADS)

Morimoto, Yuya; Baum, Peter

2018-03-01

Attosecond spectroscopy1-7 can resolve electronic processes directly in time, but a movie-like space-time recording is impeded by the too long wavelength ( 100 times larger than atomic distances) or the source-sample entanglement in re-collision techniques8-11. Here we advance attosecond metrology to picometre wavelength and sub-atomic resolution by using free-space electrons instead of higher-harmonic photons1-7 or re-colliding wavepackets8-11. A beam of 70-keV electrons at 4.5-pm de Broglie wavelength is modulated by the electric field of laser cycles into a sequence of electron pulses with sub-optical-cycle duration. Time-resolved diffraction from crystalline silicon reveals a < 10-as delay of Bragg emission and demonstrates the possibility of analytic attosecond-ångström diffraction. Real-space electron microscopy visualizes with sub-light-cycle resolution how an optical wave propagates in space and time. This unification of attosecond science with electron microscopy and diffraction enables space-time imaging of light-driven processes in the entire range of sample morphologies that electron microscopy can access.

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector

DOE Office of Scientific and Technical Information (OSTI.GOV)

Genderen, E. van; Clabbers, M. T. B.; Center for Cellular Imaging and NanoAnalytics

A specialized quantum area detector for electron diffraction studies makes it possible to solve the structure of small organic compound nanocrystals in non-cryo conditions by direct methods. Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼0.013 e{sup −} Å{sup −2} s{sup −1}) were collected at roommore » temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014)« less

Two-dimensional mapping of polarizations of rhombohedral nanostructures in the orthorhombic phase of KNbO3 by the combined use of scanning transmission electron microscopy and convergent-beam electron diffraction

NASA Astrophysics Data System (ADS)

Tsuda, Kenji; Tanaka, Michiyoshi

2015-08-01

Rhombohedral nanostructures previously found in the orthorhombic phase of KNbO3, by convergent-beam electron diffraction [Tsuda et al., Appl. Phys. Lett. 102, 051913 (2013)], have been investigated by the combined use of scanning transmission electron microscopy and convergent-beam electron diffraction. Two-dimensional distributions of the rhombohedral nanostructures, or nanometer-scale spatial fluctuations of polarization clusters, have been successfully visualized. The correlation length of the observed spatial fluctuations of local polarizations is related to the cpc/apc ratio and the transition entropy.

Characterization and activity of Pd-modified TiO2 catalysts for photocatalytic oxidation of NO in gas phase.

PubMed

Wu, Zhongbiao; Sheng, Zhongyi; Liu, Yue; Wang, Haiqiang; Tang, Nian; Wang, Jie

2009-05-30

Pd-modified TiO(2) prepared by thermal impregnation method was used in this study for photocatalytic oxidation of NO in gas phase. The physico-chemical properties of Pd/TiO(2) catalysts were characterized by X-ray diffraction analysis (XRD), Brunauer-Emmett-Teller measurements (BET), X-ray photoelectron spectrum analysis (XPS), transmission electron microscopy (TEM), high resolution-transmission electron microscopy (HR-TEM), UV-vis diffuse reflectance spectra (UV-vis DRS) and photoluminescence spectra (PL). It was found that Pd dopant existed as PdO particles in as-prepared photocatalysts. The results of PL spectra indicated that the photogenerated electrons and holes were efficiently separated after Pd doping. During in situ XPS study, it was found that the content of hydroxyl groups on the surface of Pd/TiO(2) increased when the catalyst was irradiated by UV light, which could result in the improvement of photocatalytic activity. The activity test showed that the optimum Pd dopant content was 0.05 wt.%. And the maximum conversion of NO was about 72% higher than that of P25 when the initial concentration of NO was 200 ppm, which showed that Pd/TiO(2) photocatalysts could be potentially applied to oxidize higher concentration of NO.

Teaching Diffraction of Light and Electrons: Classroom Analogies to Classic Experiments

ERIC Educational Resources Information Center

Velentzas, Athanasios

2014-01-01

Diffraction and interference are phenomena that demonstrate the wave nature of light and of particles. Experiments relating to the diffraction/interference of light can easily be carried out in an educational lab, but it may be impossible to perform experiments involving electrons because of the lack of specialized equipment needed for such…

Exploring transmission Kikuchi diffraction using a Timepix detector

NASA Astrophysics Data System (ADS)

Vespucci, S.; Winkelmann, A.; Mingard, K.; Maneuski, D.; O'Shea, V.; Trager-Cowan, C.

2017-02-01

Electron backscatter diffraction (EBSD) is a well-established scanning electron microscope (SEM)-based technique [1]. It allows the non-destructive mapping of the crystal structure, texture, crystal phase and strain with a spatial resolution of tens of nanometers. Conventionally this is performed by placing an electron sensitive screen, typically consisting of a phosphor screen combined with a charge coupled device (CCD) camera, in front of a specimen, usually tilted 70° to the normal of the exciting electron beam. Recently, a number of authors have shown that a significant increase in spatial resolution is achievable when Kikuchi diffraction patterns are acquired in transmission geometry; that is when diffraction patterns are generated by electrons transmitted through an electron-transparent, usually thinned, specimen. The resolution of this technique, called transmission Kikuchi diffraction (TKD), has been demonstrated to be better than 10 nm [2,3]. We have recently demonstrated the advantages of a direct electron detector, Timepix [4,5], for the acquisition of standard EBSD patterns [5]. In this article we will discuss the advantages of Timepix to perform TKD and for acquiring spot diffraction patterns and more generally for acquiring scanning transmission electron microscopy micrographs in the SEM. Particularly relevant for TKD, is its very compact size, which allows much more flexibility in the positioning of the detector in the SEM chamber. We will furthermore show recent results using Timepix as a virtual forward scatter detector, and will illustrate the information derivable on producing images through processing of data acquired from different areas of the detector. We will show results from samples ranging from gold nanoparticles to nitride semiconductor nanorods.

Transmission Kikuchi diffraction and transmission electron forescatter imaging of electropolished and FIB manufactured TEM specimens

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zieliński, W., E-mail: wiziel@inmat.pw.edu.pl; Płociński, T.; Kurzydłowski, K.J.

2015-06-15

We present a study of the efficiency of the utility of scanning electron microscope (SEM)-based transmission methods for characterizing grain structure in thinned bulk metals. Foils of type 316 stainless steel were prepared by two methods commonly used for transmission electron microscopy — double-jet electropolishing and focused ion beam milling. A customized holder allowed positioning of the foils in a configuration appropriate for both transmission electron forward scatter diffraction, and for transmission imaging by the use of a forescatter detector with two diodes. We found that both crystallographic orientation maps and dark-field transmitted images could be obtained for specimens preparedmore » by either method. However, for both methods, preparation-induced artifacts may affect the quality or accuracy of transmission SEM data, especially those acquired by the use of transmission Kikuchi diffraction. Generally, the quality of orientation data was better for specimens prepared by electropolishing, due to the absence of ion-induced damage. - Highlights: • The transmission imaging and diffraction techniques are emerging in scanning electron microscopy (SEM) as promising new field of materials characterization. • The manuscript titled: “Transmission Kikuchi Diffraction and Transmission Electron Forescatter Imaging of Electropolished and FIB Manufactured TEM Specimens” documents how different specimen thinning procedures can effect efficiency of transmission Kikuchi diffraction and transmission electron forescatter imaging. • The abilities to make precision crystallographic orientation maps and dark-field images in transmission was studied on electropolished versus focus ion beam manufactured TEM specimens. • Depending on the need, electropolished and focused ion beam technique may produce suitable specimens for transmission imaging and diffraction in SEM.« less

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review.

PubMed

Dwivedi, D; Lepkova, K; Becker, T

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

NASA Astrophysics Data System (ADS)

Dwivedi, D.; Lepkova, K.; Becker, T.

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

PubMed Central

Dwivedi, D.; Becker, T.

2017-01-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed. PMID:28413351

Atomic-scale diffractive imaging of sub-cycle electron dynamics in condensed matter

PubMed Central

Yakovlev, Vladislav S.; Stockman, Mark I.; Krausz, Ferenc; Baum, Peter

2015-01-01

For interaction of light with condensed-matter systems, we show with simulations that ultrafast electron and X-ray diffraction can provide a time-dependent record of charge-density maps with sub-cycle and atomic-scale resolutions. Using graphene as an example material, we predict that diffraction can reveal localised atomic-scale origins of optical and electronic phenomena. In particular, we point out nontrivial relations between microscopic electric current and density in undoped graphene. PMID:26412407

Atomic-scale diffractive imaging of sub-cycle electron dynamics in condensed matter

DOE PAGES

Yakovlev, Vladislav S.; Stockman, Mark I.; Krausz, Ferenc; ...

2015-09-28

For interaction of light with condensed-matter systems, we show with simulations that ultrafast electron and X-ray diffraction can provide a time-dependent record of charge-density maps with sub-cycle and atomic-scale resolutions. Using graphene as an example material, we predict that diffraction can reveal localised atomic-scale origins of optical and electronic phenomena. Here, we point out nontrivial relations between microscopic electric current and density in undoped graphene.

Low-kilovolt coherent electron diffractive imaging instrument based on a single-atom electron source

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Chun-Yueh; Chang, Wei-Tse; Chen, Yi-Sheng

2016-03-15

In this work, a transmission-type, low-kilovolt coherent electron diffractive imaging instrument was constructed. It comprised a single-atom field emitter, a triple-element electrostatic lens, a sample holder, and a retractable delay line detector to record the diffraction patterns at different positions behind the sample. It was designed to image materials thinner than 3 nm. The authors analyzed the asymmetric triple-element electrostatic lens for focusing the electron beams and achieved a focused beam spot of 87 nm on the sample plane at the electron energy of 2 kV. High-angle coherent diffraction patterns of a suspended graphene sample corresponding to (0.62 Å){sup −1} were recorded. This workmore » demonstrated the potential of coherent diffractive imaging of thin two-dimensional materials, biological molecules, and nano-objects at a voltage between 1 and 10 kV. The ultimate goal of this instrument is to achieve atomic resolution of these materials with high contrast and little radiation damage.« less

Growth, Structural, Electronic, and Magnetic Characterization of GaN, CrN, Fe Islands on CrN, and Fe/CrN Bilayer Thin Films

NASA Astrophysics Data System (ADS)

Alam, Khan

As a part of my Ph.D research, initially I was involved in construction and calibration of an ultra-high vacuum thin film facility, and later on I studied structural, electronic, and magnetic properties of GaN, CrN, Fe/CrN bilayers, and Fe islands on CrN thin films. All of these films were grown by molecular beam epitaxy and characterized with a variety of state-of-the-art techniques including variable temperature reflection high energy electron diffraction, low temperature scanning tunneling microscopy and spectroscopy, variable temperature vibrating sample magnetometry, variable temperature neutron diffraction and reflectometry, variable temperature x-ray diffraction, x-ray reflectometry, Rutherford backscattering, Auger electron spectroscopy, and cross-sectional tunneling electron microscopy. The experimental results are furthermore understood by comparing with numerical calculations using generalized gradient approximation, local density approximation with Hubbard correction, Refl1D, and data analysis and visual environment program. In my first research project, I studied Ga gas adatoms on GaN surfaces. We discovered frozen-out gallium gas adatoms on atomically smooth c(6x12) GaN(0001¯) surface using low temperature scanning tunneling microscopy. We identified adsorption sites of the Ga adatoms on c(6x12) reconstructed surface. Their bonding is determined by measuring low unoccupied molecular orbital level. Absorption sites of the Ga gas adatoms on centered 6x12 are identified, and their asymmetric absorption on the chiral domains is investigated. In second project, I investigated magneto-structural phase transition in chromium nitride (CrN) thin films. The CrN thin films are grown by molecular beam epitaxy. Structural and magnetic transition are studied using variable temperature reflection high energy electron diffraction and variable temperature neutron diffraction. We observed a structural phase transition at the surface at 277+/-2 K, and a sharp, first-order magnetic phase transition from paramagnetic (room temperature) to antiferromagnetic (low temperature) at 280+/-3 K. Our experiments suggest that the structural transition in CrN thin films occur in out-of-plane direction, and epitaxial constraints suppress the in-plane transition; therefore, the low temperature crystal structure of CrN is tetragonal. This new model explains our structural and magnetic data at low temperatures, but it is different than the previously published orthorhombic model. In third project, I studied exchange bias and exchange spring effect in MBE grown Fe/CrN bilayer thin films. We grew Fe/CrN bilayer thin films on MgO(001) substrate by molecular beam epitaxy, and studied them using variable temperature vibrating sample magnetometry, polarized neutron reflectometry, x-ray reflectivity, and cross-sectional transmission electron microscopy. We observed exchange bias and exchange spring effect in all bilayer thin films. We studied the relationship of exchange bias, blocking temperature, and coercivity with Fe and CrN layers thicknesses. We used polarized neutron beam reflectometry to see if spins at Fe/CrN interface are pinned. We found a thin ferromagnetically ordered CrN layer at the interface. In my final project, I studied growth of submonolayer Fe islands on CrN thin films. These films are prepared in two stages: first, a CrN layer is grown by MBE and then a submonolayer Fe is deposited at room temperature from a carefully degassed e-beam evaporator. The films are studied at liquid helium temperature using low temperature scanning tunneling microscopy and spectroscopy. Islands are seen in STM images, after the Fe deposition, at the edges as well as at the center of atomically flat CrN terraces. However, numerical calculations performed by our collaborator Ponce-P'erez from Benem'erita Universidad Aut'onoma de Puebla show that the Fe islands are energetically unstable on the surface. The Fe atoms substitute Cr atoms in the surface layer and the Cr atoms comes out and form islands. In order to find out elemental composition of the islands, we attempted to map local density of state by measuring differential conductance spectra as a function of bias voltage using LT-STS. We observed three characteristically different spectra; one in the CrN substrate and two in the islands. The CrN substrate curve has a "U" shape near Fermi level and a peak at ≈ 105 mV. The islands spectra show Kondo-like resonances at Fermi level; some islands produce a peak whereas others produce a dip the dI/dV curves near Fermi level. Further investigations are needed to determine the origin of the peak and dip in the island curves, as well as to find the composition of the islands.

Evolution in boron-based GEM detectors for diffraction measurements: from planar to 3D converters

NASA Astrophysics Data System (ADS)

Albani, Giorgia; Perelli Cippo, Enrico; Croci, Gabriele; Muraro, Andrea; Schooneveld, Erik; Scherillo, Antonella; Hall-Wilton, Richard; Kanaki, Kalliopi; Höglund, Carina; Hultman, Lars; Birch, Jens; Claps, Gerardo; Murtas, Fabrizio; Rebai, Marica; Tardocchi, Marco; Gorini, Giuseppe

2016-11-01

The so-called ‘3He-crisis’ has motivated the neutron detector community to undertake an intense R&D programme in order to develop technologies alternative to standard 3He tubes and suitable for neutron detection systems in future spallation sources such as the European spallation source (ESS). Boron-based GEM (gas electron multiplier) detectors are a promising ‘3He-free’ technology for thermal neutron detection in neutron scattering experiments. In this paper the evolution of boron-based GEM detectors from planar to 3D converters with an application in diffraction measurements is presented. The use of 3D converters coupled with GEMs allows for an optimization of the detector performances. Three different detectors were used for diffraction measurements on the INES instrument at the ISIS spallation source. The performances of the GEM-detectors are compared with those of conventional 3He tubes installed on the INES instrument. The conceptual detector with the 3D converter used in this paper reached a count rate per unit area of about 25% relative to the currently installed 3He tube. Its timing resolution is similar and the signal-to-background ratio (S/B) is 2 times lower.

Capturing Structural Dynamics in Crystalline Silicon Using Chirped Electrons from a Laser Wakefield Accelerator

PubMed Central

He, Z.-H.; Beaurepaire, B.; Nees, J. A.; Gallé, G.; Scott, S. A.; Pérez, J. R. Sánchez; Lagally, M. G.; Krushelnick, K.; Thomas, A. G. R.; Faure, J.

2016-01-01

Recent progress in laser wakefield acceleration has led to the emergence of a new generation of electron and X-ray sources that may have enormous benefits for ultrafast science. These novel sources promise to become indispensable tools for the investigation of structural dynamics on the femtosecond time scale, with spatial resolution on the atomic scale. Here, we demonstrate the use of laser-wakefield-accelerated electron bunches for time-resolved electron diffraction measurements of the structural dynamics of single-crystal silicon nano-membranes pumped by an ultrafast laser pulse. In our proof-of-concept study, we resolve the silicon lattice dynamics on a picosecond time scale by deflecting the momentum-time correlated electrons in the diffraction peaks with a static magnetic field to obtain the time-dependent diffraction efficiency. Further improvements may lead to femtosecond temporal resolution, with negligible pump-probe jitter being possible with future laser-wakefield-accelerator ultrafast-electron-diffraction schemes. PMID:27824086

Capturing Structural Dynamics in Crystalline Silicon Using Chirped Electrons from a Laser Wakefield Accelerator

DOE PAGES

He, Z. -H.; Beaurepaire, B.; Nees, J. A.; ...

2016-11-08

Recent progress in laser wakefield acceleration has led to the emergence of a new generation of electron and X-ray sources that may have enormous benefits for ultrafast science. These novel sources promise to become indispensable tools for the investigation of structural dynamics on the femtosecond time scale, with spatial resolution on the atomic scale. Here in this paper, we demonstrate the use of laser-wakefield-accelerated electron bunches for time-resolved electron diffraction measurements of the structural dynamics of single-crystal silicon nano-membranes pumped by an ultrafast laser pulse. In our proof-of-concept study, we resolve the silicon lattice dynamics on a picosecond time scalemore » by deflecting the momentum-time correlated electrons in the diffraction peaks with a static magnetic field to obtain the time-dependent diffraction efficiency. Further improvements may lead to femtosecond temporal resolution, with negligible pump-probe jitter being possible with future laser-wakefield-accelerator ultrafast-electron-diffraction schemes.« less

The significance of Bragg's law in electron diffraction and microscopy, and Bragg's second law.

PubMed

Humphreys, C J

2013-01-01

Bragg's second law, which deserves to be more widely known, is recounted. The significance of Bragg's law in electron diffraction and microscopy is then discussed, with particular emphasis on differences between X-ray and electron diffraction. As an example of such differences, the critical voltage effect in electron diffraction is described. It is then shown that the lattice imaging of crystals in high-resolution electron microscopy directly reveals the Bragg planes used for the imaging process, exactly as visualized by Bragg in his real-space law. Finally, it is shown how in 2012, for the first time, on the centennial anniversary of Bragg's law, single atoms have been identified in an electron microscope using X-rays emitted from the specimen. Hence atomic resolution X-ray maps of a crystal in real space can be formed which give the positions and identities of the different atoms in the crystal, or of a single impurity atom in the crystal.

Hierarchical assembly of urchin-like alpha-iron oxide hollow microspheres and molybdenum disulphide nanosheets for ethanol gas sensing.

PubMed

Zhang, Dongzhi; Fan, Xin; Yang, Aijun; Zong, Xiaoqi

2018-08-01

In this paper, we fabricated a high-performance ethanol sensor using layer-by-layer self-assembled urchin-like alpha-iron oxide (α-Fe 2 O 3 ) hollow microspheres/molybdenum disulphide (MoS 2 ) nanosheets heterostructure as sensitive materials. The nanostructural, morphological, and compositional properties of the as-prepared α-Fe 2 O 3 /MoS 2 heterostructure were characterized by X-ray diffraction (XRD), energy dispersive spectrometer (EDS), scanning electron microscopy (SEM), transmission electron microscope (TEM) and X-ray photoelectron spectroscopy (XPS), which confirmed its successful preparation and rationality. The α-Fe 2 O 3 /MoS 2 nanocomposite sensor shows good selectivity, excellent reproducibility, fast response/recovery time and low detection limit towards ethanol gas at room temperature, which is superior to the single component of α-Fe 2 O 3 hollow microspheres and MoS 2 nanosheets. Furthermore, the response of the α-Fe 2 O 3 /MoS 2 nanocomposite sensor as a function of ethanol gas concentration was also demonstrated. The enhanced ethanol sensing properties of the α-Fe 2 O 3 /MoS 2 nanocomposite sensor were ascribed to the synergistic effect and heterojunction between the urchin-Like α-Fe 2 O 3 hollow microspheres and MoS 2 nanosheets. This work verifies that the hierarchical α-Fe 2 O 3 /MoS 2 nanoheterostructure is a potential candidate for fabricating room-temperature ethanol gas sensor. Copyright © 2018 Elsevier Inc. All rights reserved.

Hydroquinone and Quinone-Grafted Porous Carbons for Highly Selective CO2 Capture from Flue Gases and Natural Gas Upgrading.

PubMed

Wang, Jun; Krishna, Rajamani; Yang, Jiangfeng; Deng, Shuguang

2015-08-04

Hydroquinone and quinone functional groups were grafted onto a hierarchical porous carbon framework via the Friedel-Crafts reaction to develop more efficient adsorbents for the selective capture and removal of carbon dioxide from flue gases and natural gas. The oxygen-doped porous carbons were characterized with scanning electron microscopy, transmission electron microscopy, X-ray powder diffraction, Fourier transform infrared spectroscopy, and Raman spectroscopy. CO2, CH4, and N2 adsorption isotherms were measured and correlated with the Langmuir model. An ideal adsorbed solution theory (IAST) selectivity for the CO2/N2 separation of 26.5 (298 K, 1 atm) was obtained on the hydroquinone-grafted carbon, which is 58.7% higher than that of the pristine porous carbon, and a CO2/CH4 selectivity value of 4.6 (298 K, 1 atm) was obtained on the quinone-grafted carbon (OAC-2), which represents a 28.4% improvement over the pristine porous carbon. The highest CO2 adsorption capacity on the oxygen-doped carbon adsorbents is 3.46 mmol g(-1) at 298 K and 1 atm. In addition, transient breakthrough simulations for CO2/CH4/N2 mixture separation were conducted to demonstrate the good separation performance of the oxygen-doped carbons in fixed bed adsorbers. Combining excellent adsorption separation properties and low heats of adsorption, the oxygen-doped carbons developed in this work appear to be very promising for flue gas treatment and natural gas upgrading.

Quasi-parallel precession diffraction: Alignment method for scanning transmission electron microscopes.

PubMed

Plana-Ruiz, S; Portillo, J; Estradé, S; Peiró, F; Kolb, Ute; Nicolopoulos, S

2018-06-06

A general method to set illuminating conditions for selectable beam convergence and probe size is presented in this work for Transmission Electron Microscopes (TEM) fitted with µs/pixel fast beam scanning control, (S)TEM, and an annular dark field detector. The case of interest of beam convergence and probe size, which enables diffraction pattern indexation, is then used as a starting point in this work to add 100 Hz precession to the beam while imaging the specimen at a fast rate and keeping the projector system in diffraction mode. The described systematic alignment method for the adjustment of beam precession on the specimen plane while scanning at fast rates is mainly based on the sharpness of the precessed STEM image. The complete alignment method for parallel condition and precession, Quasi-Parallel PED-STEM, is presented in block diagram scheme, as it has been tested on a variety of instruments. The immediate application of this methodology is that it renders the TEM column ready for the acquisition of Precessed Electron Diffraction Tomographies (EDT) as well as for the acquisition of slow Precessed Scanning Nanometer Electron Diffraction (SNED). Examples of the quality of the Precessed Electron Diffraction (PED) patterns and PED-STEM alignment images are presented with corresponding probe sizes and convergence angles. Copyright © 2018. Published by Elsevier B.V.

Gas Sensor Based on 3-D WO3 Inverse Opal: Design and Applications

PubMed Central

Xing, Ruiqing; Du, Yang; Zhao, Xiaonan; Zhang, Xiu

2017-01-01

A three-dimensional inverse opal (3DIO) WO3 architecture has been synthesized via a simple sacrificial template method. Morphology features of the 3DIO were characterized by scanning electron microscope (SEM) and its structure was characterized by X-ray diffraction (XRD). The shrinking ratio of the PMMA spheres was ~28.2% through measuring the distribution of the PMMA spheres and 3DIO WO3 center-to-center distance between the spheres and macropores, respectively. Beyond that, the 3DIO gas sensing properties were investigated systematically and the sensing mechanism of 3DIO WO3 was proposed. The results indicated that the response of the 3DIO sensor possessed excellent sensitivity to acetone gas, especially at trace levels. The 3DIO gas sensor response was ~7 to 5 ppm of acetone and could detect acetone low to 0.2 ppm effectively, which was in close proximity to the theoretical low detection limit of 0.14 ppm when Ra/Rg ≥ 1.2 was used as the criterion for reliable gas sensing. All in all, the obvious satisfaction of the gas-sensing properties was ascribed to the structure of the 3DIO, and the sensor could be a promising novel device in the future. PMID:28353672

Physical properties and surface/interface analysis of nanocrystalline WO3 films grown under variable oxygen gas flow rates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vemuri, R. S.; Carbjal-Franco, G.; Ferrer, D. A.

2012-10-15

Nanocrystalline WO3 films were grown by reactive magnetron sputter-deposition in a wide range of oxygen gas flow rates while keeping the deposition temperature fixed at 400 oC. The physical characteristics of WO3 films were evaluated using grazing incidence X-ray diffraction (GIXRD), X-ray reflectivity (XRR) and transmission electron microscopy (TEM) measurements. Physical characterization indicates that the thickness, grain size, and density of WO3 films are sensitive to the oxygen gas flow rate during deposition. XRD data indicates the formation of tetragonal WO3 films. The grain size increases from 21 to 25 nm with increasing oxygen gas flow rate to 65%, atmore » which point the grain size exhibits a decreasing trend to attain the lowest value of 15 nm at 100% oxygen. TEM analysis provides a model consisting of isotropic WO3 film (nanocrystalline)-SiO2 interface (amorphous)-Si(100) substrate. XRR simulations, which are based on this model, provide excellent agreement to the experimental data indicating that the normalized thickness of WO3 films decreases with the increasing oxygen gas flow rate. The density of WO3 films increases with increasing oxygen gas flow rate.« less

Comments on the paper "Bragg's law diffraction simulations for electron backscatter diffraction analysis" by Josh Kacher, Colin Landon, Brent L. Adams & David Fullwood.

PubMed

Maurice, Claire; Fortunier, Roland; Driver, Julian; Day, Austin; Mingard, Ken; Meaden, Graham

2010-06-01

This comment on the paper "Bragg's Law diffraction simulations for electron backscatter diffraction analysis" by Kacher et al. explains the limitations in determining elastic strains using synthetic EBSD patterns. Of particular importance are those due to the accuracy of determination of the EBSD geometry projection parameters. Additional references and supporting information are provided. Copyright 2010 Elsevier B.V. All rights reserved.

Anomalous Diffraction in Crystallographic Phase Evaluation

PubMed Central

Hendrickson, Wayne A.

2014-01-01

X-ray diffraction patterns from crystals of biological macromolecules contain sufficient information to define atomic structures, but atomic positions are inextricable without having electron-density images. Diffraction measurements provide amplitudes, but the computation of electron density also requires phases for the diffracted waves. The resonance phenomenon known as anomalous scattering offers a powerful solution to this phase problem. Exploiting scattering resonances from diverse elements, the methods of multiwavelength anomalous diffraction (MAD) and single-wavelength anomalous diffraction (SAD) now predominate for de novo determinations of atomic-level biological structures. This review describes the physical underpinnings of anomalous diffraction methods, the evolution of these methods to their current maturity, the elements, procedures and instrumentation used for effective implementation, and the realm of applications. PMID:24726017

Structures of Astromaterials Revealed by EBSD

NASA Technical Reports Server (NTRS)

Zolensky, M.

2018-01-01

Groups at the Johnson Space Center and the University of Tokyo have been using electron back-scattered diffraction (EBSD) to reveal the crystal structures of extraterrestrial minerals for many years. Even though we also routinely use transmission electron microscopy, synchrotron X-ray diffraction (SXRD), and conventional electron diffraction, we find that EBSD is the most powerful technique for crystal structure elucidation in many instances. In this talk I describe a few of the cases where we have found EBSD to provide crucial, unique information. See attachment.

Serial single molecule electron diffraction imaging: diffraction background of superfluid helium droplets

NASA Astrophysics Data System (ADS)

Zhang, Jie; He, Yunteng; Lei, Lei; Alghamdi, Maha; Oswalt, Andrew; Kong, Wei

2017-08-01

In an effort to solve the crystallization problem in crystallography, we have been engaged in developing a method termed "serial single molecule electron diffraction imaging" (SS-EDI). The unique features of SS-EDI are superfluid helium droplet cooling and field-induced orientation: together the two features constitute a molecular goniometer. Unfortunately, the helium atoms surrounding the sample molecule also contribute to a diffraction background. In this report, we analyze the properties of a superfluid helium droplet beam and its doping statistics, and demonstrate the feasibility of overcoming the background issue by using the velocity slip phenomenon of a pulsed droplet beam. Electron diffraction profiles and pair correlation functions of ferrocene-monomer-doped droplets and iodine-nanocluster-doped droplets are presented. The timing of the pulsed electron gun and the effective doping efficiency under different dopant pressures can both be controlled for size selection. This work clears any doubt of the effectiveness of superfluid helium droplets in SS-EDI, thereby advancing the effort in demonstrating the "proof-of-concept" one step further.

Device and method for creating Gaussian aberration-corrected electron beams

DOEpatents

McMorran, Benjamin; Linck, Martin

2016-01-19

Electron beam phase gratings have phase profiles that produce a diffracted beam having a Gaussian or other selected intensity profile. Phase profiles can also be selected to correct or compensate electron lens aberrations. Typically, a low diffraction order produces a suitable phase profile, and other orders are discarded.

Breaking resolution limits in ultrafast electron diffraction and microscopy.

PubMed

Baum, Peter; Zewail, Ahmed H

2006-10-31

Ultrafast electron microscopy and diffraction are powerful techniques for the study of the time-resolved structures of molecules, materials, and biological systems. Central to these approaches is the use of ultrafast coherent electron packets. The electron pulses typically have an energy of 30 keV for diffraction and 100-200 keV for microscopy, corresponding to speeds of 33-70% of the speed of light. Although the spatial resolution can reach the atomic scale, the temporal resolution is limited by the pulse width and by the difference in group velocities of electrons and the light used to initiate the dynamical change. In this contribution, we introduce the concept of tilted optical pulses into diffraction and imaging techniques and demonstrate the methodology experimentally. These advances allow us to reach limits of time resolution down to regimes of a few femtoseconds and, possibly, attoseconds. With tilted pulses, every part of the sample is excited at precisely the same time as when the electrons arrive at the specimen. Here, this approach is demonstrated for the most unfavorable case of ultrafast crystallography. We also present a method for measuring the duration of electron packets by autocorrelating electron pulses in free space and without streaking, and we discuss the potential of tilting the electron pulses themselves for applications in domains involving nuclear and electron motions.

A New Technique to Produce Clean and Thin Silicon Films In Situ in a UHV Electron Microscope for TEM-TED Studies of Surfaces

NASA Astrophysics Data System (ADS)

Ozawa, Soh-ichiro; Yamanaka, Akira; Kobayashi, Kunio; Tanishiro, Yasumasa; Yagi, Katsumichi

1990-04-01

A new technique of in situ oxygen gas reaction thinning of Si films at around 750-800°C in an ultrahigh-vacuum electron microscope was developed. The technique produced films as thin as 10 to 20 nm. Such a thin film allows us to observe surface atomic steps, out-of-phase boundaries and {1/7 0}, {1/7 1/7} and {2/7 0} spots from the Si(111)7× 7 surface. These spots were not observed in previous studies, having been masked by strong inelastic scattering. The technique is useful not only for detecting clear diffraction spots of kinematical intensity for surface structure analysis but also for observation of high-resolution plan-view structure images of clean and adsorbed surfaces.

Heterogeneous catalytic ozonation of hydroquinone using sewage sludge-derived carbonaceous catalysts.

PubMed

Xu, Jinglu; Yu, Yang; Ding, Kang; Liu, Zhiying; Wang, Lei; Xu, Yanhua

2018-03-01

This study converted sewage sludge into a carbonaceous catalyst via pyrolysis and employed it in the ozonation of hydroquinone. The catalyst was characterized by Mössbauer spectroscopy, X-ray photoelectron spectroscopy, temperature programmed desorption, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. Intermediate products were detected by gas chromatography-mass spectrometry, and a pathway for hydroquinone degradation was proposed. The results showed that sludge pyrolyzed at 700 °C promoted hydroquinone degradation, compared with commercial activated carbon derived from coal. When the catalyst dose was 0.5 g/L, the hydroquinone (200 mg/L) removal rate reached 97.86% after exposure to ozone (the ozone concentration was 17 mg/L and the flow rate was 50 mL/min) for 60 min. The results indicated that basic groups contributed to the catalysis.

Enhancement of diffraction efficiency and storage life of poly(vinyl chloride)-based optical recording medium with incorporation of an electron donor

NASA Astrophysics Data System (ADS)

John, Beena Mary; Ushamani, M.; Sreekumar, K.; Joseph, Rani; Sudha Kartha, C.

2007-01-01

The diffraction efficiency, sensitivity, and storage life of methylene blue-sensitized poly(vinyl chloride) film was improved by the addition of an electron donor in the matrix. The addition of pyridine enhanced the diffraction efficiency by two times, and storage life of the gratings was increased to 2-3 days.

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector.

PubMed

van Genderen, E; Clabbers, M T B; Das, P P; Stewart, A; Nederlof, I; Barentsen, K C; Portillo, Q; Pannu, N S; Nicolopoulos, S; Gruene, T; Abrahams, J P

2016-03-01

Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼ 0.013 e(-) Å(-2) s(-1)) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014).

Single-shot coherent diffraction imaging of microbunched relativistic electron beams for free-electron laser applications.

PubMed

Marinelli, A; Dunning, M; Weathersby, S; Hemsing, E; Xiang, D; Andonian, G; O'Shea, F; Miao, Jianwei; Hast, C; Rosenzweig, J B

2013-03-01

With the advent of coherent x rays provided by the x-ray free-electron laser (FEL), strong interest has been kindled in sophisticated diffraction imaging techniques. In this Letter, we exploit such techniques for the diagnosis of the density distribution of the intense electron beams typically utilized in an x-ray FEL itself. We have implemented this method by analyzing the far-field coherent transition radiation emitted by an inverse-FEL microbunched electron beam. This analysis utilizes an oversampling phase retrieval method on the transition radiation angular spectrum to reconstruct the transverse spatial distribution of the electron beam. This application of diffraction imaging represents a significant advance in electron beam physics, having critical applications to the diagnosis of high-brightness beams, as well as the collective microbunching instabilities afflicting these systems.

Electron microscopy analyses and electrical properties of the layered Bi{sub 2}WO{sub 6} phase

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taoufyq, A.; Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir, Maroc; Département d‘Études des Réacteurs, Laboratoire Dosimétrie Capteurs Instrumentation, CEA Cadarache

2013-07-15

The bismuth tungstate Bi{sub 2}WO{sub 6} was synthesized using a classical coprecipitation method followed by a calcination process at different temperatures. The samples were characterized by X-ray diffraction, simultaneous thermogravimetry and differential thermal analysis (TGA/DTA), scanning and transmission electron microscopy (SEM, TEM) analyses. The Rietveld analysis and electron diffraction clearly confirmed the Pca2{sub 1} non centrosymmetric space group previously proposed for this phase. The layers Bi{sub 2}O{sub 2}{sup 2+} and WO{sub 4}{sup 2−} have been directly evidenced from the HRTEM images. The electrical properties of Bi{sub 2}WO{sub 6} compacted pellets systems were determined from electrical impedance spectrometry (EIS) and directmore » current (DC) analyses, under air and argon, between 350 and 700 °C. The direct current analyses showed that the conduction observed from EIS analyses was mainly ionic in this temperature range, with a small electronic contribution. Electrical change above the transition temperature of 660 °C is observed under air and argon atmospheres. The strong conductivity increase observed under argon is interpreted in terms of formation of additional oxygen vacancies coupled with electron conduction. - Graphical abstract: High resolution transmission electron microscopy: inverse fast Fourier transform giving the layered structure of the Bi{sub 2}WO{sub 6} phase, with a representation of the cell dimensions (b and c vectors). The Bi{sub 2}O{sub 2}{sup 2+} and WO{sub 4}{sup 2−} sandwiches are visible in the IFFT image. - Highlights: • Using transmission electron microscopy, we visualize the layered structure of Bi{sub 2}WO{sub 6}. • Electrical analyses under argon gas show some increase in conductivity. • The phase transition at 660 °C is evidenced from electrical modification.« less

Atomic and Molecular Beam Scattering: Characterizing Structure and Dynamics of Hybrid Organic-Semiconductor Interfaces and Introducing Novel Isotope Separation Techniques

NASA Astrophysics Data System (ADS)

Nihill, Kevin John

This thesis details a range of experiments and techniques that use the scattering of atomic beams from surfaces to both characterize a variety of interfaces and harness mass-specific scattering conditions to separate and enrich isotopic components in a mixture of gases. Helium atom scattering has been used to characterize the surface structure and vibrational dynamics of methyl-terminated Ge(111), thereby elucidating the effects of organic termination on a rigid semiconductor interface. Helium atom scattering was employed as a surface-sensitive, non-destructive probe of the surface. By means of elastic gas-surface diffraction, this technique is capable of providing measurements of atomic spacing, step height, average atomic displacement as a function of surface temperature, gas-surface potential well depth, and surface Debye temperature. Inelastic time-of-flight studies provide highly resolved energy exchange measurements between helium atoms and collective lattice vibrations, or phonons; a collection of these measurements across a range of incident kinematic parameters allowed for a thorough mapping of low-energy phonons (e.g., the Rayleigh wave) across the surface Brillouin zone and subsequent comparison with complementary theoretical calculations. The scattering of molecular beams - here, hydrogen and deuterium from methyl-terminated Si(111) - enables the measurement of the anisotropy of the gas-surface interaction potential through rotationally inelastic diffraction (RID), whereby incident atoms can exchange internal energy between translational and rotational modes and diffract into unique angular channels as a result. The probability of rotational excitations as a function of incident energy and angle were measured and compared with electronic structure and scattering calculations to provide insight into the gas-surface interaction potential and hence the surface charge density distribution, revealing important details regarding the interaction of H2 with an organic-functionalized semiconductor interface. Aside from their use as probes for surface structure and dynamics, atomic beam sources are also demonstrated to enable the efficient separation of gaseous mixtures of isotopes by means of diffraction and differential condensation. In the former method, the kinematic conditions for elastic diffraction result in an incident beam of natural abundance neon diffracting into isotopically distinct angles, resulting in the enrichment of a desired isotope; this purification can be improved by exploiting the difference in arrival times of the two isotopes at a given final angle. In the latter method, the identical incident velocities of coexpanded isotopes lead to minor but important differences in their incident kinetic energies, and thus their probability of adsorbing on a sufficiently cold surface, resulting in preferential condensation of a given isotope that depends on the energy of the incident beam. Both of these isotope separation techniques are made possible by the narrow velocity distribution and velocity seeding effect offered only by high-Mach number supersonic beam sources. These experiments underscore the utility of supersonically expanded atomic and molecular beam sources as both extraordinarily precise probes of surface structure and dynamics and as a means for high-throughput, non-dissociative isotopic enrichment methods.

Solving the jitter problem in microwave compressed ultrafast electron diffraction instruments: Robust sub-50 fs cavity-laser phase stabilization

PubMed Central

Otto, M. R.; René de Cotret, L. P.; Stern, M. J.; Siwick, B. J.

2017-01-01

We demonstrate the compression of electron pulses in a high-brightness ultrafast electron diffraction instrument using phase-locked microwave signals directly generated from a mode-locked femtosecond oscillator. Additionally, a continuous-wave phase stabilization system that accurately corrects for phase fluctuations arising in the compression cavity from both power amplification and thermal drift induced detuning was designed and implemented. An improvement in the microwave timing stability from 100 fs to 5 fs RMS is measured electronically, and the long-term arrival time stability (>10 h) of the electron pulses improves to below our measurement resolution of 50 fs. These results demonstrate sub-relativistic ultrafast electron diffraction with compressed pulses that is no longer limited by laser-microwave synchronization. PMID:28852686

Aluminum surface modification by a non-mass-analyzed nitrogen ion beam

NASA Astrophysics Data System (ADS)

Ohira, Shigeo; Iwaki, Masaya

Non-mass-analyzed nitrogen ion implantation into polycrystal and single crystal aluminum sheets has been carried out at an accelerating voltage of 90 kV and a dose of 1 × 10 18 N ions/cm 2 using a Zymet implanter model Z-100. The pressure during implantation rose to 10 -3 Pa due to the influence of N gas feeding into the ion source. The characteristics of the surface layers were investigated by means of Auger electron spectroscopy (AES), X-ray diffraction (XRD), transmission electron diffraction (TED), and microscopy (TEM). The AES depth profiling shows a rectangular-like distribution of N atoms and little migration of O atoms near the surface. The high dose N-implantation forms c-axis oriented aluminum nitride (AIN) crystallines, and especially irradiation of Al single crystals with N ions leads to the formation of a hcp AlN single crystal. It is concluded that the high dose N-implantation in Al can result in the formation of AlN at room temperature without any thermal annealing. Furthermore, non-mass-analyzed N-implantation at a pressure of 10 -3 Pa of the nitrogen atmosphere causes the formation of pure AlN single crystals in the Al surface layer and consequently it can be practically used for AlN production.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mene, Ravindra U.; School of Physical Sciences, Swami Ramanand Teerth Marathwada University, Nanded 431606, M.S.; Mahabole, Megha P.

Highlights: • We report improved gas sensing and dielectric characteristics of Fe ion exchanged HAp films. • Fe doped HAp film shows maximum gas response at relatively lower temperature. • Response and gas uptake capacity of sensors is improved for appropriate amount of Fe ions in HAp matrix. • Fe-HAp films exhibit remarkable improvement in dielectric properties compared to pure HAp. • Fe doped HAp films show significant improvement in gas sensing as well as in dielectric properties. - Abstract: In the present work Fe doped hydroxyapatite (Fe-HAp) thick films has been successfully utilized to improve the gas sensing asmore » well as its dielectric properties. Initially, HAp nano powder is synthesized by chemical precipitation process and later on Fe ions are doped in HAp by ion exchange process. Structural and morphological modifications are observed by means of X-ray diffraction and scanning electron microscopy analysis. The sensing parameters such as operating temperature, response/recovery time and gas uptake capacity are experimentally determined. The Fe-HAp (0.05 M) film shows improved CO and CO{sub 2} gas sensing capacity at lower operating temperature compared to pure HAp. Moreover, variation of dielectric constant and dielectric loss for pure and Fe-HAp thick films are studied as a function of frequency in the range of 10 Hz–1 MHz. The study reveals that Fe doped HAp thick films improve the sensing and dielectric characteristics as compared to pure HAp.« less

Quantum diffraction and shielding effects on the low-energy electron-ion bremsstrahlung in two-component semiclassical plasmas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, Myoung-Jae; Jung, Young-Dae, E-mail: ydjung@hanyang.ac.kr; Department of Physics, Applied Physics, and Astronomy, Rensselaer Polytechnic Institute, 110 8th Street, Troy, New York 12180-3590

2015-10-15

The quantum diffraction and shielding effects on the low-energy bremsstrahlung process are investigated in two-component semiclassical plasmas. The impact-parameter analysis with the micropotential taking into account the quantum diffraction and shielding effects is employed to obtain the electron-ion bremsstrahlung radiation cross section as a function of the de Broglie wavelength, density parameter, impact parameter, photon energy, and projectile energy. The result shows that the influence of quantum diffraction and shielding strongly suppresses the bremsstrahlung radiation spectrum in semiclassical plasmas. It is found that the quantum diffraction and shielding effects have broaden the photon emission domain. It is also found thatmore » the photon emission domain is almost independent of the radiation photon energy. In addition, it is found that the influence of quantum diffraction and shielding on the bremsstrahlung spectrum decreases with an increase of the projectile energy. The density effect on the electron-ion bremsstrahlung cross section is also discussed.« less

Holographic Reconstruction of Photoelectron Diffraction and Its Circular Dichroism for Local Structure Probing

NASA Astrophysics Data System (ADS)

Matsui, Fumihiko; Matsushita, Tomohiro; Daimon, Hiroshi

2018-06-01

The local atomic structure around a specific element atom can be recorded as a photoelectron diffraction pattern. Forward focusing peaks and diffraction rings around them indicate the directions and distances from the photoelectron emitting atom to the surrounding atoms. The state-of-the-art holography reconstruction algorithm enables us to image the local atomic arrangement around the excited atom in a real space. By using circularly polarized light as an excitation source, the angular momentum transfer from the light to the photoelectron induces parallax shifts in these diffraction patterns. As a result, stereographic images of atomic arrangements are obtained. These diffraction patterns can be used as atomic-site-resolved probes for local electronic structure investigation in combination with spectroscopy techniques. Direct three-dimensional atomic structure visualization and site-specific electronic property analysis methods are reviewed. Furthermore, circular dichroism was also found in valence photoelectron and Auger electron diffraction patterns. The investigation of these new phenomena provides hints for the development of new techniques for local structure probing.

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

The use of analytical surface tools in the fundamental study of wear. [atomic nature of wear

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1977-01-01

Various techniques and surface tools available for the study of the atomic nature of the wear of materials are reviewed These include chemical etching, x-ray diffraction, electron diffraction, scanning electron microscopy, low-energy electron diffraction, Auger emission spectroscopy analysis, electron spectroscopy for chemical analysis, field ion microscopy, and the atom probe. Properties of the surface and wear surface regions which affect wear, such as surface energy, crystal structure, crystallographic orientation, mode of dislocation behavior, and cohesive binding, are discussed. A number of mechanisms involved in the generation of wear particles are identified with the aid of the aforementioned tools.

Local nanoscale strain mapping of a metallic glass during in situ testing

NASA Astrophysics Data System (ADS)

Gammer, Christoph; Ophus, Colin; Pekin, Thomas C.; Eckert, Jürgen; Minor, Andrew M.

2018-04-01

The local elastic strains during tensile deformation in a CuZrAlAg metallic glass are obtained by fitting an elliptic shape function to the characteristic amorphous ring in electron diffraction patterns. Scanning nanobeam electron diffraction enables strain mapping with a resolution of a few nanometers. Here, a fast direct electron detector is used to acquire the diffraction patterns at a sufficient speed to map the local transient strain during continuous tensile loading in situ in the transmission electron microscope. The elastic strain in tensile direction was found to increase during loading. After catastrophic fracture, a residual elastic strain that relaxes over time was observed.

Fabrication and Characterizations of Ethanol Sensor Based on CuO Nanoparticles.

PubMed

Al-Hadeethi, Yas; Umar, Ahmad; Kumar, Rajesh; Al-Heniti, Saleh H; Raffah, Bahaaudin M

2018-04-01

In this paper, we report the synthesis, characterization and ethanol sensing applications of CuO nanoparticles. The CuO nanoparticles were prepared by a facile, low-temperature hydrothermal method and characterized in detail in terms of their structural, morphological, compositional and crystalline properties, through different characterization techniques including X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) attached with energy dispersive spectroscopy (EDS), and Fourier transform infrared (FTIR) spectroscopy. The detailed studies revealed that the synthesized CuO nanoparticles were well-crystalline and possessed monoclinic crystal structure. The synthesized CuO nanoparticles were utilized for the fabrication of highly sensitive ethanol gas sensor. At an optimized temperature of 320 °C, high sensitivity (Ra/Rg) of 39.29 was observed for 200 ppm of ethanol gas. Additionally, very low response (τres = 14 s) and recovery (τrec = 30 s) times were observed for 100 ppm of ethanol.

Formaldehyde sensor based on Ni-doped tetrapod-shaped ZnO nanopowder induced by external magnetic field

NASA Astrophysics Data System (ADS)

Bai, Zikui; Xie, Changsheng; Hu, Mulin; Zhang, Shunping

2008-12-01

The sensors based on Ni-doped ZnO nanopowder with tetrapod-shape (T-ZnO) were fabricated by screen-printing technique with external magnetic field in different direction. The morphologies and crystal structures of the thick film were characterized by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM), respectively. Gas-sensing property of sensors responded to 100 ppm formaldehyde was also detected. The results show that the direction of magnetic field has crucial effect on the sensor sensitivity. The sensors based on 5 wt% Ni-doped T-ZnO induced by magnetic field in parallel direction to the thick film surface, has the optimization sensitivity, the shortest response and recovery time, which are 10.6, 16 and 15 s, respectively. The magnetic-field induction model and the gas-sensing mechanism of the Ni-doped T-ZnO are proposed.

Bio-green synthesis of Fe doped SnO2 nanoparticle thin film

NASA Astrophysics Data System (ADS)

Gattu, Ketan P.; Ghule, Kalyani; Huse, Nanasaheb P.; Dive, Avinash S.; Bagul, Sagar B.; Digraskar, Renuka V.; Sharma, Ramphal; Ghule, Anil V.

2017-05-01

Herein Fe doped SnO2 nanoparticles have been synthesized using simple, cost effective and ecofriendly biosynthesis method, in which remnant water (ideally kitchen waste) collected from soaked Bengal gram beans (Cicer arietinum L.) was used. This extract consists of different bio-molecules which acted as complexing as well as capping agents for synthesis of Fe-doped SnO2 nanoparticles. The X-ray powder diffraction (XRD) and Field-emission scanning electron microscopy (FE-SEM) revealed uniform size distribution with the average size of 6 nm and confirmed the formation of rutile structure with space group (P42/mnm) and nanocrystalline nature of the products with spherical morphology. Further, the gas sensing properties of the materials have been studied in comparison with other gases. The reported gas sensing results are promising, which suggest that the Fe-dopant is a promising noble metal additives to fabricate low cost SnO2 based sensor.

Mechanism of room temperature oxygen sensor based on nanocrystalline TiO2 film

NASA Astrophysics Data System (ADS)

Bakri, A. S.; Sahdan, M. Z.; Nafarizal, N.; Abdullah, S. A.; Said, N. D. M.; Raship, N. A.; Sari, Y.

2018-04-01

A titanium dioxide (TiO2) thin film is proposed as the active layer for the detection of oxygen gas. The sensor is fabricated on silicon wafer using sol-gel dip coating technique with a constant withdrawal speed. The field emission scanning electron microscope image reveals that the film has a uniform structure while the x-ray diffraction analysis indicates that the film is anatase phase with tetragonal lattice structure. The film exhibit the highest intensity peak at (101) plane. The surface roughness measurement shows that the film has low surface roughness with small grain size. The electrical studies revealed that the resistivity is about 4.02 x 10-3 Ω.cm and the thickness of TiO2 film is 127.44 nm. The gas sensor measurement showed that the sensor response of the film is about 4.21% at room temperature.

Hydrogen sensing properties of nanocomposite graphene oxide/Co-based metal organic frameworks (Co-MOFs@GO)

NASA Astrophysics Data System (ADS)

Fardindoost, Somayeh; Hatamie, Shadie; Iraji Zad, Azam; Razi Astaraei, Fatemeh

2018-01-01

This paper reports on hydrogen sensing based graphene oxide hybrid with Co-based metal organic frameworks (Co-MOFs@GO) prepared by the hydrothermal process. The texture and morphology of the hybrid were characterized by powder x-ray diffraction, scanning electron microscopy and Brunauer-Emmett-Teller analysis. Porous flower like structures assembled from Co-MOFs and GO flakes with sufficient specific surface area are obtained, which are ideal for gas molecules diffusion and interactions. Sensing performance of Co-MOFs@GO were tested and also improved by sputtering platinum (Pt) as a catalyst. The Pt-sputtered Co-MOFs@GO show outstanding hydrogen resistive-sensing with response and recovery times below 12 s at 15 °C. Also, they show stable, repeatable and selective responses to the target gas which make it suitable for the development of a high performance hydrogen sensor.

Au sensitized ZnO nanorods for enhanced liquefied petroleum gas sensing properties

NASA Astrophysics Data System (ADS)

Nakate, U. T.; Bulakhe, R. N.; Lokhande, C. D.; Kale, S. N.

2016-05-01

The zinc oxide (ZnO) nanorods have grown on glass substrate by spray pyrolysis deposition (SPD) method using zinc acetate solution. The phase formation, surface morphology and elemental composition of ZnO films have been investigated using X-ray diffraction, field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM) and energy dispersive X-ray (EDX) techniques. The liquefied petroleum gas (LPG) sensing response was remarkably improved by sensitization of gold (Au) surface noble metal on ZnO nanorods film. Maximum LPG response of 21% was observed for 1040 ppm of LPG, for pure ZnO nanorods sample. After Au sensitization on ZnO nanorods film sample, the LPG response greatly improved up to 48% at operating temperature 623 K. The improved LPG response is attributed Au sensitization with spill-over mechanism. Proposed model for LPG sensing mechanism discussed.

Low-energy transmission electron diffraction and imaging of large-area graphene

PubMed Central

Zhao, Wei; Xia, Bingyu; Lin, Li; Xiao, Xiaoyang; Liu, Peng; Lin, Xiaoyang; Peng, Hailin; Zhu, Yuanmin; Yu, Rong; Lei, Peng; Wang, Jiangtao; Zhang, Lina; Xu, Yong; Zhao, Mingwen; Peng, Lianmao; Li, Qunqing; Duan, Wenhui; Liu, Zhongfan; Fan, Shoushan; Jiang, Kaili

2017-01-01

Two-dimensional (2D) materials have attracted interest because of their excellent properties and potential applications. A key step in realizing industrial applications is to synthesize wafer-scale single-crystal samples. Until now, single-crystal samples, such as graphene domains up to the centimeter scale, have been synthesized. However, a new challenge is to efficiently characterize large-area samples. Currently, the crystalline characterization of these samples still relies on selected-area electron diffraction (SAED) or low-energy electron diffraction (LEED), which is more suitable for characterizing very small local regions. This paper presents a highly efficient characterization technique that adopts a low-energy electrostatically focused electron gun and a super-aligned carbon nanotube (SACNT) film sample support. It allows rapid crystalline characterization of large-area graphene through a single photograph of a transmission-diffracted image at a large beam size. Additionally, the low-energy electron beam enables the observation of a unique diffraction pattern of adsorbates on the suspended graphene at room temperature. This work presents a simple and convenient method for characterizing the macroscopic structures of 2D materials, and the instrument we constructed allows the study of the weak interaction with 2D materials. PMID:28879233

Low-energy transmission electron diffraction and imaging of large-area graphene.

PubMed

Zhao, Wei; Xia, Bingyu; Lin, Li; Xiao, Xiaoyang; Liu, Peng; Lin, Xiaoyang; Peng, Hailin; Zhu, Yuanmin; Yu, Rong; Lei, Peng; Wang, Jiangtao; Zhang, Lina; Xu, Yong; Zhao, Mingwen; Peng, Lianmao; Li, Qunqing; Duan, Wenhui; Liu, Zhongfan; Fan, Shoushan; Jiang, Kaili

2017-09-01

Two-dimensional (2D) materials have attracted interest because of their excellent properties and potential applications. A key step in realizing industrial applications is to synthesize wafer-scale single-crystal samples. Until now, single-crystal samples, such as graphene domains up to the centimeter scale, have been synthesized. However, a new challenge is to efficiently characterize large-area samples. Currently, the crystalline characterization of these samples still relies on selected-area electron diffraction (SAED) or low-energy electron diffraction (LEED), which is more suitable for characterizing very small local regions. This paper presents a highly efficient characterization technique that adopts a low-energy electrostatically focused electron gun and a super-aligned carbon nanotube (SACNT) film sample support. It allows rapid crystalline characterization of large-area graphene through a single photograph of a transmission-diffracted image at a large beam size. Additionally, the low-energy electron beam enables the observation of a unique diffraction pattern of adsorbates on the suspended graphene at room temperature. This work presents a simple and convenient method for characterizing the macroscopic structures of 2D materials, and the instrument we constructed allows the study of the weak interaction with 2D materials.

Protein structure determination by electron diffraction using a single three-dimensional nanocrystal.

PubMed

Clabbers, M T B; van Genderen, E; Wan, W; Wiegers, E L; Gruene, T; Abrahams, J P

2017-09-01

Three-dimensional nanometre-sized crystals of macromolecules currently resist structure elucidation by single-crystal X-ray crystallography. Here, a single nanocrystal with a diffracting volume of only 0.14 µm 3 , i.e. no more than 6 × 10 5 unit cells, provided sufficient information to determine the structure of a rare dimeric polymorph of hen egg-white lysozyme by electron crystallography. This is at least an order of magnitude smaller than was previously possible. The molecular-replacement solution, based on a monomeric polyalanine model, provided sufficient phasing power to show side-chain density, and automated model building was used to reconstruct the side chains. Diffraction data were acquired using the rotation method with parallel beam diffraction on a Titan Krios transmission electron microscope equipped with a novel in-house-designed 1024 × 1024 pixel Timepix hybrid pixel detector for low-dose diffraction data collection. Favourable detector characteristics include the ability to accurately discriminate single high-energy electrons from X-rays and count them, fast readout to finely sample reciprocal space and a high dynamic range. This work, together with other recent milestones, suggests that electron crystallography can provide an attractive alternative in determining biological structures.

Protein structure determination by electron diffraction using a single three-dimensional nanocrystal

PubMed Central

Clabbers, M. T. B.; van Genderen, E.; Wiegers, E. L.; Gruene, T.; Abrahams, J. P.

2017-01-01

Three-dimensional nanometre-sized crystals of macromolecules currently resist structure elucidation by single-crystal X-ray crystallography. Here, a single nanocrystal with a diffracting volume of only 0.14 µm3, i.e. no more than 6 × 105 unit cells, provided sufficient information to determine the structure of a rare dimeric polymorph of hen egg-white lysozyme by electron crystallography. This is at least an order of magnitude smaller than was previously possible. The molecular-replacement solution, based on a monomeric polyalanine model, provided sufficient phasing power to show side-chain density, and automated model building was used to reconstruct the side chains. Diffraction data were acquired using the rotation method with parallel beam diffraction on a Titan Krios transmission electron microscope equipped with a novel in-house-designed 1024 × 1024 pixel Timepix hybrid pixel detector for low-dose diffraction data collection. Favourable detector characteristics include the ability to accurately discriminate single high-energy electrons from X-rays and count them, fast readout to finely sample reciprocal space and a high dynamic range. This work, together with other recent milestones, suggests that electron crystallography can provide an attractive alternative in determining biological structures. PMID:28876237

Understanding the growth of micro and nano-crystalline AlN by thermal plasma process

NASA Astrophysics Data System (ADS)

Kanhe, Nilesh S.; Nawale, Ashok B.; Gawade, Rupesh L.; Puranik, Vedavati G.; Bhoraskar, Sudha V.; Das, Asoka K.; Mathe, Vikas L.

2012-01-01

We report the studies related to the growth of crystalline AlN in a DC thermal plasma reactor, operated by a transferred arc plasma torch. The reactor is capable of producing the nanoparticles of Al and AlN depending on the composition of the reacting gas. Al and AlN micro crystals are formed at the anode placed on the graphite and nano crystalline Al and AlN gets deposited on the inner surface of the plasma reactor. X-ray diffraction, Raman spectroscopy analysis, single crystal X-ray diffraction and TGA-DTA techniques are used to infer the purity of post process crystals as a hexagonal AlN. The average particle size using SEM was found to be around 30 μm. The morphology of nanoparticles of Al and AlN, nucleated by gas phase condensation in a homogeneous medium were studied by transmission electron microscopy analysis. The particle ranged in size between 15 and 80 nm in diameter. The possible growth mechanism of crystalline AlN at the anode has been explained on the basis of non-equilibrium processes in the core of the plasma and steep temperature gradient near its periphery. The gas phase species of AlN and various constituent were computed using Murphy code based on minimization of free energy. The process provides 50% yield of microcrystalline AlN and remaining of Al at anode and that of nanocrystalline h-AlN and c-Al collected from the walls of the chamber is about 33% and 67%, respectively.

Structural, compositional, optical and colorimetric characterization of TiN-nanoparticles

NASA Astrophysics Data System (ADS)

Reinholdt, A.; Pecenka, R.; Pinchuk, A.; Runte, S.; Stepanov, A. L.; Weirich, Th. E.; Kreibig, U.

2004-10-01

We present results of an investigation of TiN nanoparticles, which were produced by laser ablation/evaporation and adiabatic expansion with the nanoparticle beam apparatus LUCAS. Compositional and structural characterization, using secondary ion mass spectrometry (SIMS), electron energy loss spectroscopy (EELS), X-ray diffraction (XRD) and selected area electron diffraction (SAED), revealed that crystalline and almost stoichiometric particles were formed and that they are susceptible to oxidation. Furthermore, transmission electron microscopy (TEM) analysis showed that TiN nanoparticles exhibit cuboid shapes. The size distributions were obtained using the edge length as parameter. They are fairly broad and the mean particle diameter depends on the seeding gas flow (the pressure) that is applied to the ablation chamber during production. In situ optical transmission spectra of the TiN nanoparticles deposited on a quartz substrate indicate a pronounced single Mie resonance at around 1.7 eV and an absorption flank starting at approximately 3.0 eV. The experimental optical extinction spectra of different samples were fitted using Mie theory calculations. The dielectric function of bulk TiN was modified to account for size and interface damping of the Mie resonance. Due to the distinct absorption band, TiN may be used as a color pigment. The dependence of the color stimulus on the extinction cross-section as well as on the product of the particle concentration and the sample thickness were examined. Chromaticity coordinates were derived according to the CIE 1976 (L^*a^*b^*) color space from the in situ optical transmission spectra.

Structural, Optical and Ethanol Sensing Properties of Dy-Doped SnO2 Nanoparticles

NASA Astrophysics Data System (ADS)

Shaikh, F. I.; Chikhale, L. P.; Nadargi, D. Y.; Mulla, I. S.; Suryavanshi, S. S.

2018-04-01

We report a facile co-precipitation synthesis of dysprosium (Dy3+) doped tin oxide (SnO2) thick films and their use as gas sensors. The doping percentage (Dy3+) was varied from 1 mol.% to 4 mol.% with the step of 1 mol.%. As-produced material with varying doping levels were sintered in air; and by using a screen printing technique, their thick films were developed. Prior to sensing performance investigations, the films were examined for structural, morphological and compositional properties using x-ray diffraction, a field emission scanning electron microscope, a transmission electron microscope, selected area electron diffraction, energy dispersive analysis by x-rays, Fourier transform infrared spectroscopy and Raman spectroscopic techniques. The structural analyses revealed formation of single phase nanocrystalline material with tetragonal rutile structure of SnO2. The morphological analyses confirmed the nanocrystalline porous morphology of as-developed material. Elemental analysis defined the composition of material in accordance with the doping concentration. The produced sensor material exhibited good response towards different reducing gases (acetone, ethanol, LPG, and ammonia) at different operating temperatures. The present study confirms that the Dy3+ doping in SnO2 enhances the response towards ethanol with reduction in operating temperature. Particularly, 3 mol.% Dy3+ doped sensor exhibited the highest response (˜ 92%) at an operating temperature of 300°C with better selectivity, fast response (˜ 13 s) and recovery (˜ 22 s) towards ethanol.

Filming nuclear dynamics of iodine using x-ray diffraction at the LCLS

NASA Astrophysics Data System (ADS)

Ware, Matthew; Natan, Adi; Glownia, James; Cryan, James; Bucksbaum, Phil

2017-04-01

We will provide an overview of our analysis of the nuclear dynamics of iodine. At the LCLS, we pumped a gas cell of iodine with a weak 520nm, 50 fs pulse, and the nuclear dynamics are then probed with 9 keV, 40 fs x-rays with variable time delay. This allows us to simultaneously image nuclear wavepackets on the dissociating A state, on the bound B state, and even Raman wavepackets in the ground electronic state. We will explain at length how we isolate each of these signals using a Legendre decomposition of our x-ray data and the selection rules for each of the transitions. Likewise, we will discuss how we convert the x-ray diffraction patterns into real-space movies of the nuclear dynamics. Research supported by the U.S. Department of Energy, Office of Basic Energy Sciences, Atomic, Molecular, and Optical Science Program. Use of LCLS supported under DOE Contract No. DE-AC02-76F00515.

Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments

NASA Astrophysics Data System (ADS)

Schlicker, Lukas; Doran, Andrew; Schneppmüller, Peter; Gili, Albert; Czasny, Mathias; Penner, Simon; Gurlo, Aleksander

2018-03-01

This work describes a device for time-resolved synchrotron-based in situ and operando X-ray powder diffraction measurements at elevated temperatures under controllable gaseous environments. The respective gaseous sample environment is realized via a gas-tight capillary-in-capillary design, where the gas flow is achieved through an open-end 0.5 mm capillary located inside a 0.7 mm capillary filled with a sample powder. Thermal mass flow controllers provide appropriate gas flows and computer-controlled on-the-fly gas mixing capabilities. The capillary system is centered inside an infrared heated, proportional integral differential-controlled capillary furnace allowing access to temperatures up to 1000 °C.

Ammonia gas sensors based on In2O3/PANI hetero-nanofibers operating at room temperature

PubMed Central

Nie, Qingxin; Pang, Zengyuan; Lu, Hangyi; Cai, Yibing

2016-01-01

Summary Indium nitrate/polyvinyl pyrrolidone (In(NO3)3/PVP) composite nanofibers were synthesized via electrospinning, and then hollow structure indium oxide (In2O3) nanofibers were obtained through calcination with PVP as template material. In situ polymerization was used to prepare indium oxide/polyaniline (In2O3/PANI) composite nanofibers with different mass ratios of In2O3 to aniline. The structure and morphology of In(NO3)3/PVP, In2O3/PANI composite nanofibers and pure PANI were investigated by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM) and current–voltage (I–V) measurements. The gas sensing properties of these materials towards NH3 vapor (100 to 1000 ppm) were measured at room temperature. The results revealed that the gas sensing abilities of In2O3/PANI composite nanofibers were better than pure PANI. In addition, the mass ratio of In2O3 to aniline and the p–n heterostructure between In2O3 and PANI influences the sensing performance of the In2O3/PANI composite nanofibers. In this paper, In2O3/PANI composite nanofibers with a mass ratio of 1:2 exhibited the highest response values, excellent selectivity, good repeatability and reversibility. PMID:27826505

Water-Gas Shift and Methane Reactivity on Reducible Perovskite-Type Oxides

PubMed Central

2015-01-01

Comparative (electro)catalytic, structural, and spectroscopic studies in hydrogen electro-oxidation, the (inverse) water-gas shift reaction, and methane conversion on two representative mixed ionic–electronic conducting perovskite-type materials La0.6Sr0.4FeO3−δ (LSF) and SrTi0.7Fe0.3O3−δ (STF) were performed with the aim of eventually correlating (electro)catalytic activity and associated structural changes and to highlight intrinsic reactivity characteristics as a function of the reduction state. Starting from a strongly prereduced (vacancy-rich) initial state, only (inverse) water-gas shift activity has been observed on both materials beyond ca. 450 °C but no catalytic methane reforming or methane decomposition reactivity up to 600 °C. In contrast, when starting from the fully oxidized state, total methane oxidation to CO2 was observed on both materials. The catalytic performance of both perovskite-type oxides is thus strongly dependent on the degree/depth of reduction, on the associated reactivity of the remaining lattice oxygen, and on the reduction-induced oxygen vacancies. The latter are clearly more reactive toward water on LSF, and this higher reactivity is linked to the superior electrocatalytic performance of LSF in hydrogen oxidation. Combined electron microscopy, X-ray diffraction, and Raman measurements in turn also revealed altered surface and bulk structures and reactivities. PMID:26045733

Single-electron pulses for ultrafast diffraction

PubMed Central

Aidelsburger, M.; Kirchner, F. O.; Krausz, F.; Baum, P.

2010-01-01

Visualization of atomic-scale structural motion by ultrafast electron diffraction and microscopy requires electron packets of shortest duration and highest coherence. We report on the generation and application of single-electron pulses for this purpose. Photoelectric emission from metal surfaces is studied with tunable ultraviolet pulses in the femtosecond regime. The bandwidth, efficiency, coherence, and electron pulse duration are investigated in dependence on excitation wavelength, intensity, and laser bandwidth. At photon energies close to the cathode’s work function, the electron pulse duration shortens significantly and approaches a threshold that is determined by interplay of the optical pulse width and the acceleration field. An optimized choice of laser wavelength and bandwidth results in sub-100-fs electron pulses. We demonstrate single-electron diffraction from polycrystalline diamond films and reveal the favorable influences of matched photon energies on the coherence volume of single-electron wave packets. We discuss the consequences of our findings for the physics of the photoelectric effect and for applications of single-electron pulses in ultrafast 4D imaging of structural dynamics. PMID:21041681

Mach 1 oxidation of thoriated nickel chromium at 1204 C (2200 F)

NASA Technical Reports Server (NTRS)

Lowell, C. E.; Sanders, W. A.

1971-01-01

TD NiCr was exposed to a Mach 1, 1-atmosphere gas stream at 1204 C for times up to 50 hours. Weight change, metal thickness loss, X-ray diffraction, metallographic, and electron microprobe analyses were made. Neither surface preparation nor thermal cycling had an appreciable effect on the results. Initially, Cr2O3 formed and volatilized, allowing a rapid metal loss rate of 40 microns per hour. After about 1 hour the Cr2O3 broke down, resulting in an NiO overgrowth. The metal loss rate then slowed to 2.5 microns per hour and remained constant to 50 hours.

In situ X-ray ptychography imaging of high-temperature CO2 acceptor particle agglomerates

NASA Astrophysics Data System (ADS)

Høydalsvik, Kristin; Bø Fløystad, Jostein; Zhao, Tiejun; Esmaeili, Morteza; Diaz, Ana; Andreasen, Jens W.; Mathiesen, Ragnvald H.; Rønning, Magnus; Breiby, Dag W.

2014-06-01

Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO2 capture material, was studied at a pressure of one atmosphere in air and in CO2, at temperatures exceeding 600 °C. Images with a spatial resolution better than 200 nm were retrieved, and possibilities for improving the experiment are described.

Terahertz control of nanotip photoemission

NASA Astrophysics Data System (ADS)

Wimmer, L.; Herink, G.; Solli, D. R.; Yalunin, S. V.; Echternkamp, K. E.; Ropers, C.

2014-06-01

The active control of matter by strong electromagnetic fields is of growing importance, with applications all across the optical spectrum from the extreme-ultraviolet to the far-infrared. In recent years, phase-stable terahertz fields have shown tremendous potential for observing and manipulating elementary excitations in solids. In the gas phase, on the other hand, driving free charges with terahertz transients provides insight into ultrafast ionization dynamics. Developing such approaches for locally enhanced terahertz fields in nanostructures will create new means to govern electron currents on the nanoscale. Here, we use single-cycle terahertz transients to demonstrate extensive control over nanotip photoelectron emission. The terahertz near-field is shown to either enhance or suppress photocurrents, with the tip acting as an ultrafast rectifying diode. We record phase-resolved sub-cycle dynamics and find spectral compression and expansion arising from electron propagation within the terahertz near-field. These interactions produce rich spectro-temporal features and offer unprecedented control over ultrashort free electron pulses for imaging and diffraction.

Nanostructure ZnFe2O4 with Bacillus subtilis for Detection of LPG at Low Temperature

NASA Astrophysics Data System (ADS)

Goutham, Solleti; Kumar, Devarai Santhosh; Sadasivuni, Kishor Kumar; Cabibihan, John-John; Rao, Kalagadda Venkateswara

2017-04-01

The present study deals with the development of a chemical sensor for the detection of liquefied petroleum gas (LPG) at a low operating temperature using Zinc ferrite (ZnFe2O4)/ Bacillus subtilis ( B. subtilis) hybrid nanostructures. The nanostructure ZnFe2O4 and B. subtilis powder, taken in equal proportion was made into films using the spin coating technique. X-ray diffraction, thermal analysis, scanning electron microscopy, and transmission electron microscopy were used to study morphology, structure and crystallite size. The sensing properties of the hybrid structure were studied and excellent response was observed in the temperature range of 50-55°C for 400 ppm LPG, when compared to the individual components of the hybrid. The signal output of the proposed sensor were extremely stable for more than 30 days. This method proposes the usage of the biomolecule/metal oxide composites in electronics and helps to reduce the metal oxide usage.

Momentum microscopy of ? single crystals with detailed surface characterisation

NASA Astrophysics Data System (ADS)

Ellguth, M.; Tusche, C.; Iga, F.; Suga, S.

2016-11-01

We report the in situ preparation of surfaces of the proposed topological Kondo insulator SmB? by controlled cycles of Ar ion sputtering and annealing. The procedure provides a reproducible way for the preparation of Sm- or B-rich surface terminations by low (?1080 ?C) or high (?1200 ?C) temperature annealing. The surface quality and termination were checked by low energy electron diffraction and Auger electron spectroscopy. Photoemission studies were carried out using momentum microscopy and two laboratory light sources providing polarised radiation with an energy of 6 eV (fourth harmonic of a pulsed Ti:Sapphire laser) and unpolarised radiation with an energy of 21.2 eV (He-I line of a gas discharge lamp). Full dispersions of electronic states in a wide two-dimensional momentum space were obtained by momentum microscopy from the in situ prepared Sm-terminated surface. The shape of the Fermi surface is discussed based on the sections through the bulk Brillouin zone sampled by the different photon energies.

Publications - GMC 58 | Alaska Division of Geological & Geophysical Surveys

Science.gov Websites

DGGS GMC 58 Publication Details Title: X-ray diffraction and scanning electron microscopy mineral , Michael, and Core Laboratories, 1985, X-ray diffraction and scanning electron microscopy mineral analyses

Non-spectroscopic composition measurements of SrTiO 3-La 0.7Sr 0.3MnO 3 multilayers using scanning convergent beam electron diffraction

DOE PAGES

Ophus, Colin; Ercius, Peter; Huijben, Mark; ...

2017-02-08

The local atomic structure of a crystalline sample aligned along a zone axis can be probed with a focused electron probe, which produces a convergent beam electron diffraction pattern. The introduction of high speed direct electron detectors has allowed for experiments that can record a full diffraction pattern image at thousands of probe positions on a sample. By incoherently summing these patterns over crystalline unit cells, we demonstrate in this paper that in addition to crystal structure and thickness, we can also estimate the local composition of a perovskite superlattice sample. This is achieved by matching the summed patterns tomore » a library of simulated diffraction patterns. Finally, this technique allows for atomic-scale chemical measurements without requiring a spectrometer or hardware aberration correction.« less

The study of structural properties of carbon nanotubes decorated with NiFe₂O₄ nanoparticles and application of nano-composite thin film as H₂S gas sensor.

PubMed

Hajihashemi, R; Rashidi, Ali M; Alaie, M; Mohammadzadeh, R; Izadi, N

2014-11-01

Nano-composite of multiwall carbon nanotube, decorated with NiFe2O4 nanoparticles (NiFe2O4-MWCNT), was synthesized using the sol-gel method. NiFe2O4-MWCNTs were characterized using different methods such as X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and vibrating sample magnetometer (VSM). The average size of the crystallites is 23.93 nm. The values of the saturation magnetization (MS), coercivity (HC) and retentivity (MR) of NiFe2O4-MWCNTs are obtained as 15 emu g(-1), 21Oe and 5 emu g(-1), respectively. In this research, NiFe2O4-MWCNT thin films were prepared with the spin-coating method. These thin films were used as the H2S gas sensor. The results suggest the possibility of the utilization of NiFe2O4-MWCNT nano-composite, as the H2S detector. The sensor shows appropriate response towards 100 ppm of H2S at 300°C. Copyright © 2014 Elsevier B.V. All rights reserved.

Study on simultaneous recycling of EAF dust and plastic waste containing TBBPA.

PubMed

Grabda, Mariusz; Oleszek, Sylwia; Shibata, Etsuro; Nakamura, Takashi

2014-08-15

In the present work we investigated the fates of zinc, lead, and iron present in electric arc furnace dust during thermal treatment of the dust with tetrabromobisphenol A (TBBPA) and tetrabromobisphenol A diglycidyl ether (TBBPADGE). Mixtures of these materials were compressed into pellets and heated in a laboratory-scale furnace at 550 °C for 80 min, under oxidizing and inert conditions. The solid, condensed, and gaseous-phase products were characterized using an array of analytical methods: scanning electron microscopy, X-ray diffraction, electron probe microscopy, inductively coupled plasma, ion chromatography, and gas chromatography. The results indicated that heating the mixtures under specific conditions enabled high separation of zinc and lead from iron-rich residues, by a bromination-evaporation process. In the case of TBBPADGE, a maximum of 85% of zinc and 81% of lead were effectively separated under the above conditions. The process is based on the reaction between the highly reactive HBr gas evolved during thermal degradation of the flame-retarded materials with zinc (ZnO and ZnFe2O4) and lead in the dust, followed by complete evaporation of the formed metallic bromides from the solid residue. Copyright © 2014 Elsevier B.V. All rights reserved.

Qualitative and quantitative differentiation of gases using ZnO thin film gas sensors and pattern recognition analysis.

PubMed

Pati, Sumati; Maity, A; Banerji, P; Majumder, S B

2014-04-07

In the present work we have grown highly textured, ultra-thin, nano-crystalline zinc oxide thin films using a metal organic chemical vapor deposition technique and addressed their selectivity towards hydrogen, carbon dioxide and methane gas sensing. Structural and microstructural characteristics of the synthesized films were investigated utilizing X-ray diffraction and electron microscopy techniques respectively. Using a dynamic flow gas sensing measurement set up, the sensing characteristics of these films were investigated as a function of gas concentration (10-1660 ppm) and operating temperature (250-380 °C). ZnO thin film sensing elements were found to be sensitive to all of these gases. Thus at a sensor operating temperature of ~300 °C, the response% of the ZnO thin films were ~68, 59, and 52% for hydrogen, carbon monoxide and methane gases respectively. The data matrices extracted from first Fourier transform analyses (FFT) of the conductance transients were used as input parameters in a linear unsupervised principal component analysis (PCA) pattern recognition technique. We have demonstrated that FFT combined with PCA is an excellent tool for the differentiation of these reducing gases.

Nitrogen Dioxide-Sensing Properties at Room Temperature of Metal Oxide-Modified Graphene Composite via One-Step Hydrothermal Method

NASA Astrophysics Data System (ADS)

Zhang, Dongzhi; Liu, Jingjing; Xia, Bokai

2016-08-01

A metal oxide/graphene composite film-based sensor toward room-temperature detection of ppm-level nitrogen dioxide (NO2) gas has been demonstrated. The sensor prototype was constructed on a PCB substrate with microelectrodes, and a tin oxide-reduced graphene oxide (SnO2-rGO) composite as sensing film was prepared by one-step hydrothermal synthesis of tin tetrachloride pentahydrate solution in the presence of graphene oxide (GO). The SnO2-rGO hybrid composite was examined by scanning electron microscope and x-ray diffraction (XRD). The gas sensing properties of the SnO2-rGO composite were investigated at room temperature by exposing it to a wide concentration ranging from 1 ppm to 2000 ppm toward NO2 gas. The experiment results showed that the sensor exhibited a high response, superior selectivity, good repeatability, rapid response/recovery characteristics and low detection limit of 1 ppm, which exceeded that of a pure rGO sensor. The gas sensing mechanisms of the proposed sensor toward NO2 were possibly attributed to the nano-hybrid structures and n- p heterojunctions created at the interface of the SnO2 nanocrystals and rGO nanosheets.

A novel crack healing in steels by gas nitrocarburizing

NASA Astrophysics Data System (ADS)

Li, Ai; Chen, Xing; Zhang, Chengsong; Cui, Guodong; Zhao, Hui; Yang, Chuan

2018-06-01

In this paper, the gas nitrocarburizing technique was applied for the first time to solve the challenge in crack healing of metallic materials. The crack-healing behavior of 42CrMo steel was investigated. The gas nitrocarburizing was carried out in two steps with the decrease of the healing temperature. The mechanical properties after healing were measured using the three-point blending test. X-ray diffraction, optical microscope and scanning electron microscopy were applied to characterize the phase composition and microstructure of crack healing area and analyze healing mechanisms involved. The results show that the optimal healing effect could be obtained when it is healed at 760 °C for 2 h and then at 550 °C for 4 h. The maximum healing degree reached to 63.68%. The crack healing process could be divided into two stages, i.e. healing in crack tips at high temperatures and then in crack openings at low temperatures. The volumetric expansion and filling of formed nitrides contributed to the rapid healing of the large-sized cracks. The healing efficiency could be improved by decreasing the healing temperature. Moreover, high pressure gas nitrocarburizing was considered as another potential way to improve the healing efficiency and healing degree.

Comparative Study of Two Different TiO2 Film Sensors on Response to H2 under UV Light and Room Temperature

PubMed Central

Peng, Xiaoying; Wang, Zhongming; Huang, Pan; Chen, Xun; Fu, Xianzhi; Dai, Wenxin

2016-01-01

An anatase TiO2 film sensor was prepared by a facile in-situ method on the interdigitated Au electrode deposited on the alumina substrate. The structure, morphology and the optical properties of the in-situ TiO2 film sensor were characterized by X-ray diffraction, Scanning Electron Microscopy, and UV-vis diffuse reflectance spectra. The photo-assisted gas sensitivities of the prepared film towards H2 gas were evaluated at room temperature in N2 and synthetic air atmospheres. As compared to TiO2 film sensor prepared by drop-coating method, this in-situ TiO2 film sensor exhibited a more compact structure composed of uniform TiO2 microspheres as well as a better gas sensitivity towards H2 under UV irradiation, especially in synthetic air. The photo-electrochemical measurements suggest that these improvements may be associated with the efficient charge transfer in the TiO2 interface induced by the TiO2 microsphere structure. This study might offer a feasible approach to develop photo-assisted gas sensors at ambient temperature. PMID:27509502

Spheroidization of silica powders by radio frequency inductively coupled plasma with Ar-H2 and Ar-N2 as the sheath gases at atmospheric pressure

NASA Astrophysics Data System (ADS)

Li, Lin; Ni, Guo-hua; Guo, Qi-jia; Lin, Qi-fu; Zhao, Peng; Cheng, Jun-li

2017-09-01

Amorphous spherical silica powders were prepared by inductively coupled thermal plasma treatment at a radio frequency of 36.2 MHz. The effects of the added content of hydrogen and nitrogen into argon (serving as the sheath gas), as well as the carrier gas flow rate, on the spheroidization rate of silica powders, were investigated. The prepared silica powders before and after plasma treatment were examined by scanning electron microscopy, X-ray diffraction, and laser granulometric analysis. Results indicated that the average size of the silica particles increased, and the transformation of crystals into the amorphous state occurred after plasma treatment. Discharge image processing was employed to analyze the effect of the plasma temperature field on the spheroidization rate. The spheroidization rate of the silica powder increased with the increase of the hydrogen content in the sheath gas. On the other hand, the spheroidization rate of the silica power first increased and then decreased with the increase of the nitrogen content in the sheath gas. Moreover, the amorphous content increased with the increase of the spheroidization rate of the silica powder.

Gadolinia doped hafnia (Gd2O3- HfO 2) thermal barrier coatings for gas turbine applications

NASA Astrophysics Data System (ADS)

Gullapalli, Satya Kiran

Thermal efficiency of the gas turbines is influenced by the operating temperature of the hot gas path components. The material used for the hot gas path components can only withstand temperature up to a certain limit. Thermal barrier coatings (TBC) provide the additional thermal protection for these components and help the gas turbine achieve higher firing temperatures. Traditionally available yttria stabilized zirconia (YSZ) TBCs have a limitation up to 1200 C due to their phase transformation. The present work focuses on gadolinia based hafnia (GSH) TBCs to study their potential to replace the YSZ coatings. Different compositions of gadolinia doped hafnia coatings have been deposited using electron beam physical vapor deposition (EB-PVD) technique and characterized using x-ray diffraction (XRD) and scanning electron microscope (SEM). The crystal structure analysis performed using XRD confirmed the stabilization of the high temperature cubic phase of hafnia. Cross sectional analysis confirmed the presence of columnar structure in the coatings which is a signature of the EB-PVD coatings. Mechanical properties of the coatings were investigated using nanoindentation and nano impact testing at both room temperature and high temperature. Indentation tests indicate a reduction in hardness with an increase in temperature and gadolinia content in hafnia. Impact testing reveals the fracture resistance of the coatings as a function of stabilizer content and heat treatment. Thermal measurements and impedance testing was performed on the bulk material to study the effect of gadolinia content. Thermal cycling was performed to study the spallation behavior of the as deposited and aged samples. Finite element models were developed to study the interfacial stress development in the coatings subjected to thermal cycling.

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector

PubMed Central

van Genderen, E.; Clabbers, M. T. B.; Das, P. P.; Stewart, A.; Nederlof, I.; Barentsen, K. C.; Portillo, Q.; Pannu, N. S.; Nicolopoulos, S.; Gruene, T.; Abrahams, J. P.

2016-01-01

Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼0.013 e− Å−2 s−1) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014). PMID:26919375

Structure resolution by electron diffraction tomography of the complex layered iron-rich Fe-2234-type Sr{sub 5}Fe{sub 6}O{sub 15.4}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lepoittevin, Christophe, E-mail: christophe.lepoittevin@neel.cnrs.fr

2016-10-15

The crystal structure of the strontium ferrite Sr{sub 5}Fe{sub 6}O{sub 15.4}, was solved by direct methods on electron diffraction tomography data acquired on a transmission electron microscope. The refined cell parameters are a=27.4047(3) Å, b=5.48590(7) Å and c=42.7442(4) Å in Fm2m symmetry. Its structure is built up from the intergrowth sequence between a quadruple perovskite-type layer with a complex rock-salt (RS)-type block. In the latter iron atoms are found in two different environments : tetragonal pyramid and tetrahedron. The structural model was refined by Rietveld method based on the powder X-ray diffraction pattern. - Highlights: • Complex structure of Sr{submore » 5}Fe{sub 6}O{sub 15.4} solved by electron diffraction tomography. • Observed Fourier maps allow determining missing oxygen atoms in the structure. • Structural model refined from powder X-ray diffraction data. • Intergrowth between quadruple perovskite layer with double rock-salt-type layer.« less

Electron and lattice dynamics of transition metal thin films observed by ultrafast electron diffraction and transient optical measurements.

PubMed

Nakamura, A; Shimojima, T; Nakano, M; Iwasa, Y; Ishizaka, K

2016-11-01

We report the ultrafast dynamics of electrons and lattice in transition metal thin films (Au, Cu, and Mo) investigated by a combination of ultrafast electron diffraction (UED) and pump-probe optical methods. For a single-crystalline Au thin film, we observe the suppression of the diffraction intensity occuring in 10 ps, which direcly reflects the lattice thermalization via the electron-phonon interaction. By using the two-temperature model, the electron-phonon coupling constant ( g ) and the electron and lattice temperatures ( T e , T l ) are evaluated from UED, with which we simulate the transient optical transmittance. The simulation well agrees with the experimentally obtained transmittance data, except for the slight deviations at the initial photoexcitation and the relaxed quasi-equilibrium state. We also present the results similarly obtained for polycrystalline Au, Cu, and Mo thin films and demonstrate the electron and lattice dynamics occurring in metals with different electron-phonon coupling strengths.

The chemical and oxidation characteristics of semi-dry flue gas desulfurization ash from a steel factory.

PubMed

Liu, Ren-ping; Guo, Bin; Ren, Ailing; Bian, Jing-feng

2010-10-01

Some samples of semi-dry flue gas desulfurization (FGD) ash were taken from sinter gas of a steel factory. Scanning electron microscope (SEM) and X-ray diffraction (XRD) analyses were employed to identify the samples in order to investigate their physical and chemical characteristics. The results show that semi-dry FGD ash from a steel factory is stable under atmospheric conditions. It has irregular shape, a smooth surface and loose construction. The size of FGD ash particles is around 0.5-25 µm, the average size is about 5 µm and the median diameter is 4.18 µm. Semi-dry FGD ash from a steel factory consists of CaSO₃, CaSO₄, CaCO₃, some amorphous vitreous material and unburned carbon. An experimental method was found to study the oxidation characteristics of ash. A prediction model of the oxidation efficiency was obtained based on response surface methodology. The results show that not only the temperature, but also gas:solid ratio, play an important role in influencing the oxidation efficiency. The interactions of the gas:solid ratio with temperature play an essential role. An improved response surface model was obtained which can be helpful to describe the degree of oxidation efficiency of semi-dry FGD ash.

Synthesis and Transport Properties of Novel MOF/PIM-1/MOF Sandwich Membranes for Gas Separation

PubMed Central

Fuoco, Alessio; Khdhayyer, Muhanned R.; Attfield, Martin P.; Esposito, Elisa; Jansen, Johannes C.; Budd, Peter M.

2017-01-01

Metal-organic frameworks (MOFs) were supported on polymer membrane substrates for the fabrication of composite polymer membranes based on unmodified and modified polymer of intrinsic microporosity (PIM-1). Layers of two different MOFs, zeolitic imidazolate framework-8 (ZIF-8) and Copper benzene tricarboxylate ((HKUST-1), were grown onto neat PIM-1, amide surface-modified PIM-1 and hexamethylenediamine (HMDA) -modified PIM-1. The surface-grown crystalline MOFs were characterized by a combination of several techniques, including powder X-ray diffraction, infrared spectroscopy and scanning electron microscopy to investigate the film morphology on the neat and modified PIM-1 membranes. The pure gas permeabilities of He, H2, O2, N2, CH4, CO2 were studied to understand the effect of the surface modification on the basic transport properties and evaluate the potential use of these membranes for industrially relevant gas separations. The pure gas transport was discussed in terms of permeability and selectivity, highlighting the effect of the MOF growth on the diffusion coefficients of the gas in the new composite polymer membranes. The results confirm that the growth of MOFs on polymer membranes can enhance the selectivity of the appropriately functionalized PIM-1, without a dramatic decrease of the permeability. PMID:28208658

Development and in-vivo assessment of the bioavailability of oridonin solid dispersions by the gas anti-solvent technique.

PubMed

Li, Songming; Liu, Ying; Liu, Tao; Zhao, Ling; Zhao, Jihui; Feng, Nianping

2011-06-15

We developed solid dispersions, using the gas anti-solvent technique (GAS), to improve the oral bioavailability of the poorly water-soluble active component oridonin. The solubility of oridonin in supercritical carbon dioxide was measured under various pressures and temperatures. To prepare oridonin solid dispersions using the GAS technique, ethanol was used as the solvent, CO(2) was used as the anti-solvent and the hydrophilic polymer polyvinylpyrrolidone K17 (PVP K17) was used as the drug carrier matrix. Characterization of the obtained preparations was undertaken using scanning electron microscopy (SEM), X-ray diffraction (XRD) analyses and a drug release study. Oridonin solid dispersions were formed and oridonin was present in an amorphous form in these dispersions. Oridonin solid dispersions significantly increased the drug dissolution rate compared with that of oridonin powder, primarily through drug amorphization. Compared with the physical mixture of oridonin and PVP K17, oridonin solid dispersions gave higher values of AUC and C(max), and the absorption of oridonin from solid dispersions resulted in 26.4-fold improvement in bioavailability. The present study illustrated the feasibility of applying the GAS technique to prepare oridonin solid dispersions, and of using them for the delivery of oridonin via the oral route. Copyright © 2011 Elsevier B.V. All rights reserved.

Gas sensing behaviour of Cr{sub 2}O{sub 3} and W{sup 6+}: Cr{sub 2}O{sub 3} nanoparticles towards acetone

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kohli, Nipin, E-mail: nipinkohli82@yahoo.com; Hastir, Anita; Singh, Ravi Chand

2016-05-23

This paper reports the acetone gas sensing properties of Cr{sub 2}O{sub 3} and 2% W{sup 6+} doped Cr{sub 2}O{sub 3} nanoparticles. The simple cost-effective hydrolysis assisted co-precipitation method was adopted. Synthesized samples were characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques. XRD revealed that synthesized nanoparticles have corundum structure. The lattice parameters have been calculated by Rietveld refinement; and strain and crystallite size have been calculated by using the Williamson-Hall plots. For acetone gas sensing properties, the nanoparticles were applied as thick film onto alumina substrate and tested at different operating temperatures. The results showedmore » that the optimum operating temperature of both the gas sensors is 250°C. At optimum operating temperature, the response of Cr{sub 2}O{sub 3} and 2% W{sup 6+} doped Cr{sub 2}O{sub 3} gas sensor towards 100 ppm acetone was found to be 25.5 and 35.6 respectively. The investigations revealed that the addition of W{sup 6+} as a dopant enhanced the sensing response of Cr{sub 2}O{sub 3} nanoparticles appreciably.« less

Breaking resolution limits in ultrafast electron diffraction and microscopy

PubMed Central

Baum, Peter; Zewail, Ahmed H.

2006-01-01

Ultrafast electron microscopy and diffraction are powerful techniques for the study of the time-resolved structures of molecules, materials, and biological systems. Central to these approaches is the use of ultrafast coherent electron packets. The electron pulses typically have an energy of 30 keV for diffraction and 100–200 keV for microscopy, corresponding to speeds of 33–70% of the speed of light. Although the spatial resolution can reach the atomic scale, the temporal resolution is limited by the pulse width and by the difference in group velocities of electrons and the light used to initiate the dynamical change. In this contribution, we introduce the concept of tilted optical pulses into diffraction and imaging techniques and demonstrate the methodology experimentally. These advances allow us to reach limits of time resolution down to regimes of a few femtoseconds and, possibly, attoseconds. With tilted pulses, every part of the sample is excited at precisely the same time as when the electrons arrive at the specimen. Here, this approach is demonstrated for the most unfavorable case of ultrafast crystallography. We also present a method for measuring the duration of electron packets by autocorrelating electron pulses in free space and without streaking, and we discuss the potential of tilting the electron pulses themselves for applications in domains involving nuclear and electron motions. PMID:17056711

Structure and magnetic properties of Nd2Fe14B fine particles produced by spark erosion

NASA Astrophysics Data System (ADS)

Wan, H.; Berkowitz, A. E.

1994-11-01

At present Nd2Fe14B is the best permanent magnet because of its extremely high coercivity and energy product. Optimum properties of Nd2Fe14B magnets can be attained by producing single domain particles, and then aligning and compacting them. Due to the reactivity of the Nd constitutent, it is challenging to produce and handle a large amount of fine particles of this material. We have prepared fine particles of Nd2Fe14B by spark erosion with various dielectric media. Yield, size, size distribution, structure, and magnetic properties are discussed. The Nd2Fe14B particles were made by the sharker pot spark erosion method. Relaxation oscillators or a pulse generator were used to power the park erosion. Commercial Neomax 35 was employed as the primary material. The dielectric media were liquid Ar, Ar gas, and hydrocarbons, which provided an oxygen free environment. Structure and size were studied by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and x-ray diffraction. Magnetic properties were measured by vibrating sample magnetometer (VSM) with temperatures in range of 4.2-1200 K. The particles produced in these three different dielectric media had different microstructures and crystal structures. The particles made in Ar gas were pure Nd2Fe14B phase. The particles made in liquid Ar were a mixture of amorphous and crystalline Nd2Fe14B, because the liquid Ar provided a much higher quench rate than Ar gas, which produced some amorphous Nd2Fe14B. Upon annealing, the amorphous particles became crystalline. The fine particles produced in hydrocarbons, such as pentane and dodecane, had more complex mixed phases, since the rare earth reacted with the hydrocarbons during the sparking process. The phases were NdC2, alpha-Fe, and amorphous and crystalline Nd2Fe14B. The effects of power parameters, such as voltage and capacitance, on particle size were investigated. Particle sizes from 20 nm to 50 microns were obtained.

Disentangling atomic-layer-specific x-ray absorption spectra by Auger electron diffraction spectroscopy

NASA Astrophysics Data System (ADS)

Matsui, Fumihiko; Matsushita, Tomohiro; Kato, Yukako; Hashimoto, Mie; Daimon, Hiroshi

2009-11-01

In order to investigate the electronic and magnetic structures of each atomic layer at subsurface, we have proposed a new method, Auger electron diffraction spectroscopy, which is the combination of x-ray absorption spectroscopy (XAS) and Auger electron diffraction (AED) techniques. We have measured a series of Ni LMM AED patterns of the Ni film grown on Cu(001) surface for various thicknesses. Then we deduced a set of atomic-layer-specific AED patterns in a numerical way. Furthermore, we developed an algorithm to disentangle XANES spectra from different atomic layers using these atomic-layer-specific AED patterns. Surface and subsurface core level shift were determined for each atomic layer.

Low-energy electron point projection microscopy/diffraction study of suspended graphene

NASA Astrophysics Data System (ADS)

Hsu, Wei-Hao; Chang, Wei-Tse; Lin, Chun-Yueh; Chang, Mu-Tung; Hsieh, Chia-Tso; Wang, Chang-Ran; Lee, Wei-Li; Hwang, Ing-Shouh

2017-11-01

In this work, we present our study of suspended graphene with low-energy electrons based on a point projection microscopic/diffractive imaging technique. Both exfoliated and chemical vapor deposition (CVD) graphene samples were studied in an ultra-high vacuum chamber. This method allows imaging of individual adsorbates at the nanometer scale and characterizing graphene layers, graphene lattice orientations, ripples on graphene membranes, etc. We found that long-duration exposure to low-energy electron beams induced aggregation of adsorbates on graphene when the electron dose rate was above a certain level. We also discuss the potential of this technique to conduct coherent diffractive imaging for determining the atomic structures of biological molecules adsorbed on suspended graphene.

Feynman Path Integral Approach to Electron Diffraction for One and Two Slits: Analytical Results

ERIC Educational Resources Information Center

Beau, Mathieu

2012-01-01

In this paper we present an analytic solution of the famous problem of diffraction and interference of electrons through one and two slits (for simplicity, only the one-dimensional case is considered). In addition to exact formulae, various approximations of the electron distribution are shown which facilitate the interpretation of the results.…

Dark-field phase retrieval under the constraint of the Friedel symmetry in coherent X-ray diffraction imaging.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Nakasako, Masayoshi

2014-11-17

Coherent X-ray diffraction imaging (CXDI) is a lensless imaging technique that is suitable for visualizing the structures of non-crystalline particles with micrometer to sub-micrometer dimensions from material science and biology. One of the difficulties inherent to CXDI structural analyses is the reconstruction of electron density maps of specimen particles from diffraction patterns because saturated detector pixels and a beam stopper result in missing data in small-angle regions. To overcome this difficulty, the dark-field phase-retrieval (DFPR) method has been proposed. The DFPR method reconstructs electron density maps from diffraction data, which are modified by multiplying Gaussian masks with an observed diffraction pattern in the high-angle regions. In this paper, we incorporated Friedel centrosymmetry for diffraction patterns into the DFPR method to provide a constraint for the phase-retrieval calculation. A set of model simulations demonstrated that this constraint dramatically improved the probability of reconstructing correct electron density maps from diffraction patterns that were missing data in the small-angle region. In addition, the DFPR method with the constraint was applied successfully to experimentally obtained diffraction patterns with significant quantities of missing data. We also discuss this method's limitations with respect to the level of Poisson noise in X-ray detection.

An amino-functionalized magnetic framework composite of type Fe3O4-NH2@MIL-101(Cr) for extraction of pyrethroids coupled with GC-ECD.

PubMed

He, Xi; Yang, Wei; Li, Sijia; Liu, Yu; Hu, Baichun; Wang, Ting; Hou, Xiaohong

2018-01-24

An amino-functionalized magnetic framework composite of type Fe 3 O 4 -NH 2 @MIL-101(Cr) was synthesized using a solvothermal method. The material was characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, nitrogen adsorption, and magnetometry. The composite combines the advantages of amino-modified Fe 3 O 4 and MIL-101(Cr). The presence of amino groups facilitates the fairly specific adsorption of pyrethroids. The composite was employed as a sorbent for magnetic solid phase extraction of five pyrethroids from environmental water samples. Following desorption with acidified acetone, the pyrethroids were quantified by gas chromatography with electron capture detection. The detection limits for bifenthrin, fenpropathrin, λ-cyhalothrin, permethrin, and deltamethrin range from 5 to 9 pg·mL -1 . The method is rapid, accurate, and highly sensitive. The molecular interactions and free binding energies between MIL-101(Cr) and the five pyrethroids were calculated by means of molecular docking. Graphical abstract A novel functionalized magnetic framework composite of type Fe 3 O 4 -NH 2 @MIL-101(Cr) was synthesized. It was applied as a sorbent for magnetic solid phase extraction of pyrethroids prior to their quantitation by gas chromatography with electron capture detection. The molecular interactions of analytes and MIL-101(Cr) were studied.

Fine Structure of Diffuse Scattering Rings in Al-Li-Cu Quasicrystal: A Comparative X-ray and Electron Diffraction Study

NASA Astrophysics Data System (ADS)

Donnadieu, P.; Dénoyer, F.

1996-11-01

A comparative X-ray and electron diffraction study has been performed on Al-Li-Cu icosahedral quasicrystal in order to investigate the diffuse scattering rings revealed by a previous work. Electron diffraction confirms the existence of rings but shows that the rings have a fine structure. The diffuse aspect on the X-ray diffraction patterns is then due to an averaging effect. Recent simulations based on the model of canonical cells related to the icosahedral packing give diffractions patterns in agreement with this fine structure effect. Nous comparons les diagrammes de diffraction des rayon-X et des électrons obtenus sur les mêmes échantillons du quasicristal icosaèdrique Al-Li-Cu. Notre but est d'étudier les anneaux de diffusion diffuse mis en évidence par un travail précédent. Les diagrammes de diffraction électronique confirment la présence des anneaux mais ils montrent aussi que ces anneaux possèdent une structure fine. L'aspect diffus des anneaux révélés par la diffraction des rayons X est dû à un effet de moyenne. Des simulations récentes basées sur la décomposition en cellules canoniques de l'empilement icosaédrique produisent des diagrammes de diffraction en accord avec ces effects de structure fine.

Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes.

PubMed

Rius, Jordi; Mugnaioli, Enrico; Vallcorba, Oriol; Kolb, Ute

2013-07-01

δ Recycling is a simple procedure for directly extracting phase information from Patterson-type functions [Rius (2012). Acta Cryst. A68, 399-400]. This new phasing method has a clear theoretical basis and was developed with ideal single-crystal X-ray diffraction data. On the other hand, introduction of the automated diffraction tomography (ADT) technique has represented a significant advance in electron diffraction data collection [Kolb et al. (2007). Ultramicroscopy, 107, 507-513]. When combined with precession electron diffraction, it delivers quasi-kinematical intensity data even for complex inorganic compounds, so that single-crystal diffraction data of nanometric volumes are now available for structure determination by direct methods. To check the tolerance of δ recycling to missing data-collection corrections and to deviations from kinematical behaviour of ADT intensities, δ recycling has been applied to differently shaped nanocrystals of various inorganic materials. The results confirm that it can phase ADT data very efficiently. In some cases even more complete structure models than those derived from conventional direct methods and least-squares refinement have been found. During this study it has been demonstrated that the Wilson-plot scaling procedure is largely insensitive to sample thickness variations and missing absorption corrections affecting electron ADT intensities.

Structural and electron diffraction scaling of twisted graphene bilayers

NASA Astrophysics Data System (ADS)

Zhang, Kuan; Tadmor, Ellad B.

2018-03-01

Multiscale simulations are used to study the structural relaxation in twisted graphene bilayers and the associated electron diffraction patterns. The initial twist forms an incommensurate moiré pattern that relaxes to a commensurate microstructure comprised of a repeating pattern of alternating low-energy AB and BA domains surrounding a high-energy AA domain. The simulations show that the relaxation mechanism involves a localized rotation and shrinking of the AA domains that scales in two regimes with the imposed twist. For small twisting angles, the localized rotation tends to a constant; for large twist, the rotation scales linearly with it. This behavior is tied to the inverse scaling of the moiré pattern size with twist angle and is explained theoretically using a linear elasticity model. The results are validated experimentally through a simulated electron diffraction analysis of the relaxed structures. A complex electron diffraction pattern involving the appearance of weak satellite peaks is predicted for the small twist regime. This new diffraction pattern is explained using an analytical model in which the relaxation kinematics are described as an exponentially-decaying (Gaussian) rotation field centered on the AA domains. Both the angle-dependent scaling and diffraction patterns are in quantitative agreement with experimental observations. A Matlab program for extracting the Gaussian model parameters accompanies this paper.

Specimen preparation for cryogenic coherent X-ray diffraction imaging of biological cells and cellular organelles by using the X-ray free-electron laser at SACLA

PubMed Central

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka; Okajima, Koji; Fukuda, Asahi; Oide, Mao; Yamamoto, Masaki; Nakasako, Masayoshi

2016-01-01

Coherent X-ray diffraction imaging (CXDI) allows internal structures of biological cells and cellular organelles to be analyzed. CXDI experiments have been conducted at 66 K for frozen-hydrated biological specimens at the SPring-8 Angstrom Compact Free-Electron Laser facility (SACLA). In these cryogenic CXDI experiments using X-ray free-electron laser (XFEL) pulses, specimen particles dispersed on thin membranes of specimen disks are transferred into the vacuum chamber of a diffraction apparatus. Because focused single XFEL pulses destroy specimen particles at the atomic level, diffraction patterns are collected through raster scanning the specimen disks to provide fresh specimen particles in the irradiation area. The efficiency of diffraction data collection in cryogenic experiments depends on the quality of the prepared specimens. Here, detailed procedures for preparing frozen-hydrated biological specimens, particularly thin membranes and devices developed in our laboratory, are reported. In addition, the quality of the frozen-hydrated specimens are evaluated by analyzing the characteristics of the collected diffraction patterns. Based on the experimental results, the internal structures of the frozen-hydrated specimens and the future development for efficient diffraction data collection are discussed. PMID:27359147

Specimen preparation for cryogenic coherent X-ray diffraction imaging of biological cells and cellular organelles by using the X-ray free-electron laser at SACLA.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka; Okajima, Koji; Fukuda, Asahi; Oide, Mao; Yamamoto, Masaki; Nakasako, Masayoshi

2016-07-01

Coherent X-ray diffraction imaging (CXDI) allows internal structures of biological cells and cellular organelles to be analyzed. CXDI experiments have been conducted at 66 K for frozen-hydrated biological specimens at the SPring-8 Angstrom Compact Free-Electron Laser facility (SACLA). In these cryogenic CXDI experiments using X-ray free-electron laser (XFEL) pulses, specimen particles dispersed on thin membranes of specimen disks are transferred into the vacuum chamber of a diffraction apparatus. Because focused single XFEL pulses destroy specimen particles at the atomic level, diffraction patterns are collected through raster scanning the specimen disks to provide fresh specimen particles in the irradiation area. The efficiency of diffraction data collection in cryogenic experiments depends on the quality of the prepared specimens. Here, detailed procedures for preparing frozen-hydrated biological specimens, particularly thin membranes and devices developed in our laboratory, are reported. In addition, the quality of the frozen-hydrated specimens are evaluated by analyzing the characteristics of the collected diffraction patterns. Based on the experimental results, the internal structures of the frozen-hydrated specimens and the future development for efficient diffraction data collection are discussed.

Structural, morphological, gas sensing and photocatalytic characterization of MoO3 and WO3 thin films prepared by the thermal vacuum evaporation technique

NASA Astrophysics Data System (ADS)

Arfaoui, A.; Touihri, S.; Mhamdi, A.; Labidi, A.; Manoubi, T.

2015-12-01

Thin films of molybdenum trioxide and tungsten trioxide were deposited on glass substrates using a simplified thermal evaporation under vacuum method monitored by heat treatment in flowing oxygen at 500 °C for 1 h. The structural and morphological properties of the films were investigated using X-ray diffraction, Raman spectroscopy, atomic force microscopy and scanning electron microscopy. The X-ray diffraction analysis shows that the films of MoO3 and WO3 were well crystallized in orthorhombic and monoclinic phase respectively with the crystallites preferentially oriented toward (2 0 0) direction parallel a-axis for both samples. In literature, we have shown in previous papers that structural and surface morphology of metal thin films play an important role in the gas detection mechanism. In this article, we have studied the response evolution of MoO3 and WO3 thin films sensors ethanol versus time, working temperature and the concentration of the ethanol. It was found that these films had high sensitivity to ethanol, which made them as a good candidate for the ethanol sensor. Finally, the photocatalytic activity of the samples was evaluated with respect to the degradation reaction of a wastewater containing methylene blue (MB) under UV-visible light irradiation. The molybdenum trioxide exhibits a higher degradation rate than the tungsten trioxide thin films under similar experimental conditions.

Crystal structure, magnetic susceptibility and thermopower of superconducting and non-superconducting Nd 1.85Ce 0.15CuO 4+y

NASA Astrophysics Data System (ADS)

Magelschots, I.; Andersen, N. H.; Lebech, B.; Wisniewski, A.; Jacobsen, C. S.

1992-12-01

An experimental study of superconducting and non-superconducting Nd 1.85Ce 0.15CuO 4+ y, including structure determination by neutron powder diffraction, recording of oxygen changes by gas volumetry, and susceptibility and thermoelectric measurements, is reported. Difference neutron diffraction patterns from samples prepared on-line at the spectrometer show that the structures of superconducting and non-superconducting samples are identical within the limits set by the statistical errors of our data. Simultaneous gas volumetric measurements reveal that Δy<0.03 (1) when the sample is oxidized from the superconducting to the non-superconducting state. Structural refinements confirm that Nd 1.85Ce 0.15CuO 4+ y has the T‧-type tetragonal structure reported in the literature, but additional oxygen may be located on the apical O(3) oxygen site of the T-type structure, with a total oxygen content of 4+ y=4.03 (5). Consistent with this result, we find very small values of the thermoelectric power indicating that Nd 1.85Ce 0.15CuO 4+ y is close to the formal threshold, yc=0.075, between electron and hole conduction, but surprisingly, the thermoelectric power of the superconducting sample is positive, while it is negative in the non-superconducting sample below 210 K.

Kinetics of methane-ethane gas replacement in clathrate-hydrates studied by time-resolved neutron diffraction and Raman spectroscopy.

PubMed

Murshed, M Mangir; Schmidt, Burkhard C; Kuhs, Werner F

2010-01-14

The kinetics of CH(4)-C(2)H(6) replacement in gas hydrates has been studied by in situ neutron diffraction and Raman spectroscopy. Deuterated ethane structure type I (C(2)H(6) sI) hydrates were transformed in a closed volume into methane-ethane mixed structure type II (CH(4)-C(2)H(6) sII) hydrates at 5 MPa and various temperatures in the vicinity of 0 degrees C while followed by time-resolved neutron powder diffraction on D20 at ILL, Grenoble. The role of available surface area of the sI starting material on the formation kinetics of sII hydrates was studied. Ex situ Raman spectroscopic investigations were carried out to crosscheck the gas composition and the distribution of the gas species over the cages as a function of structure type and compared to the in situ neutron results. Raman micromapping on single hydrate grains showed compositional and structural gradients between the surface and core of the transformed hydrates. Moreover, the observed methane-ethane ratio is very far from the one expected for a formation from a constantly equilibrated gas phase. The results also prove that gas replacement in CH(4)-C(2)H(6) hydrates is a regrowth process involving the nucleation of new crystallites commencing at the surface of the parent C(2)H(6) sI hydrate with a progressively shrinking core of unreacted material. The time-resolved neutron diffraction results clearly indicate an increasing diffusion limitation of the exchange process. This diffusion limitation leads to a progressive slowing down of the exchange reaction and is likely to be responsible for the incomplete exchange of the gases.

Hydrothermal Synthesis of Various Hierarchical ZnO Nanostructures and Their Methane Sensing Properties

PubMed Central

Zhou, Qu; Chen, Weigen; Xu, Lingna; Peng, Shudi

2013-01-01

Hierarchical flower-like ZnO nanorods, net-like ZnO nanofibers and ZnO nanobulks have been successfully synthesized via a surfactant assisted hydrothemal method. The synthesized products were characterized by X-ray powder diffraction and field emission scanning electron microscopy, respectively. A possible growth mechanism of the various hierarchical ZnO nanostructures is discussed in detail. Gas sensors based on the as-prepared ZnO nanostructures were fabricated by screen-printing on a flat ceramic substrate. Furthermore, their gas sensing characteristics towards methane were systematically investigated. Methane is an important characteristic hydrocarbon contaminant found dissolved in power transformer oil as a result of faults. We find that the hierarchical flower-like ZnO nanorods and net-like ZnO nanofibers samples show higher gas response and lower operating temperature with rapid response-recovery time compared to those of sensors based on ZnO nanobulks. These results present a feasible way of exploring high performance sensing materials for on-site detection of characteristic fault gases dissolved in transformer oil. PMID:23666136

Methylcellulose-Directed Synthesis of Nanocrystalline Zeolite NaA with High CO₂ Uptake.

PubMed

Shakarova, Dilshod; Ojuva, Arto; Bergström, Lennart; Akhtar, Farid

2014-07-28

Zeolite NaA nanocrystals with a narrow particle size distribution were prepared by template-free hydrothermal synthesis in thermo-reversible methylcellulose gels. The effects of the amount of methylcellulose, crystallization time and hydrothermal treatment temperature on the crystallinity and particle size distribution of the zeolite NaA nanocrystals were investigated. We found that the thermogelation of methylcellulose in the alkaline Na₂O-SiO₂-Al₂O₃-H₂O system played an important role in controlling the particle size. The synthesized zeolite nanocrystals are highly crystalline, as demonstrated by X-ray diffraction (XRD), and scanning electron microscopy (SEM) shows that the nanocrystals can also display a well-defined facetted morphology. Gas adsorption studies on the synthesized nanocrystalline zeolite NaA showed that nanocrystals with a size of 100 nm displayed a high CO₂ uptake capacity (4.9 mmol/g at 293 K at 100 kPa) and a relatively rapid uptake rate compared to commercially available, micron-sized particles. Low-cost nanosized zeolite adsorbents with a high and rapid uptake are important for large scale gas separation processes, e.g., carbon capture from flue gas.

Removal of mercury (II), elemental mercury and arsenic from simulated flue gas by ammonium sulphide.

PubMed

Ning, Ping; Guo, Xiaolong; Wang, Xueqian; Wang, Ping; Ma, Yixing; Lan, Yi

2015-01-01

A tubular resistance furnace was used as a reactor to simulate mercury and arsenic in smelter flue gases by heating mercury and arsenic compounds. The flue gas containing Hg(2+), Hg(0) and As was treated with ammonium sulphide. The experiment was conducted to investigate the effects of varying the concentration of ammonium sulphide, the pH value of ammonium sulphide, the temperature of ammonium sulphide, the presence of SO2 and the presence of sulphite ion on removal efficiency. The prepared adsorption products were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy and scanning electron microscopy. The results showed that the optimal concentration of ammonium sulphide was 0.8 mol/L. The optimal pH value of ammonium sulphide was 10, and the optimal temperature of ammonium sulphide was 20°C.Under the optimum conditions, the removal efficiency of Hg(2+), Hg(0) and As could reach 99%, 88.8%, 98%, respectively. In addition, SO2 and sulphite ion could reduce the removal efficiency of mercury and arsenic from simulated flue gas.

Pulsed laser deposited ZnO film on side-polished fiber as a gas sensing element.

PubMed

Dikovska, Anna Og; Atanasov, Petar A; Stoyanchov, Toshko R; Andreev, Andrey T; Karakoleva, Elka I; Zafirova, Blagovesta S

2007-05-01

A simple sensor element consisting of a side-polished single-mode fiber and a planar metal oxide waveguide is described. The thin ZnO planar waveguide was produced on the polished fiber surface by pulsed laser deposition at optimized processing parameters. A measurement scheme for in situ control of the film thickness during the deposition process was developed and used. X-ray diffraction measurements and scanning electron microscopy were used to characterize the structure and the surface morphology of the planar waveguide, respectively. The numerical evaluation of the sensor sensitivity predicts the possibility to detect refractive index changes of less than 10(-4). Furthermore, preliminary gas sensor tests were performed by using a mixture of 1.5% butane diluted in N(2) and pure butane. A shift of the spectral position of the resonance points was observed from 3 to 5 s after gas exposure, which corresponds to refractive index changes of 3 x 10(-5) and 1.2 x 10(-3) for 1.5% butane and for pure butane, respectively.

Study of low-defect and strain-relaxed GeSn growth via reduced pressure CVD in H2 and N2 carrier gas

NASA Astrophysics Data System (ADS)

Margetis, J.; Mosleh, A.; Al-Kabi, S.; Ghetmiri, S. A.; Du, W.; Dou, W.; Benamara, M.; Li, B.; Mortazavi, M.; Naseem, H. A.; Yu, S.-Q.; Tolle, J.

2017-04-01

High quality, thick (up to 1.1 μm), strain relaxed GeSn alloys were grown on Ge-buffered Si (1 0 0) in an ASM Epsilon® chemical vapor deposition system using SnCl4 and low-cost commercial GeH4 precursors. The significance of surface chemistry in regards to growth rate and Sn-incorporation is discussed by comparing growth kinetics data in H2 and N2 carrier gas. The role of carrier gas is also explored in the suppression of Sn surface segregation and evolution of layer composition and strain profiles via secondary ion mass spectrometry and X-ray diffraction. Transmission electron microscopy revealed the spontaneous compositional splitting and formation of a thin intermediate layer in which dislocations are pinned. This intermediate layer enables the growth of a thick, strain relaxed, and defect-free epitaxial layer on its top. Last, we present photoluminescence results which indicate that both N2 and H2 growth methods produce optoelectronic device quality material.

Processing of carbamazepine-PEG 4000 solid dispersions with supercritical carbon dioxide: preparation, characterisation, and in vitro dissolution.

PubMed

Moneghini, M; Kikic, I; Voinovich, D; Perissutti, B; Filipović-Grcić, J

2001-07-03

The purpose of this study was to apply the attractive technique of the supercritical fluid to the preparation of solvent-free solid dispersions. In particular, the gas antisolvent crystallisation technique (GAS), using supercritical carbon dioxide as processing medium, has been considered to prepare an enhanced release dosage form for of the poorly soluble carbamazepine, employing PEG 4000 as a hydrophilic carrier. The physical characterisation of the systems using laser granulometer, powder X-ray diffraction, thermal analyses, and scanning electron microscopy was carried out in order to understand the influence of this technological process on the physical status of the drug. The results of the physical characterisation attested a substantial correspondence of the solid state of the drug before and after treatment with GAS technique, whereas a pronounced change in size and morphology of the drug crystals was noticed. The dramatic reduction of the dimensions and the better crystal shape, together with the presence of the hydrophilic polymer determined a remarkable enhancement of the in vitro drug dissolution rate.

Role of vacancy sites and UV-ozone treatment on few layered MoS2 nanoflakes for toxic gas detection

NASA Astrophysics Data System (ADS)

Burman, Debasree; Ghosh, Ruma; Santra, Sumita; Ray, Samit Kumar; Guha, Prasanta Kumar

2017-10-01

Various issues like global warming and environmental pollutions have led to the research of toxic gas detection worldwide. In this work, we have tried to develop a molybdenum disulfide (MoS2) based gas sensor to detect toxic gases like ammonia and NO. MoS2, an inorganic analog of graphene, has attracted lots of attention for many different applications recently. This paper reports the use of liquid exfoliated MoS2 nanoflakes as the sensing layer in a handheld, resistive toxic gas sensor. The nanoflakes were exfoliated from MoS2 bulk powder using a sonication based exfoliation technique at room temperature. The successful exfoliation of the nanoflakes was characterized using different techniques e.g., optical microscopy, atomic force microscopy, field emission scanning electron microscopy, high resolution transmission electron microscopy, x-ray diffraction, Raman spectroscopy, x-ray photoelectron spectroscopy and ultraviolet-visible spectrophotometry. The characterization results showed that few-layered nanoflakes have successfully been exfoliated. The MoS2 nanoflakes showed reasonable sensing towards ammonia and NO. In order to explore the effect of particle size on ammonia sensing, the MoS2 flakes were also exfoliated using different sonication times. We also observed that various factors like presence of vacancy sites, ambient oxygen, humidity, different contact electrodes have significant effect on the sensing characteristics. In fact, the response of the sensing layer against 400 ppm of ammonia increased from 54.1% to ˜80% when it was UV-ozone treated. This work holds promises to developing cost-effective, reliable and highly sensitive MoS2 based ammonia sensors.

LPG and NH3 sensing characteristics of DC electrochemically deposited Co3O4 films

NASA Astrophysics Data System (ADS)

Shelke, P. N.; Khollam, Y. B.; Gunjal, S. D.; Koinkar, P. M.; Jadkar, S. R.; Mohite, K. C.

2015-03-01

Present communication reports the LPG and NH3 sensing properties of Co3O4 films prepared on throughly cleaned stainless steel (SS) and copper (CU) substrates by using DC electrochemical deposition method followed by air annealing at 350°C/2 h. The resultant films are characterized by using X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM). The LPG and NH3 gas sensing properties of these films are measured at room temperature (RT) by using static gas sensing system at different concentrations of test gas ranging from 25 ppm to 350 ppm. The XRD and Raman spectroscopy studies clearly indicated the formation of pure cubic spinel Co3O4 in all films. The LPG and NH3 gas sensing properties of films showed (i) the increase in sensitivity factor (S.F.) with gas concentrations and (ii) more sensibility to LPG as compared to NH3 gas. In case of NH3 gas (conc. 150 ppm) and LPG gas (conc. 60 ppm) sensing, the maximum S.F. = 270 and 258 are found for the films deposited on CU substrates, respectively. For all films, the response time (3-5 min.) is found to be much higher than the recovery time (30-50 sec). For all films, the response and recovery time are found to be higher for LPG as compared to NH3 gas. Further, repeatability-reproducibility in gas sensing properties is clearly noted by analysis of data for number of cycles recorded for all films from different set of depositions.

Compression of subrelativistic space-charge-dominated electron bunches for single-shot femtosecond electron diffraction.

PubMed

van Oudheusden, T; Pasmans, P L E M; van der Geer, S B; de Loos, M J; van der Wiel, M J; Luiten, O J

2010-12-31

We demonstrate the compression of 95 keV, space-charge-dominated electron bunches to sub-100 fs durations. These bunches have sufficient charge (200 fC) and are of sufficient quality to capture a diffraction pattern with a single shot, which we demonstrate by a diffraction experiment on a polycrystalline gold foil. Compression is realized by means of velocity bunching by inverting the positive space-charge-induced velocity chirp. This inversion is induced by the oscillatory longitudinal electric field of a 3 GHz radio-frequency cavity. The arrival time jitter is measured to be 80 fs.

Removal of elemental Mercury from flue gas using wheat straw chars modified by K2FeO4 reagent.

PubMed

Zhou, Jianfei; Liu, Yangxian; Pan, Jianfeng

2017-12-01

In this article, wheat straw (WS) char, a common agricultural waste and renewable biomass, was pyrolyzed and then modified by K 2 FeO 4 reagent to develop an efficient sorbent for removal of Hg 0 from flue gas. Brunauer-Emmett-Teller, scanning electron microscopy with energy spectrum and X-ray diffraction (XRD) were employed to characterize the sorbents. The effects of K 2 FeO 4 loading, reaction temperature, Hg 0 inlet concentration and concentrations of gas mixtures O 2 , NO and SO 2 in flue gas on Hg 0 removal were investigated in a fixed-bed reactor. The results show that K 2 FeO 4 -impregnation can improve pore structure of WS char and produce new active sites, which significantly enhance Hg 0 removal. Increasing Hg 0 inlet concentration significantly decreases Hg 0 removal efficiency. O 2 in flue gas promotes Hg 0 oxidation by replenishing the oxygen groups on the surface of modified chars. The presence of NO obviously promotes Hg 0 removal since it can oxidize Hg 0 to Hg(NO 3 ) 2 . SO 2 in flue gas significantly decreases Hg 0 removal efficiency due to the competition adsorption between SO 2 and Hg 0 . The increase in reaction temperature has a dual impact on Hg 0 removal.

Digital direct electron imaging of energy-filtered electron backscatter diffraction patterns

NASA Astrophysics Data System (ADS)

Vespucci, S.; Winkelmann, A.; Naresh-Kumar, G.; Mingard, K. P.; Maneuski, D.; Edwards, P. R.; Day, A. P.; O'Shea, V.; Trager-Cowan, C.

2015-11-01

Electron backscatter diffraction is a scanning electron microscopy technique used to obtain crystallographic information on materials. It allows the nondestructive mapping of crystal structure, texture, and strain with a lateral and depth resolution on the order of tens of nanometers. Electron backscatter diffraction patterns (EBSPs) are presently acquired using a detector comprising a scintillator coupled to a digital camera, and the crystallographic information obtainable is limited by the conversion of electrons to photons and then back to electrons again. In this article we will report the direct acquisition of energy-filtered EBSPs using a digital complementary metal-oxide-semiconductor hybrid pixel detector, Timepix. We show results from a range of samples with different mass and density, namely diamond, silicon, and GaN. Direct electron detection allows the acquisition of EBSPs at lower (≤5 keV) electron beam energies. This results in a reduction in the depth and lateral extension of the volume of the specimen contributing to the pattern and will lead to a significant improvement in lateral and depth resolution. Direct electron detection together with energy filtering (electrons having energy below a specific value are excluded) also leads to an improvement in spatial resolution but in addition provides an unprecedented increase in the detail in the acquired EBSPs. An increase in contrast and higher-order diffraction features are observed. In addition, excess-deficiency effects appear to be suppressed on energy filtering. This allows the fundamental physics of pattern formation to be interrogated and will enable a step change in the use of electron backscatter diffraction (EBSD) for crystal phase identification and the mapping of strain. The enhancement in the contrast in high-pass energy-filtered EBSD patterns is found to be stronger for lighter, less dense materials. The improved contrast for such materials will enable the application of the EBSD technique to be expanded to materials for which conventional EBSD analysis is not presently practicable.

Observation of coherent optical phonons excited by femtosecond laser radiation in Sb films by ultrafast electron diffraction method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mironov, B. N.; Kompanets, V. O.; Aseev, S. A., E-mail: isanfemto@yandex.ru

2017-03-15

The generation of coherent optical phonons in a polycrystalline antimony film sample has been investigated using femtosecond electron diffraction method. Phonon vibrations have been induced in the Sb sample by the main harmonic of a femtosecond Ti:Sa laser (λ = 800 nm) and probed by a pulsed ultrashort photoelectron beam synchronized with the pump laser. The diffraction patterns recorded at different times relative to the pump laser pulse display oscillations of electron diffraction intensity corresponding to the frequencies of vibrations of optical phonons: totally symmetric (A{sub 1g}) and twofold degenerate (E{sub g}) phonon modes. The frequencies that correspond to combinationsmore » of these phonon modes in the Sb sample have also been experimentally observed.« less

Transmission electron microscope studies of extraterrestrial materials

NASA Technical Reports Server (NTRS)

Keller, Lindsay P.

1995-01-01

Transmission Electron Microscopy, X-Ray spectrometry and electron-energy-loss spectroscopy are used to analyse carbon in interplanetary dust particles. Optical micrographs are shown depicting cross sections of the dust particles embedded in sulphur. Selected-area electron diffraction patterns are shown. Transmission Electron Microscope specimens of lunar soil were prepared using two methods: ion-milling and ultramicrotomy. A combination of high resolution TEM imaging and electron diffraction is used to characterize the opaque assemblages. The opaque assemblages analyzed in this study are dominated by ilmenite with lesser rutile and spinel exsolutions, and traces of Fe metal.

A High Sensitivity Isopropanol Vapor Sensor Based on Cr₂O₃-SnO₂ Heterojunction Nanocomposites via Chemical Precipitation Route.

PubMed

Jawaher, K Rackesh; Indirajith, R; Krishnan, S; Robert, R; Pasha, S K Khadheer; Deshmukh, Kalim; Sastikumar, D; Das, S Jerome

2018-08-01

Cr2O3-SnO2 heterojunction nanocomposites were prepared via chemical precipitation method. The prepared samples were characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectra and Field Emission Electron Microscopy (FESEM). The XRD spectrum confirms the presence of both tetragonal rutile SnO2 and rhombohedral corundum Cr2O3 structure. Further investigation into the gas sensing performances of the prepared Cr2O3-SnO2 nanocomposites exhibited an enhanced sensitivity towards VOPs such as isopropanol, acetone, ethanol and formaldehyde. Especially, isopropanol vapor sensor shows excellent sensitivity at an operating temperature of 100 °C. The highest sensitivity for Cr2O3-SnO2 heterojunction nanocomposites indicate that these materials can be a good candidate for the production of high-performance isopropanol sensors.

Growth of copper-benzene-1,3,5-tricarboxylate on boron nitride nanotubes and application of the composite in methane sensing

NASA Astrophysics Data System (ADS)

Xiang, Cuili; Chen, Ting; Zhang, Haitao; Zou, Yongjin; Chu, Hailiang; Zhang, Huanzhi; Xu, Fen; Sun, Lixian; Tang, Chengying

2017-12-01

A new composite material based on copper-benzene-1,3,5-tricarboxylate (Cu-BTC) deposited on boron nitride nanotubes (BNNTs) in a hydrothermal process were investigated for methane (CH4) sensing. The composite was characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The Cu-BTC deposited on the BNNTs had an average grain size of 80 nm. The sensing performance of the as-grown product was studied for different concentrations of CH4 (20-200 ppm) at 150 °C. The results revealed that the Cu-BTC/BNNT composite exhibited high sensitivity and selectivity toward CH4. The good sensing performance of the composite was attributed to the high surface area and high affinity of Cu-BTC for CH4, which would allow the composite to act like a preconcentrator for CH4 gas sensing.

Gradient microstructure and microhardness in a nitrided 18CrNiMo7-6 gear steel

NASA Astrophysics Data System (ADS)

Yang, R.; Wu, G. L.; Zhang, X.; Fu, W. T.; Huang, X.

2017-07-01

A commercial gear steel (18CrNiMo7-6) containing a tempered martensite structure was nitrided using a pressurized gas nitriding process under a pressure of 5 atm at 530 °C for 5 hours. The mechanical properties and microstructure of the nitrided sample were characterized by Vickers hardness measurements, X-ray diffraction, and backscatter electron imaging in a scanning electron microscope. A micro-hardness gradient was identified over a distance of 500 μm with hardness values of 900 HV at the top surface and 300 HV in the core. This micro-hardness gradient corresponds to a gradient in the microstructure that changes from a nitride compound layer at the top surface (∼ 20 μm thick) to a diffusion zone with a decreasing nitrogen concentration and precipitate density with distance from the surface, finally reaching the core matrix layer with a recovered martensite structure.

Synthesis and characterization of CdS-based ternary composite for enhanced visible light-driven photocatalysis

NASA Astrophysics Data System (ADS)

Singh, Arvind; Sinha, A. S. K.

2018-09-01

Active ternary graphite and alumina-supported cadmium sulphide (CdS) composite was synthesized by impregnation method followed by high-temperature solid-gas reaction and characterized by X-ray diffraction (XRD), photoluminescence spectroscopy (PL), diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) techniques. The ternary CdS-graphite-alumina composite exhibited superior catalytic activity compared with the binary CdS-alumina composite due to its better visible-light absorption and higher charge separation. The ternary composite has a bed-type structure. It permits a greater interaction at the interface due to intimate contact between CdS and graphite in the ternary composite. This composite has a highly efficient visible light-driven photocatalytic activity for sustainable hydrogen production. It is also capable of degrading organic dyes in wastewater.

Novel perovskite coating of strontium zirconate in Inconel substrate

NASA Astrophysics Data System (ADS)

Venkatesh, G.; Blessto, B.; Rao, C. Santhosh Kumar; Subramanian, R.; Berchmans, L. John

2018-02-01

Thermal Barrier Coatings (TBC) provides a low thermal conductivity barrier to heat transfer from the hot gas in the engine to the surface of the coated alloy component. SrZrO3 powder are prepared by Sol Gel synthesis method. The synthesized powder sample is characterized by X Ray Diffraction Technique (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) and the results are interpreted. The Polycrystalline nature of SrZrO3 is confirmed and lattice spacing are determined in XRD. SEM shows sub-micron sized particles and a fringed pattern is observed in TEM. The IN718 specimen is Wire Cut and Sand Blasted. A SrZrO3 double layer is coated over the Inconel specimen through a Bond Coat made of NiCoCrAlY by Plasma spraying Process and also characterized. SEM analysis of the Coating shows diffusion of Fe, Sr into the substrate.

Low-energy Auger electron diffraction: influence of multiple scattering and angular momentum

NASA Astrophysics Data System (ADS)

Chassé, A.; Niebergall, L.; Kucherenko, Yu.

2002-04-01

The angular dependence of Auger electrons excited from single-crystal surfaces is treated theoretically within a multiple-scattering cluster model taking into account the full Auger transition matrix elements. In particular the model has been used to discuss the influence of multiple scattering and angular momentum of the Auger electron wave on Auger electron diffraction (AED) patterns in the region of low kinetic energies. Theoretical results of AED patterns are shown and discussed in detail for Cu(0 0 1) and Ni(0 0 1) surfaces, respectively. Even though Cu and Ni are very similar in their electronic and scattering properties recently strong differences have been found in AED patterns measured in the low-energy region. It is shown that the differences may be caused to superposition of different electron diffraction effects in an energy-integrated experiment. A good agreement between available experimental and theoretical results has been achieved.

Symposium N: Materials and Devices for Thermal-to-Electric Energy Conversion

DTIC Science & Technology

2010-08-24

X - ray diffraction, transmission electron microscopy, scanning electron microscopy, and dynamic light scattering. Thermal conductivity measurements...SEM), X - ray diffraction (XRD) measurements as well as Raman spectroscopy. The results from these techniques indicate a clear modification...was examined by using scanning electron microscope (SEM; HITACHI S-4500 model) attached with an energy dispersive x - ray spectroscopy. The electrical

Atomic structure solution of the complex quasicrystal approximant Al77Rh15Ru8 from electron diffraction data.

PubMed

Samuha, Shmuel; Mugnaioli, Enrico; Grushko, Benjamin; Kolb, Ute; Meshi, Louisa

2014-12-01

The crystal structure of the novel Al77Rh15Ru8 phase (which is an approximant of decagonal quasicrystals) was determined using modern direct methods (MDM) applied to automated electron diffraction tomography (ADT) data. The Al77Rh15Ru8 E-phase is orthorhombic [Pbma, a = 23.40 (5), b = 16.20 (4) and c = 20.00 (5) Å] and has one of the most complicated intermetallic structures solved solely by electron diffraction methods. Its structural model consists of 78 unique atomic positions in the unit cell (19 Rh/Ru and 59 Al). Precession electron diffraction (PED) patterns and high-resolution electron microscopy (HRTEM) images were used for the validation of the proposed atomic model. The structure of the E-phase is described using hierarchical packing of polyhedra and a single type of tiling in the form of a parallelogram. Based on this description, the structure of the E-phase is compared with that of the ε6-phase formed in Al-Rh-Ru at close compositions.

Auger electron diffraction study of Fe 1- xNi x alloys epitaxially grown on Cu(100)

NASA Astrophysics Data System (ADS)

Martin, M. G.; Foy, E.; Chevrier, F.; Krill, G.; Asensio, M. C.

1999-08-01

We have combined Auger electron diffraction (AED), low-energy electron diffraction (LEED) and high-energy electron diffraction (RHEED) to examine the structure of Fe xNi 1- x alloys when the Fe content approaches 65%. At this concentration, the 'invar effect' takes place, so the magnetization falls to zero, and the thermal expansion coefficient is very small. The Fe xNi 1- x alloys, grown as metastable thin films by molecular-beam epitaxy on Cu(100) substrates, were studied as a function of the x stoichiometry. In contrast to the related bulk alloy compounds, we observe the collapse of the fcc-to-bcc structural transition in the Fe-rich films. Furthermore, the local atomic structure around Fe and Ni in the alloy has been simultaneously determined by the angular intensity distributions of Fe L 3VV (703 eV) and Ni L 3VV (848 eV) Auger electrons measured as a function of polar and azimuthal angles. For the films deposited at room temperature, we have confirmed the pseudomorphic growth morphology and the uniformity of the alloys.

ELECTRON MICROSCOPE AND X-RAY DIFFRACTION STUDIES ON A HOMOLOGOUS SERIES OF SATURATED PHOSPHATIDYLCHOLINES.

PubMed

ELBERS, P F; VERVERGAERT, P H

1965-05-01

Three homologous saturated phosphatidylcholines were studied by electron microscopy after tricomplex fixation. The results are compared with those obtained by x-ray diffraction analysis of the same and some other homologous compounds, in the dry crystalline state and after tricomplex fixation. By electron microscopy alternating dark and light bands are observed which are likely to correspond to phosphatide double layers. X-Ray diffraction reveals the presence of lamellar structures of regular spacing. The layer spacings obtained by both methods are in good agreement. From the electron micrographs the width of the polar parts of the double layers can be derived directly. The width of the carboxylglycerylphosphorylcholine moiety of the layers is found by extrapolating the x-ray diffraction data to zero chain length of the fatty acids. When from this width the contribution of the carboxylglyceryl part of the molecules is subtracted, again we find good agreement with the electron microscope measurements. An attempt has been made to account for the different layer spacings measured in terms of orientation of the molecules within the double layers.

Investigation of the effect of phase nonuniformities and the microwave field distribution on the electronic efficiency of a diffraction-radiation generator

NASA Astrophysics Data System (ADS)

Maksimov, P. P.; Tsvyk, A. I.; Shestopalov, V. P.

1985-10-01

The effect of local phase nonuniformities of the diffraction gratings and the field distribution of the open cavity on the electronic efficiency of a diffraction-radiation generator (DRG) is analyzed numerically on the basis of a self-consistent system of nonlinear stationary equations for the DRG. It is shown that the interaction power and efficiency of a DRG can be increased by the use of an open cavity with a nonuniform diffraction grating and a complex form of microwave field distribution over the interaction space.

Modulated Electron Emission by Scattering-Interference of Primary Electrons

NASA Astrophysics Data System (ADS)

Valeri, Sergio; di Bona, Alessandro

We review the effects of scattering-interference of the primary, exciting beam on the electron emission from ordered atomic arrays. The yield of elastically and inelastically backscattered electrons, Auger electrons and secondary electrons shows a marked dependence on the incidence angle of primary electrons. Both the similarity and the relative importance of processes experienced by incident and excident electrons are discussed. We also present recent studies of electron focusing and defocusing along atomic chains. The interplay between these two processes determines the in-depth profile of the primary electron intensity anisotropy. Finally, the potential for surface-structural studies and limits for quantitative analysis are discussed, in comparison with the Auger electron diffraction (AED) and photoelectron diffraction (PD) techniques.

Imaging ultrafast dynamics of molecules with laser-induced electron diffraction.

PubMed

Lin, C D; Xu, Junliang

2012-10-14

We introduce a laser-induced electron diffraction method (LIED) for imaging ultrafast dynamics of small molecules with femtosecond mid-infrared lasers. When molecules are placed in an intense laser field, both low- and high-energy photoelectrons are generated. According to quantitative rescattering (QRS) theory, high-energy electrons are produced by a rescattering process where electrons born at the early phase of the laser pulse are driven back to rescatter with the parent ion. From the high-energy electron momentum spectra, field-free elastic electron-ion scattering differential cross sections (DCS), or diffraction images, can be extracted. With mid-infrared lasers as the driving pulses, it is further shown that the DCS can be used to extract atomic positions in a molecule with sub-angstrom spatial resolution, in close analogy to the standard electron diffraction method. Since infrared lasers with pulse duration of a few to several tens of femtoseconds are already available, LIED can be used for imaging dynamics of molecules with sub-angstrom spatial and a few-femtosecond temporal resolution. The first experiment with LIED has shown that the bond length of oxygen molecules shortens by 0.1 Å in five femtoseconds after single ionization. The principle behind LIED and its future outlook as a tool for dynamic imaging of molecules are presented.

Influence of quantum diffraction and shielding on electron-ion collision in two-component semiclassical plasmas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hong, Woo-Pyo; Jung, Young-Dae, E-mail: ydjung@hanyang.ac.kr; Department of Applied Physics and Department of Bionanotechnology, Hanyang University, Ansan, Kyunggi-Do 426-791

2015-01-15

The influence of quantum diffraction and shielding on the electron-ion collision process is investigated in two-component semiclassical plasmas. The eikonal method and micropotential taking into account the quantum diffraction and shielding are used to obtain the eikonal scattering phase shift and the eikonal collision cross section as functions of the collision energy, density parameter, Debye length, electron de Broglie wavelength, and the impact parameter. The result shows that the quantum diffraction and shielding effects suppress the eikonal scattering phase shift as well as the differential eikonal collision cross section, especially, in small-impact parameter regions. It is also shown that themore » quantum shielding effect on the eikonal collision cross section is more important in low-collision energies. In addition, it is found that the eikonal collision cross section increases with an increase in the density parameter. The variations of the eikonal cross section due to the quantum diffraction and shielding effects are also discussed.« less

Folding and stacking defects of graphene flakes probed by electron nanobeam

DOE Office of Scientific and Technical Information (OSTI.GOV)

Persichetti, L.; Fanfoni, M.; Sgarlata, A.

2011-07-25

Combining nanoscale imaging with local electron spectroscopy and diffraction has provided direct information on folding and stacking defects of graphene flakes produced by unrolled multi-walled carbon nanotubes. Structural data obtained by nanoarea electron diffraction complemented with systematic electron energy loss spectroscopy measurements of the surface plasmon losses of single flakes show the presence of flat bilayer regions coexisting with folded areas where the topology of buckled graphene resembles that of warped carbon nanostructures.

Structural changes induced by lattice-electron interactions: SiO2 stishovite and FeTiO3 ilmenite.

PubMed

Yamanaka, Takamitsu

2005-09-01

The bright source and highly collimated beam of synchrotron radiation offers many advantages for single-crystal structure analysis under non-ambient conditions. The structure changes induced by the lattice-electron interaction under high pressure have been investigated using a diamond anvil pressure cell. The pressure dependence of electron density distributions around atoms is elucidated by a single-crystal diffraction study using deformation electron density analysis and the maximum entropy method. In order to understand the bonding electrons under pressure, diffraction intensity measurements of FeTiO3 ilmenite and gamma-SiO2 stishovite single crystals at high pressures were made using synchrotron radiation. Both diffraction studies describe the electron density distribution including bonding electrons and provide the effective charge of the cations. In both cases the valence electrons are more localized around the cations with increasing pressure. This is consistent with molecular orbital calculations, proving that the bonding electron density becomes smaller with pressure. The thermal displacement parameters of both samples are reduced with increasing pressure.

Femtosecond Electron Wave Packet Propagation and Diffraction: Towards Making the ``Molecular Movie"

NASA Astrophysics Data System (ADS)

Miller, R. J. Dwayne

2003-03-01

Time-resolved electron diffraction harbors great promise for achieving atomic resolution of the fastest chemical processes. The generation of sufficiently short electron pulses to achieve this real time view of a chemical reaction has been limited by problems in maintaining short electron pulses with realistic electron densities to the sample. The propagation dynamics of femtosecond electron packets in the drift region of a photoelectron gun are investigated with an N-body numerical simulation and mean-field model. This analyis shows that the redistribution of electrons inside the packet, arising from space-charge and dispersion contributions, changes the pulse envelope and leads to the development of a spatially linear axial velocity distribution. These results have been used in the design of femtosecond photoelectron guns with higher time resolution and novel electron-optical methods of pulse characterization that are approaching 100 fs timescales. Time-resolved diffraction studies with electron pulses of approximately 500 femtoseconds have focused on solid-liquid phase transitions under far from equilibrium conditions. This work gives a microscopic description of the melting process and illustrates the promise of atomically resolving transition state processes.

Scanning tunneling microscopy study of low temperature silicon epitaxy on hydrogen/silicon(001) and phosphine adsorption on silicon(111)-7x7

NASA Astrophysics Data System (ADS)

Ji, Jeong-Young

A three-chamber ultra-high-vacuum (UHV) system with preparation, scanning tunneling microscopy (STM), and chemical vapor deposition (CVD) chambers was designed and built. Here, one can perform surface preparation, STM e-beam lithography, precursor gas dosing, ion sputtering, silicon epitaxy, and various measurements such as reflection high energy electron diffraction (RHEED), low energy electron diffraction (LEED), and Auger electron spectroscopy (AES). Processes performed in the ultra-clean preparation and gas-filled CVD chambers can be monitored by transferring the samples back to the STM chamber to take topographical images. Si deposition on H-terminated Si(001)-2x1 surfaces at temperatures 300--530 K was studied by scanning tunneling microscopy. Hydrogen apparently hinders Si adatom diffusion and enhances surface roughening. Post-growth annealing transfers the top layer atoms downward to fill in vacancies in the lower layer, restoring the crystallinity of the thin film. Hydrogen is shown to remain on the growth front up to at least 10 ML. Si deposition onto the H/Si(001)-3x1 surface at 530 K suggests that dihydride units further suppress Si adatom diffusion and increase surface roughness. PH3 adsorption on Si(111)-7x7 was studied for various exposures between 0.3--60 L at room temperature by means of the scanning-tunneling-microscopy (STM). PH3-, PH2-, H-reacted, and unreacted adatoms can be identified by analyzing STM images at different sample biases. Most of PH3 adsorbs dissociatively on the surface at initial exposure, generating H and PH2 adsorption sites, followed by molecular adsorption of PH3. Rest atoms are more reactive than the adatoms and PH 2-reacted rest atom sites are also observed in STM images. Statistical analysis shows that center adatoms are more reactive than corner adatoms and the saturation P coverage is ˜0.22 ML. Finally, 900 K annealing of a PH 3 dosed surface results in a disordered, partially P-covered surface and PH3 dosing at 900 K forms the same surface reconstruction as a P2-adsorbed surface at similar temperature.

Classification and assessment of retrieved electron density maps in coherent X-ray diffraction imaging using multivariate analysis.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Nakasako, Masayoshi

2016-01-01

Coherent X-ray diffraction imaging (CXDI) is one of the techniques used to visualize structures of non-crystalline particles of micrometer to submicrometer size from materials and biological science. In the structural analysis of CXDI, the electron density map of a sample particle can theoretically be reconstructed from a diffraction pattern by using phase-retrieval (PR) algorithms. However, in practice, the reconstruction is difficult because diffraction patterns are affected by Poisson noise and miss data in small-angle regions due to the beam stop and the saturation of detector pixels. In contrast to X-ray protein crystallography, in which the phases of diffracted waves are experimentally estimated, phase retrieval in CXDI relies entirely on the computational procedure driven by the PR algorithms. Thus, objective criteria and methods to assess the accuracy of retrieved electron density maps are necessary in addition to conventional parameters monitoring the convergence of PR calculations. Here, a data analysis scheme, named ASURA, is proposed which selects the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a diffraction pattern. Each electron density map composed of J pixels is expressed as a point in a J-dimensional space. Principal component analysis is applied to describe characteristics in the distribution of the maps in the J-dimensional space. When the distribution is characterized by a small number of principal components, the distribution is classified using the k-means clustering method. The classified maps are evaluated by several parameters to assess the quality of the maps. Using the proposed scheme, structure analysis of a diffraction pattern from a non-crystalline particle is conducted in two stages: estimation of the overall shape and determination of the fine structure inside the support shape. In each stage, the most accurate and probable density maps are objectively selected. The validity of the proposed scheme is examined by application to diffraction data that were obtained from an aggregate of metal particles and a biological specimen at the XFEL facility SACLA using custom-made diffraction apparatus.

Recombinant Reflectin-Based Optical Materials

DTIC Science & Technology

2012-01-01

sili- con substrates were placed in a sealed plastic box. The RH was controlled using a Dydra electronic cigar humidifier and monitored using a Fisher...diffraction gratings to generate diffraction patterns. Nano-spheres and la- mellar microstructures of refCBA samples were observed by scanning electron ...samples were observed by scanning electron microscopy and atomic force microscopy. Despite the reduced complexity of the refCBA protein compared to natural

Effect of screw threading dislocations and inverse domain boundaries in GaN on the shape of reciprocal-space maps.

PubMed

Barchuk, Mykhailo; Motylenko, Mykhaylo; Lukin, Gleb; Pätzold, Olf; Rafaja, David

2017-04-01

The microstructure of polar GaN layers, grown by upgraded high-temperature vapour phase epitaxy on [001]-oriented sapphire substrates, was studied by means of high-resolution X-ray diffraction and transmission electron microscopy. Systematic differences between reciprocal-space maps measured by X-ray diffraction and those which were simulated for different densities of threading dislocations revealed that threading dislocations are not the only microstructure defect in these GaN layers. Conventional dark-field transmission electron microscopy and convergent-beam electron diffraction detected vertical inversion domains as an additional microstructure feature. On a series of polar GaN layers with different proportions of threading dislocations and inversion domain boundaries, this contribution illustrates the capability and limitations of coplanar reciprocal-space mapping by X-ray diffraction to distinguish between these microstructure features.

Coherent Diffractive Imaging: From Nanometric Down to Picometric Resolution

NASA Astrophysics Data System (ADS)

De Caro, Liberato; Carlino, Elvio; Siliqi, Dritan; Giannini, Cinzia

Coherent diffractive imaging (CDI) is a novel technique for inspecting (crystalline and non-crystalline) matter from nanometric down to picometric resolution. It was used originally with X-rays and, more recently, with electrons (so-called electron diffractive imaging, or EDI). This chapter introduces basic concepts concerning CDI and addresses the different types of X-ray CDI experiments that have been conducted, namely plane wave CDI from isolated objects in forward scattering, focused-beam Fresnel CDI from isolated objects in forward scattering, Bragg CDI from nanocrystals, and keyhole CDI and ptychography from extended objects. A CDI experiment with a transmission electron microscope, alternatively named an EDI experiment, is also introduced.

TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Shirahama, Keiya; Torizuka, Yasufumi; Manoda, Masahiro; Nakasako, Masayoshi; Yamamoto, Masaki

2016-05-01

Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speed higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.

Formation of Semimetallic Cobalt Telluride Nanotube Film via Anion Exchange Tellurization Strategy in Aqueous Solution for Electrocatalytic Applications.

PubMed

Patil, Supriya A; Kim, Eun-Kyung; Shrestha, Nabeen K; Chang, Jinho; Lee, Joong Kee; Han, Sung-Hwan

2015-11-25

Metal telluride nanostructures have demonstrated several potential applications particularly in harvesting and storing green energy. Metal tellurides are synthesized by tellurization process performed basically at high temperature in reducing gas atmosphere, which makes the process expensive and complicated. The development of a facile and economical process for desirable metal telluride nanostructures without complicated manipulation is still a challenge. In an effort to develop an alternative strategy of tellurization, herein we report a thin film formation of self-standing cobalt telluride nanotubes on various conducting and nonconducting substrates using a simple binder-free synthetic strategy based on anion exchange transformation from a thin film of cobalt hydroxycarbonate nanostructures in aqueous solution at room temperature. The nanostructured films before and after ion exchange transformation reaction are characterized using field emission scanning electron microscope, energy dispersive X-ray analyzer, X-ray photoelectron spectroscopy, thin film X-ray diffraction technique, high resolution transmission electron microscope, and selected area electron diffraction analysis technique. After the ion exchange transformation of nanostructures, the film shows conversion from insulator to highly electrical conductive semimetallic characteristic. When used as a counter electrode in I3(-)/I(-) redox electrolyte based dye-sensitized solar cells, the telluride film exhibits an electrocatalytic reduction activity for I3(-) with a demonstration of solar-light to electrical power conversion efficiency of 8.10%, which is highly competitive to the efficiency of 8.20% exhibited by a benchmarked Pt-film counter electrode. On the other hand, the telluride film electrode also demonstrates electrocatalytic activity for oxygen evolution reaction from oxidation of water.

Microstructural characterization of a Zr-Ti-Ni-Mn-V-Cr based AB 2-type battery alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shi, Zhan

1999-01-01

Transmission Electron Microscopy (TEM), combined with X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) was employed to investigate a proprietary and multicomponent AB 2 type Nickel-Metal Hydride (Ni-MH) battery alloy. This material was prepared by High Pressure Gas Atomization (HPGA) and examined in both the as-atomized and heat treated condition. TEM examination showed a heavily faulted dendritic growth structure in as-atomized powder. Selected Area Diffraction (SAD) showed that this region consisted of both a cubic C15 structure with lattice constant a=7.03 and a hexagonal C14 structure with lattice parameter a=4.97 Å, c=8.11 Å. The Orientation Relationship (OR) between the C14 and C15 structures was determined to be (111)[1more » $$\\bar{1}$$0] C15//(0001)[11$$\\bar{2}$$0] C14. An interdendritic phase possessing the C14 structure was also seen. There was also a very fine grain region consisting of the C14 structure. Upon heat treatment, the faulted structure became more defined and appeared as intercalation layers within the grains. Spherical particles rich in Zr and Ni appeared scattered at the grain boundaries instead of the C14 interdendritic phase. The polycrystalline region also changed to a mixture of C14 and C15 structures. These results as well as phase stability of the C15 and C14 structures based on a consideration of atomic size factor and the average electron concentration are discussed.« less

Behavior of Quartz and Carbon Black Pellets at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Li, Fei; Tangstad, Merete

This paper studies the quartz and carbon black pellets at elevated temperature with varying temperature and gas atmosphere. High-purity quartz and commercial ultra-pure carbon black was mixed (carbon content vet. 15%), and then pelletized into particles of l-3mm in diameter. The stoichiometric analysis of the pellet during heating is studied in thermogravimetric analysis (TGA) furnace at different temperature in CO and Ar atmosphere. The microstructure, phase changes and element content of sample before/after heating is characterized by X-ray diffraction, scanning electron microscope, X-ray fluorescence and LECO analyzer. The reaction process can be divided into two stages. Higher temperature and argon atmosphere are the positive parameters for SiC formation.

In situ X-ray ptychography imaging of high-temperature CO{sub 2} acceptor particle agglomerates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Høydalsvik, Kristin; Bø Fløystad, Jostein; Esmaeili, Morteza

2014-06-16

Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO{sub 2} capture material, was studied at a pressure of one atmosphere in air and in CO{sub 2}, at temperatures exceeding 600 °C. Images with a spatial resolution better than 200 nm were retrieved, and possibilities for improving the experiment are described.

The collection of MicroED data for macromolecular crystallography.

PubMed

Shi, Dan; Nannenga, Brent L; de la Cruz, M Jason; Liu, Jinyang; Sawtelle, Steven; Calero, Guillermo; Reyes, Francis E; Hattne, Johan; Gonen, Tamir

2016-05-01

The formation of large, well-ordered crystals for crystallographic experiments remains a crucial bottleneck to the structural understanding of many important biological systems. To help alleviate this problem in crystallography, we have developed the MicroED method for the collection of electron diffraction data from 3D microcrystals and nanocrystals of radiation-sensitive biological material. In this approach, liquid solutions containing protein microcrystals are deposited on carbon-coated electron microscopy grids and are vitrified by plunging them into liquid ethane. MicroED data are collected for each selected crystal using cryo-electron microscopy, in which the crystal is diffracted using very few electrons as the stage is continuously rotated. This protocol gives advice on how to identify microcrystals by light microscopy or by negative-stain electron microscopy in samples obtained from standard protein crystallization experiments. The protocol also includes information about custom-designed equipment for controlling crystal rotation and software for recording experimental parameters in diffraction image metadata. Identifying microcrystals, preparing samples and setting up the microscope for diffraction data collection take approximately half an hour for each step. Screening microcrystals for quality diffraction takes roughly an hour, and the collection of a single data set is ∼10 min in duration. Complete data sets and resulting high-resolution structures can be obtained from a single crystal or by merging data from multiple crystals.

A pipeline for comprehensive and automated processing of electron diffraction data in IPLT.

PubMed

Schenk, Andreas D; Philippsen, Ansgar; Engel, Andreas; Walz, Thomas

2013-05-01

Electron crystallography of two-dimensional crystals allows the structural study of membrane proteins in their native environment, the lipid bilayer. Determining the structure of a membrane protein at near-atomic resolution by electron crystallography remains, however, a very labor-intense and time-consuming task. To simplify and accelerate the data processing aspect of electron crystallography, we implemented a pipeline for the processing of electron diffraction data using the Image Processing Library and Toolbox (IPLT), which provides a modular, flexible, integrated, and extendable cross-platform, open-source framework for image processing. The diffraction data processing pipeline is organized as several independent modules implemented in Python. The modules can be accessed either from a graphical user interface or through a command line interface, thus meeting the needs of both novice and expert users. The low-level image processing algorithms are implemented in C++ to achieve optimal processing performance, and their interface is exported to Python using a wrapper. For enhanced performance, the Python processing modules are complemented with a central data managing facility that provides a caching infrastructure. The validity of our data processing algorithms was verified by processing a set of aquaporin-0 diffraction patterns with the IPLT pipeline and comparing the resulting merged data set with that obtained by processing the same diffraction patterns with the classical set of MRC programs. Copyright © 2013 Elsevier Inc. All rights reserved.

A pipeline for comprehensive and automated processing of electron diffraction data in IPLT

PubMed Central

Schenk, Andreas D.; Philippsen, Ansgar; Engel, Andreas; Walz, Thomas

2013-01-01

Electron crystallography of two-dimensional crystals allows the structural study of membrane proteins in their native environment, the lipid bilayer. Determining the structure of a membrane protein at near-atomic resolution by electron crystallography remains, however, a very labor-intense and time-consuming task. To simplify and accelerate the data processing aspect of electron crystallography, we implemented a pipeline for the processing of electron diffraction data using the Image Processing Library & Toolbox (IPLT), which provides a modular, flexible, integrated, and extendable cross-platform, open-source framework for image processing. The diffraction data processing pipeline is organized as several independent modules implemented in Python. The modules can be accessed either from a graphical user interface or through a command line interface, thus meeting the needs of both novice and expert users. The low-level image processing algorithms are implemented in C++ to achieve optimal processing performance, and their interface is exported to Python using a wrapper. For enhanced performance, the Python processing modules are complemented with a central data managing facility that provides a caching infrastructure. The validity of our data processing algorithms was verified by processing a set of aquaporin-0 diffraction patterns with the IPLT pipeline and comparing the resulting merged data set with that obtained by processing the same diffraction patterns with the classical set of MRC programs. PMID:23500887

Co-synthesis and drug delivery properties of mesoporous hydroxyapatite-silica composites.

PubMed

Zhao, Y F; Loo, S C J; Ma, J

2009-06-01

In this work, mesoporous hydroxyapatite-silica (HA-silica) composite materials with four different Si:Ca:P ratios were sol-gel derived through self-assembly using triblock copolymer Pluronics P123 as template. The composition and mesoporous structure formed were characterized by X-ray diffraction and electron microscopy. The XRD patterns indicated that the intensity of the HA phase becomes stronger as the Ca/Si ratio of the composite increases. From nitrogen gas analysis at 77 K, type IV isotherm plots for typical mesoporous materials were observed for all of the samples. However, the mesoporous structure of HA-silica tends to becomes less ordered as the Ca/Si ratio increases. Promising consistency between the pore sizes from the Barrett, Joyner and Halenda (BJH) method, Transmission Electron Microscopy (TEM) and Small Angle X-ray diffraction (SAXRD) was also observed. The formation mechanism of mesoporous HA-silica composites was proposed, where the interaction between the crystallization of HA and the surfactant liquid crystal determines the regularity of the meso-structure. In vitro drug loading and release studies showed that drug loading capacity is dependent on the pore volume of the sample, and the mesoporosity of the samples were responsible for the sustained release of drugs. In vitro cell culture of the samples showed promising biocompatibility where osteosarcoma cells were observed to grow favourably on the synthesized composites.

Discontinuous precipitation in a nickel-free high nitrogen austenitic stainless steel on solution nitriding

NASA Astrophysics Data System (ADS)

Mohammadzadeh, Roghayeh; Akbari, Alireza; Grumsen, Flemming B.; Somers, Marcel A. J.

2017-10-01

Chromium-rich nitride precipitates in production of nickel-free austenitic stainless steel plates via pressurised solution nitriding of Fe-22.7Cr-2.4Mo ferritic stainless steel at 1473 K (1200 °C) under a nitrogen gas atmosphere was investigated. The microstructure, chemical and phase composition, morphology and crystallographic orientation between the resulted austenite and precipitates were investigated using optical microscopy, X-ray Diffraction (XRD), Scanning and Transmission Electron Microscopy (TEM) and Electron Back Scatter Diffraction (EBSD). On prolonged nitriding, Chromium-rich nitride precipitates were formed firstly close to the surface and later throughout the sample with austenitic structure. Chromium-rich nitride precipitates with a rod or strip-like morphology was developed by a discontinuous cellular precipitation mechanism. STEM-EDS analysis demonstrated partitioning of metallic elements between austenite and nitrides, with chromium contents of about 80 wt.% in the precipitates. XRD analysis indicated that the Chromium-rich nitride precipitates are hexagonal (Cr, Mo)2N. Based on the TEM studies, (Cr, Mo)2N precipitates presented a (1 1 1)γ//(0 0 2)(Cr, Mo)2N, ?γ//?(Cr, Mo)2N orientation relationship with respect to the austenite matrix. EBSD studies revealed that the austenite in the regions that have transformed into austenite and (Cr, Mo)2N have no orientation relation to the untransformed austenite.

Moessbauer spectroscopy study on the corrosion resistance of plasma nitrided ASTM F138 stainless steel in chloride solution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Souza, S.D. de; Olzon-Dionysio, M., E-mail: dmod@df.ufscar.br; Basso, R.L.O.

2010-10-15

Plasma nitriding of ASTM F138 stainless steel samples has been carried out using dc glow discharge under 80% H{sub 2}-20% N{sub 2} gas mixture, at 673 K, and 2, 4, and 7 h time intervals, in order to investigate the influence of treatment time on the microstructure and the corrosion resistance properties. The samples were characterized by scanning electron microscopy, glancing angle X-ray diffraction and conversion electron Moessbauer spectroscopy, besides electrochemical tests in NaCl aerated solution. A modified layer of about 6 {mu}m was observed for all the nitrided samples, independent of nitriding time. The X-ray diffraction analysis shows broadmore » {gamma}{sub N} phase peaks, signifying a great degree of nitrogen supersaturation. Besides {gamma}{sub N,} the Moessbauer spectroscopy results indicated the occurrence of {gamma}' and {epsilon} phases, as well as some other less important phases. Corrosion measurements demonstrate that the plasma nitriding time affects the corrosion resistance and the best performance is reached at 4 h treatment. It seems that the {epsilon}/{gamma}' fraction ratio plays an important role on the resistance corrosion. Additionally, the Moessbauer spectroscopy was decisive in this study, since it was able to identify and quantify the iron phases that influence the corrosion resistance of plasma nitrided ASTM F138 samples.« less

Origins of contrasting copper coordination geometries in crystalline copper sulfate pentahydrate.

PubMed

Ruggiero, Michael T; Erba, Alessandro; Orlando, Roberto; Korter, Timothy M

2015-12-14

Metal-aqua ion ([M(H2O)n](X+)) formation is a fundamental step in mechanisms that are central to enzymatic and industrial catalysis. Past investigations of such ions have yielded a wealth of information regarding their properties, however questions still exist involving the exact structures of these complexes. A prominent example of this is hexaaqua copper(II) ([Cu(H2O)6](2+)), with the solution versus gas-phase configurations under debate. The differences are often attributed to the intermolecular interactions between the bulk solvent and the aquated complex, resulting in structures stabilized by extended hydrogen-bonding networks. Yet solution phase systems are difficult to study due to the lack of atomic-level positional details. Crystalline solids are ideal models for comparative study, as they contain fixed structures that can be fully characterized using diffraction techniques. Here, crystalline copper sulfate pentahydrate (CuSO4·5H2O), which contains two unique copper-water geometries, was studied in order to elucidate the origin of these contrasting hydrated metal envrionments. A combination of solid-state density functional theory and low-temperature X-ray diffraction was used to probe the electronic origins of this phenomenon. This was accomplished through implementation of crystal orbital overlap population and crystal orbital Hamiltonian population analyses into a developmental version of the CRYSTAL14 software. These new computational methods help highlight the delicate interplay between electronic structure and metal-water geometries.

MOVPE growth of (GaIn)As/Ga(AsSb)/(GaIn)As type-II heterostructures on GaAs substrate for near infrared laser applications

NASA Astrophysics Data System (ADS)

Fuchs, C.; Beyer, A.; Volz, K.; Stolz, W.

2017-04-01

The growth of high quality (GaIn)As/Ga(AsSb)/(GaIn)As "W"-quantum well heterostructures is discussed with respect to their application in 1300 nm laser devices. The structures are grown using metal organic vapor phase epitaxy and characterized using high-resolution X-ray diffraction, scanning transmission electron microscopy and photoluminescence measurements. The agreement between experimental high-resolution X-ray diffraction patterns and full dynamical simulations is verified for these structurally challenging heterostructures. Scanning transmission electron microscopy is used to demonstrate that the structure consists of well-defined quantum wells and forms the basis for future improvements of the optoelectronic quality of this materials system. By altering the group-V gas phase ratio, it is possible to cover a large spectral range between 1200 nm and 1470 nm using a growth temperature of 550 °C and a V/III ratio of 7.5. A comparison of a sample with a photoluminescence emission wavelength at 1360 nm with single quantum well material reference samples proves the type-II character of the emission. A further optimization of these structures for application in 1300 nm lasers by applying different V/III ratios yields a stable behavior of the photoluminescence intensity using a growth temperature of 550 °C.

Metal oxide nanoparticle-modified graphene oxide for removal of elemental mercury.

PubMed

Liu, Yuxi; Chen, Gang; Tian, Chong; Gupta, Rajender; Wang, Xiaogang; Zeng, Hongbo

2018-06-05

Mercury is an extremely toxic element that is primarily released by anthropogenic activities and natural sources. Controlling Hg emissions, especially from coal combustion flue gas, is of practical importance in protecting the environment and preventing human health risks. In the present work, three metal oxides (MnO 2 , CuO, and ZnO) were loaded on graphene oxide (GO) sorbents (designated as MnO 2 -GO, CuO-GO, and ZnO-GO). All three adsorbents were successfully synthesized and were well characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The results indicated that the metal oxide nanoparticles (NPs) successfully decorated the GO. The elemental Hg adsorption capabilities of the three sorbents were subsequently evaluated using an in-house built setup for cold vapour atomic fluorescence spectrophotometry (CVAFS) with argon as the carrier gas for mercury detection. The testing temperature ranged from 50°C to 200°C at intervals of 50°C. MnO 2 -GO showed an excel lent Hg 0 adsorption capacity via chemisorption from 50 to 150°C and a mercury removal efficiency as high as 85% at 200°C, indicating that the MnO 2 -NP-modified GO is applicable for enhancing gas-phase elemental mercury removal. However, neither CuO-GO nor ZnO-GO performed well. This work provides useful insights into the development of novel sorbent materials for the elemental mercury removal from flue gases.

Hybrid SnO2/TiO2 Nanocomposites for Selective Detection of Ultra-Low Hydrogen Sulfide Concentrations in Complex Backgrounds

PubMed Central

Larin, Alexander; Womble, Phillip C.; Dobrokhotov, Vladimir

2016-01-01

In this paper, we present a chemiresistive metal oxide (MOX) sensor for detection of hydrogen sulfide. Compared to the previous reports, the overall sensor performance was improved in multiple characteristics, including: sensitivity, selectivity, stability, activation time, response time, recovery time, and activation temperature. The superior sensor performance was attributed to the utilization of hybrid SnO2/TiO2 oxides as interactive catalytic layers deposited using a magnetron radio frequency (RF) sputtering technique. The unique advantage of the RF sputtering for sensor fabrication is the ability to create ultra-thin films with precise control of geometry, morphology and chemical composition of the product of synthesis. Chemiresistive films down to several nanometers can be fabricated as sensing elements. The RF sputtering technique was found to be very robust for bilayer and multilayer oxide structure fabrication. The geometry, morphology, chemical composition and electronic structure of interactive layers were evaluated in relation to their gas sensing performance, using scanning electron microscopy (SEM), X-ray diffraction technique (XRD), atomic force microscopy (AFM), Energy Dispersive X-ray Spectroscopy (EDAX), UV visible spectroscopy, and Kelvin probe measurements. A sensor based on multilayer SnO2/TiO2 catalytic layer with 10% vol. content of TiO2 demonstrated the best gas sensing performance in all characteristics. Based on the pattern relating material’s characteristics to gas sensing performance, the optimization strategy for hydrogen sulfide sensor fabrication was suggested. PMID:27618900

Enhanced Ethanol Gas Sensing Properties of SnO2-Core/ZnO-Shell Nanostructures

PubMed Central

Tharsika, T.; Haseeb, A. S. M. A.; Akbar, Sheikh A.; Sabri, Mohd Faizul Mohd; Hoong, Wong Yew

2014-01-01

An inexpensive single-step carbon-assisted thermal evaporation method for the growth of SnO2-core/ZnO-shell nanostructures is described, and the ethanol sensing properties are presented. The structure and phases of the grown nanostructures are investigated by field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. XRD analysis indicates that the core-shell nanostructures have good crystallinity. At a lower growth duration of 15 min, only SnO2 nanowires with a rectangular cross-section are observed, while the ZnO shell is observed when the growth time is increased to 30 min. Core-shell hierarchical nanostructures are present for a growth time exceeding 60 min. The growth mechanism for SnO2-core/ZnO-shell nanowires and hierarchical nanostructures are also discussed. The sensitivity of the synthesized SnO2-core/ZnO-shell nanostructures towards ethanol sensing is investigated. Results show that the SnO2-core/ZnO-shell nanostructures deposited at 90 min exhibit enhanced sensitivity to ethanol. The sensitivity of SnO2-core/ZnO-shell nanostructures towards 20 ppm ethanol gas at 400 °C is about ∼5-times that of SnO2 nanowires. This improvement in ethanol gas response is attributed to high active sensing sites and the synergistic effect of the encapsulation of SnO2 by ZnO nanostructures. PMID:25116903

Large scale synthesis of α-Si3N4 nanowires through a kinetically favored chemical vapour deposition process

NASA Astrophysics Data System (ADS)

Liu, Haitao; Huang, Zhaohui; Zhang, Xiaoguang; Fang, Minghao; Liu, Yan-gai; Wu, Xiaowen; Min, Xin

2018-01-01

Understanding the kinetic barrier and driving force for crystal nucleation and growth is decisive for the synthesis of nanowires with controllable yield and morphology. In this research, we developed an effective reaction system to synthesize very large scale α-Si3N4 nanowires (hundreds of milligrams) and carried out a comparative study to characterize the kinetic influence of gas precursor supersaturation and liquid metal catalyst. The phase composition, morphology, microstructure and photoluminescence properties of the as-synthesized products were characterized by X-ray diffraction, fourier-transform infrared spectroscopy, field emission scanning electron microscopy, transmission electron microscopy and room temperature photoluminescence measurement. The yield of the products not only relates to the reaction temperature (thermodynamic condition) but also to the distribution of gas precursors (kinetic condition). As revealed in this research, by controlling the gas diffusion process, the yield of the nanowire products could be greatly improved. The experimental results indicate that the supersaturation is the dominant factor in the as-designed system rather than the catalyst. With excellent non-flammability and high thermal stability, the large scale α-Si3N4 products would have potential applications to the improvement of strength of high temperature ceramic composites. The photoluminescence spectrum of the α-Si3N4 shows a blue shift which could be valued for future applications in blue-green emitting devices. There is no doubt that the large scale products are the base of these applications.

Sprayed zinc oxide films: Ultra-violet light-induced reversible surface wettability and platinum-sensitization-assisted improved liquefied petroleum gas response.

PubMed

Nakate, Umesh T; Patil, Pramila; Bulakhe, R N; Lokhande, C D; Kale, Sangeeta N; Naushad, Mu; Mane, Rajaram S

2016-10-15

We report the rapid (superhydrophobic to superhydrophilic) transition property and improvement in the liquefied petroleum gas (LPG) sensing response of zinc oxide (ZnO) nanorods (NRs) on UV-irradiation and platinum (Pt) surface sensitization, respectively. The morphological evolution of ZnO NRs is evidenced from the field emission scanning electron microscope and atomic force microscope digital images and for the structural elucidation X-ray diffraction pattern is used. Elemental survey mapping is obtained from energy dispersive X-ray analysis spectrum. The optical properties have been studied by UV-Visible and photoluminescence spectroscopy measurements. The rapid (120sec) conversion of superhydrophobic (154°) ZnO NRs film to superhydrophilic (7°) is obtained under UV light illumination and the superhydrophobicity is regained by storing sample in dark. The mechanism for switching wettability behavior of ZnO NRs has thoroughly been discussed. In second phase, Pt-sensitized ZnO NRs film has demonstrated considerable gas sensitivity at 260ppm concentration of LPG. At 623K operating temperature, the maximum LPG response of 58% and the response time of 49sec for 1040ppm LPG concentration of Pt- sensitized ZnO NRs film are obtained. This higher LPG response of Pt-sensitized ZnO NRs film over pristine is primarily due to electronic effect and catalytic effect (spill-over effect) caused by an additional of Pt on ZnO NRs film surface. Copyright © 2016 Elsevier Inc. All rights reserved.

Direct Measurement of Polarization-Induced Fields in GaN/AlN by Nano-Beam Electron Diffraction

NASA Astrophysics Data System (ADS)

Carvalho, Daniel; Müller-Caspary, Knut; Schowalter, Marco; Grieb, Tim; Mehrtens, Thorsten; Rosenauer, Andreas; Ben, Teresa; García, Rafael; Redondo-Cubero, Andrés; Lorenz, Katharina; Daudin, Bruno; Morales, Francisco M.

2016-06-01

The built-in piezoelectric fields in group III-nitrides can act as road blocks on the way to maximizing the efficiency of opto-electronic devices. In order to overcome this limitation, a proper characterization of these fields is necessary. In this work nano-beam electron diffraction in scanning transmission electron microscopy mode has been used to simultaneously measure the strain state and the induced piezoelectric fields in a GaN/AlN multiple quantum well system.

Orientation and phase mapping in the transmission electron microscope using precession-assisted diffraction spot recognition: state-of-the-art results.

PubMed

Viladot, D; Véron, M; Gemmi, M; Peiró, F; Portillo, J; Estradé, S; Mendoza, J; Llorca-Isern, N; Nicolopoulos, S

2013-10-01

A recently developed technique based on the transmission electron microscope, which makes use of electron beam precession together with spot diffraction pattern recognition now offers the possibility to acquire reliable orientation/phase maps with a spatial resolution down to 2 nm on a field emission gun transmission electron microscope. The technique may be described as precession-assisted crystal orientation mapping in the transmission electron microscope, precession-assisted crystal orientation mapping technique-transmission electron microscope, also known by its product name, ASTAR, and consists in scanning the precessed electron beam in nanoprobe mode over the specimen area, thus producing a collection of precession electron diffraction spot patterns, to be thereafter indexed automatically through template matching. We present a review on several application examples relative to the characterization of microstructure/microtexture of nanocrystalline metals, ceramics, nanoparticles, minerals and organics. The strengths and limitations of the technique are also discussed using several application examples. ©2013 The Authors. Journal of Microscopy published by John Wiley & Sons Ltd on behalf of Royal Microscopical Society.

Use of reciprocal lattice layer spacing in electron backscatter diffraction pattern analysis

PubMed

Michael; Eades

2000-03-01

In the scanning electron microscope using electron backscattered diffraction, it is possible to measure the spacing of the layers in the reciprocal lattice. These values are of great use in confirming the identification of phases. The technique derives the layer spacing from the higher-order Laue zone rings which appear in patterns from many materials. The method adapts results from convergent-beam electron diffraction in the transmission electron microscope. For many materials the measured layer spacing compares well with the calculated layer spacing. A noted exception is for higher atomic number materials. In these cases an extrapolation procedure is described that requires layer spacing measurements at a range of accelerating voltages. This procedure is shown to improve the accuracy of the technique significantly. The application of layer spacing measurements in EBSD is shown to be of use for the analysis of two polytypes of SiC.

Characterization of calcium crystals in Abelia using x-ray diffraction and electron microscopes

USDA-ARS?s Scientific Manuscript database

Localization, chemical composition, and morphology of calcium crystals in leaves and stems of Abelia mosanensis and A. ×grandiflora were analyzed with a variable pressure scanning electron microscope (VP-SEM) equipped with an X-ray diffraction system, low temperature SEM (LT-SEM) and a transmission ...

Development of Thin Films as Potential Structural Cathodes to Enable Multifunctional Energy-Storage Structural Composite Batteries for the U.S. Army’s Future Force

DTIC Science & Technology

2011-09-01

glancing angle X - ray diffraction (GAXRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), and electrochemical...Emission SEM FWHM full width at half maximum GAXRD glancing angle X - ray diffraction H3COCH2CH2OH 2-methoxyethanol LiMn2O4 lithium manganese oxide...were characterized by scanning electron microscopy (SEM), X - ray diffraction (XRD), and atomic force microscopy (AFM). In addition,

Multiple defocused coherent diffraction imaging: method for simultaneously reconstructing objects and probe using X-ray free-electron lasers.

PubMed

Hirose, Makoto; Shimomura, Kei; Suzuki, Akihiro; Burdet, Nicolas; Takahashi, Yukio

2016-05-30

The sample size must be less than the diffraction-limited focal spot size of the incident beam in single-shot coherent X-ray diffraction imaging (CXDI) based on a diffract-before-destruction scheme using X-ray free electron lasers (XFELs). This is currently a major limitation preventing its wider applications. We here propose multiple defocused CXDI, in which isolated objects are sequentially illuminated with a divergent beam larger than the objects and the coherent diffraction pattern of each object is recorded. This method can simultaneously reconstruct both objects and a probe from the coherent X-ray diffraction patterns without any a priori knowledge. We performed a computer simulation of the prposed method and then successfully demonstrated it in a proof-of-principle experiment at SPring-8. The prposed method allows us to not only observe broad samples but also characterize focused XFEL beams.

Kinetic studies of methane-ethane mixed gas hydrates by neutron diffraction and Raman spectroscopy.

PubMed

Murshed, M Mangir; Kuhs, Werner F

2009-04-16

In situ formations of CH(4)-C(2)H(6) mixed gas hydrates were made using high flux neutron diffraction at 270 K and 5 MPa. For this purpose, a feed gas composition of CH(4) and C(2)H(6) (95 mol% CH(4)) was employed. The rates of transformation of spherical grains of deuterated ice Ih into hydrates were measured by time-resolved neutron powder diffraction on D20 at ILL, Grenoble. Phase fractions of the crystalline constituents were obtained from Rietveld refinements. A concomitant formation of structure type I (sI) and structure type II (sII) hydrates were observed soon after the gas pressure was applied. The initial fast formation of sII hydrate reached its maximum volume and started declining very slowly. The formation of sI hydrate followed a sigmoid growth kinetics that slowed down due to diffusion limitation. This observation has been interpreted in terms of a kinetically favored nucleation of the sII hydrate along with a slow transformation into sI. Both powder diffraction and Raman spectroscopic results suggest that a C(2)H(6)-rich sII hydrate was formed at the early part of the clathration, which slowly decreased to approximately 3% after a reaction of 158 days as confirmed by synchrotron XRD. The final persistence of a small portion of sII hydrate points to a miscibility gap between CH(4)-rich sI and C(2)H(6)-rich sII hydrates.

Electron-spectroscopy and -diffraction study of the conductivity of CVD diamond ( 0 0 1 )2×1 surface

NASA Astrophysics Data System (ADS)

Kono, S.; Takano, T.; Shimomura, M.; Goto, T.; Sato, K.; Abukawa, T.; Tachiki, M.; Kawarada, H.

2003-04-01

A chemical vapor deposition as-grown diamond (0 0 1) single-domain 2 × 1 surface was studied by electron-spectroscopy and electron-diffraction in ultrahigh vacuum (UHV). In order to change the surface conductivity (SC) of the diamond in UHV, three annealing stages were used; without annealing, annealing at 300 °C and annealing at 550 °C. From low energy electron diffraction and X-ray photoelectron spectroscopic (XPS) studies, an existence of SC was suggested for the first two stages of annealing and an absence of SC was suggested for the last stage of annealing. Changes in C KVV Auger electron spectroscopic spectra, C KVV Auger electron diffraction (AED) patterns and C 1s XPS peak positions were noticed between the annealing stages at 300 and 550 °C. These changes are interpreted as such that the state of hydrogen involvement in a subsurface of diamond (0 0 1)2 × 1 changes as SC changes. In particular, the presence of local disorder in diamond configuration in SC subsurface is pointed out from C KVV AED. From C 1s XPS peak shifts, a lower bound for the Fermi-level for SC layers from the valence band top is presented to be ˜0.5 eV.

Cr2O3 nanoparticle-functionalized WO3 nanorods for ethanol gas sensors

NASA Astrophysics Data System (ADS)

Choi, Seungbok; Bonyani, Maryam; Sun, Gun-Joo; Lee, Jae Kyung; Hyun, Soong Keun; Lee, Chongmu

2018-02-01

Pristine WO3 nanorods and Cr2O3-functionalized WO3 nanorods were synthesized by the thermal evaporation of WO3 powder in an oxidizing atmosphere, followed by spin-coating of the nanowires with Cr2O3 nanoparticles and thermal annealing in an oxidizing atmosphere. Scanning electron microscopy was used to examine the morphological features and X-ray diffraction was used to study the crystallinity and phase formation of the synthesized nanorods. Gas sensing tests were performed at different temperatures in the presence of test gases (ethanol, acetone, CO, benzene and toluene). The Cr2O3-functionalized WO3 nanorods sensor showed a stronger response to these gases relative to the pristine WO3 nanorod sensor. In particular, the response of the Cr2O3-functionalized WO3 nanorods sensor to 200 ppm ethanol gas was 5.58, which is approximately 4.4 times higher that of the pristine WO3 nanorods sensor. Furthermore, the Cr2O3-functionalized WO3 nanorods sensor had a shorter response and recovery time. The pristine WO3 nanorods had no selectivity toward ethanol gas, whereas the Cr2O3-functionalized WO3 nanorods sensor showed good selectivity toward ethanol. The gas sensing mechanism of the Cr2O3-functionalized WO3 nanorods sensor toward ethanol is discussed in detail.

A new life for the wavelength-dispersive X-ray spectrometer (WDS): incorporation of a silicon drift detector into the WDS for improved quantification and X-ray mapping

NASA Astrophysics Data System (ADS)

Wuhrer, R.; Moran, K.

2018-01-01

The wavelength-dispersive X-ray spectrometer (WDS) has been around for a long time and the design has not changed much since its original development. The electron microprobe operator using WDS has to be meticulous in monitoring items such as gas flow, gas purity, gas pressure, noise levels of baseline and window, gas flow proportional counter (GFPC) voltage levels, count rate suppression, anode wire contamination and other detector parameters. Recent development and improvements of silicon drift detectors (SDD’s) has allowed the incorporation of a SDD as the X-ray detector in place of the proportional counter (PC) and/or gas flow proportional counter (GFPC). This allows minimal mechanical alteration and no loss of movement range. The superiority of a WDS with a SDD, referred to as SD-WDS, is easily seen once in operation. The SD-WDS removes many artefacts including the worse of all high order diffraction, thus allowing more accurate analysis. The incorporation of the SDD has been found to improve the light and mid element range and consequently improving the detection limit for these elements. It is also possible to obtain much more reliable results at high count rates with almost no change in resolution, gain and zero-peak characteristics of the energy spectrum.

Two-Dimensional Light Diffraction from an EPROM Chip

ERIC Educational Resources Information Center

Ekkens, Tom

2018-01-01

In introductory physics classes, a laser pointer and a compact disc are all the items required to illustrate diffraction of light in a single dimension. If a two-dimensional diffraction pattern is desired, double axis diffraction grating material is available or a CCD sensor can be extracted from an unused electronics device. This article presents…

Vanadium As a Potential Membrane Material for Carbon Capture: Effects of Minor Flue Gas Species.

PubMed

Yuan, Mengyao; Liguori, Simona; Lee, Kyoungjin; Van Campen, Douglas G; Toney, Michael F; Wilcox, Jennifer

2017-10-03

Vanadium and its surface oxides were studied as a potential nitrogen-selective membrane material for indirect carbon capture from coal or natural gas power plants. The effects of minor flue gas components (SO 2 , NO, NO 2 , H 2 O, and O 2 ) on vanadium at 500-600 °C were investigated by thermochemical exposure in combination with X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and in situ X-ray diffraction (XRD). The results showed that SO 2 , NO, and NO 2 are unlikely to have adsorbed on the surface vanadium oxides at 600 °C after exposure for up to 10 h, although NO and NO 2 may have exhibited oxidizing effects (e.g., exposure to 250 ppmv NO/N 2 resulted in an 2.4 times increase in surface V 2 O 5 compared to exposure to just N 2 ). We hypothesize that decomposition of surface vanadium oxides and diffusion of surface oxygen into the metal bulk are both important mechanisms affecting the composition and morphology of the vanadium membrane. The results and hypothesis suggest that the carbon capture performance of the vanadium membrane can potentially be strengthened by material and process improvements such as alloying, operating temperature reduction, and flue gas treatment.

(18)O(2) label mechanism of sulfur generation and characterization in properties over mesoporous Sm-based sorbents for hot coal gas desulfurization.

PubMed

Liu, B S; Wan, Z Y; Wang, F; Zhan, Y P; Tian, M; Cheung, A S C

2014-02-28

Using a sol-gel method, SmMeOx/MCM-41 or SBA-15 (Me=Fe, Co and Zn) and corresponding unsupported sorbents were prepared. The desulfurization performance of these sorbents was evaluated over a fixed-bed reactor and the effects of reaction temperature, feed and sorbent composition on desulfurization performance were studied. Samarium-based sorbents used to remove H2S from hot coal gas were reported for the first time. The results of successive sulfidation/regeneration cycles revealed that SmFeO3/SBA-15 sorbent was suitable for desulfurization of hot coal gas in the chemical industry. The formation of elemental sulfur during both sulfidation and regeneration processes depended strongly on the catalytic action of Sm2O2S species, which was confirmed for the first time via high sensitive time of flight mass spectrometer (TOF-MS) using 6%vol(18)O2/Ar regeneration gas and can reduce markedly procedural complexity. The sorbents were characterized using N2-adsorption, high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), temperature-programmed reduction of H2 (H2-TPR), thermogravimetry (TG) and time-of-flight mass spectrometry (TOF-MS) techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

Characterization of X80 and X100 Microalloyed Pipeline Steel Using Quantitative X-ray Diffraction

NASA Astrophysics Data System (ADS)

Wiskel, J. B.; Li, X.; Ivey, D. G.; Henein, H.

2018-06-01

Quantitative X-ray diffraction characterization of four (4) X80 and three (3) X100 microalloyed steels was undertaken. The effect of through-thickness position, processing parameters, and composition on the measured crystallite size, microstrain, and J index (relative magnitude of crystallographic texture) was determined. Microstructure analysis using optical microscopy, scanning electron microscopy, transmission electron microscopy, and electron-backscattered diffraction was also undertaken. The measured value of microstrain increased with increasing alloy content and decreasing cooling interrupt temperature. Microstructural features corresponding to crystallite size in the X80 steels were both above and below the detection limit for quantitative X-ray diffraction. The X100 steels consistently exhibited microstructure features below the crystallite size detection limit. The yield stress of each steel increased with increasing microstrain. The increase in microstrain from X80 to X100 is also associated with a change in microstructure from predominantly polygonal ferrite to bainitic ferrite.

Mapping of reciprocal space of La{sub 0.30}CoO{sub 2} in 3D: Analysis of superstructure diffractions and intergrowths with Co{sub 3}O{sub 4}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brázda, Petr, E-mail: brazda@fzu.cz; Palatinus, Lukáš; Klementová, Mariana

2015-07-15

We have used electron diffraction tomography and powder X-ray diffraction to elucidate the structural properties of layered cobaltate γ-La{sub 0.30}CoO{sub 2}. The structure consists of hexagonal sheets of edge-sharing CoO{sub 6} octahedra interleaved by lanthanum monolayers. The La{sup 3+} cations occupy only one third of available P2 sites, forming a 2-dimensional a√3×a√3 superstructure in a–b plane. The results show that there exists no order in the mutual relative shift between the neighbouring La interlayers within the a–b plane. This is manifested in the observed monotonous decrease of the diffracted intensity of the superstructure diffractions along c{sup ⁎} in both X-raymore » and electron diffraction data. The observed lack of stacking order differentiates the La{sub x}CoO{sub 2} from its Ca and Sr analogues where at least a partial stacking order of the cationic interlayers is manifested in experimental data published in literature. - Highlights: • We use electron diffraction tomography for reciprocal space mapping of La{sub 0.30}CoO{sub 2}. • We observed a complete disorder of the stacking of Lanthanum interlayers. • Co{sub 3}O{sub 4} intergrown with La{sub 0.30}CoO{sub 2} crystals brings about fake superstructure diffractions. • Twinning of Co{sub 3}O{sub 4} enhances the problem of fake superstructure diffractions.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Hongfen, E-mail: wanghongfen11@163.com; Wang, Zhiqi; Chen, Shougang

Molybdenum carbides with surfactants as carbon sources were prepared using the carbothermal reduction of the appropriate precursors (molybdenum oxides deposited on surfactant micelles) at 1023 K under hydrogen gas. The carburized products were characterized using scanning electron microscopy (SEM), X-ray diffraction and BET surface area measurements. From the SEM images, hollow microspherical and rod-like molybdenum carbides were observed. X-ray diffraction patterns showed that the annealing time of carburization had a large effect on the conversion of molybdenum oxides to molybdenum carbides. And BET surface area measurements indicated that the difference of carbon sources brought a big difference in specific surfacemore » areas of molybdenum carbides. - Graphical abstract: Molybdenum carbides having hollow microspherical and hollow rod-like morphologies that are different from the conventional monodipersed platelet-like morphologies. Highlights: Black-Right-Pointing-Pointer Molybdenum carbides were prepared using surfactants as carbon sources. Black-Right-Pointing-Pointer The kinds of surfactants affected the morphologies of molybdenum carbides. Black-Right-Pointing-Pointer The time of heat preservation at 1023 K affected the carburization process. Black-Right-Pointing-Pointer Molybdenum carbides with hollow structures had larger specific surface areas.« less

Three-dimensional rotation electron diffraction: software RED for automated data collection and data processing

PubMed Central

Wan, Wei; Sun, Junliang; Su, Jie; Hovmöller, Sven; Zou, Xiaodong

2013-01-01

Implementation of a computer program package for automated collection and processing of rotation electron diffraction (RED) data is described. The software package contains two computer programs: RED data collection and RED data processing. The RED data collection program controls the transmission electron microscope and the camera. Electron beam tilts at a fine step (0.05–0.20°) are combined with goniometer tilts at a coarse step (2.0–3.0°) around a common tilt axis, which allows a fine relative tilt to be achieved between the electron beam and the crystal in a large tilt range. An electron diffraction (ED) frame is collected at each combination of beam tilt and goniometer tilt. The RED data processing program processes three-dimensional ED data generated by the RED data collection program or by other approaches. It includes shift correction of the ED frames, peak hunting for diffraction spots in individual ED frames and identification of these diffraction spots as reflections in three dimensions. Unit-cell parameters are determined from the positions of reflections in three-dimensional reciprocal space. All reflections are indexed, and finally a list with hkl indices and intensities is output. The data processing program also includes a visualizer to view and analyse three-dimensional reciprocal lattices reconstructed from the ED frames. Details of the implementation are described. Data collection and data processing with the software RED are demonstrated using a calcined zeolite sample, silicalite-1. The structure of the calcined silicalite-1, with 72 unique atoms, could be solved from the RED data by routine direct methods. PMID:24282334

Three-dimensional rotation electron diffraction: software RED for automated data collection and data processing.

PubMed

Wan, Wei; Sun, Junliang; Su, Jie; Hovmöller, Sven; Zou, Xiaodong

2013-12-01

Implementation of a computer program package for automated collection and processing of rotation electron diffraction (RED) data is described. The software package contains two computer programs: RED data collection and RED data processing. The RED data collection program controls the transmission electron microscope and the camera. Electron beam tilts at a fine step (0.05-0.20°) are combined with goniometer tilts at a coarse step (2.0-3.0°) around a common tilt axis, which allows a fine relative tilt to be achieved between the electron beam and the crystal in a large tilt range. An electron diffraction (ED) frame is collected at each combination of beam tilt and goniometer tilt. The RED data processing program processes three-dimensional ED data generated by the RED data collection program or by other approaches. It includes shift correction of the ED frames, peak hunting for diffraction spots in individual ED frames and identification of these diffraction spots as reflections in three dimensions. Unit-cell parameters are determined from the positions of reflections in three-dimensional reciprocal space. All reflections are indexed, and finally a list with hkl indices and intensities is output. The data processing program also includes a visualizer to view and analyse three-dimensional reciprocal lattices reconstructed from the ED frames. Details of the implementation are described. Data collection and data processing with the software RED are demonstrated using a calcined zeolite sample, silicalite-1. The structure of the calcined silicalite-1, with 72 unique atoms, could be solved from the RED data by routine direct methods.

Enhanced photocatalytic hydrogen production from water-ethanol solution by Ruthenium doped La-NaTaO3

NASA Astrophysics Data System (ADS)

Husin, H.; Alam, P. N.; Zaki, M.; Sofyana; Jakfar; Husaini; Hasfita, F.

2018-04-01

The photocatalytic hydrogen production from ethanol aqueous solution, with the use ruthenium doped La-NaTaO3 has been investigated. Ruthenium doped La-NaTaO3 catalysts are prepared by impregnation method. The catalysts are by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The Ru co-catalyst demonstrated from the TEM image shows a good dispersion on the surface of La-C-NaTaO3 with an average particle size between 4-5 nm. The photocatalytic reaction is carried out in a closed reactor with a gas circulation system. The catalytic activity of La-NaTaO3 improved markedly (6.6 times from pure water) when Ru is loaded onto its surface. The hydrogen production is notably enhanced in the presence of ethanol as electron donors. This result is much higher when compared with the rate of hydrogen production in the sample without co- catalysts about 9.4 times higher after Ru deposition from ethanol aqueous solution. Increasing the production of hydrogen on the Ru/La-NaTaO3 closely related to the decrease in recombination between electron-hole pairs.

Study of residual stresses in CT test specimens welded by electron beam

NASA Astrophysics Data System (ADS)

Papushkin, I. V.; Kaisheva, D.; Bokuchava, G. D.; Angelov, V.; Petrov, P.

2018-03-01

The paper reports result of residual stress distribution studies in CT specimens reconstituted by electron beam welding (EBW). The main aim of the study is evaluation of the applicability of the welding technique for CT specimens’ reconstitution. Thus, the temperature distribution during electron beam welding of a CT specimen was calculated using Green’s functions and the residual stress distribution was determined experimentally using neutron diffraction. Time-of-flight neutron diffraction experiments were performed on a Fourier stress diffractometer at the IBR-2 fast pulsed reactor in FLNP JINR (Dubna, Russia). The neutron diffraction data estimates yielded a maximal stress level of ±180 MPa in the welded joint.

In-situ TEM investigations of graphic-epitaxy and small particles

NASA Technical Reports Server (NTRS)

Heinemann, K.

1983-01-01

Palladium was deposited inside a controlled-vacuum specimen chamber of a transmission electron microscope (TEM) onto MgO and alpha-alumina substrate surfaces. Annealing and various effects of gas exposure of the particulate Pd deposits were studied in-situ by high resolution TEM and electron diffraction. Whereas substrate temperatures of 500 C or annealing of room temperature (RT) deposits to 500 C were needed to obtain epitaxy on sapphire, RT deposits on MgO were perfectly epitaxial. For Pd/MgO a lattice expansion of 2 to 4% was noted; the highest values of expansion were found for the smallest particles. The lattice expansion of small Pd particles on alumina substrates was less than 1%. Long-time RT exposure of Pd/MgO in a vacuum yielded some moblity and coalescence events, but notably fewer than for Pd on sapphire. Exposure to air or oxygen greatly enhanced the particle mobility and coalescence and also resulted in the flattening of Pd particles on MgO substrates. Electron-beam irradiation further enhanced this effect. Exposure to air for several tens of hours of Pd/MgO led to strong coalescence.

Geometry of phase-separated domains in phospholipid bilayers by diffraction-contrast electron microscopy.

PubMed Central

Hui, S W

1981-01-01

The sizes and shapes of solidus (gel) phase domains in the hydrated molecular bilayers of dilauroylphosphatidylcholine/dipalmitoylphasphatidylcholine (DLPC/DPPC) (1:1) and phosphatidylserine (PS)/DPPC (1:2) are visualized directly by low dose diffraction-contrast electron microscopy. The temperature and humidity of the bilayers are controlled by an environmental chamber set in an electron microscope. The contrast between crystalline domains is enhanced by electron optical filtering of the diffraction patterns of the bilayers. The domains are seen as a patchwork in the plane of the bilayer, with an average width of 0.2-0.5 micrometer. The percentage of solidus area measured from diffraction-contrast micrographs at various temperatures agrees in general with those depicted by known phase diagrams. The shape and size of the domains resemble those seen by freeze-fracture in multilamellar vesicles. Temperature-related changes in domain size and in phase boundary per unit area are more pronounced in the less miscible DLPC/DPPC mixture. No significant change in these geometric parameters with temperature is found in the PS/DPPC mixture. Mapping domains by their molecular diffraction signals not only verifies the existance of areas of different molecular packing during phase separation but also provides a quantitative measurement of structural boundaries and defects in lipid bilayers. Images FIGURE 1 FIGURE 3 FIGURE 6 PMID:6894707

The synthesis of multifunctional porous honey comb-like La2O3 thin film for supercapacitor and gas sensor applications.

PubMed

Yadav, A A; Lokhande, A C; Pujari, R B; Kim, J H; Lokhande, C D

2016-12-15

The porous honey comb-like La 2 O 3 thin films have been synthesized using one step spray pyrolysis method. The influence of sprayed solution quantity on properties of La 2 O 3 thin films is studied using X-ray diffraction, Fourier transform spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, optical absorption and Brunauer-Emmett-Teller techniques. Morphology of La 2 O 3 electrode is controlled with sprayed solution quantity. The supercapacitive properties of La 2 O 3 thin film electrode are investigated using cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance techniques. The La 2 O 3 film electrode exhibited the specific capacitance of the 166Fg -1 with 85% stability for the 3000 cycles. The La 2 O 3 film electrode exhibited sensitivity of 68 at 523K for 500ppm CO 2 gas concentration. The possible CO 2 sensing mechanism is discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

Microstructure and thermal conductivity of surfactant-free NiO nanostructures

NASA Astrophysics Data System (ADS)

Sahoo, Pranati; Misra, Dinesh K.; Salvador, Jim; Makongo, Julien P. A.; Chaubey, Girija S.; Takas, Nathan J.; Wiley, John B.; Poudeu, Pierre F. P.

2012-06-01

High purity, nanometer sized surfactant-free nickel oxide (NiO) particles were produced in gram scale using a solution combustion method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), gas pycnometry and gas adsorption analysis (BET). The average particle size of the as-synthesized NiO increases significantly with the preheating temperature of the furnace, while the specific surface area decreases. A BET specific surface area of ∼100 m2/g was obtained for NiO nanoparticles with size as small as 3 nm synthesized at 300 °C. The thermal conductivity (κ) of pressed pellets of the synthesized NiO nanoparticles obtained using spark plasma sintering (SPS) and uniaxial hot pressing is drastically decreased (∼60%) compared to that of NiO single crystal. This strong reduction in κ with particle size suggests the suitability of the synthesized surfactant-free NiO nanoparticles for use as nanoinclusions when designing high performance materials for waste heat recovery.

Carbon Nanotubes Blended Hydroxyapatite Ethanol Sensor

NASA Astrophysics Data System (ADS)

Anjum, S. R.; Khairnar, R. S.

2016-12-01

Nano crystals of Hydroxyapatite (HAp) were synthesized by a wet chemical precipitation method. The nano composite materials were developed by doping various weight concentrations of carbon nanotubes in HAp, followed by characterization using scanning electron microscopy, and X-ray diffraction. Thick films of these materials were prepared by using screen printing technique. The ethanol sensing properties of these nano crystals and nano composite films were investigated by two probe electrical method. The gas sensing features such as operating temperature, response and recovery time, maximum gas detection limit, etc. were studied, since these parameters are of prime importance for sensor. The results revealed that at room temperature, the composite materials exhibited improved sensing performance towards 100 ppm ethanol with fast response times. It also showed shorter recovery time with higher vapor uptake capacity. The ethanol adsorption processes on doped and undoped substrates can be explained by surface chemical reactions as well as providing the possible adsorption models. The novelty of this work lies in developing reusable sensor substrates for room temperature sensing.

Cyclic oxidation behavior of plasma sprayed NiCrAlY/WC-Co/cenosphere coating

NASA Astrophysics Data System (ADS)

Mathapati, Mahantayya; Ramesh M., R.; Doddamani, Mrityunjay

2018-04-01

Components working at elevated temperature like boiler tubes of coal and gas fired power generation plants, blades of gas and steam turbines etc. experience degradation owing to oxidation. Oxidation resistance of such components can be increased by developing protective coatings. In the present investigation NiCrAlY-WC-Co/Cenosphere coating is deposited on MDN 321 steel substrate using plasma spray coating. Thermo cyclic oxidation behavior of coating and substrate is studied in static air at 600 °C for 20 cycles. The thermo gravimetric technique is used to approximate the kinetics of oxidation. X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy (EDS) and X-ray mapping techniques are used to characterize the oxidized samples. NiCrAlY-WC-Co/Cenosphere coating exhibited lower oxidation rate in comparison to MDN 321 steel substrate. The lower oxidation rate of coating is attributed to formation of Al2O3, Cr2O3, NiO and CoWO4 oxides on the outermost surface.

Nanocrystalline Pd:NiFe2O4 thin films: A selective ethanol gas sensor

NASA Astrophysics Data System (ADS)

Rao, Pratibha; Godbole, R. V.; Bhagwat, Sunita

2016-10-01

In this work, Pd:NiFe2O4 thin films were investigated for the detection of reducing gases. These films were fabricated using spray pyrolysis technique and characterized using X-ray diffraction (XRD) to confirm the crystal structure. The surface morphology was studied using scanning electron microscopy (SEM). Magnetization measurements were carried out using SQUID VSM, which shows ferrimagnetic behavior of the samples. These thin film sensors were tested against methanol, ethanol, hydrogen sulfide and liquid petroleum gas, where they were found to be more selective to ethanol. The fabricated thin film sensors exhibited linear response signal for all the gases with concentrations up to 5 w/o Pd. Reduction in optimum operating temperature and enhancement in response was also observed. Pd:NiFe2O4 thin films exhibited faster response and recovery characteristic. These sensors have potential for industrial applications because of their long-term stability, low power requirement and low production cost.

Comparative characteristic and erosion behavior of NiCr coatings deposited by various high-velocity oxyfuel spray processes

NASA Astrophysics Data System (ADS)

Sidhu, Hazoor Singh; Sidhu, Buta Singh; Prakash, S.

2006-12-01

The purpose of this study is to analyze and compare the mechanical properties and microstructure details at the interface of high-velocity oxyfuel (HVOF)-sprayed NiCr-coated boiler tube steels, namely ASTM-SA-210 grade A1, ASTM-SA213-T-11, and ASTM-SA213-T-22. Coatings were developed by two different techniques, and in these techniques liquefied petroleum gas was used as the fuel gas. First, the coatings were characterized by metallographic, scanning electron microscopy/energy-dispersive x-ray analysis, x-ray diffraction, surface roughness, and microhardness, and then were subjected to erosion testing. An attempt has been made to describe the transformations taking place during thermal spraying. It is concluded that the HVOF wire spraying process offers a technically viable and cost-effective alternative to HVOF powder spraying process for applications in an energy generation power plant with a point view of life enhancement and to minimize the tube failures because it gives a coating having better resistance to erosion.

Synthesis of ZnO nanopencils using wet chemical method and its investigation as LPG sensor

NASA Astrophysics Data System (ADS)

Shimpi, Navinchandra G.; Jain, Shilpa; Karmakar, Narayan; Shah, Akshara; Kothari, D. C.; Mishra, Satyendra

2016-12-01

ZnO nanopencils (NPCs) were prepared by a novel wet chemical process, using triethanolamine (TEA) as a mild base, which is relatively simple and cost effective method as compared to hydrothermal method. ZnO NPCs were characterized using powder X-ray diffraction (XRD), Fourier Transform Infra-Red (FTIR) spectroscopy in mid-IR and far-IR regions, X-ray Photoelectron Spectroscopy (XPS), UV-vis (UV-vis) absorption spectroscopy, room temperature Photoluminescence (PL) spectroscopy and Field Emission Scanning Electron Microscopy (FESEM). ZnO NPCs obtained, were highly pure, uniform and monodispersed.XRD pattern indicated hexagonal unit cell structure with preferred orientation along the c-axis. Sensing behaviour of ZnO NPCs was studied towards Liquefied Petroleum Gas (LPG) at different operating temperatures. The study shows that ZnO NPCs were most sensitive and promising candidate for detection of LPG at 250 °C with gas sensitivity > 60%. The high response towards LPG is due to high surface area of ZnO NPCs and their parallel alignment.

Effect of CO2 partial pressure and different CO2 phases on carbon steel corrosion

NASA Astrophysics Data System (ADS)

Mahlobo, MGR; Premlall, K.; Olubambi, PA

2017-12-01

Carbon capture and storage (CCS) is the recent promising technology aimed at reducing greenhouse gas emission. Like many other developed technologies, CCS is faced with great challenges such as pipeline transportation failure due to corrosion. There are many factors contributing to steel corrosion during the pipeline transportation of carbon dioxide (CO2). This study focuses on CO2 partial pressure and different phases of CO2 as some of the factors contributing to steel corrosion. Carbon steel was used as a testing specimen. High pressure reactor was used in this study to compress CO2 from low to high pressures ultimately changing the CO2 from gaseous phase to gas/liquid phase (subcritical) and to dense phase (supercritical). Weight loss method was employed to determine the corrosion rate while scanning electron microscopy (SEM) and X-Ray diffraction (XRD) were used to study the carbon steel morphology and phase analysis. Using low magnification digital camera, the type of corrosion that took place on the carbon steel surface was identified.

Fabrication and characterization of nano-gas sensor arrays

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hassan, H. S., E-mail: hassan.shokry@gmail.com; Kashyout, A. B., E-mail: hady8@yahoo.com; Morsi, I., E-mail: drimanmorsi@yahoo.com

2015-03-30

A novel structures of Nanomaterials gas sensors array constructed using ZnO, and ZnO doped with Al via sol-gel technique. Two structure arrays are developed; the first one is a double sensor array based on doping with percentages of 1% and 5%. The second is a quadrature sensor array based on several doping ratios concentrations (0%, 1%, 5% and 10%). The morphological structures of prepared ZnO were revealed using scanning electron microscope (SEM). X-ray diffraction (XRD) patterns reveal a highly crystallized wurtzite structure and used for identifying phase structure and chemical state of both ZnO and ZnO doped with Al undermore » different preparation conditions and different doping ratios. Chemical composition of Al-doped ZnO nanopowders was performed using energy dispersive x-ray (EDS) analysis. The electrical characteristics of the sensor are determined by measuring the two terminal sensor’s output resistance for O{sub 2}, H{sub 2} and CO{sub 2} gases as a function of temperature.« less

Synthesis of ZnMn₂O₄ Nanoparticles by a Microwave-Assisted Colloidal Method and their Evaluation as a Gas Sensor of Propane and Carbon Monoxide.

PubMed

Morán-Lázaro, Juan Pablo; Guillen-López, Erwin Said; López-Urias, Florentino; Muñoz-Sandoval, Emilio; Blanco-Alonso, Oscar; Guillén-Bonilla, Héctor; Guillén-Bonilla, Alex; Rodríguez-Betancourtt, Verónica María; Sanchez-Tizapa, Marciano; Olvera-Amador, María de la Luz

2018-02-27

Spinel-type ZnMn₂O₄ nanoparticles were synthesized via a simple and inexpensive microwave-assisted colloidal route. Structural studies by X-ray diffraction showed that a spinel crystal phase of ZnMn₂O₄ was obtained at a calcination temperature of 500 °C, which was confirmed by Raman and UV-vis characterizations. Spinel-type ZnMn₂O₄ nanoparticles with a size of 41 nm were identified by transmission electron microscopy. Pellet-type sensors were fabricated using ZnMn₂O₄ nanoparticles as sensing material. Sensing measurements were performed by exposing the sensor to different concentrations of propane or carbon monoxide at temperatures in the range from 100 to 300 °C. Measurements performed at an operating temperature of 300 °C revealed a good response to 500 ppm of propane and 300 ppm of carbon monoxide. Hence, ZnMn₂O₄ nanoparticles possess a promising potential in the gas sensors field.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Elihn, K.; Landstroem, L.; Alm, O.

Iron nanoparticles enclosed in carbon shells were formed by laser-assisted chemical vapor decomposition of ferrocene (Fe(C{sub 5}H{sub 5}){sub 2}) vapor in Ar gas atmosphere. The particle size dependence on the total ambient gas pressure and on laser fluence of the pulsed ArF excimer laser was examined and, e.g., an effective size decrease of the iron core was observed at elevated laser fluences. Characterizations of the iron and carbon microstructures were performed by x-ray diffraction and transmission electron microscopy, while relative iron deposition rates were measured by x-ray fluorescence spectroscopy. Both {alpha}-Fe and {gamma}-Fe phases were found for the single crystallinemore » iron cores, surrounded by graphitic (inner) and amorphous (outer) carbon layers. The temperature rise of the laser-excited particles was also determined by optical spectroscopy of the emitted thermal radiation, which allowed an estimation of the iron loss of the nanoparticles due to evaporation. The estimated and measured iron losses are in good agreement.« less

Diffraction of real and virtual photons in a pyrolytic graphite crystal as source of intensive quasimonochromatic X-ray beam

NASA Astrophysics Data System (ADS)

Bogomazova, E. A.; Kalinin, B. N.; Naumenko, G. A.; Padalko, D. V.; Potylitsyn, A. P.; Sharafutdinov, A. F.; Vnukov, I. E.

2003-01-01

A series of experiments on the parametric X-rays radiation (PXR) generation and radiation soft component diffraction of relativistic electrons in pyrolytic graphite (PG) crystals have been carried out at the Tomsk synchrotron. It is shown that the experimental results with PG crystals are explained by the kinematic PXR theory if we take into account a contribution of the real photons diffraction (transition radiation, bremsstrahlung and PXR photons as well). The measurements of the emission spectrum of channeled electrons in the photon energy range much smaller than the characteristic energy of channeling radiation have been performed with a crystal-diffraction spectrometer. For electrons incident along the <1 1 0> axis of a silicon crystal, the radiation intensity in the energy range 30⩽ ω⩽360 keV exceeds the bremsstrahlung one almost by an order of magnitude. Different possibilities to create an effective source of the monochromatic X-ray beam based on the real and virtual photons diffraction in the PG crystals have been considered.

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

The molecular structure of 5-X-isatines where (X = F, Cl, and Br) determined by gas-phase electron diffraction with theoretical calculations

NASA Astrophysics Data System (ADS)

Belyakov, Alexander V.; Nikolaenko, Kirill O.; Davidovich, Pavel B.; Ivanov, Anatolii D.; Ponyaev, Alexander I.; Rykov, Anatolii N.; Shishkov, Igor F.

2018-01-01

The molecular structures of 5-X-isatines where X = F (1), Cl (2), and Br (3) were studied by gas-phase electron diffraction (GED) and theoretical calculations at M062X/aug-cc-pVTZ and MP2/aug-cc-pVTZ levels. The best fit of the experimental scattering intensities was obtained for a molecular model of Cs symmetry. The small differences between similar geometric parameters were constrained at the values calculated at the M062X level. The bond distances in the benzene ring are in agreement with their standard values. The (Odbnd)Csbnd C(dbnd O) carbon-carbon bonds of the pyrrole moiety in title compounds (1.581(11), 1.578(8), 1.574(12) Å, respectively) are remarkably lengthened in comparison with standard C(sp2)-C(sp2) value, 1.425(11) Å for N-methylpyrrole. According to NBO analysis this lengthening cannot be attributed to the electrostatic repulsion of oxygen lone pairs alone and is, mainly, due to the hyperconjugation, that is delocalization of oxygen lone pairs of π-type into the corresponding carbon-carbon antibonding orbital, nπ(O)→σ*(Csbnd C). Deletion of σ*(Csbnd C) orbital followed by subsequent geometry optimization led to shortening of the corresponding Csbnd C bond by 0.05-0.06 Å. Electronegative halogen atoms led to increase of Csbnd CXsbnd C endocyclic bond angles at ipso carbon atom as compared with the value of 120° in regular hexagon. According to different aromaticity descriptors, aromaticity of benzene moiety of title compounds is smaller in comparison with benzene molecule. External magnetic field induces diatropic ring current in benzene moiety. Local reactivity descriptors that indicate sites in a molecule that are susceptible to nucleophilic, electrophilic and radical attack are calculated.

Determination of molecular structure of succinic acid in a very complex conformational landscape: Gas-phase electron diffraction (GED) and ab initio studies

NASA Astrophysics Data System (ADS)

Vogt, Natalja; Abaev, Maxim A.; Rykov, Anatolii N.; Shishkov, Igor F.

2011-06-01

The molecular structure of succinic acid has been investigated by the gas-phase electron diffraction (GED) method for the first time. According to predictions of MP2/cc-pVTZ calculations, the molecule has 18 stable conformers with the C sbnd C sbnd C sbnd C chain in the gauche ( G) or anti ( A) configuration, and four of them, I ( G), II ( A), III ( G) and IV ( A) belonging to the C 2, C 2h, C 1 and C 1 point groups, respectively, with relative energies ΔE ZPE within 2.2 kcal/mol can be present at the experimental temperature of 445 K in noticeable amounts. The ratio of the conformers I:II:III:IV = 45(15):20(15):10(assumed):25(15) (in %) has been determined in the GED analysis guided by theoretical predictions. To take into account vibrational effects, the corrections Δ( r e - r a) to the experimental r a bond lengths were calculated from the MP2/cc-pVTZ quadratic and cubic force constants. The obtained equilibrium structural parameters of the dominant conformer I are the following (bond lengths in Å, angles in degrees): r e(C sp3sbnd C sp3) = 1.508(3), r e(C sp3sbnd C sp2) = 1.499(2), r e(C sbnd O) = 1.343(2), r e(C dbnd O) = 1.202(1), e(C sbnd C sbnd C) = 111.8(4), e(C sbnd C sbnd O) = 112.0(4), e(O sbnd C dbnd O) = 123.0(1), τ(C sbnd C sbnd C sbnd C) = 69.9(11). Yielding the best agreement with the GED structure, the MP2/cc-pVQZ approximation overestimates the C sbnd O and C dbnd O bond lengths by ca. 0.005(2) Å.

Molecular structure and conformational composition of methyl chloroacetate: An electron-diffraction and ab initio molecular orbital investigation

NASA Astrophysics Data System (ADS)

Aarset, Kirsten; Boldermo, Kjell Gunnar; Hagen, Kolbjørn

2010-08-01

The molecular structure and conformational composition of methyl chloroacetate, H 2ClC sbnd C( dbnd O) sbnd O sbnd CH 3, have been determined by gas-phase electron-diffraction (GED), using results from ab initio molecular orbital calculations (HF, MP2 and MP3/6-311+G(d,p)) to obtain constraints on some of the structural parameters. The molecules exist in the gas-phase at 25 °C as a mixture of two stable conformers: syn with C sbnd Cl eclipsing C dbnd O and gauche with C sbnd H approximately eclipsing C dbnd O. In both of these conformers O sbnd CH 3 is also eclipsing C dbnd O. The experimentally observed conformational composition at 25 °C was 36(8)% syn and 64(8)% gauche (parenthesised values are 2 σ), corresponding to a free energy difference between conformers of ΔGexp° = 1.4(9) kJ/mol. The corresponding theoretical values obtained for Δ G° are 1.1 kJ/mol (HF), 2.3 kJ/mol (MP2), and 2.4 kJ/mol (MP3). The results for the principal distances ( rh1) and angles ( ∠h1) for the major gauche conformer obtained from the combined GED/ ab initio study (2 σ uncertainties) are r(CO sbnd CCl) = 1.502(9) Å, r(C sbnd H) = 1.084(6) Å (average value), r(C sbnd Cl) = 1.782(4) Å, r(C dbnd O) = 1.213(4) Å, r(CO sbnd O) = 1.346(4) Å, r(CH 3sbnd O) = 1.468(10) Å, ∠C sbnd C sbnd Cl = 110.0(6)°, ∠C sbnd C dbnd O = 124.7(6)°, ∠C sbnd C sbnd O = 108.3(10)°, ∠C sbnd O sbnd C = 115.9(8)°, ϕ(Cl sbnd C sbnd C dbnd O) = 111(2)°, ϕ(C sbnd O sbnd C dbnd O) = 3(3)°.

Molecular structure of tris(cyclopropylsilyl)amine as determined by gas electron diffraction and quantum-chemical calculations

NASA Astrophysics Data System (ADS)

Vishnevskiy, Yuri V.; Abaev, Maxim A.; Ivanov, Arkadii A.; Vilkov, Lev V.; Dakkouri, Marwan

2008-10-01

The molecular structure and conformation of tris(cyclopropylsilyl)amine (TCPSA) has been studied by means of gas-phase electron diffraction at 338 K and quantum-chemical calculations. A total of 12 relatively stable conformations of TCPSA molecule were considered. According to the experimental results and the DFT calculations the most stable conformer corresponds to a configuration (according to the Prelog-Klyne notation) of the type (-ac)(-ac)(+ac)-(-ac)(-ac)(+ac), where the first three parentheses describe the three different Si-N-Si-C torsional angles and the latter ones depict the rotation of the three cyclopropyl groups about the C ring-Si axes, respectively. The quantum-mechanical calculations were performed using various density functional (B3LYP, X3LYP and O3LYP) and perturbation MP2 methods in combination with double- and triple- ζ basis sets plus polarization and diffuse functions. The most important experimental geometrical parameters of TCPSA ( ra Å, ∠ h1 degrees) are: (Si-N) av = 1.741(3), (Si-C) av = 1.866(4), (C-C) av = 1.510(3), (C-C(Si)) av = 1.535(3), (N-Si-C) av = 115.1(18)°. For the purpose of comparison and searching for reasons leading to the planarity of the Si 3N moiety in trisilylated amines we carried out NBO analysis and optimized the geometries of numerous silylamines. Among these compounds was tris(allylsilyl)amine (TASA), which is isovalent and isoelectronic to TCPSA. Utilizing the structural results we obtained we could show that Si +⋯Si + electrostatic repulsive interaction is predominantly responsible for the planarity of the Si 3N skeleton in TCPSA and in all other trisilylamines we considered. We also found that regardless the size and partial charges of the substituents the Si-N-Si bond angle in various disilylamines amounts to 130 ± 2°.

Dynamical electron diffraction simulation for non-orthogonal crystal system by a revised real space method.

PubMed

Lv, C L; Liu, Q B; Cai, C Y; Huang, J; Zhou, G W; Wang, Y G

2015-01-01

In the transmission electron microscopy, a revised real space (RRS) method has been confirmed to be a more accurate dynamical electron diffraction simulation method for low-energy electron diffraction than the conventional multislice method (CMS). However, the RRS method can be only used to calculate the dynamical electron diffraction of orthogonal crystal system. In this work, the expression of the RRS method for non-orthogonal crystal system is derived. By taking Na2 Ti3 O7 and Si as examples, the correctness of the derived RRS formula for non-orthogonal crystal system is confirmed by testing the coincidence of numerical results of both sides of Schrödinger equation; moreover, the difference between the RRS method and the CMS for non-orthogonal crystal system is compared at the accelerating voltage range from 40 to 10 kV. Our results show that the CMS method is almost the same as the RRS method for the accelerating voltage above 40 kV. However, when the accelerating voltage is further lowered to 20 kV or below, the CMS method introduces significant errors, not only for the higher-order Laue zone diffractions, but also for zero-order Laue zone. These indicate that the RRS method for non-orthogonal crystal system is necessary to be used for more accurate dynamical simulation when the accelerating voltage is low. Furthermore, the reason for the increase of differences between those diffraction patterns calculated by the RRS method and the CMS method with the decrease of the accelerating voltage is discussed. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Study of sensing properties of SnO2 prepared by spray-pyrolysis deposition towards ethanol gas

NASA Astrophysics Data System (ADS)

Saadaldin, Nasser M.; Hussain, Nabiha; AlZouabi, Abla

2018-05-01

Ethanol is widely used in all kinds of products with direct exposure to the human skin (e.g. medicinal products like hand disinfectants in occupational settings, cosmetics like hairsprays or mouthwashes, in this study, thin films of (SnO2) were deposited by using the thermal spray method (SPD) on quartz at 450°C substrate temperature using tin chloride SnCl2.2H2O, (1.0M). A gas sensor was constructed with the prepared SnO2, used to detect ethanol gas and some other gases. The films were characterized by X-ray diffraction (XRD), and scanning electron microscopy (SEM). The grain size was calculated the results showed nanostructure polycrystalline and crystallize in a tetragonal, S.G:P42/m nm, reaching grain Size approximately 27nm. The sensing properties of the films were studied towards ethanol at different concentrations ranging within (1-200 ppm,) the results showed that the sensitivity of the film increases with the concentration of ethanol, the best operating temperature reached about 300 °C, We studied the sensing properties of the films towards Ethanol alcohol gas, The first and foremost concerns of topical ethanol applications for public health are its carcinogenic effects, high selectivity and sensitivity of the film towards ethanol gas was found compared to other tested toxic gases such as methanol gas, acetone and methylbenzene. Yet an upto-date risk assessment of ethanol application on the skin and inside the oral cavity is currently lacking.

Attosecond electron pulses for 4D diffraction and microscopy

PubMed Central

Baum, Peter; Zewail, Ahmed H.

2007-01-01

In this contribution, we consider the advancement of ultrafast electron diffraction and microscopy to cover the attosecond time domain. The concept is centered on the compression of femtosecond electron packets to trains of 15-attosecond pulses by the use of the ponderomotive force in synthesized gratings of optical fields. Such attosecond electron pulses are significantly shorter than those achievable with extreme UV light sources near 25 nm (≈50 eV) and have the potential for applications in the visualization of ultrafast electron dynamics, especially of atomic structures, clusters of atoms, and some materials. PMID:18000040

TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka

Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speedmore » higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.« less

Electron diffraction study of the sillenites Bi{sub 12}SiO{sub 20}, Bi{sub 25}FeO{sub 39} and Bi{sub 25}InO{sub 39}: Evidence of short-range ordering of oxygen-vacancies in the trivalent sillenites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Scurti, Craig A.; Arenas, D. J.; Auvray, Nicolas

We present an electron diffraction study of three sillenites, Bi{sub 12}SiO{sub 20}, Bi{sub 25}FeO{sub 39}, and Bi{sub 25}InO{sub 39} synthesized using the solid-state method. We explore a hypothesis, inspired by optical studies in the literature, that suggests that trivalent sillenites have additional disorder not present in the tetravalent compounds. Electron diffraction patterns of Bi{sub 25}FeO{sub 39} and Bi{sub 25}InO{sub 39} show streaks that confirm deviations from the ideal sillenite structure. Multi-slice simulations of electron-diffraction patterns are presented for different perturbations to the sillenite structure - partial substitution of the M site by Bi{sup 3+}, random and ordered oxygen-vacancies, and amore » frozen-phonon model. Although comparison of experimental data to simulations cannot be conclusive, we consider the streaks as evidence of short-range ordered oxygen-vacancies.« less

Electron Matter Optics and the Quantum Electron Stern-Gerlach Magnet

NASA Astrophysics Data System (ADS)

McGregor, Scot; Bach, Roger; Yin, Xiaolu; Liou, Sy-Hwang; Batelaan, Herman; Gronniger, Glen

2011-05-01

We explore electron interferometry for the purpose of performing fundamental quantum mechanical experiments and sensing applications. To this end electron matter optics elements, in particular, a diffraction limited single slit, a double slit, and a nano-fabricated grating diffraction apparatus as well as a Mach-Zehnder IFM were previously developed. The double slit diffraction pattern has been recorded one electron at a time. Furthermore, the capability of closing each slit on demand has been developed, in that way realizing the thought experiment that Feynman explains in his lectures. The capability of the Mach-Zehnder interferometer to sense DC and AC electromagnetic fields for industrial applications is currently under investigation. Also, the construction of a new type of interferometer that has the potential to significantly increase the enclosed area and thus its sensitivity is in progress. Finally an idea to separate an electron beam fully into its two spin component using an electron interferometer is presented. We gratefully acknowledge funding by NSF Grant No. 0969506 and R. B. and S. M. acknowledge DOE-GAANN fellowships.

A protocol for searching the most probable phase-retrieved maps in coherent X-ray diffraction imaging by exploiting the relationship between convergence of the retrieved phase and success of calculation.

PubMed

Sekiguchi, Yuki; Hashimoto, Saki; Kobayashi, Amane; Oroguchi, Tomotaka; Nakasako, Masayoshi

2017-09-01

Coherent X-ray diffraction imaging (CXDI) is a technique for visualizing the structures of non-crystalline particles with size in the submicrometer to micrometer range in material sciences and biology. In the structural analysis of CXDI, the electron density map of a specimen particle projected along the direction of the incident X-rays can be reconstructed only from the diffraction pattern by using phase-retrieval (PR) algorithms. However, in practice, the reconstruction, relying entirely on the computational procedure, sometimes fails because diffraction patterns miss the data in small-angle regions owing to the beam stop and saturation of the detector pixels, and are modified by Poisson noise in X-ray detection. To date, X-ray free-electron lasers have allowed us to collect a large number of diffraction patterns within a short period of time. Therefore, the reconstruction of correct electron density maps is the bottleneck for efficiently conducting structure analyses of non-crystalline particles. To automatically address the correctness of retrieved electron density maps, a data analysis protocol to extract the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a single diffraction pattern is proposed. Through monitoring the variations of the phase values during PR calculations, the tendency for the PR calculations to succeed when the retrieved phase sets converged on a certain value was found. On the other hand, if the phase set was in persistent variation, the PR calculation tended to fail to yield the correct electron density map. To quantify this tendency, here a figure of merit for the variation of the phase values during PR calculation is introduced. In addition, a PR protocol to evaluate the similarity between a map of the highest figure of merit and other independently reconstructed maps is proposed. The protocol is implemented and practically examined in the structure analyses for diffraction patterns from aggregates of gold colloidal particles. Furthermore, the feasibility of the protocol in the structure analysis of organelles from biological cells is examined.

Carbonate formation in non-aqueous environments by solid-gas carbonation of silicates

NASA Astrophysics Data System (ADS)

Day, S. J.; Thompson, S. P.; Evans, A.; Parker, J. E.

2012-02-01

We have produced synthetic analogues of cosmic silicates using the Sol Gel method, producing amorphous silicates of composition Mg(x)Ca(1-x)SiO3. Using synchrotron X-ray powder diffraction on Beamline I11 at the Diamond Light Source, together with a newly-commissioned gas cell, real-time powder diffraction scans have been taken of a range of silicates exposed to CO2 under non-ambient conditions. The SXPD is complemented by other techniques including Raman and Infrared Spectroscopy and SEM imaging.

Carrier Dynamics and Application of the Phase Coherent Photorefractive Effect in ZnSe Quantum Wells

NASA Astrophysics Data System (ADS)

Dongol, Amit

The intensity dependent diffraction efficiency of a phase coherent photorefractive (PCP) ZnSe quantum well (QW) is investigated at 80 K in a two-beam four-wave mixing (FWM) configuration using 100 fs laser pulses with a repetition rate of 80 MHz. The observed diffraction efficiencies of the first and second-order diffracted beam are on the order of 10-3 and 10-5, respectively, revealing nearly no intensity dependence. The first-order diffraction is caused by the PCP effect where the probe-pulse is diffracted due to a long-living incoherent electron density grating in the QW. The second-order diffraction is created by a combination of diffraction processes. For negative probe-pulse delay, the exciton polarization is diffracted at the electron grating twice by a cascade effect. For positive delay, the diffracted signal is modified by the destructive interference with a chi(5) generated signal due to a dynamical screening effect. Model calculations of the signal traces based on the optical Bloch equations considering inhomogeneous broadening of exciton energies are in good agreement with the experimental data. To study the carrier dynamics responsible for the occurrence of the PCP effect, threebeam FWM experiments are carried out. The non-collinear wave-vectors k1 , k2 and k3 at central wavelength of 441 nm (~2.81 eV) were resonantly tuned to the heavy-hole exciton transition energy at 20 K. In the FWM experiment the time coincident strong pump pulses k1 and k2 create both an exciton density grating in the QW and an electron-hole pair grating in the GaAs while the delayed weak pulse k3 simultaneously probes the exciton lifetime as well as the electron grating capture time. The model calculations are in good agreement with the experimental results also providing information about the transfer delay of electrons arriving from the substrate to the QW. For negative probe-pulse delay we still observe a diffracted signal due to the long living electron density grating in the QW. The electron grating build-up and decay times are also studied with the modified three-beam FWM set-up. Using an optical shutter for pump pulses k1and k2, the dynamics of the electron grating formation and its decay is continuously probed by a delayed pulse k3. The obtained build-up and decay times are found to depend nearly linearly on the intensity of incident pulses k1 and k2 being on the order of several microseconds at low pump intensities. The PCP effect in ZnSe QW possesses a time-gating capability which can be used for real-time holographic imaging. In this work we demonstrate contrast enhanced real time holographic imaging (CEHI) of floating glass beads and of living unicellular animals (Paramecium and Euglena cells) in aqueous solution. We also demonstrate CEHI of a ~100 im thick wire concealed behind a layer of chicken skin. The results demonstrate the potential of PCP QWs for real-time and depth-resolved imaging of moving micrometer sized biological objects in transparent media or of obscured objects in turbid media.

The effect of heat treatment on structural and electronic properties of niobium nitride prepared by a thermal diffusion method

DOE PAGES

Farha, Ashraf Hassan; Ozkendir, Osman Murat; Elsayed-Ali, Hani E.; ...

2016-11-15

NbN coatings are prepared onto Nb substrate by thermal diffusion at high temperatures. The formation of NbN coating by thermal diffusion was studied in the range of 1250-1500 °C at constant nitrogen background gas pressure (1.3x10 -3 Pa) and processing time (180 min). The electronic and crystal structures of the NbN coatings were investigated. It was found that nitrogen diffuses into Nb forming the Nb-N solid solution (bcc) a-NbN phase that starts to appear above 1250 °C. Increasing the processing temperature gives richer a-phase concentration. Besides, X-ray absorption spectroscopy (XAS) was performed to study the electronic structure of the NbNmore » layer. The results of the electronic structural study corroborate the crystal structural analysis. The Nb M 3,2 edge X-ray absorption spectroscopy (XAS) spectrum shows strong temperature dependence. At the highest processing temperature (1500 °C), the number of d holes increased. Nitrogen diffusion into Nb is resulting to increase electrostatic interaction between d electron and core hole. Lastly, for the studied conditions, only the α-NbN was observed in the X-ray diffraction patterns.« less

The effect of heat treatment on structural and electronic properties of niobium nitride prepared by a thermal diffusion method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Farha, Ashraf Hassan; Ozkendir, Osman Murat; Elsayed-Ali, Hani E.

NbN coatings are prepared onto Nb substrate by thermal diffusion at high temperatures. The formation of NbN coating by thermal diffusion was studied in the range of 1250-1500 °C at constant nitrogen background gas pressure (1.3x10 -3 Pa) and processing time (180 min). The electronic and crystal structures of the NbN coatings were investigated. It was found that nitrogen diffuses into Nb forming the Nb-N solid solution (bcc) a-NbN phase that starts to appear above 1250 °C. Increasing the processing temperature gives richer a-phase concentration. Besides, X-ray absorption spectroscopy (XAS) was performed to study the electronic structure of the NbNmore » layer. The results of the electronic structural study corroborate the crystal structural analysis. The Nb M 3,2 edge X-ray absorption spectroscopy (XAS) spectrum shows strong temperature dependence. At the highest processing temperature (1500 °C), the number of d holes increased. Nitrogen diffusion into Nb is resulting to increase electrostatic interaction between d electron and core hole. Lastly, for the studied conditions, only the α-NbN was observed in the X-ray diffraction patterns.« less

Microstructural characterization of weld joints of 9Cr reduced activation ferritic martensitic steel fabricated by different joining methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thomas Paul, V.; Saroja, S.; Albert, S.K.

This paper presents a detailed electron microscopy study on the microstructure of various regions of weldment fabricated by three welding methods namely tungsten inert gas welding, electron beam welding and laser beam welding in an indigenously developed 9Cr reduced activation ferritic/martensitic steel. Electron back scatter diffraction studies showed a random micro-texture in all the three welds. Microstructural changes during thermal exposures were studied and corroborated with hardness and optimized conditions for the post weld heat treatment have been identified for this steel. Hollomon–Jaffe parameter has been used to estimate the extent of tempering. The activation energy for the tempering processmore » has been evaluated and found to be corresponding to interstitial diffusion of carbon in ferrite matrix. The type and microchemistry of secondary phases in different regions of the weldment have been identified by analytical transmission electron microscopy. - Highlights: • Comparison of microstructural parameters in TIG, electron beam and laser welds of RAFM steel • EBSD studies to illustrate the absence of preferred orientation and identification of prior austenite grain size using phase identification map • Optimization of PWHT conditions for indigenous RAFM steel • Study of kinetics of tempering and estimation of apparent activation energy of the process.« less

Structure Evolution and Distributions of Grain-Boundary Misorientainons in Submicrocrystalline Molybdenum Irradiated with a Pulsed Electron Beam

NASA Astrophysics Data System (ADS)

Stepanova, E. N.; Grabovetskaya, G. P.; Teresov, A. D.; Mishin, I. P.

2018-05-01

Using the methods of electron backscatter diffraction, electron microscopy and X-ray diffraction analysis, it is demonstrated that irradiation of the surface of a submicrocrystalline molybdenum specimen with a pulsed electron beam in a non-melt regime results in the formation of a gradient structure in its bulk. The irradiation temperature is shown to affect the density of defects, the value of stress, and the distributions of grain-boundary misorientations in the surface and bulk of the submicrocrystalline molybdenum specimens.

Sulfur Nanoparticles Synthesis and Characterization from H2S Gas, Using Novel Biodegradable Iron Chelates in W/O Microemulsion

NASA Astrophysics Data System (ADS)

Deshpande, Aniruddha S.; Khomane, Ramdas B.; Vaidya, Bhalchandra K.; Joshi, Renuka M.; Harle, Arti S.; Kulkarni, Bhaskar D.

2008-06-01

Sulfur nanoparticles were synthesized from hazardous H2S gas using novel biodegradable iron chelates in w/o microemulsion system. Fe3+ malic acid chelate (0.05 M aqueous solution) was studied in w/o microemulsion containing cyclohexane, Triton X-100 and n-hexanol as oil phase, surfactant, co-surfactant, respectively, for catalytic oxidation of H2S gas at ambient conditions of temperature, pressure, and neutral pH. The structural features of sulfur nanoparticles have been characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), energy dispersive spectroscopy (EDS), diffused reflectance infra-red Fourier transform technique, and BET surface area measurements. XRD analysis indicates the presence of α-sulfur. TEM analysis shows that the morphology of sulfur nanoparticles synthesized in w/o microemulsion system is nearly uniform in size (average particle size 10 nm) and narrow particle size distribution (in range of 5 15 nm) as compared to that in aqueous surfactant systems. The EDS analysis indicated high purity of sulfur (>99%). Moreover, sulfur nanoparticles synthesized in w/o microemulsion system exhibit higher antimicrobial activity (against bacteria, yeast, and fungi) than that of colloidal sulfur.

Morphology controlled synthesis of platinum nanoparticles performed on the surface of graphene oxide using a gas-liquid interfacial reaction and its application for high-performance electrochemical sensing.

PubMed

Bai, Wushuang; Sheng, Qinglin; Zheng, Jianbin

2016-07-21

In this paper, we report a novel morphology-controlled synthetic method. Platinum (Pt) nanoparticles with three kinds of morphology (aggregation-like, cube-like and globular) were grown on the surface of graphene oxide (GO) using a simple gas-liquid interfacial reaction and Pt/GO nanocomposites were obtained successfully. According to the experimental results, the morphology of the Pt nanoparticles can be controlled by adjusting the reaction temperature with the protection of chitosan. The obtained Pt/GO nanocomposites were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy (FTIR). Then the Pt/GO nanocomposites with the three kinds of morphology were all used to fabricate electrochemical sensors. The electrochemical experimental results indicated that compared with various reported electrochemical sensors, the Pt/GO modified sensors in this work exhibit a low detection limit, high sensitivity and an extra wide linear range for the detection of nitrite. In addition, the synthesis of Pt particles based on a gas-liquid interfacial reaction provides a new platform for the controllable synthesis of nanomaterials.

Characterization of commercially cold sprayed copper coatings and determination of the effects of impacting copper powder velocities

NASA Astrophysics Data System (ADS)

Jakupi, P.; Keech, P. G.; Barker, I.; Ramamurthy, S.; Jacklin, R. L.; Shoesmith, D. W.; Moser, D. E.

2015-11-01

Copper coated steel containers are being developed for the disposal of high level nuclear waste using processes such as cold spray and electrodeposition. Electron Back-Scatter Diffraction has been used to determine the microstructural properties and the quality of the steel-copper coating interface. The influence of the nature of the cold-spray carrier gas as well as its temperature and pressure (velocity) on the coating's plastic strain and recrystallization behaviour have been investigated, and one commercially-produced electrodeposited coating characterized. The quality of the coatings was assessed using the coincident site lattice model to analyse the properties of the grain boundaries. For cold spray coatings the grain size and number of coincident site lattice grain boundaries increased, and plastic strain decreased, with carrier gas velocity. In all cases annealing improved the quality of the coatings by increasing texture and coincidence site-lattices, but also increased the number of physical voids, especially when a low temperature cold spray carrier gas was used. Comparatively, the average grain size and number of coincident site-lattices was considerably larger for the strongly textured electrodeposited coating. Tensile testing showed the electrodeposited coating was much more strongly adherent to the steel substrate.

Sulfur Nanoparticles Synthesis and Characterization from H2S Gas, Using Novel Biodegradable Iron Chelates in W/O Microemulsion

PubMed Central

2008-01-01

Sulfur nanoparticles were synthesized from hazardous H2S gas using novel biodegradable iron chelates in w/o microemulsion system. Fe3+–malic acid chelate (0.05 M aqueous solution) was studied in w/o microemulsion containing cyclohexane, Triton X-100 andn-hexanol as oil phase, surfactant, co-surfactant, respectively, for catalytic oxidation of H2S gas at ambient conditions of temperature, pressure, and neutral pH. The structural features of sulfur nanoparticles have been characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), energy dispersive spectroscopy (EDS), diffused reflectance infra-red Fourier transform technique, and BET surface area measurements. XRD analysis indicates the presence of α-sulfur. TEM analysis shows that the morphology of sulfur nanoparticles synthesized in w/o microemulsion system is nearly uniform in size (average particle size 10 nm) and narrow particle size distribution (in range of 5–15 nm) as compared to that in aqueous surfactant systems. The EDS analysis indicated high purity of sulfur (>99%). Moreover, sulfur nanoparticles synthesized in w/o microemulsion system exhibit higher antimicrobial activity (against bacteria, yeast, and fungi) than that of colloidal sulfur.

Structural, dielectric and gas sensing behavior of Mn substituted spinel MFe2O4 (M=Zn, Cu, Ni, and Co) ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Ranjith Kumar, E.; Siva Prasada Reddy, P.; Sarala Devi, G.; Sathiyaraj, S.

2016-01-01

Spinel ferrite (MnZnFe2O4, MnCuFe2O4, MnNiFe2O4 and MnCoFe2O4) nanoparticles have been prepared by evaporation method. The annealing temperature plays an important role on changing particle size of the spinel ferrite nanoparticles was found out by X-ray diffraction and transmission electron microscopy. The role of manganese substitution in the spinel ferrite nanoparticles were also analyzed for different annealing temperature. The substitution of Mn also creates a vital change in dielectric properties have been measured in the frequency range of 100 kHz to 5 MHz. These spinel ferrites are decomposed to α-Fe2O3 after annealing above 550 °C in air. Through the characterization of the prepared powder, the effect of annealing temperature, chemical composition and preparation technique on the microstructure, particle size and dielectric properties of the Mn substituted spinel ferrite nanoparticles are discussed. Furthermore, Conductance response of Mn substituted MFe2O4 ferrite nanoparticles were measured by exposing the materials to reducing gas like liquefied petroleum gas (LPG).

Synthesis and Phase Stability of Scandia, Gadolinia, and Ytterbia Co-doped Zirconia for Thermal Barrier Coating Application

NASA Astrophysics Data System (ADS)

Li, Qi-Lian; Cui, Xiang-Zhong; Li, Shu-Qing; Yang, Wei-Hua; Wang, Chun; Cao, Qian

2015-01-01

Scandia, gadolinia, and ytterbia co-doped zirconia (SGYZ) ceramic powder was synthesized by chemical co-precipitation and calcination processes for application in thermal barrier coatings to promote the durability of gas turbines. The ceramic powder was agglomerated and sintered at 1150 °C for 2 h, and the powder exhibited good flowability and apparent density to be suitable for plasma spraying process. The microstructure, morphology and phase stability of the powder and plasma-sprayed SGYZ coatings were analyzed by means of scanning electron microscope and x-ray diffraction. Thermal conductivity of plasma-sprayed SGYZ coatings was measured. The results indicated that the SGYZ ceramic powder and the coating exhibit excellent stability to retain single non-transformable tetragonal zirconia even after high temperature (1400 °C) exposure for 500 h and do not undergo a tetragonal-to-monoclinic phase transition upon cooling. Furthermore, the plasma-sprayed SGYZ coating also exhibits lower thermal conductivity than yttria stabilized zirconia coating currently used in gas turbine engine industry. SGYZ can be explored as a candidate material of ultra-high temperature thermal barrier coating for advanced gas turbine engines.

Synthesis of nano-structured tin oxide thin films with faster response to LPG and ammonia by spray pyrolysis

NASA Astrophysics Data System (ADS)

PrasannaKumari, K.; Thomas, Boben

2018-01-01

Nanostructured SnO2 thin film have been efficiently fabricated by spray pyrolysis using atomizers of different types. The structure and morphology of as-prepared samples are investigated by techniques such as x-ray diffraction, and field-emission scanning electron microscopy. Significant morphological changes are observed in films by modifying the precursor atomization as a result of change of spray device. The optical characterization indicates that change in atomization, affects the absorbance and the band gap, following the varied crystallite size. Gas sensing investigations on ultrasonically prepared tin oxide films show NH3 response at operating temperatures lower down to 50 °C. For 1000 ppm of LPG the response at 350 °C for air blast atomizer film is about 99%, with short response and recovery times. The photoluminescence emmision spectra reveal the correlation between atomization process and the quantity of oxygen vacancies present in the samples. The favorable size reduction in microstructure with good crystallinity with slight change in lattice properties suggest their scope in gas sensing applications. On the basis of these characterizations, the mechanism of LPG and NH3 gas sensing of nanostructured SnO2 thin films has been proposed.

Recrystallization of puerarin using the supercritical fluid antisolvent process

NASA Astrophysics Data System (ADS)

Li, Y.; Yang, D. J.; Zhou, W.; Chen, S. B.; Chen, S. L.

2012-02-01

The purpose of this study was to investigate the influence of supercritical fluid (SCF) processing on the polymorphism of puerarin (Pur), a poorly soluble drug. The gas anti-solvent (GAS) technique was used to crystalize the drug in different conditions. The samples were analyzed by scanning electron microscopy and laser granulometry for changes in the habitus and particle size. The solid state was studied by X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC), Fourier-transform infrared spectroscopy (FT-IR) and melting point determination. Finally, the dissolution and solubility tests were carried out. It was attested that compared with the commercial Pur in Crystal form I, at the optimum and most of conditions, Pur changed into crystal form II with more orderly and pure appearances. At the concentration of 60 mg/ml and at the solvent of methanol, two other new crystal forms (named form III and form IV) were produced. It was demonstrated that the particles mean diameter, size distribution and morphology can be strongly controlled through the manipulation of the process parameters and more importantly, Pur in the new crystal forms, which were not reported before with better physico-chemical properties could be produced by recrystalization by GAS.

Detection of expansion at large angle grain boundaries using electron diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Balluffi, R.W.; Bristowe, P.D.

1984-02-01

Lamarre and Sass (LS) (Scripta Metall. 17: 1141(1983)) observed a grain boundary electron diffraction effect from a large angle twist boundary which they claim can be used to obtain the volume expansion at the grain boundary in a direction normal to it. This paper considers the case where the intensity from the grain boundary region, is close to lattice reflections on the same element of the boundary diffraction lattice. Analysis of this complex problem show that the simplified model of LS is misleading in this case. (DLC)

Graphene unit cell imaging by holographic coherent diffraction.

PubMed

Longchamp, Jean-Nicolas; Latychevskaia, Tatiana; Escher, Conrad; Fink, Hans-Werner

2013-06-21

We have imaged a freestanding graphene sheet of 210 nm in diameter with 2 Å resolution by combining coherent diffraction and holography with low-energy electrons. The entire sheet is reconstructed from a single diffraction pattern displaying the arrangement of 660.000 individual graphene unit cells at once. Given the fact that electrons with kinetic energies of the order of 100 eV do not damage biological molecules, it will now be a matter of developing methods for depositing individual proteins onto such graphene sheets.

Design and implementation of an optimal laser pulse front tilting scheme for ultrafast electron diffraction in reflection geometry with high temporal resolution.

PubMed

Pennacchio, Francesco; Vanacore, Giovanni M; Mancini, Giulia F; Oppermann, Malte; Jayaraman, Rajeswari; Musumeci, Pietro; Baum, Peter; Carbone, Fabrizio

2017-07-01

Ultrafast electron diffraction is a powerful technique to investigate out-of-equilibrium atomic dynamics in solids with high temporal resolution. When diffraction is performed in reflection geometry, the main limitation is the mismatch in group velocity between the overlapping pump light and the electron probe pulses, which affects the overall temporal resolution of the experiment. A solution already available in the literature involved pulse front tilt of the pump beam at the sample, providing a sub-picosecond time resolution. However, in the reported optical scheme, the tilted pulse is characterized by a temporal chirp of about 1 ps at 1 mm away from the centre of the beam, which limits the investigation of surface dynamics in large crystals. In this paper, we propose an optimal tilting scheme designed for a radio-frequency-compressed ultrafast electron diffraction setup working in reflection geometry with 30 keV electron pulses containing up to 10 5 electrons/pulse. To characterize our scheme, we performed optical cross-correlation measurements, obtaining an average temporal width of the tilted pulse lower than 250 fs. The calibration of the electron-laser temporal overlap was obtained by monitoring the spatial profile of the electron beam when interacting with the plasma optically induced at the apex of a copper needle (plasma lensing effect). Finally, we report the first time-resolved results obtained on graphite, where the electron-phonon coupling dynamics is observed, showing an overall temporal resolution in the sub-500 fs regime. The successful implementation of this configuration opens the way to directly probe structural dynamics of low-dimensional systems in the sub-picosecond regime, with pulsed electrons.

Design and implementation of an optimal laser pulse front tilting scheme for ultrafast electron diffraction in reflection geometry with high temporal resolution

PubMed Central

Pennacchio, Francesco; Vanacore, Giovanni M.; Mancini, Giulia F.; Oppermann, Malte; Jayaraman, Rajeswari; Musumeci, Pietro; Baum, Peter; Carbone, Fabrizio

2017-01-01

Ultrafast electron diffraction is a powerful technique to investigate out-of-equilibrium atomic dynamics in solids with high temporal resolution. When diffraction is performed in reflection geometry, the main limitation is the mismatch in group velocity between the overlapping pump light and the electron probe pulses, which affects the overall temporal resolution of the experiment. A solution already available in the literature involved pulse front tilt of the pump beam at the sample, providing a sub-picosecond time resolution. However, in the reported optical scheme, the tilted pulse is characterized by a temporal chirp of about 1 ps at 1 mm away from the centre of the beam, which limits the investigation of surface dynamics in large crystals. In this paper, we propose an optimal tilting scheme designed for a radio-frequency-compressed ultrafast electron diffraction setup working in reflection geometry with 30 keV electron pulses containing up to 105 electrons/pulse. To characterize our scheme, we performed optical cross-correlation measurements, obtaining an average temporal width of the tilted pulse lower than 250 fs. The calibration of the electron-laser temporal overlap was obtained by monitoring the spatial profile of the electron beam when interacting with the plasma optically induced at the apex of a copper needle (plasma lensing effect). Finally, we report the first time-resolved results obtained on graphite, where the electron-phonon coupling dynamics is observed, showing an overall temporal resolution in the sub-500 fs regime. The successful implementation of this configuration opens the way to directly probe structural dynamics of low-dimensional systems in the sub-picosecond regime, with pulsed electrons. PMID:28713841

Quantitative Analysis of Electron Beam Damage in Organic Thin Films

PubMed Central

2017-01-01

In transmission electron microscopy (TEM) the interaction of an electron beam with polymers such as P3HT:PCBM photovoltaic nanocomposites results in electron beam damage, which is the most important factor limiting acquisition of structural or chemical data at high spatial resolution. Beam effects can vary depending on parameters such as electron dose rate, temperature during imaging, and the presence of water and oxygen in the sample. Furthermore, beam damage will occur at different length scales. To assess beam damage at the angstrom scale, we followed the intensity of P3HT and PCBM diffraction rings as a function of accumulated electron dose by acquiring dose series and varying the electron dose rate, sample preparation, and the temperature during acquisition. From this, we calculated a critical dose for diffraction experiments. In imaging mode, thin film deformation was assessed using the normalized cross-correlation coefficient, while mass loss was determined via changes in average intensity and standard deviation, also varying electron dose rate, sample preparation, and temperature during acquisition. The understanding of beam damage and the determination of critical electron doses provides a framework for future experiments to maximize the information content during the acquisition of images and diffraction patterns with (cryogenic) transmission electron microscopy. PMID:28553431

Development of splitting convergent beam electron diffraction (SCBED).

PubMed

Houdellier, Florent; Röder, Falk; Snoeck, Etienne

2015-12-01

Using a combination of condenser electrostatic biprism with dedicated electron optic conditions for sample illumination, we were able to split a convergent beam electron probe focused on the sample in two half focused probes without introducing any tilt between them. As a consequence, a combined convergent beam electron diffraction pattern is obtained in the back focal plane of the objective lens arising from two different sample areas, which could be analyzed in a single pattern. This splitting convergent beam electron diffraction (SCBED) pattern has been tested first on a well-characterized test sample of Si/SiGe multilayers epitaxially grown on a Si substrate. The SCBED pattern contains information from the strained area, which exhibits HOLZ lines broadening induced by surface relaxation, with fine HOLZ lines observed in the unstrained reference part of the sample. These patterns have been analyzed quantitatively using both parts of the SCBED transmitted disk. The fine HOLZ line positions are used to determine the precise acceleration voltage of the microscope while the perturbed HOLZ rocking curves in the stained area are compared to dynamical simulated ones. The combination of these two information leads to a precise evaluation of the sample strain state. Finally, several SCBED setups are proposed to tackle fundamental physics questions as well as applied materials science ones and demonstrate how SCBED has the potential to greatly expand the range of applications of electron diffraction and electron holography. Copyright © 2015 Elsevier B.V. All rights reserved.

Zemax simulations describing collective effects in transition and diffraction radiation.

PubMed

Bisesto, F G; Castellano, M; Chiadroni, E; Cianchi, A

2018-02-19

Transition and diffraction radiation from charged particles is commonly used for diagnostics purposes in accelerator facilities as well as THz sources for spectroscopy applications. Therefore, an accurate analysis of the emission process and the transport optics is crucial to properly characterize the source and precisely retrieve beam parameters. In this regard, we have developed a new algorithm, based on Zemax, to simulate both transition and diffraction radiation as generated by relativistic electron bunches, therefore considering collective effects. In particular, unlike other previous works, we take into account electron beam physical size and transverse momentum, reproducing some effects visible on the produced radiation, not observable in a single electron analysis. The simulation results have been compared with two experiments showing an excellent agreement.

On the Use of Dynamical Diffraction Theory To Refine Crystal Structure from Electron Diffraction Data: Application to KLa5O5(VO4)2, a Material with Promising Luminescent Properties.

PubMed

Colmont, Marie; Palatinus, Lukas; Huvé, Marielle; Kabbour, Houria; Saitzek, Sébastien; Djelal, Nora; Roussel, Pascal

2016-03-07

A new lanthanum oxide, KLa5O5(VO4)2, was synthesized using a flux growth technique that involved solid-state reaction under an air atmosphere at 900 °C. The crystal structure was solved and refined using an innovative approach recently established and based on three-dimensional (3D) electron diffraction data, using precession of the electron beam and then validated against Rietveld refinement and denisty functional theory (DFT) calculations. It crystallizes in a monoclinic unit cell with space group C2/m and has unit cell parameters of a = 20.2282(14) Å, b = 5.8639(4) Å, c = 12.6060(9) Å, and β = 117.64(1)°. Its structure is built on Cresnel-like two-dimensional (2D) units (La5O5) of 4*3 (OLa4) tetrahedra, which run parallel to (001) plane, being surrounded by isolated VO4 tetrahedra. Four isolated vanadate groups create channels that host K(+) ions. Substitution of K(+) cations by another alkali metal is possible, going from lithium to rubidium. Li substitution led to a similar phase with a primitive monoclinic unit cell. A complementary selected area electron diffraction (SAED) study highlighted diffuse streaks associated with stacking faults observed on high-resolution electron microscopy (HREM) images of the lithium compound. Finally, preliminary catalytic tests for ethanol oxidation are reported, as well as luminescence evidence. This paper also describes how solid-state chemists can take advantages of recent progresses in electron crystallography, assisted by DFT calculations and powder X-ray diffraction (PXRD) refinements, to propose new structural types with potential applications to the physicist community.

Strain analysis from nano-beam electron diffraction: Influence of specimen tilt and beam convergence.

PubMed

Grieb, Tim; Krause, Florian F; Schowalter, Marco; Zillmann, Dennis; Sellin, Roman; Müller-Caspary, Knut; Mahr, Christoph; Mehrtens, Thorsten; Bimberg, Dieter; Rosenauer, Andreas

2018-07-01

Strain analyses from experimental series of nano-beam electron diffraction (NBED) patterns in scanning transmission electron microscopy are performed for different specimen tilts. Simulations of NBED series are presented for which strain analysis gives results that are in accordance with experiment. This consequently allows to study the relation between measured strain and actual underlying strain. A two-tilt method which can be seen as lowest-order electron beam precession is suggested and experimentally implemented. Strain determination from NBED series with increasing beam convergence is performed in combination with the experimental realization of a probe-forming aperture with a cross inside. It is shown that using standard evaluation techniques, the influence of beam convergence on spatial resolution is lower than the influence of sharp rings around the diffraction disc which occur at interfaces and which are caused by the tails of the intensity distribution of the electron probe. Copyright © 2018 Elsevier B.V. All rights reserved.

Applications of the diffraction and interference of light and electronic waves

NASA Astrophysics Data System (ADS)

Bahrim, Cristian; Lanning, Robert

2010-10-01

As part of a NSF sponsored program, called STAIRSTEP, at Lamar University we work on improving the basic knowledge of our physics majors in topics with broader impact in various areas of science and engineering [1]. The purpose is to facilitate a deeper understanding of some fundamental concepts in the field of optics through hands-on experience [2]. We choose to study the interference/diffraction of light and matter waves, because of its fundamental importance in physics with many applications. We target multiple goals in our field of study such as to understand the formation of electronic waves (wave packets) and their interaction with atoms in crystals (electron diffraction); the Fourier analysis of light with applications in spectroscopy, etc. We can show that a crystal lattice Fourier transforms the sinusoidal waves associated to free electrons fired toward the crystal. Our studies led to a simple and instructive recipe for discovering the arrangement of atoms in crystals from the analysis of the diffraction patterns produced by radiation or by electrons transmitted through crystals. [1] Doerschuk P. et al., 39th ASEE/IEEE Frontiers in Education Conference, San Antonio 2009, M3F-1. [2] Bahrim C, Innovation 2006 -- World Innovations in Engineering Education and Research, Chapter 17, iNEER Innovation Series, ISBN 0-9741252-5-3.

Diffraction contrast as a sensitive indicator of femtosecond sub-nanoscale motion in ultrafast transmission electron microscopy

NASA Astrophysics Data System (ADS)

Cremons, Daniel R.; Schliep, Karl B.; Flannigan, David J.

2013-09-01

With ultrafast transmission electron microscopy (UTEM), access can be gained to the spatiotemporal scales required to directly visualize rapid, non-equilibrium structural dynamics of materials. This is achieved by operating a transmission electron microscope (TEM) in a stroboscopic pump-probe fashion by photoelectrically generating coherent, well-timed electron packets in the gun region of the TEM. These probe photoelectrons are accelerated down the TEM column where they travel through the specimen before reaching a standard, commercially-available CCD detector. A second laser pulse is used to excite (pump) the specimen in situ. Structural changes are visualized by varying the arrival time of the pump laser pulse relative to the probe electron packet at the specimen. Here, we discuss how ultrafast nanoscale motions of crystalline materials can be visualized and precisely quantified using diffraction contrast in UTEM. Because diffraction contrast sensitively depends upon both crystal lattice orientation as well as incoming electron wavevector, minor spatial/directional variations in either will produce dynamic and often complex patterns in real-space images. This is because sections of the crystalline material that satisfy the Laue conditions may be heterogeneously distributed such that electron scattering vectors vary over nanoscale regions. Thus, minor changes in either crystal grain orientation, as occurs during specimen tilting, warping, or anisotropic expansion, or in the electron wavevector result in dramatic changes in the observed diffraction contrast. In this way, dynamic contrast patterns observed in UTEM images can be used as sensitive indicators of ultrafast specimen motion. Further, these motions can be spatiotemporally mapped such that direction and amplitude can be determined.

Electron-beam-irradiation-induced crystallization of amorphous solid phase change materials

NASA Astrophysics Data System (ADS)

Zhou, Dong; Wu, Liangcai; Wen, Lin; Ma, Liya; Zhang, Xingyao; Li, Yudong; Guo, Qi; Song, Zhitang

2018-04-01

The electron-beam-irradiation-induced crystallization of phase change materials in a nano sized area was studied by in situ transmission electron microscopy and selected area electron diffraction. Amorphous phase change materials changed to a polycrystalline state after being irradiated with a 200 kV electron beam for a long time. The results indicate that the crystallization temperature strongly depends on the difference in the heteronuclear bond enthalpy of the phase change materials. The selected area electron diffraction patterns reveal that Ge2Sb2Te5 is a nucleation-dominated material, when Si2Sb2Te3 and Ti0.5Sb2Te3 are growth-dominated materials.

Electron crystallography with the EIGER detector

PubMed Central

Tinti, Gemma; Fröjdh, Erik; van Genderen, Eric; Gruene, Tim; Schmitt, Bernd; de Winter, D. A. Matthijs; Weckhuysen, Bert M.; Abrahams, Jan Pieter

2018-01-01

Electron crystallography is a discipline that currently attracts much attention as method for inorganic, organic and macromolecular structure solution. EIGER, a direct-detection hybrid pixel detector developed at the Paul Scherrer Institut, Switzerland, has been tested for electron diffraction in a transmission electron microscope. EIGER features a pixel pitch of 75 × 75 µm2, frame rates up to 23 kHz and a dead time between frames as low as 3 µs. Cluster size and modulation transfer functions of the detector at 100, 200 and 300 keV electron energies are reported and the data quality is demonstrated by structure determination of a SAPO-34 zeotype from electron diffraction data. PMID:29765609