Effect of Electron Beam Irradiation on Structural and Optical Properties of Cu-Doped In2O3 Films Prepared by RF Magnetron Sputtering

NASA Astrophysics Data System (ADS)

Krishnan, R. Reshmi; Sanjeev, Ganesh; Prabhu, Radhakrishna; Pillai, V. P. Mahadevan

2018-02-01

Undoped and Cu-doped In2O3 films were prepared by radiofrequency magnetron sputtering technique. The effects of Cu doping and high-energy electron beam irradiation on the structural and optical properties of as-prepared films were investigated using techniques such as x-ray diffraction, x-ray photoelectron spectroscopy (XPS), lateral scanning electron microscopic image analysis, energy-dispersive x-ray (EDX) spectroscopy, micro-Raman, and ultraviolet-visible (UV-vis) spectroscopy. Moderate doping of Cu in In2O3 enhanced the intensity of (222) peak, indicating alignment of crystalline grains along <111>. Electron beam irradiation promoted orientation of crystalline grains along <111> in undoped and moderately Cu-doped films. EDX spectroscopic and XPS analyses revealed incorporation of Cu2+ ions in the lattice. The transmittance of Cu-doped films decreased with e-beam irradiation. Systematic reduction of the bandgap energy with increase in Cu doping concentration was seen in unirradiated and electron-beam-irradiated films.

Electron Effective-Attenuation-Length Database

National Institute of Standards and Technology Data Gateway

SRD 82 NIST Electron Effective-Attenuation-Length Database (PC database, no charge)   This database provides values of electron effective attenuation lengths (EALs) in solid elements and compounds at selected electron energies between 50 eV and 2,000 eV. The database was designed mainly to provide EALs (to account for effects of elastic-eletron scattering) for applications in surface analysis by Auger-electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS).

Lattice and Valence Electronic Structures of Crystalline Octahedral Molybdenum Halide Clusters-Based Compounds, Cs2[Mo6X14] (X = Cl, Br, I), Studied by Density Functional Theory Calculations.

PubMed

Saito, Norio; Cordier, Stéphane; Lemoine, Pierric; Ohsawa, Takeo; Wada, Yoshiki; Grasset, Fabien; Cross, Jeffrey S; Ohashi, Naoki

2017-06-05

The electronic and crystal structures of Cs 2 [Mo 6 X 14 ] (X = Cl, Br, I) cluster-based compounds were investigated by density functional theory (DFT) simulations and experimental methods such as powder X-ray diffraction, ultraviolet-visible spectroscopy, and X-ray photoemission spectroscopy (XPS). The experimentally determined lattice parameters were in good agreement with theoretically optimized ones, indicating the usefulness of DFT calculations for the structural investigation of these clusters. The calculated band gaps of these compounds reproduced those experimentally determined by UV-vis reflectance within an error of a few tenths of an eV. Core-level XPS and effective charge analyses indicated bonding states of the halogens changed according to their sites. The XPS valence spectra were fairly well reproduced by simulations based on the projected electron density of states weighted with cross sections of Al K α , suggesting that DFT calculations can predict the electronic properties of metal-cluster-based crystals with good accuracy.

X-ray Photoelectron Spectroscopy Database (Version 4.1)

National Institute of Standards and Technology Data Gateway

SRD 20 X-ray Photoelectron Spectroscopy Database (Version 4.1) (Web, free access)   The NIST XPS Database gives access to energies of many photoelectron and Auger-electron spectral lines. The database contains over 22,000 line positions, chemical shifts, doublet splittings, and energy separations of photoelectron and Auger-electron lines.

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.

Surface Functionalization of Diamond Films by Photoreaction of Elemental Sulfur and Their Surface Properties

NASA Astrophysics Data System (ADS)

Nakamura, Takako; Ohana, Tsuguyori

2012-08-01

A useful method for direct sulfurization of diamond film surfaces by photoreaction of elemental sulfur was developed. The introduction of thiol groups onto the diamond films was confirmed by X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, and scanning electron microscopy (SEM) analyses. The sulfur-modified diamond films attached to gold nanoparticles by self-assembly. The degrees of thiol group introduction and gold attachment were found to depend on photoirradiation time by monitoring by XPS. The gold-modified diamond film was observed to act as a surface-enhanced Raman scattering substrate for measurement of picric acid.

A study of the UV and VUV degradation of FEP

NASA Technical Reports Server (NTRS)

George, Graeme A.; Hill, David J. T.; Odonnell, James H.; Pomery, Peter J.; Rasoul, Firas A.

1993-01-01

UV and VUV degradation of fluorinated ethylene propylene (FEP) copolymer was studied using electron spin resonance (ESR) spectroscopy, x-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). The ESR study revealed the formation of a terminal polymer radical. The stability of this radical was investigated under different environments. An XPS study of FEP film exposed to VUV and atomic oxygen showed that oxidation takes place on the polymer surface. The study revealed also that the percentage of CF2 in the polymer surface decreased with exposure time and the percentage of CF, CF3, and carbon attached to oxygen increased. SEM micrographs of FEP film exposed to VUV and atomic oxygen identified a rough surface with undulations similar to sand dunes.

X-ray photoelectron and mass spectroscopic study of electron irradiation and thermal stability of polytetrafluoroethylene

NASA Technical Reports Server (NTRS)

Wheeler, Donald R.; Pepper, Stephen V.

1990-01-01

Polytetrafluoroethylene (PTFE) was subjected to 3 keV electron bombardment and then heated in vacuum to 300 C. The behavior of the material as a function of radiation dose and temperature was studied by X-ray photoelectron spectroscopy (XPS) of the surface and mass spectroscopy of the species evolved. A quantitative comparison of the radiation dose rate with that in other reported studies showed that, for a given total dose, the damage observed by XPS is greater for higher dose rates. Lightly damaged material heated to 300 C evolved saturated fluorocarbon species, whereas unsaturated fluorocarbon species evolved from heavily damaged material. After heating the heavily damaged material, those features in the XPS that were associated with damage diminished, giving the appearance that the radiation damage annealed. The apparent annealing of the radiation damage was found to be due to the covering of the network by saturated fragments that easily diffused through the decomposed material to the surface region upon heating.

Scanning electron and atomic force microscopy, and raman and x-ray photoelectron spectroscopy characterization of near-isogenic soft and hard wheat kernels and corresponding flours

USDA-ARS?s Scientific Manuscript database

Atomic force microscopy (AFM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) are used to investigate vitreous (hard) and non-vitreous (soft) wheat kernels and their corresponding wheat flours. AFM data reveal two different microstructures. The vitreous kernel reveals a granular text...

A New NIST Database for the Simulation of Electron Spectra for Surface Analysis (SESSA): Application to Angle-Resolved X-ray Photoelectron Spectroscopy of HfO2, ZrO2, HfSiO4, and ZrSiO4 Films on Silicon

NASA Astrophysics Data System (ADS)

Powell, C. J.; Smekal, W.; Werner, W. S. M.

2005-09-01

We describe a new NIST database for the Simulation of Electron Spectra for Surface Analysis (SESSA). This database provides data for the many parameters needed in quantitative Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). In addition, AES and XPS spectra can be simulated for layered samples. The simulated spectra, for layer compositions and thicknesses specified by the user, can be compared with measured spectra. The layer compositions and thicknesses can then be adjusted to find maximum consistency between simulated and measured spectra. In this way, AES and XPS can provide more detailed characterization of multilayer thin-film materials. We report on the use of SESSA for determining the thicknesses of HfO2, ZrO2, HfSiO4, and ZrSiO4 films on Si by angle-resolved XPS. Practical effective attenuation lengths (EALs) have been computed from SESSA as a function of film thickness and photoelectron emission angle (i.e., to simulate the effects of tilting the sample). These EALs have been compared with similar values obtained from the NIST Electron Effective-Attenuation-Length Database (SRD 82). Generally good agreement was found between corresponding EAL values, but there were differences for film thicknesses less than the inelastic mean free path of the photoelectrons in the overlayer film. These differences are due to a simplifying approximation in the algorithm used to compute EALs in SRD 82. SESSA, with realistic cross sections for elastic and inelastic scattering in the film and substrate materials, is believed to provide more accurate EALs than SRD 82 for thin-film thickness measurements, particularly in applications where the film and substrate have different electron-scattering properties.

A New NIST Database for the Simulation of Electron Spectra for Surface Analysis (SESSA): Application to Angle-Resolved X-ray Photoelectron Spectroscopy of HfO2, ZrO2, HfSiO4, and ZrSiO4 Films on Silicon

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

Powell, C.J.; Smekal, W.; Werner, W.S.M.

2005-09-09

We describe a new NIST database for the Simulation of Electron Spectra for Surface Analysis (SESSA). This database provides data for the many parameters needed in quantitative Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). In addition, AES and XPS spectra can be simulated for layered samples. The simulated spectra, for layer compositions and thicknesses specified by the user, can be compared with measured spectra. The layer compositions and thicknesses can then be adjusted to find maximum consistency between simulated and measured spectra. In this way, AES and XPS can provide more detailed characterization of multilayer thin-film materials. Wemore » report on the use of SESSA for determining the thicknesses of HfO2, ZrO2, HfSiO4, and ZrSiO4 films on Si by angle-resolved XPS. Practical effective attenuation lengths (EALs) have been computed from SESSA as a function of film thickness and photoelectron emission angle (i.e., to simulate the effects of tilting the sample). These EALs have been compared with similar values obtained from the NIST Electron Effective-Attenuation-Length Database (SRD 82). Generally good agreement was found between corresponding EAL values, but there were differences for film thicknesses less than the inelastic mean free path of the photoelectrons in the overlayer film. These differences are due to a simplifying approximation in the algorithm used to compute EALs in SRD 82. SESSA, with realistic cross sections for elastic and inelastic scattering in the film and substrate materials, is believed to provide more accurate EALs than SRD 82 for thin-film thickness measurements, particularly in applications where the film and substrate have different electron-scattering properties.« less

Characterization of BN rich layer on ammonia treated Nextel{trademark}312 fibers

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

Khasgiwale, N.R.; Butler, E.P.; Tsakalakos, L.

A BN rich layer grown on Nextel{trademark}312 fibers by appropriate ammonia treatments was evaluated using various complimentary techniques including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM)/Parallel Electron Energy Loss Spectroscopy (PEELS in TEM). Three different ammonia treatments were studied. Ammonia treatment resulted in crystallization of the Nextel{trademark}312 fiber. The BN rich surface layer formed due to ammonia treatment was clearly detected in XPS and PEELS both before and after oxidation. The layer thickness was estimated to be between 5--10 nm. The layer was stable after oxidation treatment at 600 C formore » 100 hours. High resolution TEM observations of the fiber surface revealed a variable BN rich layer thickness. Patches of turbostratic BN were observed under certain conditions, however mostly the layer appeared to be amorphous.« less

Investigation of nanoparticulate silicon as printed layers using scanning electron microscopy, transmission electron microscopy, X-ray absorption spectroscopy and X-ray photoelectron spectroscopy

DOE PAGES

Unuigbe, David M.; Harting, Margit; Jonah, Emmanuel O.; ...

2017-08-21

The presence of native oxide on the surface of silicon nanoparticles is known to inhibit charge transport on the surfaces. Scanning electron microscopy (SEM) studies reveal that the particles in the printed silicon network have a wide range of sizes and shapes. High-resolution transmission electron microscopy reveals that the particle surfaces have mainly the (111)- and (100)-oriented planes which stabilizes against further oxidation of the particles. X-ray absorption spectroscopy (XANES) and X-ray photoelectron spectroscopy (XPS) measurements at the O 1s-edge have been utilized to study the oxidation and local atomic structure of printed layers of silicon nanoparticles which were milledmore » for different times. XANES results reveal the presence of the +4 (SiO 2) oxidation state which tends towards the +2 (SiO) state for higher milling times. Si 2pXPS results indicate that the surfaces of the silicon nanoparticles in the printed layers are only partially oxidized and that all three sub-oxide, +1 (Si 2O), +2 (SiO) and +3 (Si 2O 3), states are present. The analysis of the change in the sub-oxide peaks of the silicon nanoparticles shows the dominance of the +4 state only for lower milling times.« less

XPS and EELS characterization of Mn2SiO4, MnSiO3 and MnAl2O4

NASA Astrophysics Data System (ADS)

Grosvenor, A. P.; Bellhouse, E. M.; Korinek, A.; Bugnet, M.; McDermid, J. R.

2016-08-01

X-ray Photoelectron Spectroscopy (XPS) and Electron Energy Loss Spectroscopy (EELS) are strong candidate techniques for characterizing steel surfaces and substrate-coating interfaces when investigating the selective oxidation and reactive wetting of advanced high strength steels (AHSS) during the continuous galvanizing process. However, unambiguous identification of ternary oxides such as Mn2SiO4, MnSiO3, and MnAl2O4 by XPS or EELS, which can play a significant role in substrate reactive wetting, is difficult due to the lack of fully characterized standards in the literature. To resolve this issue, samples of Mn2SiO4, MnSiO3 and MnAl2O4 were synthesized and characterized by XPS and EELS. The unique features of the XPS and EELS spectra for the Mn2SiO4, MnSiO3 and MnAl2O4 standards were successfully derived, thereby allowing investigators to fully differentiate and identify these oxides at the surface and subsurface of Mn, Si and Al alloyed AHSS using these techniques.

Characterization of Colloidal Quantum Dot Ligand Exchange by X-ray Photoelectron Spectroscopy

NASA Astrophysics Data System (ADS)

Atewologun, Ayomide; Ge, Wangyao; Stiff-Roberts, Adrienne D.

2013-05-01

Colloidal quantum dots (CQDs) are chemically synthesized semiconductor nanoparticles with size-dependent wavelength tunability. Chemical synthesis of CQDs involves the attachment of long organic surface ligands to prevent aggregation; however, these ligands also impede charge transport. Therefore, it is beneficial to exchange longer surface ligands for shorter ones for optoelectronic devices. Typical characterization techniques used to analyze surface ligand exchange include Fourier-transform infrared spectroscopy, x-ray diffraction, transmission electron microscopy, and nuclear magnetic resonance spectroscopy, yet these techniques do not provide a simultaneously direct, quantitative, and sensitive method for evaluating surface ligands on CQDs. In contrast, x-ray photoelectron spectroscopy (XPS) can provide nanoscale sensitivity for quantitative analysis of CQD surface ligand exchange. A unique aspect of this work is that a fingerprint is identified for shorter surface ligands by resolving the regional XPS spectrum corresponding to different types of carbon bonds. In addition, a deposition technique known as resonant infrared matrix-assisted pulsed laser evaporation is used to improve the CQD film uniformity such that stronger XPS signals are obtained, enabling more accurate analysis of the ligand exchange process.

Improving the oxidation resistance and stability of Ag nanoparticles by coating with multilayered reduced graphene oxide

NASA Astrophysics Data System (ADS)

Li, Yahui; Zhang, Huayu; Wu, Bowen; Guo, Zhuo

2017-12-01

A kind of coating nanostructure, Ag nanoparticles coated with multilayered reduced graphene oxide (RGO), is fabricated by employing a three-step reduction method in an orderly manner, which is significantly different from the conventional structures that are simply depositing or doping with Ag nanoparticles on RGO via chemical reduction. The as-prepared nanostructure is investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electronic diffraction (SEAD), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR). The results show that the obtained Ag/RGO nanostructure is observed to be a perfect coating structure with well dispersed Ag particles, which is responsible for the remarkable oxidation resistance. The results of XPS spectra indicate the content of metallic Ag is far greater than that of Ag oxides despite of prolonged exposure to the air, which fully demonstrate the excellent stability of thus coating nanostructure.

Effects of 160 keV electron irradiation on the optical properties and microstructure of "Panda" type Polarization-Maintaining optical fibers

NASA Astrophysics Data System (ADS)

Hong-Chen, Zhang; Hai, Liu; Hui-Jie, Xue; Wen-Qiang, Qiao; Shi-Yu, He

2012-11-01

In this paper, effects of 160 keV electron irradiated "Panda" type Polarization-Maintaining optical fiber at 1310 nm are investigated by us. Attenuation coefficient induced in optical fiber by electron beams at 1310 nm increases with increase in electron fluence. Electron irradiation-induced damage mechanism are studied by means of CASINO simulation program, the X-ray photoelectron spectroscopy (XPS), electron spin resonance spectrometer (EPR) and Fourier transform infrared spectroscopy (FTIR). The results show that Si-OH impurity defect concentration is the main reason of increasing attenuation coefficient at 1310 nm.

Facile Synthesis and Characterization of ZrO₂ Nanoparticles via Modified Co-Precipitation Method.

PubMed

Ramachandran, M; Subadevi, R; Liu, Wei-Ren; Sivakumar, M

2018-01-01

The crystalline Zirconium oxide (ZrO2) nano particles were synthesized using optimized content of Zirconium nitrate (Zr(NO3)2·3H2O) with varying KOH concentration (0.5, 1 and 1.5 M) by co-precipitation method. The thermal history of the precursor was carefully analyzed through Thermogravimetric (TG/DTA) measurement. The as prepared samples were characterized to ensure structural, functional, morphological, compositional, chemical composition and band gap by X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), Laser Raman, scanning electron microscopy (SEM), High resolution Transverse Electron Microscopy (HR-TEM), X-ray photo electron spectroscopy (XPS), EDX, Photo luminescence spectroscopy (PL). The monoclinic structure with space group P21/c has been confirmed from XRD (JCPDS 89-9066). The Zr-O stretching vibration and Zr-O2-Zr bending vibrations were confirmed through FTIR analysis. The well dispersed particles with spherical morphology were confirmed through SEM and TEM analysis. The oxidation states of Zr, O and C were confirmed through XPS analysis. The oxygen vacancies and band gap of the particles were investigated through PL analysis.

Schottky Barrier Height of Pd/MoS2 Contact by Large Area Photoemission Spectroscopy.

PubMed

Dong, Hong; Gong, Cheng; Addou, Rafik; McDonnell, Stephen; Azcatl, Angelica; Qin, Xiaoye; Wang, Weichao; Wang, Weihua; Hinkle, Christopher L; Wallace, Robert M

2017-11-08

MoS 2 , as a model transition metal dichalcogenide, is viewed as a potential channel material in future nanoelectronic and optoelectronic devices. Minimizing the contact resistance of the metal/MoS 2 junction is critical to realizing the potential of MoS 2 -based devices. In this work, the Schottky barrier height (SBH) and the band structure of high work function Pd metal on MoS 2 have been studied by in situ X-ray photoelectron spectroscopy (XPS). The analytical spot diameter of the XPS spectrometer is about 400 μm, and the XPS signal is proportional to the detection area, so the influence of defect-mediated parallel conduction paths on the SBH does not affect the measurement. The charge redistribution by Pd on MoS 2 is detected by XPS characterization, which gives insight into metal contact physics to MoS 2 and suggests that interface engineering is necessary to lower the contact resistance for the future generation electronic applications.

Raman enhancement by graphene-Ga2O3 2D bilayer film.

PubMed

Zhu, Yun; Yu, Qing-Kai; Ding, Gu-Qiao; Xu, Xu-Guang; Wu, Tian-Ru; Gong, Qian; Yuan, Ning-Yi; Ding, Jian-Ning; Wang, Shu-Min; Xie, Xiao-Ming; Jiang, Mian-Heng

2014-01-28

2D β-Ga2O3 flakes on a continuous 2D graphene film were prepared by a one-step chemical vapor deposition on liquid gallium surface. The composite was characterized by optical microscopy, scanning electron microscopy, Raman spectroscopy, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy (XPS). The experimental results indicate that Ga2O3 flakes grew on the surface of graphene film during the cooling process. In particular, tenfold enhancement of graphene Raman scattering signal was detected on Ga2O3 flakes, and XPS indicates the C-O bonding between graphene and Ga2O3. The mechanism of Raman enhancement was discussed. The 2D Ga2O3-2D graphene structure may possess potential applications.

Thickness and composition of ultrathin SiO2 layers on Si

NASA Astrophysics Data System (ADS)

van der Marel, C.; Verheijen, M. A.; Tamminga, Y.; Pijnenburg, R. H. W.; Tombros, N.; Cubaynes, F.

2004-07-01

Ultrathin SiO2 layers are of importance for the semiconductor industry. One of the techniques that can be used to determine the chemical composition and thickness of this type of layers is x-ray photoelectron spectroscopy (XPS). As shown by Seah and Spencer [Surf. Interface Anal. 33, 640 (2002)], it is not trivial to characterize this type of layer by means of XPS in a reliable way. We have investigated a series of ultrathin layers of SiO2 on Si (in the range from 0.3 to 3 nm) using XPS. The samples were also analyzed by means of transmission electron microscopy (TEM), Rutherford backscattering (RBS), and ellipsometry. The thickness of the SiO2 layers (d) was determined from the XPS results using three different approaches: the ``standard'' equation (Seah and Spencer) for d, an overlayer-substrate model calculation, and the QUASES-Tougaard [Surf. Interface Anal. 26, 249 (1998), QUASES-Tougaard: Software package for Quantitative Analysis of Surfaces by Electron Spectroscopy, version 4.4 (2000); http://www.quases.com] method. Good agreement was obtained between the results of XPS analyses using the ``standard'' equation, the overlayer-substrate model calculation, and RBS results. The QUASES-Tougaard results were approximately 62% above the other XPS results. The optical values for the thickness were always slightly higher than the thickness according to XPS or RBS. Using the model calculation, these (relatively small) deviations from the optical results could be explained as being a consequence of surface contaminations with hydrocarbons. For a thickness above 2.5 nm, the TEM results were in good agreement with the results obtained from the other techniques (apart from QUASES-Tougaard). Below 2.5 nm, significant deviations were found between RBS, XPS, and optical data on the one hand and TEM results on the other hand; the deviations became larger as the thickness of the SiO2 decreased. This effect may be related to interface states of oxygen, which have been investigated [D. A. Muller, T. Sorsch, S. Moccio, F. H. Baumann, K. Evans-Lutterodt, and G. Timp, Nature (London) 399, 758 (1999); D. A. Muller and J. B. Neaton, Structure and Energetics of the Interface Between Si and Amorphous SiO2 in Fundamental Aspects of Silicon Oxidation, edited by Y. J. Chabal (Springer, Berlin, 2001), pp. 219-246.] by means of high-resolution electron energy loss spectroscopy measurements of the O K edge in ultrathin gate oxides of SiO2. .

Epitaxial corundum-VTiO 3 thin films grown on c-cut sapphire

DOE PAGES

Kramer, Alan; Sutter, Eli; Su, Dong; ...

2017-04-12

Corundum structured VTiO 3 has been grown as epitaxial films on c-cut sapphire by laser molecular beam epitaxy. The properties of the film were characterized by reflection high energy electron diffraction, x-ray diffraction, transmission electron microscopy, and photoemission spectroscopy. All the structural probes clearly indicate the corundum structure of the film. X-ray photoemission spectroscopy (XPS) indicates that V is in a 3+ charge state implying that Ti also needs to adopt a 3+ charge state in order for the corundum structure to form. However, the Ti-2p XPS, while clearly broadened to the lower binding energy side compared to TiO 2,more » also exhibits a pronounced Ti 4+ component. This is tentatively assigned to a final state effect in XPS measurements and not as the true cation state. In conclusion, the valence band spectra show occupation of 3d metal states that resemble more closely those of Ti 2O 3 than for V 2O 3, suggesting that only the a1g molecular states are occupied.« less

Redirected charge transport arising from diazonium grafting of carbon coated LiFePO4.

PubMed

Madec, L; Seid, K A; Badot, J-C; Humbert, B; Moreau, P; Dubrunfaut, O; Lestriez, B; Guyomard, D; Gaubicher, J

2014-11-07

The morphological and the electrical properties of carbon coated LiFePO4 (LFPC) active material functionalized by 4-ethynylbenzene tetrafluoroboratediazonium salt were investigated. For this purpose, FTIR, Raman, XPS, High Resolution Transmission Electron Microscopy (HRTEM) and Broadband Dielectric Spectroscopy (BDS) were considered. Electronic conductivities of LFPC samples at room temperature were found to decrease in a large frequency range upon simple immersion in polar solvents and to decrease further upon functionalization. Due to their high dipole moment, strongly physisorbed molecules detected by XPS likely add barriers to electron hopping. Significant alteration of the carbon coating conductivity was only observed, however, upon functionalization. This effect is most presumably associated with an increase in the sp(3) content determined by Raman spectroscopy, which is a strong indication of the formation of a covalent bond between the organic layer and the carbon coating. In this case, the electron flux appears to be redirected and relayed by short-range (intra chain) and long-range (inter chain) electron transport through molecular oligomers anchored at the LFPC surface. The latter are controlled by tunnelling and slightly activated hopping, which enable higher conductivity at low temperature (T < 250 K). Alteration of the electron transport within the carbon coating also allows detection of a relaxation phenomenon that corresponds to small polaron hopping in bulk LiFePO4. XPS and HRTEM images allow a clear correlation of these findings with the island type oligomeric structure of grafted molecules.

Effect of intrinsic electronic defect states on the morphology and optoelectronic properties of Sn-rich SnS particles

NASA Astrophysics Data System (ADS)

Singh, Chetan C.; Panda, Emila

2018-05-01

A small variation in the elemental composition of a chemical compound can cause the formation of additional electronic defect states in the material, thereby altering the overall microstructure and thus induced properties. In this work, we observed chemical constitution-induced modification in the morphology and optoelectronic properties of SnS. To this end, SnS particles were prepared using the solution chemical route and were characterized using a wide range of experimental techniques, such as x-ray diffractometry, field emission scanning electron microscopy, high resolution transmission electron microscopy, energy dispersive spectroscopy (EDS), x-ray photoelectron spectroscopy (XPS), UV-Vis spectrophotometry, and scanning tunneling spectroscopy (STS). All these SnS particles are found to be Sn-rich and p-type. However, distinctly different morphologies (i.e., flower-like and aggregated ones) are observed. These are then correlated with the electronic defect states, which are induced because of the presence of Sn vacancies, Sn antisites, and/or Sn interstitials. A combination of EDS, XPS, and STS data confirmed the presence of a higher concentration of Sn vacancies along with lower quantities of Sn interstitials and/or antisites in the SnS particles with flower-like morphologies giving rise to higher hole concentration, which subsequently leads to reduced transport, optical band gaps, and barrier heights.

Electronic structure evolution in doping of fullerene (C{sub 60}) by ultra-thin layer molybdenum trioxide

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

Wang, Chenggong; Wang, Congcong; Kauppi, John

2015-08-28

Ultra-thin layer molybdenum oxide doping of fullerene has been investigated using ultraviolet photoemission spectroscopy (UPS) and X-ray photoemission spectroscopy (XPS). The highest occupied molecular orbital (HOMO) can be observed directly with UPS. It is observed that the Fermi level position in fullerene is modified by ultra-thin-layer molybdenum oxide doping, and the HOMO onset is shifted to less than 1.3 eV below the Fermi level. The XPS results indicate that charge transfer was observed from the C{sub 60} to MoO{sub x} and Mo{sup 6+} oxides is the basis as hole dopants.

Structure and magnetic properties of mono- and bi-layer graphene films on ultraprecision figured 4H-SiC(0001) surfaces.

PubMed

Hattori, Azusa N; Okamoto, Takeshi; Sadakuni, Shun; Murata, Junji; Oi, Hideo; Arima, Kenta; Sano, Yasuhisa; Hattori, Ken; Daimon, Hiroshi; Endo, Katsuyoshi; Yamauchi, Kazuto

2011-04-01

Monolayer and bilayer graphene films with a few hundred nm domain size were grown on ultraprecision figured 4H-SiC(0001) on-axis and 8 degrees -off surfaces by annealing in ultra-high vacuum. Using X-ray photoelectron spectroscopy (XPS), atomic force microscopy, reflection high-energy electron diffraction, low-energy electron diffraction (LEED), Raman spectroscopy, and scanning tunneling microscopy, we investigated the structure, number of graphene layers, and chemical bonding of the graphene surfaces. Moreover, the magnetic property of the monolayer graphene was studied using in-situ surface magneto-optic Kerr effect at 40 K. LEED spots intensity distribution and XPS spectra for monolayer and bilayer graphene films could become an obvious and accurate fingerprint for the determination of graphene film thickness on SiC surface.

Green synthesis of nitrogen-doped graphitic carbon sheets with use of Prunus persica for supercapacitor applications

NASA Astrophysics Data System (ADS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Perumal, Suguna; Lee, Yong Rok

2017-01-01

Nitrogen-doped graphitic carbon sheets (N-GCSs) were prepared from the extract of unripe Prunus persica fruit by a direct hydrothermal method. The synthesized N-GCSs were examined by high resolution transmission electron microscopy (HRTEM), nitrogen adsorption-desorption isotherms, X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FT-IR) spectroscopy. HRTEM showed that the synthesized carbon sheets were graphitic with lattice fringes and an inter-layer distance of 0.36 nm. Doping with the nitrogen moiety present over the synthesized GCSs was confirmed by XPS, FT-IR spectroscopy, and energy dispersive X-ray spectroscopy elemental mapping. The fruit extract associated with hydrothermal-carbonization method is economical and eco-friendly with a single step process. The resulting carbon sheets could be modified and are promising candidates for nano-electronic applications, including supercapacitors. The synthesized N-GCSs-2 provided a high specific capacitance of 176 F g-1 at a current density of 0.1 A g-1. This electrode material has excellent cyclic stability, even after 2000 cycles of charge-discharge at a current density of 0.5 A g-1.

Soft x-ray spectroscopy studies of novel electronic materials using synchrotron radiation

NASA Astrophysics Data System (ADS)

Newby, David, Jr.

Soft x-ray spectroscopy can provide a wealth of information on the electronic structure of solids. In this work, a suite of soft x-ray spectroscopies is applied to organic and inorganic materials with potential applications in electronic and energy generation devices. Using the techniques of x-ray absorption (XAS), x-ray emission spectroscopy (XES), and x-ray photoemission spectroscopy (XPS), the fundamental properties of these different materials are explored. Cycloparaphenylenes (CPPs) are a recently synthesized family of cyclic hydrocarbons with very interesting properties and many potential applications. Unusual UV/Visible fluorescence trends have spurred a number of theoretical investigations into the electronic properties of the CPP family, but thus far no comprehensive electronic structure measurements have been conducted. XPS, XAS, and XES data for two varieties, [8]- and [10]-CPP, are presented here, and compared with the results of relevant DFT calculations. Turning towards more application-centered investigations, similar measurements are applied to two materials commonly used in solid oxide fuel cell (SOFC) cathodes: La1-xSrxMnO 3 (LSMO) and La1-xSr1- xCo1-yFe yO3 (LSCF). Both materials are structurally perovskites, but they exhibit strikingly different electronic properties. SOFC systems very efficiently produce electricity by catalyzing reactions between oxygen and petroleum-based hydrocarbons at high temperatures (> 800 C). Such systems are already utilized to great effect in many industries, but more widespread adoption could be had if the cells could operate at lower temperatures. Understanding the electronic structure and operational evolution of the cathode materials is essential for the development of better low-temperature fuel cells. LSCF is a mixed ion-electron conductor which holds promise for low-temperature SOFC applications. XPS spectra of LSCF thin films are collected as the films are heated and gas-dosed in a controlled environment. The surface evolution of these films is discussed, and the effects of different gas environments on oxygen vacancy concentration are elucidated. LSMO is commonly used in commercial fuel cell devices. Here the resonant soft x-ray emission (RIXS) spectrum of LSMO is examined, and it is shown that the inelastic x-ray emission structure of LSMO arises from local atomic multiplet effects.

A comparative theoretical study on core-hole excitation spectra of azafullerene and its derivatives

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

Deng, Yunfeng; Department of Physics, Guizhou University, Guiyang 550025; Gao, Bin, E-mail: bin.gao@uit.no

2014-03-28

The core-hole excitation spectra—near-edge x-ray absorption spectroscopy (NEXAFS), x-ray emission spectroscopy (XES), and x-ray photoelectron spectroscopy (XPS) shake-up satellites have been simulated at the level of density functional theory for the azafullerene C{sub 59}N and its derivatives (C{sub 59}N){sup +}, C{sub 59}HN, (C{sub 59}N){sub 2}, and C{sub 59}N–C{sub 60}, in which the XPS shake-up satellites were simulated using our developed equivalent core hole Kohn-Sham (ECH-KS) density functional theory approach [B. Gao, Z. Wu, and Y. Luo, J. Chem. Phys. 128, 234704 (2008)] which aims for the study of XPS shake-up satellites of large-scale molecules. Our calculated spectra are generally inmore » good agreement with available experimental results that validates the use of the ECH-KS method in the present work. The nitrogen K-edge NEXAFS, XES, and XPS shake-up satellites spectra in general can be used as fingerprints to distinguish the azafullerene C{sub 59}N and its different derivatives. Meanwhile, different carbon K-edge spectra could also provide detailed information of (local) electronic structures of different molecules. In particular, a peak (at around 284.5 eV) in the carbon K-edge NEXAFS spectrum of the heterodimer C{sub 59}N–C{sub 60} is confirmed to be related to the electron transfer from the C{sub 59}N part to the C{sub 60} part in this charge-transfer complex.« less

Impact of ambient environment on the electronic structure of CuPc/Au sample

NASA Astrophysics Data System (ADS)

Sinha, Sumona; Mukherjee, M.

2018-02-01

The performances of organic devices are crucially connected with their stability in the ambient environment. The impact of 24 h. Ambient environment exposure to the electronic structures of about 12 nm thick CuPc thin film on clean Au substrate have been studied employing UV photoemission spectroscopy technique. X-ray photoemission spectroscopy (XPS) was used to find out the origin of the change of the electronic structures in the sample with the exposure. The XPS study suggests that the oxidation occurs at the CuPc thin film. Due to the adsorption of oxygen in the CuPc film from the ambient air, charge carriers are formed within the CuPc film. Moreover, the XPS results imply that the CuPc film is sufficiently thinner for diffusing oxygen molecules through it and gets physically absorbed on Au substrate during the ambient exposure. Consequently, the hole injection barrier height of pristine CuPc film, grown on Au substrate, is reduced by about 0.50 eV and work-function of the pristine CuPc sample is enhanced by around 0.25 eV in the exposure. The findings will help to understand the mechanism that governs the degradation of performance of CuPc based devices in ambient environment.

A simple method to synthesize polyhedral hexagonal boron nitride nanofibers

NASA Astrophysics Data System (ADS)

Lin, Liang-xu; Zheng, Ying; Li, Zhao-hui; shen, Xiao-nv; Wei, Ke-mei

2007-12-01

Hexagonal boron nitride (h-BN) fibers with polyhedral morphology were synthesized with a simple-operational, large-scale and low-cost method. The sample obtained was studied by X-ray photoelectron spectrometer (XPS), electron energy lose spectroscopy (EELS), X-ray powder diffraction (XRD), Fourier transformation infrared spectroscopy (FT-IR), etc., which matched with h-BN. Environment scanning electron microscopy (ESEM) and transmission electron microscope (TEM) indicated that the BN fibers possess polyhedral morphology. The diameter of the BN fibers is mainly in the range of 100-500 nm.

Raman enhancement by graphene-Ga2O3 2D bilayer film

PubMed Central

2014-01-01

2D β-Ga2O3 flakes on a continuous 2D graphene film were prepared by a one-step chemical vapor deposition on liquid gallium surface. The composite was characterized by optical microscopy, scanning electron microscopy, Raman spectroscopy, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy (XPS). The experimental results indicate that Ga2O3 flakes grew on the surface of graphene film during the cooling process. In particular, tenfold enhancement of graphene Raman scattering signal was detected on Ga2O3 flakes, and XPS indicates the C-O bonding between graphene and Ga2O3. The mechanism of Raman enhancement was discussed. The 2D Ga2O3-2D graphene structure may possess potential applications. PMID:24472433

Chrome-free Samarium-based Protective Coatings for Magnesium Alloys

NASA Astrophysics Data System (ADS)

Hou, Legan; Cui, Xiufang; Yang, Yuyun; Lin, Lili; Xiao, Qiang; Jin, Guo

The microstructure of chrome-free samarium-based conversion coating on magnesium alloy was investigated and the corrosion resistance was evaluated as well. The micro-morphology, transverse section, crystal structure and composition of the coating were observed by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS) and X- ray photoelectron spectroscopy (XPS), respectively. The corrosion resistance was evaluated by potentiodynamic polarization curve and electrochemical impedance spectroscopy (EIS). The results reveal that the morphology of samarium conversion coating is of crack-mud structure. Tiny cracks distribute in the compact coating deposited by samarium oxides. XRD, EDS and XPS results characterize that the coating is made of amorphous and trivalent-samarium oxides. The potentiodynamic polarization curve, EIS and OCP indicate that the samarium conversion coating can improve the corrosion resistance of magnesium alloys.

Facile fabrication of BiVO4 nanofilms with controlled pore size and their photoelectrochemical performances

NASA Astrophysics Data System (ADS)

Feng, Chenchen; Jiao, Zhengbo; Li, Shaopeng; Zhang, Yan; Bi, Yingpu

2015-12-01

We demonstrate a facile method for the rational fabrication of pore-size controlled nanoporous BiVO4 photoanodes, and confirmed that the optimum pore-size distributions could effectively absorb visible light through light diffraction and confinement functions. Furthermore, in situ X-ray photoelectron spectroscopy (XPS) reveals more efficient photoexcited electron-hole separation than conventional particle films, induced by light confinement and rapid charge transfer in the inter-crossed worm-like structures.We demonstrate a facile method for the rational fabrication of pore-size controlled nanoporous BiVO4 photoanodes, and confirmed that the optimum pore-size distributions could effectively absorb visible light through light diffraction and confinement functions. Furthermore, in situ X-ray photoelectron spectroscopy (XPS) reveals more efficient photoexcited electron-hole separation than conventional particle films, induced by light confinement and rapid charge transfer in the inter-crossed worm-like structures. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr06584d

Electrochemically Controlled Ion-exchange Property of Carbon Nanotubes/Polypyrrole Nanocomposite in Various Electrolyte Solutions

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

Choi, Daiwon; Zhu, Chengzhou; Fu, Shaofang

2016-09-15

The electrochemically controlled ion-exchange properties of multi-wall carbon nanotube (MWNT)/electronically conductive polypyrrole (PPy) polymer composite in the various electrolyte solutions have been investigated. The ion-exchange behavior, rate and capacity of the electrochemically deposited polypyrrole with and without carbon nanotube (CNT) were compared and characterized using cyclic voltammetry (CV), chronoamperometry (CA), electrochemical quartz crystal microbalance (EQCM), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). It has been found that the presence of carbon nanotube backbone resulted in improvement in ion-exchange rate, stability of polypyrrole, and higher anion loading capacity per PPy due to higher surface area, electronic conductivity, porous structuremore » of thin film, and thinner film thickness providing shorter diffusion path. Chronoamperometric studies show that electrically switched anion exchange could be completed more than 10 times faster than pure PPy thin film. The anion selectivity of CNT/PPy film is demonstrated using X-ray photoelectron spectroscopy (XPS).« less

Hexadecylamine Adsorption at the Iron Oxide–Oil Interface

PubMed Central

2013-01-01

The adsorption behavior of a model additive, hexadecylamine, onto an iron surface from hexadecane oil has been characterized using polarized neutron reflectometry, sum-frequency generation spectroscopy, solution depletion isotherm, and X-ray photoelectron spectroscopy (XPS). The amine showed a strong affinity for the metal surface, forming a dense monolayer at relatively low concentrations; a layer thickness of 16 (±3) Å at low concentrations, increasing to 20 (±3) Å at greater amine concentrations, was determined from the neutron data. These thicknesses suggest that the molecules in the layer are tilted. Adsorption was also indicated by sum-frequency generation spectroscopy and XPS, the latter indicating that the most dominant amine–surface interaction was via electron donation from the nitrogen lone pair to the positively charged iron ions. Sum-frequency generation spectroscopy was used to determine the alkyl chain conformation order and orientation on the surface. PMID:24106786

Tunable Stoichiometry of BCxNy Thin Films Through Multitarget Pulsed Laser Deposition Monitored via In Situ Ellipsometry (Postprint)

DTIC Science & Technology

2014-02-05

X - ray photoelectron spectroscopy (XPS), Raman spectroscopy , and atomic ...calculate thickness, n and k. X - ray photoelectron spectroscopy (XPS), Raman spectroscopy , and atomic force microscopy (AFM) were all performed on each of the... X - ray photoelectron spectroscopy (XPS) and Raman spectroscopy were used to measure and compare the composition of the films.6 In this paper,

Morphological, chemical and structural characterisation of deciduous enamel: SEM, EDS, XRD, FTIR and XPS analysis.

PubMed

Zamudio-Ortega, C M; Contreras-Bulnes, R; Scougall-Vilchis, R J; Morales-Luckie, R A; Olea-Mejía, O F; Rodríguez-Vilchis, L E

2014-09-01

The purpose of this study was to characterise the enamel surface of sound deciduous teeth in terms of morphology, chemical composition, structure and crystalline phases. The enamel of 30 human deciduous teeth was examined by: Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), X-ray Powder Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and X-ray Photoelectron Spectroscopy (XPS). Chemical differences between incisors and canines were statistically evaluated using the Mann-Whitney U test (p ≤ 0.05). Three enamel patterns were observed by SEM: 'mostly smooth with some groves', 'abundant microporosities' and 'exposed prisms'. The average Ca/P molar ratios were 1.37 and 1.03 by EDS and XPS, respectively. The crystallite size determined by XRD was 210.82 ± 16.78 Å. The mean ratio between Ca bonded to phosphate and Ca bonded to hydroxyl was approximately 10:1. The enamel of sound deciduous teeth showed two main patterns: 'mostly smooth with some groves' and 'abundant microporosities'. 'Exposed prisms' was a secondary pattern. There were slight variations among the Ca/P molar ratios found by EDS and XPS, suggesting differences in the mineral content from the enamel surface to the interior. The crystalline phases found in enamel were hydroxyapatite and carbonate apatite, with major type B than type A carbonate incorporation.

Electronic structure of the indium tin oxide/nanocrystalline anatase (TiO2)/ruthenium-dye interfaces in dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Lyon, J. E.; Rayan, M. K.; Beerbom, M. M.; Schlaf, R.

2008-10-01

The electronic structure of two interfaces commonly found in dye-sensitized photovoltaic cells based on nanocrystalline anatase TiO2 ("Grätzel cells") was investigated using photoemission spectroscopy (PES). X-ray photoemission spectroscopy (XPS) and ultraviolet photoemission spectroscopy (UPS) measurements were carried out on the indium tin oxide (ITO)/TiO2 and the TiO2/cis-bis(isothiocyanato)bis(2,2'-bipyridyl-4,4'-dicarboxylato)-ruthenium(II)bis-tetrabutylammonium dye ("N719" or "Ruthenium 535-bisTBA") interfaces. Both contacts were investigated using a multistep deposition procedure where the entire structure was prepared in vacuum using electrospray deposition. In between deposition steps the surface was characterized with XPS and UPS resulting in a series of spectra, allowing the determination of the orbital and band lineup at the interfaces. The results of these efforts confirm previous PES measurements on TiO2/dye contacts prepared under ambient conditions, suggesting that ambient contamination might not have significant influence on the electronic structure at the dye/TiO2 interface. The results also demonstrate that there may be a significant barrier for electron injection at the sputtered ITO/TiO2 interface and that this interface should be viewed as a semiconductor heterojunction rather than as metal-semiconductor (Schottky) contact.

Hydrothermal Synthesis and Biocompatibility Study of Highly Crystalline Carbonated Hydroxyapatite Nanorods

NASA Astrophysics Data System (ADS)

Xue, Caibao; Chen, Yingzhi; Huang, Yongzhuo; Zhu, Peizhi

2015-08-01

Highly crystalline carbonated hydroxyapatite (CHA) nanorods with different carbonate contents were synthesized by a novel hydrothermal method. The crystallinity and chemical structure of synthesized nanorods were studied by Fourier transform infrared spectroscopy (FTIR), X-ray photo-electronic spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM). The biocompatibility of synthesized CHA nanorods was evaluated by cell viability and alkaline phosphatase (ALP) activity of MG-63 cell line. The biocompatibility evaluation results show that these CHA nanorods are biologically active apatites and potentially promising bone-substitute biomaterials for orthopedic application.

Facile green synthesis of fluorescent N-doped carbon dots from Actinidia deliciosa and their catalytic activity and cytotoxicity applications

NASA Astrophysics Data System (ADS)

Arul, Velusamy; Sethuraman, Mathur Gopalakrishnan

2018-04-01

Green synthesis of fluorescent nitrogen doped carbon dots (N-CDs) using Actinidia deliciosa (A. deliciosa) fruit extract as a carbon precursor and aqueous ammonia as a nitrogen dopant is reported here. The synthesized N-CDs were characterized by high resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), UV-Visible spectroscopy (UV-Vis), fluorescence spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The average size of the N-CDs was approximately 3.59 nm and the calculated inter layer distance was found to be 0.21 nm. Raman spectroscopy and SAED pattern revealed the graphitic nature of the synthesized N-CDs. The N-CDs were found to emit intense blue color at 405 nm under the excitation of 315 nm. The doping of nitrogen over the surface of the N-CDs was confirmed by EDS, FT-IR and XPS studies. The synthesized N-CDs were found to exhibit excellent catalytic activity in the reduction of Rhodamine-B using sodium borohydrate. The MTT assay was used to evaluate the cytotoxicity and biocompatibility of N-CDs towards L-929 and MCF-7 cells. From the results obtained, it was found that the N-CDs exhibit low cytotoxicity and superior biocompatibility on both L-929 and MCF-7 cells.

Kinetics of electron-induced decomposition of CF2Cl2 coadsorbed with water (ice): A comparison with CCl4

NASA Astrophysics Data System (ADS)

Faradzhev, N. S.; Perry, C. C.; Kusmierek, D. O.; Fairbrother, D. H.; Madey, T. E.

2004-11-01

The kinetics of decomposition and subsequent chemistry of adsorbed CF2Cl2, activated by low-energy electron irradiation, have been examined and compared with CCl4. These molecules have been adsorbed alone and coadsorbed with water ice films of different thicknesses on metal surfaces (Ru; Au) at low temperatures (25 K; 100 K). The studies have been performed with temperature programmed desorption (TPD), reflection absorption infrared spectroscopy (RAIRS), and x-ray photoelectron spectroscopy (XPS). TPD data reveal the efficient decomposition of both halocarbon molecules under electron bombardment, which proceeds via dissociative electron attachment (DEA) of low-energy secondary electrons. The rates of CF2Cl2 and CCl4 dissociation increase in an H2O (D2O) environment (2-3×), but the increase is smaller than that reported in recent literature. The highest initial cross sections for halocarbon decomposition coadsorbed with H2O, using 180 eV incident electrons, are measured (using TPD) to be 1.0±0.2×10-15 cm2 for CF2Cl2 and 2.5±0.2×10-15 cm2 for CCl4. RAIRS and XPS studies confirm the decomposition of halocarbon molecules codeposited with water molecules, and provide insights into the irradiation products. Electron-induced generation of Cl- and F- anions in the halocarbon/water films and production of H3O+, CO2, and intermediate compounds COF2 (for CF2Cl2) and COCl2, C2Cl4 (for CCl4) under electron irradiation have been detected using XPS, TPD, and RAIRS. The products and the decomposition kinetics are similar to those observed in our recent experiments involving x-ray photons as the source of ionizing irradiation.

X-PEEM, XPS and ToF-SIMS characterisation of xanthate induced chalcopyrite flotation: Effect of pulp potential

NASA Astrophysics Data System (ADS)

Kalegowda, Yogesh; Chan, Yuet-Loy; Wei, Der-Hsin; Harmer, Sarah L.

2015-05-01

Synchrotron-based X-ray photoemission electron microscopy (X-PEEM), X-ray photo-electron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and ultraviolet visible spectroscopy were used to characterize the flotation behaviour of chalcopyrite with xanthate at different processing conditions. The flotation recovery of chalcopyrite decreased from 97% under oxidative conditions (Eh ~ 385 mV SHE, pH 4) to 41% at a reductive potential of - 100 mV SHE (at pH 9). X-PEEM images constructed from the metal L3 absorption edges were used to produce near-edge X-ray absorption fine structure (NEXAFS) spectra from regions of interest, allowing the variability in mineral surface chemistry of each mineral particle to be analysed, and the effect of pulp potential (Eh) on the flotation of chalcopyrite to be determined. XPS, ToF-SIMS and NEXAFS analyses of chalcopyrite particles at oxidative conditions show that the surface was mildly oxidised and covered with adsorbed molecular CuEX. The Cu 2p XPS and Cu L2,3 NEXAFS spectra were dominated by CuI species attributed to bulk chalcopyrite and adsorbed CuEX. At a reductive potential of - 100 mV SHE, an increase in concentration of CuI and FeIII oxides and hydroxides was observed. X-PEEM analysis was able to show the presence of a low percentage of CuII oxides (CuO or Cu(OH)2) with predominantly CuI oxide (Cu2O) which is not evident in Cu 2p XPS spectra.

New Generation Materials and Structures for Nanophotonics and Nanoelectronics

DTIC Science & Technology

2006-04-30

been investigated using thermogravimetric analysis and FTIR spectroscopy. The nanoparticles appear to have excess surfactants on their surface, but...processes. We continued analysis of the vibrational modes of the InP/II- VI core-shell nanoparticles determined by IR and Raman studies, and initiated...photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), BET surface area analysis , transmission electron microscopy (TEM), and SQUID magnetometry. In

UHV AFM based colloidal probe studies of adhesive properties of VAlN hard coatings

NASA Astrophysics Data System (ADS)

Wiesing, M.; de los Arcos, T.; Grundmeier, G.

2018-01-01

The adhesion of polystyrene (PS) on V0.27Al0.29N0.44 and the related influence of the oxidation states of both surfaces was investigated using X-Ray Photoelectron Spectroscopy (XPS) and Colloidal Force Spectroscopy (CFS) in Ultra-High Vacuum (UHV). Complementary, the intimate relation between the adhesion force, the chemical structure and surface polarizability was investigated by XPS valence band spectroscopy and the calculation of non-retarded Hamaker coefficients using Lifshitz theory based on optical data as derived from Reflection Electron Energy Loss Spectroscopy (REELS) spectra. The combined electron and force spectroscopic analysis of the interaction forces disclosed quantitatively the separation of the adhesion force in van der Waals and Lewis acid-base contributions. Further, the surface polarizability of VAlN was shown to be unaffected by oxygen incorporation due to the formation of an only gradually oxidized surface comprising a range of vanadium oxidation states. In contrast, the adhesion force analysis revealed additional Lewis acid-base interactions between the oxidized and non-oxidized VAlN surfaces and carboxyl groups present in the surface of PS after an oxidative oxygen beam treatment.

Biogenic hydroxysulfate green rust, a potential electron acceptor for SRB activity

NASA Astrophysics Data System (ADS)

Zegeye, Asfaw; Huguet, Lucie; Abdelmoula, Mustapha; Carteret, Cédric; Mullet, Martine; Jorand, Frédéric

2007-11-01

Microbiological reduction of a biogenic sulfated green rust (GR2(SO42-)), was examined using a sulfate reducing bacterium ( Desulfovibrio alaskensis). Experiments investigated whether GR2(SO42-) could serve as a sulfate source for D. alaskensis anaerobic respiration by analyzing mineral transformation. Batch experiments were conducted using lactate as the electron donor and biogenic GR2(SO42-) as the electron acceptor, at circumneutral pH in unbuffered medium. GR2(SO42-) transformation was monitored with time by X-ray diffraction (XRD), Transmission Mössbauer Spectroscopy (TMS), Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS), Transmission Electron Microscopy (TEM) and X-ray Photoelectron Spectroscopy (XPS). The reduction of sulfate anions and the formation of iron sulfur mineral were clearly identified by XPS analyses. TMS showed the formation of additional mineral as green rust (GR) and vivianite. XRD analyses discriminated the type of the newly formed GR as GR1. The formed GR1 was GR1(CO32-) as indicated by DRIFTS analysis. Thus, the results presented in this study indicate that D. alaskensis cells were able to use GR2(SO42-) as an electron acceptor. GR1(CO32-), vivianite and an iron sulfur compound were formed as a result of GR2(SO42-) reduction by D. alaskensis. Hence, in environments where geochemical conditions promote biogenic GR2(SO42-) formation, this mineral could stimulate the anaerobic respiration of sulfate reducing bacteria.

Interfacial chemical and electronic structure of cobalt deposition on 2,7-dioctyl[1]benzothieno[3,2-b]benzothiophene (C8-BTBT)

NASA Astrophysics Data System (ADS)

Zhu, Menglong; Lyu, Lu; Niu, Dongmei; Zhang, Hong; Zhang, Yuhe; Liu, Peng; Gao, Yongli

2017-04-01

Interfacial chemical and electronic structure of Co deposition on 2,7-dioctyl[1]benzothieno[3,2-b]benzothiophene(C8-BTBT) was investigated by ultraviolet photoemission spectroscopy (UPS) and X-ray photoemission spectroscopy (XPS). Chemical reaction of cobalt with C8-BTBT at the interface is confirmed by a new component of S 2s peak which is electron-rich compared to the original one of C8-BTBT molecules. Intensity evolution of the core level in XPS indicates that the adsorption of Co atoms is mainly at the surface without deeper diffusion into C8-BTBT layer. Initial deposition of Co atoms downward shifts the core levels of C8-BTBT by electron transfer from isolated Co atoms or clusters to the C8-BTBT. Further deposition of Co upward shifts the core levels of C8-BTBT because of the neutralization of the thicker metal Co film. Our investigation suggests an inert buffer layer inserted to protect organic layer from reaction or decomposition and to lower the carrier barriers for both the electron and hole to improve the performance of Co/C8-BTBT-based OFETs.

Structural characteristics of phosphorus-doped C60 thin film prepared by radio frequency-plasma assisted thermal evaporation technique.

PubMed

Arie, Arenst Andreas; Lee, Joong Kee

2012-02-01

Phosphorus doped C60 (P:C60) thin films were prepared by a radio frequency plasma assisted thermal evaporation technique using C60 powder as a carbon source and a mixture of argon and phosphine (PH3) gas as a dopant precursor. The effects of the plasma power on the structural characteristics of the as-prepared films were then studied using Raman spectroscopy, Auger electron spectroscopy (AES) and X-ray photo-electrons spectroscopy (XPS). XPS and Auger analysis indicated that the films were mainly composed of C and P and that the concentration of P was proportional to the plasma power. The Raman results implied that the doped films contained a more disordered carbon structure than the un-doped samples. The P:C60 films were then used as a coating layer for the Si anodes of lithium ion secondary batteries. The cyclic voltammetry (CV) analysis of the P:C60 coated Si electrodes demonstrated that the P:C60 coating layer might be used to improve the transport of Li-ions at the electrode/electrolyte interface.

Arsenopyrite and pyrite bioleaching: evidence from XPS, XRD and ICP techniques.

PubMed

Fantauzzi, Marzia; Licheri, Cristina; Atzei, Davide; Loi, Giovanni; Elsener, Bernhard; Rossi, Giovanni; Rossi, Antonella

2011-10-01

In this work, a multi-technical bulk and surface analytical approach was used to investigate the bioleaching of a pyrite and arsenopyrite flotation concentrate with a mixed microflora mainly consisting of Acidithiobacillus ferrooxidans. X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and X-ray-induced Auger electron spectroscopy mineral surfaces investigations, along with inductively coupled plasma-atomic emission spectroscopy and carbon, hydrogen, nitrogen and sulphur determination (CHNS) analyses, were carried out prior and after bioleaching. The flotation concentrate was a mixture of pyrite (FeS(2)) and arsenopyrite (FeAsS); after bioleaching, 95% of the initial content of pyrite and 85% of arsenopyrite were dissolved. The chemical state of the main elements (Fe, As and S) at the surface of the bioreactor feed particles and of the residue after bioleaching was investigated by X-ray photoelectron and X-ray excited Auger electron spectroscopy. After bioleaching, no signals of iron, arsenic and sulphur originating from pyrite and arsenopyrite were detected, confirming a strong oxidation and the dissolution of the particles. On the surfaces of the mineral residue particles, elemental sulphur as reaction intermediate of the leaching process and precipitated secondary phases (Fe-OOH and jarosite), together with adsorbed arsenates, was detected. Evidence of microbial cells adhesion at mineral surfaces was also produced: carbon and nitrogen were revealed by CHNS, and nitrogen was also detected on the bioleached surfaces by XPS. This was attributed to the deposition, on the mineral surfaces, of the remnants of a bio-film consisting of an extra-cellular polymer layer that had favoured the bacterial action. © Springer-Verlag 2011

Synthesis and Structural Characterization of Silver Nanoparticles Stabilized with 3-Mercapto-1-Propansulfonate and 1-Thioglucose Mixed Thiols for Antibacterial Applications

PubMed Central

Porcaro, Francesco; Carlini, Laura; Ugolini, Andrea; Visaggio, Daniela; Visca, Paolo; Fratoddi, Ilaria; Venditti, Iole; Meneghini, Carlo; Simonelli, Laura; Marini, Carlo; Olszewski, Wojciech; Ramanan, Nitya; Luisetto, Igor; Battocchio, Chiara

2016-01-01

The synthesis, characterization and assessment of the antibacterial properties of hydrophilic silver nanoparticles (AgNPs) were investigated with the aim to probe their suitability for innovative applications in the field of nanobiotechnology. First, silver nanoparticles were synthetized and functionalized with two capping agents, namely 3-mercapto-1-propansulfonate (3MPS) and 1-β-thio-d-glucose (TG). The investigation of the structural and electronic properties of the nano-systems was carried out by means of X-ray Photoelectron Spectroscopy (XPS) and X-ray Absorption Spectroscopy (XAS). XPS data provided information about the system stability and the interactions between the metallic surface and the organic ligands. In addition, XPS data allowed us to achieve a deep understanding of the influence of the thiols stoichiometric ratio on the electronic properties and stability of AgNPs. In order to shed light on the structural and electronic local properties at Ag atoms sites, XAS at Ag K-Edge was successfully applied; furthermore, the combination of Dynamic Light Scattering (DLS) and XAS results allowed determining AgNPs sizes, ranging between 3 and 13 nm. Finally, preliminary studies on the antibacterial properties of AgNPs showed promising results on four of six multidrug-resistant bacteria belonging to the ESKAPE group (Enterococcus faecium, Staphylococcus aureus, Klebsiella pneumoniae, Acinetobacter baumannii, Pseudomonas aeruginosa, and Enterobacter sp.). PMID:28774148

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

Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de

A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ballmore » milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.« less

Quantifying the Impact of Nanoparticle Coatings and Non-uniformities on XPS Analysis: Gold/silver Core-shell Nanoparticles

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

Wang, Yung-Chen Andrew; Engelhard, Mark H.; Baer, Donald R.

2016-03-07

Abstract or short description: Spectral modeling of photoelectrons can serve as a valuable tool when combined with X-ray photoelectron spectroscopy (XPS) analysis. Herein, a new version of the NIST Simulation of Electron Spectra for Surface Analysis (SESSA 2.0) software, capable of directly simulating spherical multilayer NPs, was applied to model citrate stabilized Au/Ag-core/shell nanoparticles (NPs). The NPs were characterized using XPS and scanning transmission electron microscopy (STEM) to determine the composition and morphology of the NPs. The Au/Ag-core/shell NPs were observed to be polydispersed in size, non-circular, and contain off-centered Au-cores. Using the average NP dimensions determined from STEM analysis,more » SESSA spectral modeling indicated that washed Au/Ag-core shell NPs were stabilized with a 0.8 nm l« less

XPS Spectra Analysis of Ti2+, Ti3+ Ions and Dye Photodegradation Evaluation of Titania-Silica Mixed Oxide Nanoparticles

NASA Astrophysics Data System (ADS)

Chinh, Vu Duc; Broggi, Alessandra; Di Palma, Luca; Scarsella, Marco; Speranza, Giorgio; Vilardi, Giorgio; Thang, Pham Nam

2018-04-01

TiO2-SiO2 mixed oxides have been prepared by the sol-gel technique from tetrabutyl orthotitanate and tetraethyl orthosilicate. The prepared materials were characterized by x-ray diffraction, scanning electron microscopy, energy dispersive x-ray spectroscopy, nitrogen physisorption, Fourier-transform infrared spectroscopy (FT-IR) and x-ray photoelectron spectroscopy (XPS). The results indicate that the TiO2-SiO2 mixed oxides have a large surface area and a nanoscale size. FT-IR spectra show that Ti atoms are bonded to silica by oxygen bridging atoms in Ti-O-Si bonds. The titanium valence states in TiO2-SiO2 mixed oxides were investigated by XPS, and their spectra report the presence of Ti2+ and Ti3+ cations for high silica concentration, suggesting the formation of oxygen vacancies. The photocatalytic activity of the prepared materials has been evaluated for the photodegradation of methylene blue (MB). The mixed oxides were activated by means of a UV light source, and the concentration of MB was monitored by UV-Vis spectroscopy. The synthesized TiO2-SiO2 shows significantly higher MB removal efficiency in comparison with that of the commercial TiO2 Degussa, P25.

An investigation of adhesive/adherend and fiber matrix interactions. [Ti 6-4 surfaces

NASA Technical Reports Server (NTRS)

Beck, B.; Siriwardane, R.; Wightman, J. P.

1981-01-01

Research during the report period focused on continued scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) of lap shear samples and flatwise tensile specimens and on the surface characterization of TiO2, Ti 6-4, and Ti powders with particular emphasis on their interaction with primer solutions of both polyphenylquinoxaline and LaRC-13 polyimide. The use of SEM and XPS in the analysis of Ti 6-4 adherend surfaces is described as well as differences in Ti 6-4 surface composition after different chemical pretreatments. Analysis of fractured surfaces is used to established the failure mode. The surface acidity of Ti 6-4 coupons can be established by reflectance visible spectroscopy using indicator dyes.

X-ray photoelectron spectroscopy and secondary electron yield analysis of Al and Cu samples exposed to an accelerator environment

NASA Astrophysics Data System (ADS)

Rosenberg, R. A.; McDowell, M. W.; Ma, Q.; Harkay, K. C.

2003-09-01

It is well known that exposure to an accelerator environment can cause ``conditioning'' of the vacuum chamber surfaces. In order to understand the manner in which the surface structure might influence the production of gases and electrons in the accelerator, such surfaces should be studied both before and after exposure to accelerator conditions. Numerous studies have been performed on representative materials prior to being inserted into an accelerator, but very little has been done on materials that have ``lived'' in the accelerator for extended periods. In the present work, we mounted Al and Cu coupons at different positions in a section of the Advanced Photon Source storage ring and removed them following exposures ranging from 6 to 18 months. X-ray photoelectron spectroscopy (XPS) of the surface was performed before and after exposure. Changes were observed that depended on the location and whether the coupon was facing the chamber interior or chamber wall. These results will be presented and compared to XPS and secondary electron yield data obtained from laboratory measurements meant to simulate the accelerator conditions.

Empirical optimization of DFT  +  U and HSE for the band structure of ZnO.

PubMed

Bashyal, Keshab; Pyles, Christopher K; Afroosheh, Sajjad; Lamichhane, Aneer; Zayak, Alexey T

2018-02-14

ZnO is a well-known wide band gap semiconductor with promising potential for applications in optoelectronics, transparent electronics, and spintronics. Computational simulations based on the density functional theory (DFT) play an important role in the research of ZnO, but the standard functionals, like Perdew-Burke-Erzenhof, result in largely underestimated values of the band gap and the binding energies of the Zn 3d electrons. Methods like DFT  +  U and hybrid functionals are meant to remedy the weaknesses of plain DFT. However, both methods are not parameter-free. Direct comparison with experimental data is the best way to optimize the computational parameters. X-ray photoemission spectroscopy (XPS) is commonly considered as a benchmark for the computed electronic densities of states. In this work, both DFT  +  U and HSE methods were parametrized to fit almost exactly the binding energies of electrons in ZnO obtained by XPS. The optimized parameterizations of DFT  +  U and HSE lead to significantly worse results in reproducing the ion-clamped static dielectric tensor, compared to standard high-level calculations, including GW, which in turn yield a perfect match for the dielectric tensor. The failure of our XPS-based optimization reveals the fact that XPS does not report the ground state electronic structure for ZnO and should not be used for benchmarking ground state electronic structure calculations.

Empirical optimization of DFT  +  U and HSE for the band structure of ZnO

NASA Astrophysics Data System (ADS)

Bashyal, Keshab; Pyles, Christopher K.; Afroosheh, Sajjad; Lamichhane, Aneer; Zayak, Alexey T.

2018-02-01

ZnO is a well-known wide band gap semiconductor with promising potential for applications in optoelectronics, transparent electronics, and spintronics. Computational simulations based on the density functional theory (DFT) play an important role in the research of ZnO, but the standard functionals, like Perdew-Burke-Erzenhof, result in largely underestimated values of the band gap and the binding energies of the Zn3d electrons. Methods like DFT  +  U and hybrid functionals are meant to remedy the weaknesses of plain DFT. However, both methods are not parameter-free. Direct comparison with experimental data is the best way to optimize the computational parameters. X-ray photoemission spectroscopy (XPS) is commonly considered as a benchmark for the computed electronic densities of states. In this work, both DFT  +  U and HSE methods were parametrized to fit almost exactly the binding energies of electrons in ZnO obtained by XPS. The optimized parameterizations of DFT  +  U and HSE lead to significantly worse results in reproducing the ion-clamped static dielectric tensor, compared to standard high-level calculations, including GW, which in turn yield a perfect match for the dielectric tensor. The failure of our XPS-based optimization reveals the fact that XPS does not report the ground state electronic structure for ZnO and should not be used for benchmarking ground state electronic structure calculations.

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

Brown, Matthew A.; Redondo, Amaia Beloqui; Duyckaerts, Nicolas

A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutionsmore » and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.« less

Structural and magnetic characterization of copper sulfonated phthalocyanine grafted onto treated polyethylene

NASA Astrophysics Data System (ADS)

Reznickova, A.; Kolska, Z.; Orendac, M.; Cizmar, E.; Sajdl, P.; Svorcik, V.

2016-08-01

This study focuses on high density polyethylene (HDPE) activated by Ar plasma treatment, subsequently grafted with copper sulfonated phthalocyanine (CuPc) especially pointing out to the surface and magnetic properties of those composites. Properties of pristine PE and their plasma treated counterparts were studied by different experimental techniques: X-ray photoelectron spectroscopy (XPS), UV-vis spectroscopy, zeta potential and by electron spin resonance (ESR). XPS analysis confirmed the successful grafting of phthalocyanine. The highest absorption was found for the sample grafted with bCuPc for 1 h. Electrokinetic analysis also confirmed the plasma treatment and also subsequent CuPc grafting influence significantly the surface chemistry and charge. These results correspond well with XPS determination. ESR studies confirmed the presence of CuPc grafted on HDPE. It was found, that grafting is mediated by magnetically inactive functional groups, rather than radicals. Magnetic properties of CuPc do not seem to change significantly after grafting CuPc on polyethylene surface.

Production of sp3 hybridization by swift heavy ion irradiation of HOPG

NASA Astrophysics Data System (ADS)

Zeng, J.; Zhai, P. F.; Liu, J.; Yao, H. J.; Duan, J. L.; Hou, M. D.; Sun, Y. M.; Li, G. P.

2013-07-01

Highly oriented pyrolytic graphite (HOPG) samples were irradiated by swift heavy ions (86Kr, 209Bi and 238U) with the fluence of 1011-1013 ions/cm2 at room temperature. The production of sp3 hybridization by the irradiation process has been confirmed directly by X-ray photoelectron spectroscopy (XPS). In this work, both irradiated and pristine HOPG samples were investigated by XPS and Raman spectroscopy. The existence of sp3 component is confirmed on the surface of the irradiated HOPG samples. XPS result shows that the acreage ratio Isp3/Isp2 increases with the ion fluence and saturates at a higher value of irradiation. It is found that the amount of hybridization (Isp3/Isp2) strongly depends on the electronic energy loss in the sample. Raman spectra of the irradiated samples show the increasing of acreage ratio ID/IG with the ion fluence, which indicates the change of the atomic structure and the phase transition from sp2 to sp3.

Quantitative interpretation of molecular dynamics simulations for X-ray photoelectron spectroscopy of aqueous solutions

NASA Astrophysics Data System (ADS)

Olivieri, Giorgia; Parry, Krista M.; Powell, Cedric J.; Tobias, Douglas J.; Brown, Matthew A.

2016-04-01

Over the past decade, energy-dependent ambient pressure X-ray photoelectron spectroscopy (XPS) has emerged as a powerful analytical probe of the ion spatial distributions at the vapor (vacuum)-aqueous electrolyte interface. These experiments are often paired with complementary molecular dynamics (MD) simulations in an attempt to provide a complete description of the liquid interface. There is, however, no systematic protocol that permits a straightforward comparison of the two sets of results. XPS is an integrated technique that averages signals from multiple layers in a solution even at the lowest photoelectron kinetic energies routinely employed, whereas MD simulations provide a microscopic layer-by-layer description of the solution composition near the interface. Here, we use the National Institute of Standards and Technology database for the Simulation of Electron Spectra for Surface Analysis (SESSA) to quantitatively interpret atom-density profiles from MD simulations for XPS signal intensities using sodium and potassium iodide solutions as examples. We show that electron inelastic mean free paths calculated from a semi-empirical formula depend strongly on solution composition, varying by up to 30% between pure water and concentrated NaI. The XPS signal thus arises from different information depths in different solutions for a fixed photoelectron kinetic energy. XPS signal intensities are calculated using SESSA as a function of photoelectron kinetic energy (probe depth) and compared with a widely employed ad hoc method. SESSA simulations illustrate the importance of accounting for elastic-scattering events at low photoelectron kinetic energies (<300 eV) where the ad hoc method systematically underestimates the preferential enhancement of anions over cations. Finally, some technical aspects of applying SESSA to liquid interfaces are discussed.

Surfactant Mediated Growth of Co on MgO(111)

NASA Astrophysics Data System (ADS)

Johnson-Steigelman, H. Trevor; Parihar, Somendra S.; Lyman, Paul F.

2010-03-01

Monolayer films of Co were deposited using an electrostatic electron-beam evaporator on single-crystal MgO(111)- √3 x√3 R 30^o substrates held at room temperature, with subsequent annealing of temperatures 400 C to 800 C. These films were characterized using low-energy electron diffraction (LEED), x-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and x-ray diffraction (XRD). After short anneals of 400 C, AFM, LEED, and XPS suggest that islanding has occurred at the surface. XPS and XRD indicate the presence of elemental Co. 1-2 ML films of Ag were examined as a potential surfactant to aid in the growth of smooth Co films. Despite the fact that Ag itself formed islands, it was found that the presence of Ag did have a surfactant effect upon the thin-film growth of Co on Ag/MgO(111)- √3 x√3 R 30^o. Co islands were still present, but much more smooth than islands formed without Ag. XPS and AFM suggest strongly that Ag floated to the top of these samples at temperatures above 400 ^oC.

Adsorption of Atoms of 3 d Metals on the Surfaces of Aluminum and Magnesium Oxide Films

NASA Astrophysics Data System (ADS)

Ramonova, A. G.; Kibizov, D. D.; Kozyrev, E. N.; Zaalishvili, V. B.; Grigorkina, G. S.; Fukutani, K.; Magkoev, T. T.

2018-01-01

The adsorption and formation of submonolayer structures of Ti, Cr, Fe, Ni, Cu on the surfaces of aluminum and magnesium oxide films formed on Mo(110) under ultrahigh vacuum conditions are studied via X-ray, ultraviolet photo-, and Auger electron spectroscopy (XPS, UVES, AES); spectroscopy of energy losses of high-resolution electrons (SELHRE); spectroscopy of the backscattering of low-energy ions (SBSLEI); infrared absorption spectroscopy (IAS); and the diffraction of slow electrons (DSE). Individual atoms and small clusters of all the investigated metals deposited on oxides acquire a positive charge, due presumably to interaction with surface defects. As the concentration of adatoms increases when the adsorption centers caused by defects are filled, charge transfer from adatoms to substrates is reduced. This is accompanied by further depolarization caused by the lateral interaction of adatoms.

Effect of oxygen deficiency on electronic properties and local structure of amorphous tantalum oxide thin films

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

Denny, Yus Rama; Firmansyah, Teguh; Oh, Suhk Kun

2016-10-15

Highlights: • The effect of oxygen flow rate on electronic properties and local structure of tantalum oxide thin films was studied. • The oxygen deficiency induced the nonstoichiometric state a-TaOx. • A small peak at 1.97 eV above the valence band side appeared on nonstoichiometric Ta{sub 2}O{sub 5} thin films. • The oxygen flow rate can change the local electronic structure of tantalum oxide thin films. - Abstract: The dependence of electronic properties and local structure of tantalum oxide thin film on oxygen deficiency have been investigated by means of X-ray photoelectron spectroscopy (XPS), Reflection Electron Energy Loss Spectroscopy (REELS),more » and X-ray absorption spectroscopy (XAS). The XPS results showed that the oxygen flow rate change results in the appearance of features in the Ta 4f at the binding energies of 23.2 eV, 24.4 eV, 25.8, and 27.3 eV whose peaks are attributed to Ta{sup 1+}, Ta{sup 2+}, Ta{sup 3+}/Ta{sup 4+}, and Ta{sup 5+}, respectively. The presence of nonstoichiometric state from tantalum oxide (TaOx) thin films could be generated by the oxygen vacancies. In addition, XAS spectra manifested both the increase of coordination number of the first Ta-O shell and a considerable reduction of the Ta-O bond distance with the decrease of oxygen deficiency.« less

Green Synthesis of Novel Polyaniline Nanofibers: Application in pH Sensing.

PubMed

Tanwar, Shivani; Ho, Ja-an Annie

2015-10-13

An optically active polyaniline nanomaterial (PANI-Nap), doped with (S)-naproxen, was developed and evaluated as a potent pH sensor. We synthesized the material in one pot by the addition of the dopant, (S)-naproxen, prior to polymerization, followed by the addition of the oxidizing agent (ammonium persulfate) that causes polymerization of the aniline. This green chemistry approach allowed us to take only 1 h to produce a water-soluble and stable nanomaterial. UV-visible spectroscopy, fluorescence spectroscopy, FT-IR spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) were used to characterize the designed nanomaterial. This nanomaterial exhibited excellent pH sensing properties and showed long term stability (up to one month) without loss of sensor performance.

Boron difluoride dibenzoylmethane derivatives: Electronic structure and luminescence

NASA Astrophysics Data System (ADS)

Tikhonov, Sergey A.; Vovna, Vitaliy I.; Osmushko, Ivan S.; Fedorenko, Elena V.; Mirochnik, Anatoliy G.

2018-01-01

Electronic structure and optical properties of boron difluoride dibenzoylmethanate and four of its derivatives have been studied by X-ray photoelectron spectroscopy, absorption and luminescence spectroscopy and quantum chemistry (DFT, TDDFT). The relative quantum luminescence yields have been revealed to correlate with charge transfers of HOMO-LUMO transitions, energy barriers of aromatic substituents rotation and the lifetime of excited states in the investigated complexes. The bathochromic shift of intensive bands in the optical spectra has been observed to occur when the functional groups are introduced into p-positions of phenyl cycles due to destabilizing HOMO levels. Calculated energy intervals between electronic levels correlate well with XPS spectra structure of valence and core electrons.

Synthesis of adenine-modified reduced graphene oxide nanosheets.

PubMed

Cao, Huaqiang; Wu, Xiaoming; Yin, Gui; Warner, Jamie H

2012-03-05

We report here a facile strategy to synthesize the nanocomposite of adenine-modified reduced graphene oxide (AMG) via reaction between adenine and GOCl which is generated from SOCl(2) reacted with graphite oxide (GO). The as-synthesized AMG was characterized by transmission electron microscopy (TEM), atomic force microscopy (AFM), UV-vis absorption spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), and galvanostatic discharge analysis. The AMG owns about one adenine group per 53 carbon atoms on a graphene sheet, which improves electronic conductivity compared with reduced graphene oxide (RGO). The AMG displays enhanced supercapacitor performance compared with RGO accompanying good stability and good cycling behavior in the supercapacitor.

Surface Reactivity of Li2MnO3: First-Principles and Experimental Study.

PubMed

Quesne-Turin, Ambroise; Flahaut, Delphine; Croguennec, Laurence; Vallverdu, Germain; Allouche, Joachim; Charles-Blin, Youn; Chotard, Jean-Noël; Ménétrier, Michel; Baraille, Isabelle

2017-12-20

This article deals with the surface reactivity of (001)-oriented Li 2 MnO 3 crystals investigated from a multitechnique approach combining material synthesis, X-ray photoemission spectroscopy (XPS), scanning electron microscopy, Auger electron spectroscopy, and first-principles calculations. Li 2 MnO 3 is considered as a model compound suitable to go further in the understanding of the role of tetravalent manganese atoms in the surface reactivity of layered lithium oxides. The knowledge of the surface properties of such materials is essential to understand the mechanisms involved in parasitic phenomena responsible for early aging or poor storage performances of lithium-ion batteries. The surface reactivity was probed through the adsorption of SO 2 gas molecules on large Li 2 MnO 3 crystals to be able to focus the XPS beam on the top of the (001) surface. A chemical mapping and XPS characterization of the material before and after SO 2 adsorption show in particular that the adsorption is homogeneous at the micro- and nanoscale and involves Mn reduction, whereas first-principles calculations on a slab model of the surface allow us to conclude that the most energetically favorable species formed is a sulfate with charge transfer implying reduction of Mn.

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

Sarkar, S.; Mondal, A.; Dey, K.

Highlights: • Reduced graphene oxides (RGO) are prepared by two chemical routes. • Defects in RGO are characterized by Raman, FTIR and XPS studies. • Defects tailor colossal dielectricity in RGO. - Abstract: Reduced graphene oxide (RGO) is prepared in two different chemical routes where reduction of graphene oxide is performed by hydrazine hydrate and through high pressure in hydrothermal reactor. Samples are characterized by X-ray powdered diffraction (XRD), thermo gravimetric analysis (TGA), field emission scanning electron microscopy (FESEM) and tunneling electron microscopy (TEM). Types of defects are probed by Raman, FTIR spectroscopy and X-ray photoelectron spectroscopy (XPS). UV–vis absorptionmore » reveals different optical band gaps of the two RGOs. Conductivity mechanism is studied through I–V measurements displaying different characteristic features which are addressed due to the presence of defects appeared in different synthesis. Significantly high value (∼10{sup 4}) of dielectric permittivity at 10 MHz is attractive for technological application which could be tuned by the defects present in RGO.« less

Thermal stability of electron-irradiated poly(tetrafluoroethylene) - X-ray photoelectron and mass spectroscopic study

NASA Technical Reports Server (NTRS)

Wheeler, Donald R.; Pepper, Stephen V.

1990-01-01

Polytetrafluoroethylene (PTFE) was subjected to 3 keV electron bombardment and then heated in vacuum to 300 C. The behavior of the material as a function of radiation dose and temperature was studied by X-ray photoelectron spectroscopy (XPS) of the surface and mass spectroscopy of the species evolved. Lightly damaged material heated to 300 C evolved saturated fluorocarbon species, whereas unsaturated fluorocarbon species were evolved from heavily damaged material. After heating the heavily damaged material, those features in the XPS spectrum that were associated with damage diminished, giving the appearance that the radiation damage had annealed. The observations were interpreted by incorporating mass transport of severed chain fragments and thermal decomposition of severely damaged material into the branched and cross-linked network model of irradiated PTFE. The apparent annealing of the radiation damage was due to covering of the network by saturated fragments that easily diffused through the decomposed material to the surface region upon heating.

Characterization of bimetallic Fe/Pd nanoparticles by grape leaf aqueous extract and identification of active biomolecules involved in the synthesis.

PubMed

Luo, Fang; Yang, Die; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravi

2016-08-15

This paper reports the detailed composition and morphology of one-step green synthesized bimetallic Fe/Pd nanoparticles (NPs) using grape leaf aqueous extract and identification of active biomolecules involved in the synthesis employing various techniques. Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) revealed that Fe/Pd NPs were polydispersed and quasi-spherical with a diameter ranging from 2 to 20nm. X-ray Photoelectron Spectroscopy (XPS) and Energy Dispersive X-ray Spectroscopy (EDS) provided evidence for the composition of Fe and Pd and for their species existing on the surface of Fe/Pd NPs. In addition, biomolecules in the grape leaf aqueous extract were identified but their functions are still unclear. Biomolecules in the aqueous extract such as methoxy-phenyl-oxime, N-benzoyl-2-cyano-histamine, 2-ethyl-phenol, 1,2-benzenediol, β-hydroxyquebracamine, hydroquinone, 2-methoxy-4-vinylphenol, 5-methyl-2-furancarboxaldehyde, 4-(3-hydroxybutyl)-3,5,5-trimethyl-2-cyclohexen and some polyphenolic compounds were identified as reducing and capping agents, which were studied by Chromatography-Mass Spectroscopy (GC-MS), XPS and Fourier Transform Infrared Spectroscopy (FTIR). Our finding suggests a new insight into cost-effective, simple, and environmentally benign production of bimetallic Fe/Pd NPs. Copyright © 2016 Elsevier B.V. All rights reserved.

Surface characterization of LDEF carbon fiber/polymer matrix composites

NASA Technical Reports Server (NTRS)

Grammer, Holly L.; Wightman, James P.; Young, Philip R.; Slemp, Wayne S.

1995-01-01

XPS (x-ray photoelectron spectroscopy) and SEM (scanning electron microscopy) analysis of both carbon fiber/epoxy matrix and carbon fiber/polysulfone matrix composites revealed significant changes in the surface composition as a result of exposure to low-earth orbit. The carbon 1s curve fit XPS analysis in conjunction with the SEM photomicrographs revealed significant erosion of the polymer matrix resins by atomic oxygen to expose the carbon fibers of the composite samples. This erosion effect on the composites was seen after 10 months in orbit and was even more obvious after 69 months.

A critical study of the role of the surface oxide layer in titanium bonding

NASA Technical Reports Server (NTRS)

Dias, S.; Wightman, J. P.

1983-01-01

Scanning electron microscope/X-ray photoelectron spectroscopy (SEM/XPS) analysis of fractured adhesively bonded Ti 6-4 samples is discussed. The text adhesives incuded NR 056X polyimide, polypheylquinoxaline (PPQ), and LARC-13 polyimide. Differentiation between cohesive and interfacial failure was based on the absence of presence of a Ti 2p XPS photopeak. In addition, the surface oxide layer on Ti-(6A1-4V) adherends is characterized and bond strength and durability are addressed. Bond durability in various environmental conditions is discussed.

Deduction of the chemical state and the electronic structure of Nd{sub 2}Fe{sub 14}B compound from X-ray photoelectron spectroscopy core-level and valence-band spectra

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

Wang, Jing; Liang, Le; Zhang, Lanting, E-mail: lantingzh@sjtu.edu.cn, E-mail: lmsun@sjtu.edu.cn

2014-10-28

Characterization of chemical state and electronic structure of the technologically important Nd{sub 2}Fe{sub 14}B compound is attractive for understanding the physical nature of its excellent magnetic properties. X-ray photoelectron spectroscopy (XPS) study of such rare-earth compound is important and also challenging due to the easy oxidation of surface and small photoelectron cross-sections of rare-earth 4f electrons and B 2p electrons, etc. Here, we reported an investigation based on XPS spectra of Nd{sub 2}Fe{sub 14}B compound as a function of Ar ion sputtering time. The chemical state of Fe and that of B in Nd{sub 2}Fe{sub 14}B compound can be clearlymore » determined to be 0 and −3, respectively. The Nd in Nd{sub 2}Fe{sub 14}B compound is found to have the chemical state of close to +3 instead of +3 as compared with the Nd in Nd{sub 2}O{sub 3}. In addition, by comparing the valence-band spectrum of Nd{sub 2}Fe{sub 14}B compound to that of the pure Fe, the contributions from Nd, Fe, and B to the valence-band structure of Nd{sub 2}Fe{sub 14}B compound is made more clear. The B 2p states and B 2s states are identified to be at ∼11.2 eV and ∼24.6 eV, respectively, which is reported for the first time. The contribution from Nd 4f states can be identified both in XPS core-level spectrum and XPS valence-band spectrum. Although Nd 4f states partially hybridize with Fe 3d states, Nd 4f states are mainly localized in Nd{sub 2}Fe{sub 14}B compound.« less

Charge transfer and injection barrier at the metal-organic interfaces

NASA Astrophysics Data System (ADS)

Yan, Li

2002-09-01

The metal-organic interface plays a critical role in determining the functionality and performance of many innovative organic based devices. It has attracted extensive research interests in recent years. This thesis presents investigations of the electronic structures of organic materials, such as tris-(8-hydroxyquinoline) aluminum (Alq3) and copper phthalocyanine (CuPc), during their interface formation with metals. The characterization is accomplished by X-ray and ultraviolet photoelectron spectroscopes (XPS and UPS) and inverse photoelectron spectroscopy (IPES). As discussed herein, both occupied and unoccupied electronic states at the interfaces are carefully examined in different aspects. In Chapter 4, the charge transfer and chemical reaction at various metal/Alq3 interfaces are investigated using XPS and UPS to study the electron injection into the Alga film. Electron transfer from the low work function metal and Al/LiF(CsF) bilayer to the Alga has been observed. The role of the dielectric and possible chemistry at the interface are discussed in comparison of the low work function metals. Further in Chapter 5, the origin of the metal-interface dipole and the estimation of charge injection barrier is explored using several organic materials. A thermodynamic equilibrium model is extended to explain the relation between the charge transfer process ad the interface dipole. Further, in Chapter 6 the combination of XPS, UPS and IPES detailed the evolution of both occupied and unoccupied energy states during the alkali metal doping. The energy gap modification in organic due to metal doping is observed directly for the spectra. Chapter 7 provides stability study of the organic thin films under x-ray and UV light. The results verify the usability of UPS and XPS for the organic materials used in the thesis. Chapter 7 also shows the secondary ion mass spectroscopy results of metal diffusion in organic thin films.

Electronic structure study of wide band gap magnetic semiconductor (La0.6Pr0.4)0.65Ca0.35MnO3 nanocrystals in paramagnetic and ferromagnetic phases

NASA Astrophysics Data System (ADS)

Dwivedi, G. D.; Joshi, Amish G.; Kumar, Shiv; Chou, H.; Yang, K. S.; Jhong, D. J.; Chan, W. L.; Ghosh, A. K.; Chatterjee, Sandip

2016-04-01

X-ray circular magnetic dichroism (XMCD), X-ray photoemission spectroscopy (XPS), and ultraviolet photoemission spectroscopy (UPS) techniques were used to study the electronic structure of nanocrystalline (La0.6Pr0.4)0.65Ca0.35MnO3 near Fermi-level. XMCD results indicate that Mn3+ and Mn4+ spins are aligned parallel to each other at 20 K. The low M-H hysteresis curve measured at 5 K confirms ferromagnetic ordering in the (La0.6Pr0.4)0.65Ca0.35MnO3 system. The low temperature valence band XPS indicates that coupling between Mn3d and O2p is enhanced and the electronic states near Fermi-level have been suppressed below TC. The valence band UPS also confirms the suppression of electronic states near Fermi-level below Curie temperature. UPS near Fermi-edge shows that the electronic states are almost absent below 0.5 eV (at 300 K) and 1 eV (at 115 K). This absence clearly demonstrates the existence of a wide band-gap in the system since, for hole-doped semiconductors, the Fermi-level resides just above the valence band maximum.

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach

NASA Astrophysics Data System (ADS)

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material.Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. Electronic supplementary information (ESI) available: Fig. S1, AFM image (5 μm × 5 μm) of graphene nanoplate-MnO2 composite obtained at 3 h; Fig. S2, nitrogen adsorption/desorption isotherm of graphene nanoplate-MnO2 composite obtained at 3 h. See DOI: 10.1039/c1nr10229j

Low-temperature thermal reduction of graphene oxide: In situ correlative structural, thermal desorption, and electrical transport measurements

NASA Astrophysics Data System (ADS)

Lipatov, Alexey; Guinel, Maxime J.-F.; Muratov, Dmitry S.; Vanyushin, Vladislav O.; Wilson, Peter M.; Kolmakov, Andrei; Sinitskii, Alexander

2018-01-01

Elucidation of the structural transformations in graphene oxide (GO) upon reduction remains an active and important area of research. We report the results of in situ heating experiments, during which electrical, mass spectrometry, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and transmission electron microscopy (TEM) measurements were carried out correlatively. The simultaneous electrical and temperature programmed desorption measurements allowed us to correlate the onset of the increase in the electrical conductivity of GO by five orders of magnitude at about 150 °C with the maxima of the rates of desorption of H2O, CO, and CO2. Interestingly, this large conductivity change happens at an intermediate level of the reduction of GO, which likely corresponds to the point when the graphitic domains become large enough to enable percolative electronic transport. We demonstrate that the gas desorption is intimately related to (i) the changes in the chemical structure of GO detected by XPS and Raman spectroscopy and (ii) the formation of nanoscopic holes in GO sheets revealed by TEM. These in situ observations provide a better understanding of the mechanism of the GO thermal reduction.

Synthesis of Cr3+-doped TiO2 nanoparticles: characterization and evaluation of their visible photocatalytic performance and stability.

PubMed

Mendiola-Alvarez, Sandra Yadira; Guzmán-Mar, Jorge Luis; Turnes-Palomino, Gemma; Maya-Alejandro, Fernando; Caballero-Quintero, Adolfo; Hernández-Ramírez, Aracely; Hinojosa-Reyes, Laura

2017-09-28

Cr 3+ -doped TiO 2 nanoparticles (Ti-Cr) were synthesized by microwave-assisted sol-gel method. The Ti-Cr catalyst was characterized by X-ray diffraction, ultraviolet-visible diffuse reflectance spectroscopy, N 2 adsorption-desorption analysis, Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, photoluminescence spectroscopy, X-ray photoelectron spectroscopy (XPS) and zetametry. The anatase mesoporous Ti-Cr material exhibited a specific surface area of 54.5 m 2 /g. XPS analysis confirmed the proper substitution of Ti 4+ cations by Cr 3+ cations in the TiO 2 matrix. The particle size was of average size of 17 nm for the undoped TiO 2 but only 9.5 nm for Ti-Cr. The Cr atoms promoted the formation of hydroxyl radicals and modified the surface adsorptive properties of TiO 2 due to the increase in surface acidity of the material. The photocatalytic evaluation demonstrated that the Ti-Cr catalyst completely degraded (4-chloro-2-methylphenoxy) acetic acid under visible light irradiation, while undoped TiO 2 and P25 allowed 45.7% and 31.1%, respectively. The rate of degradation remained 52% after three cycles of catalyst reuse. The higher visible light photocatalytic activity of Ti-Cr was attributed to the beneficial effect of Cr 3+ ions on the TiO 2 surface creating defects within the TiO 2 crystal lattice, which can act as charge-trapping sites, reducing the electron-hole recombination process.

A Study of Ziegler–Natta Propylene Polymerization Catalysts by Spectroscopic Methods

PubMed Central

Tkachenko, Olga P.; Kucherov, Alexey V.; Kustov, Leonid M.; Virkkunen, Ville; Leinonen, Timo; Denifl, Peter

2017-01-01

Ziegler–Natta polymerization catalysts were characterized by a complex of surface- and bulk-sensitive methods (DRIFTS, XPS, ESR, and XAS = XANES + EXAFS). A diffuse-reflectance Fourier-transform IR spectroscopy (DRIFTS) study showed the presence of strong Lewis acid sites in different concentrations and absence of strong basic sites in the polymerization catalysts. X-ray photoelectron spectroscopy (XPS), electron-spin resonance (ESR), and (X-ray absorption near-edge structure (XANES) analysis revealed the presence of Ti4+, Ti3+, Ti2+, and Ti1+ species in the surface layers and in the bulk of catalysts. The samples under study differ drastically in terms of the number of ESR-visible paramagnetic sites. The EXAFS study shows the presence of a Cl atom as a nearest neighbor of the absorbing Ti atom. PMID:28772850

Electro-optic investigation of the n-alkanethiol GaAs(001) interface: Surface phenomena and applications to photoluminescence-based biosensing

NASA Astrophysics Data System (ADS)

Marshall, Gregory M.

Semiconductor surfaces coupled to molecular structures derived from organic chemistry form the basis of an emerging class of field-effect devices. In addition to molecular electronics research, these interfaces are developed for a variety of sensor applications in the electronic and optical domains. Of practical interest are self-assembled monolayers (SAMs) comprised of n-alkanethiols [HS(CH2)n], which couple to the GaAs(001) surface through S-GaAs covalent bond formation. These SAMs offer potential functionality in terms of the requisite sensor chemistry and the passivation effect such coupling is known to afford. In this thesis, the SAM-GaAs interface is investigated in the context of a photonic biosensor based on photoluminescence (PL) variation. The scope of the work is categorized into three parts: i) the structural and compositional analysis of the surface using X-ray photoelectron spectroscopy (XPS), ii) the investigation of electronic properties at the interface under equilibrium conditions using infrared (IR) spectroscopy, the Kelvin probe method, and XPS, and iii) the analysis of the electro-optic response under steady-state photonic excitation, specifically, the surface photovoltage (SPV) and PL intensity. Using a partial overlayer model of angle-resolved XPS spectra in which the component assignments are shown to be quantitatively valid, the coverage fraction of methyl-terminated SAMs is shown to exceed 90%. Notable among the findings are a low-oxide, Ga-rich surface with elemental As present in sub-monolayer quantities consistent with theoretical surface morphologies. Modal analysis of transmission IR spectra show that the SAM molecular order is sufficient to support a Beer-Lambert determination of the IR optical constants, which yields the observation of a SAM-specific absorbance enhancement. By correlation of the IR absorbance with the SAM dipole layer potential, the enhancement mechanism is attributed to the vibrational moments added by the electronic polarizability in the static field of the SAM. Lastly, the surface Fermi level position is determined by XPS and is used to interpret SPV results in terms of a thiol-induced reduction of the surface cross-section for minority carrier-capture. Numerical analysis confirms this result based on the carrier transport theory of PL intensity by means of a reduction of the surface recombination velocity. Keywords: photonics, biosensor, GaAs, self-assembled monolayers, X-ray photoelectron spectroscopy, IR spectroscopy, photoluminescence, surface Fermi level, surface photovoltage.

Facile and fast synthesis of SnS2 nanoparticles by pulsed laser ablation in liquid

NASA Astrophysics Data System (ADS)

Johny, J.; Sepulveda-Guzman, S.; Krishnan, B.; Avellaneda, D.; Shaji, S.

2018-03-01

Nanoparticles (NPs) of tin disulfide (SnS2) were synthesized using pulsed laser ablation in liquid (PLAL) technique. Effects of different liquid media and ablation wavelengths on the morphology and optical properties of the nanoparticles were studied. Nd: YAG laser wavelengths of 532 nm and 1064 nm (frequency 10 Hz and pulse width 10 ns) were used to irradiate SnS2 target immersed in liquid for the synthesis of SnS2 nanoparticles. Here PLAL was a fast synthesis technique, the ablation was only for 30 s. Transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, UV-vis absorption spectroscopy and photoluminescence spectroscopy were used to characterize the SnS2 NPs. TEM images showed that the liquid medium and laser wavelength influence the morphology of the NPs. SAED patterns and high resolution TEM (HRTEM) images confirmed the crystallinity of the particles. XRD and XPS analyses confirmed that SnS2 NPs were having exact crystalline structure and chemical states as that of the target. Raman analysis also supported the results obtained by XRD and XPS. Optical band gaps of the nanocolloids evaluated from their UV-vis absorption spectra were 2.4-3.05 eV. SnS2 NPs were having luminescence spectra in the blue-green region irrespective of the liquid media and ablation wavelength.

Auger electron diffraction study of the growth of Fe(001) films on ZnSe(001)

NASA Astrophysics Data System (ADS)

Jonker, B. T.; Prinz, G. A.

1991-03-01

The growth of Fe films on ZnSe(001) epilayers and bulk GaAs(001) substrates has been studied to determine the mode of film growth, the formation of the interface, and the structure of the overlayer at the 1-10 monolayer level. Auger electron diffraction (AED), x-ray photoelectron spectroscopy (XPS), and reflection high-energy electron diffraction data are obtained for incremental deposition of the Fe(001) overlayer. The coverage dependence of the AED forward scattering peaks reveals a predominantly layer-by-layer mode of film growth at 175 °C on ZnSe, while a more three-dimensional growth mode occurs on the oxide-desorbed GaAs(001) substrate. XPS studies of the semiconductor 3d levels indicate that the Fe/ZnSe interface is less reactive than the Fe/GaAs interface.

Electronic structure of LiGaS 2

NASA Astrophysics Data System (ADS)

Atuchin, V. V.; Isaenko, L. I.; Kesler, V. G.; Lobanov, S.; Huang, H.; Lin, Z. S.

2009-04-01

X-ray photoelectron spectroscopy (XPS) measurement has been performed to determine the valence band structure of LiGaS 2 crystals. The experimental measurement is compared with the electronic structure obtained from the density functional calculations. It is found that the Ga 3d states in the XPS spectrum are much higher than the calculated results. In order to eliminate this discrepancy, the LDA+ U method is employed and reasonable agreement is achieved. Further calculations show that the difference of the linear and nonlinear optical coefficients between LDA and LDA+ U calculations is negligibly small, indicating that the Ga 3d states are actually independent of the excited properties of LiGaS 2 crystals since they are located at a very deep position in the valence bands.

Effects of the electron-hole pair in Auger and X-ray photoemission spectroscopy from surfaces of Fe-Si

NASA Astrophysics Data System (ADS)

Gervasoni, J. L.; Jenko, M.; Poniku, B.; Belič, I.; Juan, A.

2015-07-01

In this work, we investigate in detail the effects due to the interaction between an electron and a stationary positive ion (or atomic hole) in the neighborhood of a surface of Fe-Si, having a strong plasmon peak in their electron energy loss spectra, when it is excited with synchrotron radiation. We take into account the effects due to the sudden creation of an electron and the residual holes, one in the case of X-ray photoemission spectroscopy (XPS) and two in the case of Auger electron spectroscopy (AES). We use a semi classical dielectric formulation for the photoelectron trajectory, and we estimated the parameter rs, the radius of the sphere occupied by one electron in the solid, which is critical in order to define the electron density of the alloy. With the cited formulation, we have obtained a detailed behavior of the different contributions of the collective excitations in both processes.

Auger electron spectroscopy, secondary ion mass spectroscopy and optical characterization of a-C-H and BN films

NASA Technical Reports Server (NTRS)

Pouch, J. J.; Alterovitz, S. A.; Warner, J. D.

1986-01-01

The amorphous dielectrics a-C:H and BN were deposited on III-V semiconductors. Optical band gaps as high as 3 eV were measured for a-C:H generated by C4H10 plasmas; a comparison was made with bad gaps obtained from films prepared by CH4 glow discharges. The ion beam deposited BN films exhibited amorphous behavior with band gaps on the order of 5 eV. Film compositions were studied by Auger electron spectroscopy (AES), x-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS). The optical properties were characterized by ellipsometry, UV/VIS absorption, and IR reflection and transmission. Etching rates of a-C:H subjected to O2 dicharges were determined.

Spontaneous grafting: a novel approach to graft diazonium cations on gold nanoparticles in aqueous medium and their self-assembly on electrodes.

PubMed

Kesavan, Srinivasan; John, S Abraham

2014-08-15

The spontaneous grafting of aminophenyl groups on gold nanoparticles (AuNPs) by reaction with in situ generated 4-aminophenyl diazonium cations (APD) in an aqueous medium was described. The spontaneous grafting was likely to proceed by transfer of electrons from AuNPs to the APD cations to form an aminophenyl radical and subsequent attachment with AuNPs. The aminophenyl (AP) functionalized gold nanoparticles (AP-AuNPs) were characterized by UV-visible spectroscopy, high resolution-transmission electron microscopy (HR-TEM), X-ray diffraction, FT-IR spectroscopy, X-ray photoelectron spectroscopy (XPS) and surface-enhanced Raman spectroscopy (SERS). The absence of characteristic vibrational bands corresponding to diazonium group in the FT-IR spectrum confirmed the reduction of the aminophenyl diazonium cations at the surface of AuNPs. The spontaneous attachment of AP on AuNPs was confirmed by XPS from the observed binding energy values for -NH2 at 399.4 eV and -N=N- at 400.2 eV. The SERS spectrum reveals the presence Au-C (437 cm(-1)) bond on AP-AuNPs. Further, the AP-AuNPs were self-assembled on GC/ITO electrode (AP-AuNPs modified electrode) with the aid of free amine groups present on the surface of AP-AuNPs via Michael's nucleophilic addition reaction. The AP-AuNPs modified electrode was characterized by cyclic voltammetry, impedance spectroscopy, UV-visible spectroscopy and scanning electron microscopy. Impedance studies show that the electron transfer reaction of [Fe(CN)6](3-/4-) was higher at the AP-AuNPs modified electrode (1.81×10(-4) cm s(-1)) than at bare (3.77×10(-5) cm s(-1)) GC electrode. Finally, the electrocatalytic activity of the AP-AuNPs modified electrode was demonstrated by studying the oxidation of dopamine (DA). Copyright © 2014 Elsevier Inc. All rights reserved.

Auger Electrons as Probes for Composite Micro- and Nano- structured Materials: Application to Solid Electrolyte Interphases in Graphite and Silicon-Graphite Electrodes

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

Kalaga, Kaushik; Shkrob, Ilya A.; Haasch, Richard T.

In this study, Auger electron spectroscopy (AES) combined with ion sputtering profilometry, Xray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM) have been used in a complementary fashion to examine chemical and microstructural changes in graphite (Gr) and silicon/graphite (Si/Gr) blends contained in the negative electrodes of lithium-ion cells. We demonstrate how AES can be used to characterize morphology of the solid-electrolyte interphase (SEI) deposits in such heterogeneous media, complementing well-established methods, such as XPS and SEM. In this way we demonstrate that the SEI does not consist of uniformly thick layers on the graphite and silicon; the thickness ofmore » the SEI layers in cycle-life aged electrodes follows an exponential distribution with a mean of ca. 13 nm for the graphite and ca. 20-25 nm for the silicon nanoparticles (with a crystalline core of 50-70 nm in diameter). Furthermore, a “sticky-sphere” model, in which Si nanoparticles are covered with a layer of polymer binder (that is replaced by the SEI during cycling) of variable thickness is introduced to account for the features observed.« less

Auger Electrons as Probes for Composite Micro- and Nano- structured Materials: Application to Solid Electrolyte Interphases in Graphite and Silicon-Graphite Electrodes

DOE PAGES

Kalaga, Kaushik; Shkrob, Ilya A.; Haasch, Richard T.; ...

2017-10-05

In this study, Auger electron spectroscopy (AES) combined with ion sputtering profilometry, Xray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM) have been used in a complementary fashion to examine chemical and microstructural changes in graphite (Gr) and silicon/graphite (Si/Gr) blends contained in the negative electrodes of lithium-ion cells. We demonstrate how AES can be used to characterize morphology of the solid-electrolyte interphase (SEI) deposits in such heterogeneous media, complementing well-established methods, such as XPS and SEM. In this way we demonstrate that the SEI does not consist of uniformly thick layers on the graphite and silicon; the thickness ofmore » the SEI layers in cycle-life aged electrodes follows an exponential distribution with a mean of ca. 13 nm for the graphite and ca. 20-25 nm for the silicon nanoparticles (with a crystalline core of 50-70 nm in diameter). Furthermore, a “sticky-sphere” model, in which Si nanoparticles are covered with a layer of polymer binder (that is replaced by the SEI during cycling) of variable thickness is introduced to account for the features observed.« less

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

NASA Astrophysics Data System (ADS)

Zemlyanov, Dmitry Y.; Jespersen, Michael; Zakharov, Dmitry N.; Hu, Jianjun; Paul, Rajib; Kumar, Anurag; Pacley, Shanee; Glavin, Nicholas; Saenz, David; Smith, Kyle C.; Fisher, Timothy S.; Voevodin, Andrey A.

2018-03-01

X-ray photoelectron spectroscopy (XPS) has been utilized as a versatile method for thickness characterization of various two-dimensional (2D) films. Accurate thickness can be measured simultaneously while acquiring XPS data for chemical characterization of 2D films having thickness up to approximately 10 nm. For validating the developed technique, thicknesses of few-layer graphene (FLG), MoS2 and amorphous boron nitride (a-BN) layer, produced by microwave plasma chemical vapor deposition (MPCVD), plasma enhanced chemical vapor deposition (PECVD), and pulsed laser deposition (PLD) respectively, were accurately measured. The intensity ratio between photoemission peaks recorded for the films (C 1s, Mo 3d, B 1s) and the substrates (Cu 2p, Al 2p, Si 2p) is the primary input parameter for thickness calculation, in addition to the atomic densities of the substrate and the film, and the corresponding electron attenuation length (EAL). The XPS data was used with a proposed model for thickness calculations, which was verified by cross-sectional transmission electron microscope (TEM) measurement of thickness for all the films. The XPS method determines thickness values averaged over an analysis area which is orders of magnitude larger than the typical area in cross-sectional TEM imaging, hence provides an advanced approach for thickness measurement over large areas of 2D materials. The study confirms that the versatile XPS method allows rapid and reliable assessment of the 2D material thickness and this method can facilitate in tailoring growth conditions for producing very thin 2D materials effectively over a large area. Furthermore, the XPS measurement for a typical 2D material is non-destructive and does not require special sample preparation. Therefore, after XPS analysis, exactly the same sample can undergo further processing or utilization.

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

DOE PAGES

Zemlyanov, Dmitry Y.; Jespersen, Michael; Zakharov, Dmitry N.; ...

2018-02-07

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

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

PubMed

Zemlyanov, Dmitry Y; Jespersen, Michael; Zakharov, Dmitry N; Hu, Jianjun; Paul, Rajib; Kumar, Anurag; Pacley, Shanee; Glavin, Nicholas; Saenz, David; Smith, Kyle C; Fisher, Timothy S; Voevodin, Andrey A

2018-03-16

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

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

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

Zemlyanov, Dmitry Y.; Jespersen, Michael; Zakharov, Dmitry N.

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

New insights into micro/nanoscale combined probes (nanoAuger, μXPS) to characterize Ag/Au@SiO2 core-shell assemblies

NASA Astrophysics Data System (ADS)

Ledeuil, J. B.; Uhart, A.; Soulé, S.; Allouche, J.; Dupin, J. C.; Martinez, H.

2014-09-01

This work has examined the elemental distribution and local morphology at the nanoscale of core@shell Ag/Au@SiO2 particles. The characterization of such complex metal/insulator materials becomes more efficient when using an initial cross-section method of preparation of the core@shell nanoparticles (ion milling cross polisher). The originality of this route of preparation allows one to obtain undamaged, well-defined and planar layers of cross-cut nano-objects. Once combined with high-resolution techniques of characterization (XPS, Auger and SEM), the process appears as a powerful way to minimize charging effects and enhance the outcoming electron signal (potentially affected by the topography of the material) during analysis. SEM experiments have unambiguously revealed the hollow-morphology of the metal core, while Auger spectroscopy observations showed chemical heterogeneity within the particles (as silver and gold are randomly found in the core ring). To our knowledge, this is the first time that Auger nano probe spectroscopy has been used and successfully optimized for the study of some complex metal/inorganic interfaces at such a high degree of resolution (~12 nm). Complementarily, XPS Au 4f and Ag 3d peaks were finally detected attesting the possibility of access to the whole chemistry of such nanostructured assemblies.This work has examined the elemental distribution and local morphology at the nanoscale of core@shell Ag/Au@SiO2 particles. The characterization of such complex metal/insulator materials becomes more efficient when using an initial cross-section method of preparation of the core@shell nanoparticles (ion milling cross polisher). The originality of this route of preparation allows one to obtain undamaged, well-defined and planar layers of cross-cut nano-objects. Once combined with high-resolution techniques of characterization (XPS, Auger and SEM), the process appears as a powerful way to minimize charging effects and enhance the outcoming electron signal (potentially affected by the topography of the material) during analysis. SEM experiments have unambiguously revealed the hollow-morphology of the metal core, while Auger spectroscopy observations showed chemical heterogeneity within the particles (as silver and gold are randomly found in the core ring). To our knowledge, this is the first time that Auger nano probe spectroscopy has been used and successfully optimized for the study of some complex metal/inorganic interfaces at such a high degree of resolution (~12 nm). Complementarily, XPS Au 4f and Ag 3d peaks were finally detected attesting the possibility of access to the whole chemistry of such nanostructured assemblies. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr03211j

Polyethylene imine modified hydrochar adsorption for chromium (VI) and nickel (II) removal from aqueous solution.

PubMed

Shi, Yuanji; Zhang, Tao; Ren, Hongqiang; Kruse, Andrea; Cui, Ruofan

2018-01-01

An adsorbent hydrochar was synthesized from corn cobs and modified with polyethylene imine (PEI). The hydrochars before and after modification were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and thermogravimetric analysis. FTIR and XPS revealed that the PEI was grafted onto the hydrochar via ether and imine bonds formed with glutaraldehyde. The maximum adsorption capacities for Cr(VI) (33.663mg/g) and Ni(II) (29.059mg/g) on the modified hydrochars were 365% and 43.7% higher, respectively, than those on the unmodified hydrochar. A pseudo-second-order model described the adsorption of Ni(II) and Cr(VI) on all the adsorbents. The adsorption of Cr(VI) was endothermic, spontaneous, increased disorder, and obeyed the Langmuir model. By contrast, the adsorption of Ni(II) was exothermic, spontaneous, decreased disorder, and obeyed the Freundlich model. XPS confirmed that the adsorption sites and mechanisms for Ni(II) and Cr(VI) on the modified hydrochars were different. Copyright © 2017 Elsevier Ltd. All rights reserved.

Surface characterization in composite and titanium bonding: Carbon fiber surface treatments for improved adhesion to thermoplastic polymers

NASA Technical Reports Server (NTRS)

Devilbiss, T. A.; Wightman, J. P.

1987-01-01

The effect of anodization in NaOH, H2SO4, and amine salts on the surface chemistry of carbon fibers was examined by X-ray photoelectron spectroscopy (XPS). The surfaces of carbon fibers after anodization in NaOH and H2SO4 were examined by scanning transmission electron microscopy (STEM), angular dependent XPS, UV absorption spectroscopy of the anodization bath, secondary ion mass spectrometry, and polar/dispersive surface energy analysis. Hercules AS-4, Dexter Hysol XAS, and Union Carbide T-300 fibers were examined by STEM, angular dependent XPS, and breaking strength measurement before and after commercial surface treatment. Oxygen and nitrogen were added to the fiber surfaces by anodization in amine salts. Analysis of the plasmon peak in the carbon 1s signal indicated that H2SO4 anodization affected the morphological structure of the carbon fiber surface. The work of adhesion of carbon fibers to thermoplastic resins was calculated using the geometric mean relationship. A correlation was observed between the dispersive component of the work of adhesion and the interfacial adhesion.

Deposition and characterization of stoichiometric films of V2O5 on Pd(111)

NASA Astrophysics Data System (ADS)

Feng, Xu; Abdel-Rahman, Mohammed K.; Kruppe, Christopher M.; Trenary, Michael

2017-10-01

A simple and efficient method has been used to grow V2O5 thin films on Pd(111) at a substrate temperature of 300 K through physical vapor deposition by heating a fine powder of V2O5 in a non-oxidative, UHV environment. X-ray photoelectron spectroscopy (XPS), reflection absorption infrared spectroscopy (RAIRS) and low energy electron diffraction (LEED) were used to characterize the thin films. When the as-grown films exceed a minimum thickness, characteristic features of V2O5 were revealed by XPS and RAIRS, which confirms the presence of stoichiometric V2O5. LEED indicates no long range order of the as-grown films at 300 K. Annealing to temperatures between 600 and 700 K causes a reduction of V2O5 to VO2 as identified by XPS and the formation of ordered structures as determined by LEED, and VO2 is predominant after annealing to 800 K. After further annealing to 1000 K, only an ordered form of V2O3 is present on Pd(111).

Quantification of Efficiency of Beneficiation of Lunar Regolith

NASA Technical Reports Server (NTRS)

Trigwell, Steve; Lane, John; Captain, James; Weis, Kyle; Quinn, Jacqueline; Watanabe, Fumiya

2011-01-01

Electrostatic beneficiation of lunar regolith is being researched at Kennedy Space Center to enhance the ilmenite concentration of the regolith for the production of oxygen in in-situ resource utilization on the lunar surface. Ilmenite enrichment of up to 200% was achieved using lunar simulants. For the most accurate quantification of the regolith particles, standard petrographic methods are typically followed, but in order to optimize the process, many hundreds of samples were generated in this study that made the standard analysis methods time prohibitive. In the current studies, X-ray photoelectron spectroscopy (XPS) and Secondary Electron microscopy/Energy Dispersive Spectroscopy (SEM/EDS) were used that could automatically, and quickly, analyze many separated fractions of lunar simulant. In order to test the accuracy of the quantification, test mixture samples of known quantities of ilmenite (2, 5, 10, and 20 wt%) in silica (pure quartz powder), were analyzed by XPS and EDS. The results showed that quantification for low concentrations of ilmenite in silica could be accurately achieved by both XPS and EDS, knowing the limitations of the techniques. 1

Insights into electrochemical reactions from ambient pressure photoelectron spectroscopy.

PubMed

Stoerzinger, Kelsey A; Hong, Wesley T; Crumlin, Ethan J; Bluhm, Hendrik; Shao-Horn, Yang

2015-11-17

The understanding of fundamental processes in the bulk and at the interfaces of electrochemical devices is a prerequisite for the development of new technologies with higher efficiency and improved performance. One energy storage scheme of great interest is splitting water to form hydrogen and oxygen gas and converting back to electrical energy by their subsequent recombination with only water as a byproduct. However, kinetic limitations to the rate of oxygen-based electrochemical reactions hamper the efficiency in technologies such as solar fuels, fuel cells, and electrolyzers. For these reactions, the use of metal oxides as electrocatalysts is prevalent due to their stability, low cost, and ability to store oxygen within the lattice. However, due to the inherently convoluted nature of electrochemical and chemical processes in electrochemical systems, it is difficult to isolate and study individual electrochemical processes in a complex system. Therefore, in situ characterization tools are required for observing related physical and chemical processes directly at the places where and while they occur and can help elucidate the mechanisms of charge separation and charge transfer at electrochemical interfaces. X-ray photoelectron spectroscopy (XPS), also known as ESCA (electron spectroscopy for chemical analysis), has been used as a quantitative spectroscopic technique that measures the elemental composition, as well as chemical and electronic state of a material. Building from extensive ex situ characterization of electrochemical systems, initial in situ studies were conducted at or near ultrahigh vacuum (UHV) conditions (≤10(-6) Torr) to probe solid-state electrochemical systems. However, through the integration of differential-pumping stages, XPS can now operate at pressures in the torr range, comprising a technique called ambient pressure XPS (AP-XPS). In this Account, we briefly review the working principles and current status of AP-XPS. We use several recent in situ studies on model electrochemical components as well as operando studies performed by our groups at the Advanced Light Source (ALS) at Lawrence Berkeley National Laboratory to illustrate that AP-XPS is both a chemically and an electrically specific tool since photoelectrons carry information on both the local chemistry and electrical potentials. The applications of AP-XPS to oxygen electrocatalysis shown in this Account span well-defined studies of (1) the oxide/oxygen gas interface, (2) the oxide/water vapor interface, and (3) operando measurements of half and full electrochemical cells. Using specially designed model devices, we can expose and isolate the electrode or interface of interest to the incident X-ray beam and AP-XPS analyzer to relate the electrical potentials to the composition/chemical state of the key components and interfaces. We conclude with an outlook on new developments of AP-XPS end stations, which may provide significant improvement in the observation of dynamics over a wide range of time scales, higher spatial resolution, and improved characterization of boundary or interface layers (solid/solid and liquid/solid).

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

Masuda, Takuya; PRESTO, Japan Science and Technology Agency; Yoshikawa, Hideki

In situ electrochemical X-ray photoelectron spectroscopy (XPS) apparatus, which allows XPS at solid/liquid interfaces under potential control, was constructed utilizing a microcell with an ultra-thin Si membrane, which separates vacuum and a solution. Hard X-rays from a synchrotron source penetrate into the Si membrane surface exposed to the solution. Electrons emitted at the Si/solution interface can pass through the membrane and be analyzed by an analyzer placed in vacuum. Its operation was demonstrated for potential-induced Si oxide growth in water. Effect of potential and time on the thickness of Si and Si oxide layers was quantitatively determined at sub-nanometer resolution.

Co-axial Electrospun Polyacrylonitrile-Poly(methylmethacrylate) Nanofibers: Atomic Force Microscopy and Compositional Characterization

PubMed Central

Zander, N.E.; Strawhecker, K.E.; Orlicki, J.A.; Rawlett, A.M.; Beebe, T.P.

2011-01-01

Poly(methylmethacrylate) (PMMA)- Polyacrylonitrile (PAN) fibers were prepared using a conventional single-nozzle electrospinning technique. The as-spun fibers exhibited core-shell morphology as verified by transmission electron microscopy (TEM) and atomic force microscopy (AFM). AFM-phase and modulus mapping images of the fiber cross-section and x-ray photoelectron spectroscopy (XPS) analysis indicated PAN formed the shell and PMMA the core material. XPS, thermal gravimetric analysis (TGA), and elemental analysis were used to determine fiber compositional information. Soaking the fibers in solvent demonstrated removal of the core material, generating hollow PAN fibers. PMID:21928836

Local Fine Structural Insight into Mechanism of Electrochemical Passivation of Titanium.

PubMed

Wang, Lu; Yu, Hongying; Wang, Ke; Xu, Haisong; Wang, Shaoyang; Sun, Dongbai

2016-07-20

Electrochemically formed passive film on titanium in 1.0 M H2SO4 solution and its thickness, composition, chemical state, and local fine structure are examined by Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and X-ray absorption fine structure. AES analysis reveals that the thickness and composition of oxide film are proportional to the reciprocal of current density in potentiodynamic polarization. XPS depth profiles of the chemical states of titanium exhibit the coexistence of various valences cations in the surface. Quantitative X-ray absorption near edge structure analysis of the local electronic structure of the topmost surface (∼5.0 nm) shows that the ratio of [TiO2]/[Ti2O3] is consistent with that of passivation/dissolution of electrochemical activity. Theoretical calculation and analysis of extended X-ray absorption fine structure spectra at Ti K-edge indicate that both the structures of passivation and dissolution are distorted caused by the appearance of two different sites of Ti-O and Ti-Ti. And the bound water in the topmost surface plays a vital role in structural disorder confirmed by XPS. Overall, the increase of average Ti-O coordination causes the electrochemical passivation, and the dissolution is due to the decrease of average Ti-Ti coordination. The structural variations of passivation in coordination number and interatomic distance are in good agreement with the prediction of point defect model.

Surface chemical properties of eutectic and frozen NaCl solutions probed by XPS and NEXAFS.

PubMed

Křepelová, Adéla; Huthwelker, Thomas; Bluhm, Hendrik; Ammann, Markus

2010-12-17

We study the surface of sodium chloride-water mixtures above, at, and below the eutectic temperature using X-ray photoelectron spectroscopy (XPS) and electron-yield near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. The NaCl frozen solutions are mimicking sea-salt deposits in ice or snow. Sea-salt particles emitted from the oceans are a major contributor to the global aerosol burden and can act as a catalyst for heterogeneous chemistry or as cloud condensation nuclei. The nature of halogen ions at ice surfaces and their influence on surface melting of ice are of significant current interest. We found that the surface of the frozen solution, depending on the temperature, consists of ice and different NaCl phases, that is, NaCl, NaCl·2H(2)O, and surface-adsorbed water.

Sliding friction and wear behaviors of surface-coated natural serpentine mineral powders as lubricant additive

NASA Astrophysics Data System (ADS)

Zhang, Baosen; Xu, Yi; Gao, Fei; Shi, Peijing; Xu, Binshi; Wu, Yixiong

2011-01-01

This work aims to investigate the friction and wear properties of surface-coated natural serpentine powders (SP) suspended in diesel engine oil using an Optimal SRV oscillating friction and wear tester. The worn surface was characterized by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS). Results indicated that the additives can improve the wear resistance and decrease friction coefficient of carbon steel friction couples. The 0.5 wt% content of serpentine powders is found most efficient in reducing friction and wear at the load of 50 N. The SEM and XPS analysis results demonstrate that a tribofilm forms on the worn surface, which is responsible for the decrease in friction and wear, mainly with iron oxides, silicon oxides, graphite and organic compounds.

Local electrical properties of thermally grown oxide films formed on duplex stainless steel surfaces

NASA Astrophysics Data System (ADS)

Guo, L. Q.; Yang, B. J.; He, J. Y.; Qiao, L. J.

2018-06-01

The local electrical properties of thermally grown oxide films formed on ferrite and austenite surfaces of duplex stainless steel at different temperatures were investigated by Current sensing atomic force microscopy, X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). The current maps and XPS/AES analyses show that the oxide films covering austenite and ferrite surfaces formed at different temperatures exhibit different local electrical characteristics, thickness and composition. The dependence of electrical conductivity of oxide films covering austenite and ferrite surface on the formation temperature is attributed to the film thickness and semiconducting structures, which is intrinsically related to thermodynamics and kinetics process of film grown at different temperature. This is well elucidated by corresponding semiconductor band structures of oxide films formed on austenite and ferrite phases at different temperature.

Electrochemical and thermal grafting of alkyl grignard reagents onto (100) silicon surfaces.

PubMed

Vegunta, Sri Sai S; Ngunjiri, Johnpeter N; Flake, John C

2009-11-03

Passivation of (100) silicon surfaces using alkyl Grignard reagents is explored via electrochemical and thermal grafting methods. The electrochemical behavior of silicon in methyl or ethyl Grignard reagents in tetrahydrofuran is investigated using cyclic voltammetry. Surface morphology and chemistry are investigated using atomic force microscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy (XPS). Results show that electrochemical pathways provide an efficient and more uniform passivation method relative to thermal methods, and XPS results demonstrate that electrografted terminations are effective at limiting native oxide formation for more than 55 days in ambient conditions. A two-electron per silicon mechanism is proposed for electrografting a single (1:1) alkyl group per (100) silicon atom. The mechanism includes oxidation of two Grignard species and subsequent hydrogen abstraction and alkylation reaction resulting in a covalent attachment of alkyl groups with silicon.

Hydrogenation and hydrogen intercalation of hexagonal boron nitride on Ni(1 1 1): reactivity and electronic structure

NASA Astrophysics Data System (ADS)

Späth, F.; Gebhardt, J.; Düll, F.; Bauer, U.; Bachmann, P.; Gleichweit, C.; Görling, A.; Steinrück, H.-P.; Papp, C.

2017-09-01

We investigate the reactivity of hexagonal boron nitride (h-BN) on a Ni(1 1 1) single crystal towards atomic hydrogen over a wide exposure range. Near edge x-ray absorption fine structure and x-ray photoelectron spectroscopy (XPS) show that for low hydrogen exposures hydrogenation of the h-BN sheet is found. In contrast, intercalation of hydrogen between h-BN and the Ni(1 1 1) substrate occurs for high exposures. For intermediate regimes, a mixture of intercalation and hydrogenation is observed. From temperature-programmed desorption and temperature-programmed XPS experiments, we conclude that the hydrogen covalently bound to h-BN is rather stable with a desorption temperature of 600 K, while intercalated hydrogen is desorbing already at 390 K. Further insight into the structural arrangements and the thermodynamics of the system is obtained by comparing our experimental results with extensive density-functional theory calculations. Together with ultraviolet photoelectron spectroscopy measurements, the calculations provide detailed insight into the influence of hydrogenation on the electronic structure of h-BN.

Ab initio calculations of the electronic structure and specific optical features of β-LiNH4SO4 single crystals

NASA Astrophysics Data System (ADS)

Rudysh, M. Ya.; Brik, M. G.; Stadnyk, V. Yo.; Brezvin, R. S.; Shchepanskyi, P. A.; Fedorchuk, A.; Khyzhun, O. Y.; Kityk, I. V.; Piasecki, M.

2018-01-01

In the present work complex experimental and theoretical studies of electronic and optical properties for β-lithium-ammonium sulfate crystals of good optical quality are performed using the X-ray photoelectron spectroscopy (XPS) and X-ray emission spectroscopy (XES). Standard immersion and spectroscopic techniques accompanied by the theoretical quantum-chemical calculations in the density functional theory (DFT) framework were applied. Calculations of band structure and related properties were carried out within a framework of local density and generalized gradient approximations as well as hybrid B3LYP functionals. The energy levels features and their origin are established from the DFT calculations and they were ferified by XPS and XES measurements. Theoretical and experimental refractive indices dispersions along the principal crystallographic directions (nx, ny and nz) as well as birefringence dispersion (Δnx, Δny and Δnz) in the visible spectral range are obtained. It was found a closeness of nx and ny curves for the titled crystals. More precise birefringence examining predicts their intersection at λ ≈ 190 nm.

Sonochemical fabrication of fluorinated mesoporous titanium dioxide microspheres

NASA Astrophysics Data System (ADS)

Yu, Changlin; Yu, Jimmy C.; Chan, Mui

2009-05-01

A sonochemical-hydrothermal method for preparing fluorinated mesoporous TiO 2 microspheres was developed. Formation of mesoporous TiO 2 and doping of fluorine was achieved by sonication and then hydrothermal treatment of a solution containing titanium isopropoxide, template, and sodium fluoride. The as-synthesized TiO 2 microspheres were characterized by X-ray diffraction (XRD), Fourier translation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX) spectroscopy, photoluminescence spectroscopy (PL), and BET surface areas. The P123 template was removed completely during the hydrothermal and washing steps, which was different from the conventional calcination treatment. The as- synthesized TiO 2 microspheres had good crystallinity and high stability. Results from the photocatalytic degradation of methylene blue (MB) showed that fluorination could remarkably improve the photocatalytic activity of titanium dioxide.

Characterization of Arsenic Contamination on Rust from Ton Containers

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

Gary S. Groenewold; Recep Avci; Robert V. Fox

The speciation and spatial distribution of arsenic on rusted steel surfaces affects both measurement and removal approaches. The chemistry of arsenic residing in the rust of ton containers that held the chemical warfare agents bis(2-chloroethyl)sulfide (sulfur mustard) and 2-chlorovinyldichloroarsine (Lewisite) is of particular interest, because while the agents have been decontaminated, residual arsenic could pose a health or environmental risk. The chemistry and distribution of arsenic in rust samples was probed using imaging secondary ion mass spectrometry (SIMS), X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy, and scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDX). Arsenic in the +3 and or +5more » oxidation state is homogeneously distributed at the very top-most layer of the rust samples, and is intimately associated with iron. Sputter depth profiling followed by SIMS and XPS shows As at a depth of several nm, in some cases in a reduced form. The SEM/EDX experiments show that As is present at a depth of several microns, but is inhomogeneously distributed; most locations contained oxidized As at concentrations of a few percent, however several locations showed very high As in a metallic form. These results indicate that the rust material must be removed if the steel containers are to be cleared of arsenic.« less

X-ray photoelectron spectroscopy for identification of morphological defects and disorders in graphene devices

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

Aydogan, Pinar; Suzer, Sefik, E-mail: suzer@fen.bilkent.edu.tr; Polat, Emre O.

The progress in the development of graphene devices is promising, and they are now considered as an option for the current Si-based electronics. However, the structural defects in graphene may strongly influence the local electronic and mechanical characteristics. Although there are well-established analytical characterization methods to analyze the chemical and physical parameters of this material, they remain incapable of fully understanding of the morphological disorders. In this study, x-ray photoelectron spectroscopy (XPS) with an external voltage bias across the sample is used for the characterization of morphological defects in large area of a few layers graphene in a chemically specificmore » fashion. For the XPS measurements, an external +6 V bias applied between the two electrodes and areal analysis for three different elements, C1s, O1s, and Au4f, were performed. By monitoring the variations of the binding energy, the authors extract the voltage variations in the graphene layer which reveal information about the structural defects, cracks, impurities, and oxidation levels in graphene layer which are created purposely or not. Raman spectroscopy was also utilized to confirm some of the findings. This methodology the authors offer is simple but provides promising chemically specific electrical and morphological information.« less

Surface analysis of anodized aluminum clamps from NASA-LDEF satellite

NASA Technical Reports Server (NTRS)

Grammer, H. L.; Wightman, J. P.; Young, Philip R.

1992-01-01

Surface analysis results of selected anodized aluminum clamps containing black (Z306) and white (A276) paints which received nearly six years of Low Earth Orbit (LEO) exposure on the Long Duration Exposure Facility are reported. Surface analytical techniques, including x-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and scanning electron microscopy/energy dispersive analysis by x-ray (SEM/EDAX), showed significant differences in the surface composition of these materials depending upon the position on the LDEF. Differences in the surface composition are attributed to varying amounts of atomic oxygen and vacuum ultraviolet radiation (VUV). Silicon containing compounds were the primary contaminant detected on the materials.

Surface characterization of LDEF materials

NASA Astrophysics Data System (ADS)

Wightman, J. P.; Grammer, Holly Little

1993-10-01

The NASA Long Duration Exposure Facility (LDEF), a passive experimental satellite, was placed into low-Earth orbit by the Shuttle Challenger in Apr. 1984. The LDEF spent an unprecedented 69 months in space. The flight and recovery of the LDEF provided a wealth of information on the longterm space environmental effects of a variety of materials exposed to the low-Earth orbit environment. Surface characterization of LDEF materials included polymers, composites, thermal control paints, and aluminum. X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), scanning electron microscopy (SEM), and contact angle analysis were used to document changes in both the surface composition and surface chemistry of these materials. Detailed XPS analysis of the polymer systems, such as Kapton, polyimide polysiloxane copolymers, and fluorinated ethylene propylene thermal blankets on the backside of the LDEF revealed significant changes in both the surface composition and surface chemistry as a result of exposure to the low-Earth orbit environment. Polymer systems such as Kapton, polyimide polysiloxane copolymers, and polysulfone showed a common trend of decreasing carbon content and increasing oxygen content with respect to the control sample. Carbon 1s curve fit XPS analysis of the composite samples, in conjunction with SEM photomicrographs, revealed significant ablation of the polymer matrix resin to expose the carbon fibers of the composite during exposure to the space environment. Surface characterization of anodized aluminum tray clamps, which were located at regular intervals over the entire LDEF frame, provided the first results to evaluate the extent of contamination with respect to position on the LDEF. The XPS results clearly showed that the amount and state of both silicon and fluorine contamination were directly dependent upon the position of the tray clamp on the LDEF.

Surface characterization of LDEF materials

NASA Technical Reports Server (NTRS)

Wightman, J. P.; Grammer, Holly Little

1993-01-01

The NASA Long Duration Exposure Facility (LDEF), a passive experimental satellite, was placed into low-Earth orbit by the Shuttle Challenger in Apr. 1984. The LDEF spent an unprecedented 69 months in space. The flight and recovery of the LDEF provided a wealth of information on the longterm space environmental effects of a variety of materials exposed to the low-Earth orbit environment. Surface characterization of LDEF materials included polymers, composites, thermal control paints, and aluminum. X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), scanning electron microscopy (SEM), and contact angle analysis were used to document changes in both the surface composition and surface chemistry of these materials. Detailed XPS analysis of the polymer systems, such as Kapton, polyimide polysiloxane copolymers, and fluorinated ethylene propylene thermal blankets on the backside of the LDEF revealed significant changes in both the surface composition and surface chemistry as a result of exposure to the low-Earth orbit environment. Polymer systems such as Kapton, polyimide polysiloxane copolymers, and polysulfone showed a common trend of decreasing carbon content and increasing oxygen content with respect to the control sample. Carbon 1s curve fit XPS analysis of the composite samples, in conjunction with SEM photomicrographs, revealed significant ablation of the polymer matrix resin to expose the carbon fibers of the composite during exposure to the space environment. Surface characterization of anodized aluminum tray clamps, which were located at regular intervals over the entire LDEF frame, provided the first results to evaluate the extent of contamination with respect to position on the LDEF. The XPS results clearly showed that the amount and state of both silicon and fluorine contamination were directly dependent upon the position of the tray clamp on the LDEF.

Nitrogen-doped carbon dots originating from unripe peach for fluorescent bioimaging and electrocatalytic oxygen reduction reaction.

PubMed

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Lee, Yong Rok

2016-11-15

This paper reports the robust hydrothermal synthesis of nitrogen doped carbon dots (N-CDs) using the unripe fruit of Prunus persica (peach) as the carbon precursor and aqueous ammonia as the nitrogen source. The optical properties of synthesized N-CDs were characterized by ultraviolet visible (UV-Vis) and fluorescence spectroscopy techniques. The synthesized N-CDs were emitted blue light when excitated with a portable UV lamp. The materials with the optical properties were characterized further by high resolution transmission electron microscope (HRTEM), X-ray diffraction (XRD), Raman, Fourier transform infrared (FT-IR) and X-ray photoelectron spectroscopy (XPS). The mean size of the N-CDs was approximately 8nm, as calculated from the HRTEM image. The d-spacing of N-CDs, calculated using Bragg law, was approximately 0.21nm, which was consistent with the interlayer distance calculated from the HRTEM image. FT-IR spectroscopy and XPS revealed the presence of the phytoconstituents functionalities of peach fruit over the N-CDs surface and a high level of nitrogen doping on carbon dots (CDs) was confirmed by XPS studies. These results suggest that the unripe fruit extract of peach is an ideal candidate for the preparation of N-CDs. The resulting N-CDs showed excellent optical properties in water. The synthesized N-CDs exhibited a high fluorescence quantum yield and low cytotoxicity, and can be used as fluorescence imaging probes. In addition, the N-CDs were catalytically activite towards the oxygen reduction reaction (ORR). The N-CDs exhibited good catalytic activity in an alkaline medium (0.1M KOH) with a remarkable ORR of approximately 0.72V vs reversible hydrogen electrode (RHE), and O2 reduction follows mainly a 2 electron pathway by being reduced to hydrogen peroxide. The 2-electron reduction pathway is used in industry for H2O2 production. Copyright © 2016 Elsevier Inc. All rights reserved.

Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

NASA Astrophysics Data System (ADS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Sethuraman, Mathur Gopalakrishnan; Lee, Yong Rok

2016-10-01

Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV-vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.

Application of modern surface analytical tools in the investigation of surface deterioration processes

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1983-01-01

Surface profilometry and scanning electron microscopy were utilized to study changes in the surface of polymers when eroded. The X-ray photoelectron spectroscopy (XPS) and depth profile analysis indicate the corrosion of metal and ceramic surfaces and reveal the diffusion of certain species into the surface to produce a change in mechanical properties. Ion implantation, nitriding and plating and their effects on the surface are characterized. Auger spectroscopy analysis identified morphological properties of coatings applied to surfaces by sputter deposition.

Electron-beam-induced post-grafting polymerization of acrylic acid onto the surface of Kevlar fibers

NASA Astrophysics Data System (ADS)

Xu, Lu; Hu, Jiangtao; Ma, Hongjuan; Wu, Guozhong

2018-04-01

The surface of Kevlar fibers was successfully modified by electron beam (EB)-induced post-grafting of acrylic acid (AA). The generation of radicals in the fibers was confirmed by electron spin resonance (ESR) measurements, and the concentration of radicals was shown to increase as the absorbed dose increased, but decrease with increasing temperature. The influence of the synthesis conditions on the degree of grafting was also investigated. The surface microstructure and chemical composition of the modified Kevlar fibers were characterized by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The SEM images revealed that the surface of the grafted fibers was rougher than those of the pristine and irradiated fibers. XPS analysis confirmed an increase in C(O)OH groups on the surface of the Kevlar fibers, suggesting successful grafting of AA. These results indicate that EB-induced post-grafting polymerization is effective for modifying the surface properties of Kevlar fibers.

Atomic charges of sulfur in ionic liquids: experiments and calculations.

PubMed

Fogarty, Richard M; Rowe, Rebecca; Matthews, Richard P; Clough, Matthew T; Ashworth, Claire R; Brandt, Agnieszka; Corbett, Paul J; Palgrave, Robert G; Smith, Emily F; Bourne, Richard A; Chamberlain, Thomas W; Thompson, Paul B J; Hunt, Patricia A; Lovelock, Kevin R J

2017-12-14

Experimental near edge X-ray absorption fine structure (NEXAFS) spectra, X-ray photoelectron (XP) spectra and Auger electron spectra are reported for sulfur in ionic liquids (ILs) with a range of chemical structures. These values provide experimental measures of the atomic charge in each IL and enable the evaluation of the suitability of NEXAFS spectroscopy and XPS for probing the relative atomic charge of sulfur. In addition, we use Auger electron spectroscopy to show that when XPS binding energies differ by less than 0.5 eV, conclusions on atomic charge should be treated with caution. Our experimental data provides a benchmark for calculations of the atomic charge of sulfur obtained using different methods. Atomic charges were computed for lone ions and ion pairs, both in the gas phase (GP) and in a solvation model (SMD), with a wide range of ion pair conformers considered. Three methods were used to compute the atomic charges: charges from the electrostatic potential using a grid based method (ChelpG), natural bond orbital (NBO) population analysis and Bader's atoms in molecules (AIM) approach. By comparing the experimental and calculated measures of the atomic charge of sulfur, we provide an order for the sulfur atoms, ranging from the most negative to the most positive atomic charge. Furthermore, we show that both ChelpG and NBO are reasonable methods for calculating the atomic charge of sulfur in ILs, based on the agreement with both the XPS and NEXAFS spectroscopy results. However, the atomic charges of sulfur derived from ChelpG are found to display significant, non-physical conformational dependence. Only small differences in individual atomic charge of sulfur were observed between lone ion (GP) and ion pair IL(SMD) model systems, indicating that ion-ion interactions do not strongly influence individual atomic charges.

Applications of XPS in the characterization of Battery materials

DOE PAGES

Shutthanandan, Vaithiyalingam; Nandasiri, Manjula; Zheng, Jianming; ...

2018-05-26

In this study, technological development requires reliable power sources where energy storage devices are emerging as a critical component. Wide range of energy storage devices, Redox-flow batteries (RFB), Lithium ion based batteries (LIB), and Lithium-sulfur (LSB) batteries are being developed for various applications ranging from grid-scale level storage to mobile electronics. Material complexities associated with these energy storage devices with unique electrochemistry are formidable challenge which needs to be address for transformative progress in this field. X-ray photoelectron spectroscopy (XPS) - a powerful surface analysis tool - has been widely used to study these energy storage materials because of itsmore » ability to identify, quantify and image the chemical distribution of redox active species. However, accessing the deeply buried solid-electrolyte interfaces (which dictates the performance of energy storage devices) has been a challenge in XPS usage. Herein we report our recent efforts to utilize the XPS to gain deep insight about these interfaces under realistic conditions with varying electrochemistry involving RFB, LIB and LSB.« less

Applications of XPS in the characterization of Battery materials

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

Shutthanandan, Vaithiyalingam; Nandasiri, Manjula; Zheng, Jianming

In this study, technological development requires reliable power sources where energy storage devices are emerging as a critical component. Wide range of energy storage devices, Redox-flow batteries (RFB), Lithium ion based batteries (LIB), and Lithium-sulfur (LSB) batteries are being developed for various applications ranging from grid-scale level storage to mobile electronics. Material complexities associated with these energy storage devices with unique electrochemistry are formidable challenge which needs to be address for transformative progress in this field. X-ray photoelectron spectroscopy (XPS) - a powerful surface analysis tool - has been widely used to study these energy storage materials because of itsmore » ability to identify, quantify and image the chemical distribution of redox active species. However, accessing the deeply buried solid-electrolyte interfaces (which dictates the performance of energy storage devices) has been a challenge in XPS usage. Herein we report our recent efforts to utilize the XPS to gain deep insight about these interfaces under realistic conditions with varying electrochemistry involving RFB, LIB and LSB.« less

Simple quantification of surface carboxylic acids on chemically oxidized multi-walled carbon nanotubes

NASA Astrophysics Data System (ADS)

Gong, Hyejin; Kim, Seong-Taek; Lee, Jong Doo; Yim, Sanggyu

2013-02-01

The surface of multi-walled carbon nanotube (MWCNT) was chemically oxidized using nitric acid and sulfuric-nitric acid mixtures. Thermogravimetric analysis, transmission electron microscopy and infrared spectroscopy revealed that the use of acid mixtures led to higher degree of oxidation. More quantitative identification of surface carboxylic acids was carried out using X-ray photoelectron spectroscopy (XPS) and acid-base titration. However, these techniques are costly and require very long analysis times to promptly respond to the extent of the reaction. We propose a much simpler method using pH measurements and pre-determined pKa value in order to estimate the concentration of carboxylic acids on the oxidized MWCNT surfaces. The results from this technique were consistent with those obtained from XPS and titration, and it is expected that this simple quantification method can provide a cheap and fast way to monitor and control the oxidation reaction of MWCNT.

Initial stages of microbiologically influenced tarnishing on titanium after 20 months of immersion in freshwater.

PubMed

Moreno, D A; Cano, E; Ibars, J R; Polo, J L; Montero, F; Bastidas, J M

2004-05-01

This paper studies the initial stages of iridescent tarnishes on titanium heat exchanger tubes in contact with running freshwater on the river Tagus in Spain for up to 20 months. Electrochemical impedance spectroscopy (EIS), scanning electron microscopy [(SEM with energy dispersive X-ray (EDX)] and X-ray photoelectron spectroscopy (XPS) in conjunction with argon-ion sputtering were the techniques used. The EIS data indicated a capacitive behavior, showing a semicircle that was better defined as the experimental time increased, indicating a decreasing tarnishing resistance of titanium. XPS and EDX results indicated that the main elements identified were calcium, phosphorus, nitrogen, and iron. The amount of these elements was higher on the tarnished titanium specimens than on the untarnished specimens. SEM analysis showed the presence of diatoms in the iridescent tarnishes on titanium tubes. Copyright 2003 Springer-Verlag

Physicochemical properties of chars at different treatment temperatures.

PubMed

Kim, Sung Su; Kang, Youn Suk; Lee, Hyun Dong; Kim, Jae Kwan; Hong, Sung Chang

2012-02-01

In this study, the physicochemical properties of the char of Indonesian SM coal following heat treatment at various temperatures were evaluated using X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and morphological and specific surface area analysis. Based on these analyses, heat treatment of coal was determined to be the most effective in increasing the coal rank. In the XPS analysis, the C-O and C-O-C groups and quaternary-N species were found to be of a lower grade coal when the pretreatment temperature decreased, meanwhile the C-C group and pyridinic species increased. In the FT-IR analysis, the collapse of the C-O and C-O-C group was observed due to the collapse of the ether group. In SEM and Brunauer-Emmett-Teller (BET) analysis, a decrease in the ether group was shown to be accompanied with the formation of micropores.

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

Tang, Mingyi; Xu, Xiaoyang, E-mail: xiaoyangxu2012@163.com; Wu, Tao

Highlights: • Graphene oxide (GO) was modified by chemical reactions to functionalized GO (FGO). • The FGOs and the GO were then subjected to in situ free radical polymerization. • Hydroxyl groups of GO were the most reactive grafting sites. - Abstract: Graphene oxide (GO) was modified using chemical reactions to obtain three types of functionalized GO sheets (FGO). The FGO sheets and the GO were then subjected to in situ free radical polymerization in order to study the grafting polymerization. The FGO and grafted-.FGO were analyzed with Fourier transform infrared spectroscopy, scanning electronic microscopy, thermo-gravimetric analysis (TGA) and X-raymore » photoelectron spectroscopy (XPS). The grafting percentages in the materials were calculated using the TGA and XPS results. The FGO sheets with different functional groups exhibited different grafting abilities, and hydroxyl groups were proven to be the most reactive grafting sites for the in situ free radical grafting polymerization of polyacrylamide.« less

Corrosion product layers on magnesium alloys AZ31 and AZ61: Surface chemistry and protective ability

NASA Astrophysics Data System (ADS)

Feliu, S.; Llorente, I.

2015-08-01

This paper studies the chemical composition of the corrosion product layers formed on magnesium alloys AZ31 and AZ61 following immersion in 0.6 M NaCl, with a view to better understanding their protective action. Relative differences in the chemical nature of the layers were quantified by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDX) and low-angle X-ray diffraction (XRD). Corrosion behavior was investigated by Electrochemical Impedance Spectroscopy (EIS) and hydrogen evolution measurement. An inhibitive effect from the corrosion product layers was observed from EIS, principally in the case of AZ31, as confirmed by hydrogen evolution tests. A link was found between carbonate enrichment observed by XPS in the surface of the corrosion product layer, concomitant with the increase in the protective properties observed by EIS.

X-Ray Photoelectron Spectroscopic Characterization of Iron Oxide Nanoparticles

NASA Astrophysics Data System (ADS)

Radu, T.; Iacovita, C.; Benea, D.; Turcu, R.

2017-05-01

We report X-ray photoelectron spectroscopy (XPS) results on iron oxide magnetic nanoparticle (Fe3O4) synthesized using solvothermal reduction in the presence of polyethylene glycol. The magnetite obtained was employed as precursor for the synthesis of γ-Fe2O3 (by oxygen dissociation) which in turn was transformed into α-Fe2O3. We confirmed the magnetite, maghemite and hematite structure by Fourier Transformed Spectroscopy (FTIR) and X-ray diffraction (XRD). The analysis of the XPS core level and valence band (VB) photoemission spectra for all investigated samples is discussed in terms of the degree of iron oxidation. This is of fundamental importance to better understand the electronic structure of the obtained iron oxide nanoparticles in order to control and improve their quality for specific biomedical applications. Moreover, theoretical band structure calculations are performed for magnetite and the separate contributions of Fe in tetragonal and octahedral environment are shown.

Role of C–N Configurations in the Photoluminescence of Graphene Quantum Dots Synthesized by a Hydrothermal Route

PubMed Central

Permatasari, Fitri Aulia; Aimon, Akfiny Hasdi; Iskandar, Ferry; Ogi, Takashi; Okuyama, Kikuo

2016-01-01

Graphene quantum dots (GQDs) containing N atoms were successfully synthesized using a facile, inexpensive, and environmentally friendly hydrothermal reaction of urea and citric acid, and the effect of the GQDs’ C–N configurations on their photoluminescence (PL) properties were investigated. High-resolution transmission electron microscopy (HR-TEM) images confirmed that the dots were spherical, with an average diameter of 2.17 nm. X-ray photoelectron spectroscopy (XPS) analysis indicated that the C–N configurations of the GQDs substantially affected their PL intensity. Increased PL intensity was obtained in areas with greater percentages of pyridinic-N and lower percentages of pyrrolic-N. This enhanced PL was attributed to delocalized π electrons from pyridinic-N contributing to the C system of the GQDs. On the basis of energy electron loss spectroscopy (EELS) and UV-Vis spectroscopy analyses, we propose a PL mechanism for hydrothermally synthesized GQDs. PMID:26876153

Preparation of high performance NBR/HNTs nanocomposites using an electron transferring interaction method

NASA Astrophysics Data System (ADS)

Yang, Shuyan; Zhou, Yanxue; Zhang, Peng; Cai, Zhuodi; Li, Yangping; Fan, Hongbo

2017-12-01

Interfacial interaction is one of the key factors to improve comprehensive properties of polymer/inorganic filler nanocomposites. In this work, a new interfacial interaction called electron transferring interaction is reported in the nitrile-butadiene rubber/halloysite nanotubes (NBR/HNTs) nanocomposites. The X-ray photoelectron spectroscopy (XPS) and in-situ controlling temperature Fourier transform infrared spectroscopy (FTIR) have confirmed that electrons of electron-rich -CN groups in NBR can transfer to the electron-deficiency aluminum atoms of HNTs, which packs a part of NBR molecules onto the surface of HNTs to form bound rubber and stabilize the homogeneous dispersion of HNTs with few agglomeration as revealed by scanning electron microscope (SEM) and dynamic mechanical analysis (DMA) performances, even at high HNTs addition, resulting in high light transmittance. The tensile strength of NBR/30wt%HNTs nanocomposites is about 291% higher than pure NBR, without sacrificing the elongation at break.

Characterization of thin films on the nanometer scale by Auger electron spectroscopy and X-ray photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Powell, C. J.; Jablonski, A.; Werner, W. S. M.; Smekal, W.

2005-01-01

We describe two NIST databases that can be used to characterize thin films from Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS) measurements. First, the NIST Electron Effective-Attenuation-Length Database provides values of effective attenuation lengths (EALs) for user-specified materials and measurement conditions. The EALs differ from the corresponding inelastic mean free paths on account of elastic-scattering of the signal electrons. The database supplies "practical" EALs that can be used to determine overlayer-film thicknesses. Practical EALs are plotted as a function of film thickness, and an average value is shown for a user-selected thickness. The average practical EAL can be utilized as the "lambda parameter" to obtain film thicknesses from simple equations in which the effects of elastic-scattering are neglected. A single average practical EAL can generally be employed for a useful range of film thicknesses and for electron emission angles of up to about 60°. For larger emission angles, the practical EAL should be found for the particular conditions. Second, we describe a new NIST database for the Simulation of Electron Spectra for Surface Analysis (SESSA) to be released in 2004. This database provides data for many parameters needed in quantitative AES and XPS (e.g., excitation cross-sections, electron-scattering cross-sections, lineshapes, fluorescence yields, and backscattering factors). Relevant data for a user-specified experiment are automatically retrieved by a small expert system. In addition, Auger electron and photoelectron spectra can be simulated for layered samples. The simulated spectra, for layer compositions and thicknesses specified by the user, can be compared with measured spectra. The layer compositions and thicknesses can then be adjusted to find maximum consistency between simulated and measured spectra, and thus, provide more detailed characterizations of multilayer thin-film materials. SESSA can also provide practical EALs, and we compare values provided by the NIST EAL database and SESSA for hafnium dioxide. Differences of up to 10% were found for film thicknesses less than 20 Å due to the use of different physical models in each database.

Metal-passivated PbS nanoparticles: fabrication and characterization.

PubMed

Tchaplyguine, M; Mikkelä, M-H; Mårsell, E; Polley, C; Mikkelsen, A; Zhang, W; Yartsev, A; Hetherington, C J D; Wallenberg, L R; Björneholm, O

2017-03-08

Organic-shell-free PbS nanoparticles have been produced in the size range relevant for quantum-dot solar cells (QDSCs) by a vapor aggregation method involving magnetron reactive sputtering. This method creates a beam of free 5-10 nm particles in a vacuum. The dimensions of the particles were estimated after their deposition on a substrate by imaging them using ex situ SEM and HRTEM electron microscopy. The particle structure and chemical composition could be deduced "on the fly", prior to deposition, using X-ray photoelectron spectroscopy (XPS) with tunable synchrotron radiation. Our XPS results suggest that under certain conditions it is possible to fabricate particles with a semiconductor core and 1 to 2 monolayer shells of metallic lead. For this case the absolute energy of the highest occupied molecular orbital (HOMO) in PbS has been determined to be (5.0 ± 0.5) eV below the vacuum level. For such particles deposited on a substrate HRTEM has confirmed the XPS-based conclusions on the crystalline PbS structure of the semiconductor core. Absorption spectroscopy on the deposited film has given a value of ∼1 eV for the lowest exciton. Together with the valence XPS results this has allowed us to reconstruct the energy level scheme of the particles. The results obtained are discussed in the context of the properties of PbS QDSCs.

Modern Material Analysis Instruments Add a New Dimension to Materials Characterization and Failure Analysis

NASA Technical Reports Server (NTRS)

Panda, Binayak

2009-01-01

Modern analytical tools can yield invaluable results during materials characterization and failure analysis. Scanning electron microscopes (SEMs) provide significant analytical capabilities, including angstrom-level resolution. These systems can be equipped with a silicon drift detector (SDD) for very fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations, chambers that admit large samples, variable pressure for wet samples, and quantitative analysis software to examine phases. Advanced solid-state electronics have also improved surface and bulk analysis instruments: Secondary ion mass spectroscopy (SIMS) can quantitatively determine and map light elements such as hydrogen, lithium, and boron - with their isotopes. Its high sensitivity detects impurities at parts per billion (ppb) levels. X-ray photo-electron spectroscopy (XPS) can determine oxidation states of elements, as well as identifying polymers and measuring film thicknesses on coated composites. This technique is also known as electron spectroscopy for chemical analysis (ESCA). Scanning Auger electron spectroscopy (SAM) combines surface sensitivity, spatial lateral resolution (10 nm), and depth profiling capabilities to describe elemental compositions of near and below surface regions down to the chemical state of an atom.

X-ray photoelectron spectroscopy for characterization of wood surfaces in adhesion studies

Treesearch

James F. Beecher; Charles R. Frihart

2005-01-01

X-ray photoelectron spectroscopy (XPS) is one of a set of tools that have been used to characterize wood surfaces. Among the advantages of XPS are surface sensitivity, identification of nearly all elements, and frequently, discrimination of bonding states. For these reasons, XPS seemed to be an appropriate tool to help explain the differences in bond strength under wet...

Scanning tunnelling microscope for boron surface studies

NASA Astrophysics Data System (ADS)

Trenary, Michael

1990-10-01

The equipment purchased is to be used in an experimental study of the relationship between atomic structure and chemical reactivity for boron and carbon surfaces. This research is currently being supported by grant AFOSR-88-0111. A renewal proposal is currently pending with AFOSR to continue these studies. Carbon and boron are exceptionally stable, covalently bonded solids with highly unique crystal structures. The specific reactions to be studied are loosely related to the problems of oxidation and oxidation inhibition of carbon/carbon composites. The main experimental instrument to be used is a scanning tunneling microscope (STM) purchased under grant number AFSOR-89-0146. Other techniques to be used include Auger electron spectroscopy, X-ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UPS), low energy electron diffraction (LEED), temperature programmed desorption (TPD) and scanning tunneling microscopy (STM).

X-ray photoemission study of the infinite-layer cuprate superconductor Sr(0.9) La (0.1) CuO(2)

NASA Technical Reports Server (NTRS)

Vasquez, R. P.; Jung, C. U.; Kim, J. Y.; Kim, M. S.; Lee, S. Y.; Lee, S. I.

2001-01-01

The electron-doped infinite-layer superconductor Sr(0.9)La(0.1) CuO(2) is studied with x-ray photoemission spectroscopy (XPS). A nonaqueous chemical etchant is shown to effectively remove contaminants and to yield surfaces from which signals intrinsic to the superconductor dominate.

Novel mesoporous FeAl bimetal oxides for As(III) removal: Performance and mechanism.

PubMed

Ding, Zecong; Fu, Fenglian; Cheng, Zihang; Lu, Jianwei; Tang, Bing

2017-02-01

In this study, novel mesoporous FeAl bimetal oxides were successfully synthesized, characterized, and employed for As(III) removal. Batch experiments were conducted to investigate the effects of Fe/Al molar ratio, dosage, and initial solution pH values on As(III) removal. The results showed that the FeAl bimetal oxide with Fe/Al molar ratio 4:1 (shorten as FeAl-4) can quickly remove As(III) from aqueous solution in a wide pH range. The FeAl-4 before and after reaction with As(III) was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), Brunauer-Emmett-Teller (BET) surface area measurement, and X-ray photoelectron spectroscopy (XPS). The BET results showed that the original FeAl-4 with a high surface area of 223.9 m 2 /g was a mesoporous material. XPS analysis indicated that the surface of FeAl-4 possessed a high concentration of M-OH (where M represents Fe and Al), which was beneficial to the immobility of As(III). The excellent performance of FeAl-4 makes it a potentially attractive material for As(III) removal from aqueous solution. Copyright © 2016 Elsevier Ltd. All rights reserved.

Dehydration of the Uranyl Peroxide Studtite, [UO 2(η 2-O 2)(H 2O) 2]·2H 2O, Affords a Drastic Change in the Electronic Structure: A Combined X-ray Spectroscopic and Theoretical Analysis

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

Vitova, Tonya; Pidchenko, Ivan; Biswas, Saptarshi

The dehydration of studtite, [UO 2(2-O 2)(H 2O)2]·2H 2O, to metastudtite, [UO 2(2-O 2)(H 2O) 2], uranyl peroxide minerals that are major oxidative alteration phases of UO2 under conditions of geological storage, has been studied using X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy. XPS of the U 4f region shows small but significant differences between studtite and metastudtite, with the 4f binding energy of studtite the highest reported for a uranyl mineral studied by this technique. Further information on the changes in the electronic structure was elucidated using U M4-edge High Energy Resolution XANES (HR-XANES) spectroscopy, which directly probesmore » f-orbital states. The transition from the 3d to the 5f* orbital is sensitive to variations of the U=Oaxial bond length and to changes in the bond covalency. We report evidences that the covalence in the uranyl fragment decreases upon dehydration. Photoluminescence spectroscopy at near liquid helium temperatures reveals significant spectral differences between the two materials, correlating with the X-ray spectroscopy results. A theoretical investigation has been conducted on the structures of both studtite and metastudtite and benchmarked to the HR-XANES spectra. These illustrate the sensitivity of the 3d to the 5f * transition towards U=Oaxial bond variation.« less

Probing the interaction of Rh, Co and bimetallic Rh-Co nanoparticles with the CeO2 support: catalytic materials for alternative energy generation.

PubMed

Varga, E; Pusztai, P; Óvári, L; Oszkó, A; Erdőhelyi, A; Papp, C; Steinrück, H-P; Kónya, Z; Kiss, J

2015-10-28

The interaction of CeO2-supported Rh, Co and bimetallic Rh-Co nanoparticles, which are active catalysts in hydrogen production via steam reforming of ethanol, a process related to renewable energy generation, was studied by X-ray diffraction (XRD), high resolution electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and low energy ion scattering (LEIS). Furthermore, diffuse reflectance infrared spectroscopy (DRIFTS) of adsorbed CO as a probe molecule was used to characterize the morphology of metal particles. At small loadings (0.1%), Rh is in a much dispersed state on ceria, while at higher contents (1-5%), Rh forms 2-8 nm particles. Between 473-673 K pronounced oxygen transfer from ceria to Rh is observed and at 773 K significant agglomeration of Rh occurs. On reduced ceria, XPS indicates a possible electron transfer from Rh to ceria. The formation of smaller ceria crystallites upon loading with Co was concluded from XRD and HRTEM; for 10% Co, the CeO2 particle size decreased from 27.6 to 10.7 nm. A strong dissolution of Co into ceria and a certain extent of encapsulation by ceria were deduced by XRD, XPS and LEIS. In the bimetallic system, the presence of Rh enhances the reduction of cobalt and ceria. During thermal treatments, reoxidation of Co occurs, and Rh agglomeration as well as oxygen migration from ceria to Rh are hindered in the presence of cobalt.

Electronic structure and phase separation of superconducting and nonsuperconducting KxFe2-ySe2 revealed by x-ray photoemission spectroscopy

NASA Astrophysics Data System (ADS)

Oiwake, M.; Ootsuki, D.; Noji, T.; Hatakeda, T.; Koike, Y.; Horio, M.; Fujimori, A.; Saini, N. L.; Mizokawa, T.

2013-12-01

We have investigated the electronic structure of superconducting (SC) and nonsuperconducting (non-SC) KxFe2-ySe2 using x-ray photoemission spectroscopy (XPS). The spectral shape of the Fe 2p XPS is found to depend on the amount of Fe vacancies. The Fe 2p3/2 peak of the SC and non-SC Fe-rich samples is accompanied by a shoulder structure on the lower binding energy side, which can be attributed to the metallic phase embedded in the Fe2+ insulating phase. The absence of the shoulder structure in the non-SC Fe-poor sample allows us to analyze the Fe 2p spectra using a FeSe4 cluster model. The Fe 3d-Se 4p charge-transfer energy of the Fe2+ insulating phase is found to be ˜2.3 eV which is smaller than the Fe 3d-Fe 3d Coulomb interaction of ˜3.5 eV. This indicates that the Fe2+ insulating state is the charge-transfer type in the Zaanen-Sawatzky-Allen scheme. We also find a substantial change in the valence-band XPS as a function of Fe content and temperature. The metallic state at the Fermi level is seen in the SC and non-SC Fe-rich samples and tends to be enhanced with cooling in the SC sample.

MBE growth of few-layer 2H-MoTe2 on 3D substrates

NASA Astrophysics Data System (ADS)

Vishwanath, Suresh; Sundar, Aditya; Liu, Xinyu; Azcatl, Angelica; Lochocki, Edward; Woll, Arthur R.; Rouvimov, Sergei; Hwang, Wan Sik; Lu, Ning; Peng, Xin; Lien, Huai-Hsun; Weisenberger, John; McDonnell, Stephen; Kim, Moon J.; Dobrowolska, Margaret; Furdyna, Jacek K.; Shen, Kyle; Wallace, Robert M.; Jena, Debdeep; Xing, Huili Grace

2018-01-01

MoTe2 is the least explored material in the Molybdenum-chalcogen family. Molecular beam epitaxy (MBE) provides a unique opportunity to tackle the small electronegativity difference between Mo and Te while growing layer by layer away from thermodynamic equilibrium. We find that for a few-layer MoTe2 grown at a moderate rate of ∼6 min per monolayer, a narrow window in temperature (above Te cell temperature) and Te:Mo ratio exists, where we can obtain pure phase 2H-MoTe2. This is confirmed using reflection high-energy electron diffraction (RHEED), Raman spectroscopy and X-ray photoemission spectroscopy (XPS). For growth on CaF2, Grazing incidence X-ray diffraction (GI-XRD) reveals a grain size of ∼90 Å and presence of twinned grains. In this work, we hypothesis the presence of excess Te incorporation in MBE grown few layer 2H-MoTe2. For film on CaF2, it is based on >2 Te:Mo stoichiometry using XPS as well as 'a' and 'c' lattice spacing greater than bulk 2H-MoTe2. On GaAs, its based on observations of Te crystallite formation on film surface, 2 × 2 superstructure observed in RHEED and low energy electron diffraction, larger than bulk c-lattice spacing as well as the lack of electrical conductivity modulation by field effect. Finally, thermal stability and air sensitivity of MBE 2H-MoTe2 is investigated by temperature dependent XRD and XPS, respectively.

Occurrence of photoluminescence and onion like structures decorating graphene oxide with europium using sodium dodecyl sulfate surfactant

NASA Astrophysics Data System (ADS)

Cedeño, V. J.; Rangel, R.; Cervantes, J. L.; Lara, J.; Alvarado, J. J.; Galván, D. H.

2017-07-01

Graphene oxide decoration with europium was carried out using SDS (sodium dodecyl sulfate) as the surfactant. The reaction was performed in a microwave oven and subsequently underwent thermal treatment under hydrogen flow. The results found in the present work demonstrate that through the use of SDS surfactant aggregates of hemi-cylindrical and onion-like structures could be obtained; which propitiate an enhanced synergistic photoluminescence located at the red wavelength. On the other hand, after thermal treatment the aggregates disappear providing a good dispersion of europium, however a decrease in the photoluminescence signal is observed. The graphene oxide decorated with europium was characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Fourier infrared transform spectroscopy (FTIR), RAMAN spectroscopy, x-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) techniques, showing the characteristic features of graphene oxide and europium.

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.

CuInGaSe{sub 2} nanoparticles by pulsed laser ablation in liquid medium

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

Mendivil, M.I.; García, L.V.; Krishnan, B.

2015-12-15

Highlights: • CIGS nanocolloids were synthesized using PLAL technique. • Characterized their morphology, structure, composition and optical properties. • Morphologies were dependent on ablation wavelength and liquid medium. • Optical absorption and bandgap of these nanocolloids were tunable. - Abstract: Pulsed laser ablation in liquid medium (PLALM) is a nanofabrication technique to produce complex nanostructures. CuInGaSe{sub 2} (CIGS) is an alloy with applications in photovoltaic industry. In this work, we studied the effects of laser ablation wavelength, energy fluence and liquid medium on the properties of the CIGS nanoparticles synthesized by PLALM. The nanoparticles obtained were analyzed by transmission electronmore » microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), selected area electron diffraction (SAED), X-ray photoelectron spectroscopy (XPS) and UV–vis absorption spectroscopy. XPS results confirmed the chemical states and composition of the ablated products. TEM analysis showed different morphologies for the nanomaterials obtained in different liquid media and ablation wavelengths. The optical properties for these CIGS nanocolloids were analyzed using UV–vis absorption spectroscopy. The results demonstrated the use of PLALM as a useful synthesis technique for nanoparticles of quaternary photovoltaic materials.« less

Defect-driven interfacial electronic structures at an organic/metal-oxide semiconductor heterojunction.

PubMed

Winget, Paul; Schirra, Laura K; Cornil, David; Li, Hong; Coropceanu, Veaceslav; Ndione, Paul F; Sigdel, Ajaya K; Ginley, David S; Berry, Joseph J; Shim, Jaewon; Kim, Hyungchui; Kippelen, Bernard; Brédas, Jean-Luc; Monti, Oliver L A

2014-07-16

The electronic structure of the hybrid interface between ZnO and the prototypical organic semiconductor PTCDI is investigated via a combination of ultraviolet and X-ray photoelectron spectroscopy (UPS/XPS) and density functional theory (DFT) calculations. The interfacial electronic interactions lead to a large interface dipole due to substantial charge transfer from ZnO to 3,4,9,10-perylenetetracarboxylicdiimide (PTCDI), which can be properly described only when accounting for surface defects that confer ZnO its n-type properties. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Adsorption and electron-induced polymerization of methyl methacrylate on Ru(101xAF0)

NASA Astrophysics Data System (ADS)

Hedhili, M. N.; Yakshinskiy, B. V.; Wasielewski, R.; Ciszewski, A.; Madey, T. E.

2008-05-01

The adsorption and electron irradiation of methyl methacrylate (MMA) on a Ru(101¯0) surface have been studied using x-ray photoelectron spectroscopy (XPS), temperature programmed desorption (TPD), and low energy ion scattering. TPD analysis indicates that a monolayer of MMA chemisorbs and dissociates on the Ru(101¯0) surface. The reaction products observed upon heating include H2, CO, CO2, and a small amount of MMA. Physisorbed multilayers of MMA desorb at temperatures around 170K. Electron irradiation of physisorbed MMA at 140K leads to a modification of the MMA film: The XPS spectra show an increase in thermal stability of the film with retention of the MMA structure, and indicate that electron irradiation induces polymerization. An increase in the electron bombardment fluence induces a degradation of the formed polymerized species and leads to the accumulation of carbon on the Ru surface. These results are relevant to the accumulation of carbon on surfaces of Ru films that serve as capping layers on Mo /Si multilayer mirrors used in extreme ultraviolet lithography.

Influence of square wave anodization on the electronic properties and structures of the passive films on Ti in sulfuric acid solution

NASA Astrophysics Data System (ADS)

Long, Y.; Li, D. G.; Chen, D. R.

2017-12-01

Two types of square wave anodization (type 1 and type 2) were employed in this work to form a passive film on Ti in a 0.5 M H2SO4 solution. The influences of the anodization potential and duration on the electronic properties and structures of the passive films were studied by Mott-Schottky plots, auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). The results showed that the donor density, ND, of the passive film decreased and the flat band potential, EFB, shifted to the positive direction with the increase of the anodization duration and high anodization potential irrespective of whether type 1 or type 2 was used. Moreover, the passive film that formed on Ti using type 1 had a lower donor density and a more positive flat band potential than that on Ti using type 2 at one fixed anodization duration (only exchanging the anodization order of 1 V and the high potential). XPS analysis revealed that the outmost passive film was only composed of TiO2, the inner passive film was mainly composed of TiO2 with some amount of TiO and Ti2O3, and the TiO2 concentration in the outermost passive film increased with the increase of the anodization duration and the high potential in the case of using type 1 or type 2, implying an increased degree of crystallinity. The AES results showed that the O/Ti atomic ratio of the passive film obviously increased with the increasing anodization duration and high potential, demonstrating the increased homogeneous characteristic of the passive film; this was in agreement with the Mott-Schottky and XPS results.

Electronic structure study of wide band gap magnetic semiconductor (La{sub 0.6}Pr{sub 0.4}){sub 0.65}Ca{sub 0.35}MnO{sub 3} nanocrystals in paramagnetic and ferromagnetic phases

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

Dwivedi, G. D.; Chou, H.; Yang, K. S.

2016-04-25

X-ray circular magnetic dichroism (XMCD), X-ray photoemission spectroscopy (XPS), and ultraviolet photoemission spectroscopy (UPS) techniques were used to study the electronic structure of nanocrystalline (La{sub 0.6}Pr{sub 0.4}){sub 0.65}Ca{sub 0.35}MnO{sub 3} near Fermi-level. XMCD results indicate that Mn{sup 3+} and Mn{sup 4+} spins are aligned parallel to each other at 20 K. The low M-H hysteresis curve measured at 5 K confirms ferromagnetic ordering in the (La{sub 0.6}Pr{sub 0.4}){sub 0.65}Ca{sub 0.35}MnO{sub 3} system. The low temperature valence band XPS indicates that coupling between Mn3d and O2p is enhanced and the electronic states near Fermi-level have been suppressed below T{sub C}. The valence bandmore » UPS also confirms the suppression of electronic states near Fermi-level below Curie temperature. UPS near Fermi-edge shows that the electronic states are almost absent below 0.5 eV (at 300 K) and 1 eV (at 115 K). This absence clearly demonstrates the existence of a wide band-gap in the system since, for hole-doped semiconductors, the Fermi-level resides just above the valence band maximum.« less

Polyphenylsilole multilayers--an insight from X-ray electron spectroscopy and density functional theory.

PubMed

Diller, Katharina; Ma, Yong; Luo, Yi; Allegretti, Francesco; Liu, Jianzhao; Tang, Ben Zhong; Lin, Nian; Barth, Johannes V; Klappenberger, Florian

2015-12-14

We present a combined investigation by means of X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine-structure (NEXAFS) spectroscopy of condensed multilayers of two polyphenylsiloles, namely hexaphenylsilole (HPS) and tetraphenylsilole (TPS). Both compounds exhibit very similar spectroscopic signatures, whose interpretation is aided by density functional theory (DFT) calculations. High-resolution XPS spectra of the Si 2p and C 1s core levels of these multilayers indicate a positively charged silicon ion flanked by two negatively charged adjacent carbon atoms in the silole core of both molecules. This result is corroborated quantitatively by DFT calculations on isolated HPS (TPS) molecules, which show a natural bond orbital partial charge of +1.67 e (+1.58 e) on the silicon and -0.34 e (-0.58 e) on the two neighbouring carbon atoms in the silole ring. These charges are conserved in direct contact with a Cu(111) substrate for films of submonolayer coverage, as evidenced by the Si 2p XPS data. The C K-edge NEXAFS spectra of HPS and TPS multilayers exhibit distinct and differing features. Their main characteristics reappear in the simulated spectra and are assigned to the different inequivalent carbon species in the molecule. The angle-dependent measurements hardly reveal any dichroism, i.e., the molecular π-systems are not uniformly oriented parallel or perpendicular with respect to the surface. Changes in the growth conditions of TPS, i.e., a reduction of the substrate temperature from 240 K to 80 K during deposition, lead to a broadening of both XPS and NEXAFS signatures, as well as an upward shift of the Si 2p and C 1s binding energies, indicative of a less ordered growth mode at low temperature.

Nanoparticle formation of deposited Agn-clusters on free-standing graphene

NASA Astrophysics Data System (ADS)

Al-Hada, M.; Peters, S.; Gregoratti, L.; Amati, M.; Sezen, H.; Parisse, P.; Selve, S.; Niermann, T.; Berger, D.; Neeb, M.; Eberhardt, W.

2017-11-01

Size-selected Agn-clusters on unsupported graphene of a commercial Quantifoil sample have been investigated by surface and element-specific techniques such as transmission electron microscopy (TEM), spatially-resolved inner-shell X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). An agglomeration of the highly mobile clusters into nm-sized Ag-nanodots of 2-3 nm is observed. Moreover, crystalline as well as non-periodic fivefold symmetric structures of the Ag-nanoparticles are evident by high-resolution TEM. Using a lognormal size-distribution as revealed by TEM, the measured positive binding energy shift of the air-exposed Ag-nanodots can be explained by the size-dependent dynamical liquid-drop model.

Characterization of tetraethylene glycol passivated iron nanoparticles

NASA Astrophysics Data System (ADS)

Nunes, Eloiza da Silva; Viali, Wesley Renato; da Silva, Sebastião William; Coaquira, José Antonio Huamaní; Garg, Vijayendra Kumar; de Oliveira, Aderbal Carlos; Morais, Paulo César; Jafelicci Júnior, Miguel

2014-10-01

The present study describes the synthesis and characterization of iron@iron oxide nanoparticles produced by passivation of metallic iron in tetraethylene glycol media. Structural and chemical characterizations were performed using transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Mössbauer spectroscopy. Pomegranate-like core@shell nanoparticulate material in the size range of 90-120 nm was obtained. According to quantitative phase analysis using Rietveld structure refinement the synthesized iron oxide was identified as magnetite (Fe3O4) whereas the iron to magnetite mass fractions was found to be 47:53. These findings are in good agreement with the data obtained from Mössbauer and thermal gravimetric analysis (TGA). The XPS data revealed the presence of a surface organic layer with higher hydrocarbon content, possibly due to the tetraethylene glycol thermal degradation correlated with iron oxidation. The room-temperature (300 K) saturation magnetization measured for the as-synthesized iron and for the iron-iron oxide were 145 emu g-1 and 131 emu g-1, respectively. The measured saturation magnetizations are in good agreement with data obtained from TEM, XRD and Mössbauer spectroscopy.

Structural, magnetic, dielectric, and electrical properties of NiFe2O4 spinel ferrite nanoparticles prepared by honey-mediated sol-gel combustion

NASA Astrophysics Data System (ADS)

Yadav, Raghvendra Singh; Kuřitka, Ivo; Vilcakova, Jarmila; Havlica, Jaromir; Masilko, Jiri; Kalina, Lukas; Tkacz, Jakub; Enev, Vojtěch; Hajdúchová, Miroslava

2017-08-01

In this study, NiFe2O4 nanoparticles were synthesized using a honey-mediated sol-gel combustion method. The synthesized nanoparticles and samples annealed at 800 °C and 1100 °C were characterized by X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and vibrating sample magnetometry (VSM). XRD and Raman spectroscopy confirmed the formation of a cubic spinel ferrite structure. FE-SEM demonstrated the octahedral morphology of the NiFe2O4 spinel ferrite nanoparticles with sizes ranging from 10 to 70 nm. Quantitative analysis based on XPS suggested a mixed spinel structure comprising NiFe2O4 nanoparticles. XPS analysis determined occupation formulae of (Ni0.212+ Fe0.443+)[Ni0.792+ Fe1.563+]O4 and (Ni0.232+ Fe0.503+)[Ni0.772+ Fe1.503+]O4, for the as-prepared NiFe2O4 nanoparticles and those annealed at 1100 °C, respectively. Magnetic measurements showed that the saturation magnetization increased with the crystallite size from 32.3 emu/g (20 nm) to 49.9 emu/g (163 nm), whereas the coercivity decreased with the crystallite size from 162 Oe (20 nm) to 47 Oe (163 nm). Furthermore, the dielectric constant, dielectric loss tangent, and AC conductivity of the NiFe2O4 nanoparticles were dependent on the frequency (1-107 Hz) and grain size. The influence of the grain size was also observed by modulus spectroscopy based on the Cole-Cole plot.

Novel Electrochemical Process for Treatment of Perchlorate in Waste Water

DTIC Science & Technology

2011-03-06

Prepared in Different Processes: (b) in 0.1 M Pyrrole Solution with 0.1 M NaCl at 0.8 V for 20 min; (c) at 0.5 V for 400 s in 0.1 M ClO4- Solution and...polypyrrole Py pyrrole SEM scanning electron microscopy SON statement of need XPS X-ray photoelectron spectroscopy v Acknowledgments This work is...shows the scanning electron microscopy (SEM) images of carbon fiber paper and a CNT array grown on carbon fiber paper. Pyrrole (Py) deposition

Mg-doped ZnO nanoparticles for efficient sunlight-driven photocatalysis.

PubMed

Etacheri, Vinodkumar; Roshan, Roshith; Kumar, Vishwanathan

2012-05-01

Magnesium-doped ZnO (ZMO) nanoparticles were synthesized through an oxalate coprecipitation method. Crystallization of ZMO upon thermal decomposition of the oxalate precursors was investigated using differential scanning calorimetry (DSC) and X-ray diffraction (XRD) techniques. XRD studies point toward a significant c-axis compression and reduced crystallite sizes for ZMO samples in contrast to undoped ZnO, which was further confirmed by HRSEM studies. X-ray photoelectron spectroscopy (XPS), UV/vis spectroscopy and photoluminescence (PL) spectroscopy were employed to establish the electronic and optical properties of these nanoparticles. (XPS) studies confirmed the substitution of Zn(2+) by Mg(2+), crystallization of MgO secondary phase, and increased Zn-O bond strengths in Mg-doped ZnO samples. Textural properties of these ZMO samples obtained at various calcination temperatures were superior in comparison to the undoped ZnO. In addition to this, ZMO samples exhibited a blue-shift in the near band edge photoluminescence (PL) emission, decrease of PL intensities and superior sunlight-induced photocatalytic decomposition of methylene blue in contrast to undoped ZnO. The most active photocatalyst 0.1-MgZnO obtained after calcination at 600 °C showed a 2-fold increase in photocatalytic activity compared to the undoped ZnO. Band gap widening, superior textural properties and efficient electron-hole separation were identified as the factors responsible for the enhanced sunlight-driven photocatalytic activities of Mg-doped ZnO nanoparticles.

Theoretical and experimental studies on wide-band-gap p-type conductive BaCuSeF and related compounds

NASA Astrophysics Data System (ADS)

Sakakima, Hiroshi; Nishitani, Mikihiko; Yamamoto, Koichi; Wada, Takahiro

2015-08-01

BaCuSeF and related compounds, MCuQF (M = Ba, Sr; Q = Se, S), are known to show p-type conduction. The formation energies of the Cu vacancy ΔH[VCu] in a MCuQF system were computed by first-principles calculation with a generalized gradient approximation (GGA) of the Perdew-Burke-Ernzerhof (PBE) functional as an electron exchange and correlation functional. The density of states (DOS) of BaCuSeF was calculated with the hybrid functional of Heyd-Scuseria-Ernzerhof (HSE) 06. ΔH[VCu] was found to be very small under both the Cu- and Q-rich conditions, which probably contributes to p-type conduction. The electronic structure of BaCuSeF was studied by X-ray photoelectron spectroscopy (XPS) with UV photoelectron yield spectroscopy (UVPYS) and photoemission yield spectroscopy (PYS). The determined depth of the top of the valence band relative to the vacuum level was about 4.9 eV. This value is desirable for applications in compound semiconductor thin-film tandem solar cells since the absorbers of polycrystalline thin-film solar cells, such as CdTe and Cu(In,Ga)Se2, are p-type semiconductors. The DOS of BaCuSeF calculated with the HSE06 functional was almost consistent with the XPS spectrum.

Magnesium oxide grafted carbon nanotubes based impedimetric genosensor for biomedical application.

PubMed

Patel, Manoj Kumar; Ali, Md Azahar; Srivastava, Saurabh; Agrawal, Ved Varun; Ansari, S G; Malhotra, Bansi D

2013-12-15

Nanostructured magnesium oxide (size<10nm) grafted carboxyl (COOH) functionalized multi-walled carbon nanotubes (nMgO-cMWCNTs) deposited electrophoretically onto indium tin oxide (ITO) coated glass electrode and have been utilized for Vibrio cholerae detection. Aminated 23 bases single stranded DNA (NH2-ssDNA) probe sequence (O1 gene) of V. cholerae has been covalently functionalized onto nMgO-cMWCNTs/ITO electrode surface using EDC-NHS chemistry. This DNA functionalized MgO grafted cMWCNTs electrode has been characterized using X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electrochemical techniques. The results of XPS studies reveal that sufficient O-C=O groups present at the nMgO-cMWCNTs surface are utilized for DNA binding. The results of hybridization studies conducted with fragmented target DNA (ftDNA) of V. cholerae using electrochemical impedance spectroscopy (EIS) reveal sensitivity as 3.87 Ω ng(-1) cm(-2), detection limit of ~21.70 ng µL(-1) in the linear range of 100-500 ng µL(-1) and stability of about 120 days. The proposed DNA functionalized nMgO-cMWCNTs nanomatrix provides a novel impedimetric platform for the fabrication of a compact genosensor device for biomedical application. © 2013 Elsevier B.V. All rights reserved.

Adequacy of surface analytical tools for studying the tribology of ceramics

NASA Technical Reports Server (NTRS)

Sliney, H. E.

1986-01-01

Surface analytical tools are very beneficial in tribological studies of ceramics. Traditional methods of optical microscopy, XRD, XRF, and SEM should be combined with newer surface sensitive techniques especially AES and XPS. ISS and SIMS can also be useful in providing additional compositon details. Tunneling microscopy and electron energy loss spectroscopy are less known techniques that may also prove useful.

Synthesis of SiO(x) powder using DC arc plasma.

PubMed

Jung, Chan-Ok; Park, Dong-Wha

2013-02-01

SiO(x) was prepared by DC arc plasma and applied to the anode material of lithium ion batteries. A pellet of a mixture of Si and SiO2 was used as the raw material. The ratios of the silicon and silicon dioxide (SiO2) mixtures were varied by controlling the Si-SiO2 molar ratio (Si-SiO2 = 1-4). Hydrogen gas was used as the reduction atmosphere in the chamber. The prepared SiO(x) was collected on the chamber wall. The obtained SiO(x) was characterized by X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). XRD and TEM showed that the phase composition of the prepared particles was composed of amorphous SiO(x) and crystalline Si. The prepared SiO(x) showed wire and spherical morphology. XPS indicated the bonding state and 'x' value of the prepared SiO(x), which was close to one. The result of prepared SiO(x) is discussed from thermodynamic equilibrium calculations. The electrochemical behavior of the silicon monoxide anode was investigated.

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

Unuigbe, David M.; Harting, Margit; Jonah, Emmanuel O.

The presence of native oxide on the surface of silicon nanoparticles is known to inhibit charge transport on the surfaces. Scanning electron microscopy (SEM) studies reveal that the particles in the printed silicon network have a wide range of sizes and shapes. High-resolution transmission electron microscopy reveals that the particle surfaces have mainly the (111)- and (100)-oriented planes which stabilizes against further oxidation of the particles. X-ray absorption spectroscopy (XANES) and X-ray photoelectron spectroscopy (XPS) measurements at the O 1s-edge have been utilized to study the oxidation and local atomic structure of printed layers of silicon nanoparticles which were milledmore » for different times. XANES results reveal the presence of the +4 (SiO 2) oxidation state which tends towards the +2 (SiO) state for higher milling times. Si 2pXPS results indicate that the surfaces of the silicon nanoparticles in the printed layers are only partially oxidized and that all three sub-oxide, +1 (Si 2O), +2 (SiO) and +3 (Si 2O 3), states are present. The analysis of the change in the sub-oxide peaks of the silicon nanoparticles shows the dominance of the +4 state only for lower milling times.« less

Microbial reduction of uranium (VI) by Bacillus sp. dwc-2: A macroscopic and spectroscopic study.

PubMed

Li, Xiaolong; Ding, Congcong; Liao, Jiali; Du, Liang; Sun, Qun; Yang, Jijun; Yang, Yuanyou; Zhang, Dong; Tang, Jun; Liu, Ning

2017-03-01

The microbial reduction of U(VI) by Bacillus sp. dwc-2, isolated from soil in Southwest China, was explored using transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray absorption near edge spectroscopy (XANES). Our studies indicated that approximately 16.0% of U(VI) at an initial concentration of 100mg/L uranium nitrate could be reduced by Bacillus sp. dwc-2 at pH8.2 under anaerobic conditions at room temperature. Additionally, natural organic matter (NOM) played an important role in enhancing the bioreduction of U(VI) by Bacillus sp. dwc-2. XPS results demonstrated that the uranium presented mixed valence states (U(VI) and U(IV)) after bioreduction, which was subsequently confirmed by XANES. Furthermore, the TEM and high resolution transmission electron microscopy (HRTEM) analysis suggested that the reduced uranium was bioaccumulated mainly within the cell and as a crystalline structure on the cell wall. These observations implied that the reduction of uranium may have a significant effect on its fate in the soil environment in which these bacterial strains occur. Copyright © 2016. Published by Elsevier B.V.

Effect of Cr doping on the structural, morphological, optical and electrical properties of indium tin oxide films

NASA Astrophysics Data System (ADS)

Mirzaee, Majid; Dolati, Abolghasem

2015-03-01

We report on the preparation and characterization of high-purity chromium (0.5-2.5 at.%)-doped indium tin oxide (ITO, In:Sn = 90:10) films deposited by sol-gel-mediated dip coating. The effects of different Cr-doping contents on structural, morphological, optical and electrical properties of the films were characterized by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV-Vis spectroscopy and four-point probe methods. XRD showed high phase purity cubic In2O3 and indicated a contraction of the lattice with Cr doping. FESEM micrographs show that grain size decreased with increasing the Cr-doping content. A method to determine chromium species in the sample was developed through the decomposition of the Cr 2 p XPS spectrum in Cr6+ and Cr3+ standard spectra. Optical and electrical studies revealed that optimum opto-electronic properties, including minimum sheet resistance of 4,300 Ω/Sq and an average optical transmittance of 85 % in the visible region with a band gap of 3.421 eV, were achieved for the films doped with Cr-doping content of 2 at.%.

Incommensurate growth of Co thin film on close-packed Ag(111) surface

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

Barman, Sukanta, E-mail: sukanta.ac@gmail.com; Menon, Krishna Kumar S. R., E-mail: krishna.menon@saha.ac.in

2016-05-06

Growth of ultrathin Co layers on close-packed Ag(111)were investigated by means of Low Energy Electron Diffraction (LEED), X-ray Photoelectron Spectroscopy (XPS) and Angle-resolved Photoemission Spectroscopy(ARPES) techniques. The close-packed hexagonal face of Co(0001), exhibits a lattice misfit about 13% with Ag(111) surface which manipulates the growth to be incommensurate up to a certain thickness. The strain field causes aperiodic height undulation in the sub-angstrom regime of the film which was confirmed by p(1 × 1) LEED pattern along with a 6-fold moiré reconstruction pattern in the lower film thickness (up to ∼2ML). The evolution of the LEED pattern was studied withmore » increasing film coverage. Lattice strain was measured with respect to the relative positions of these double spots as a functionof film thickness. Almost a constant strain (∼13%) in the full range of film thickness explains the moiré pattern formation in order to stabilize the incommensurate growth. For higher film coverages, an epitaxial well-ordered commensurate growth was observed. Core level and valance band electronic structures of these films were studied by XPS and ARPES techniques.« less

Reduced graphene oxide-induced recrystallization of NiS nanorods to nanosheets and the improved Na-storage properties.

PubMed

Pan, Qin; Xie, Jian; Zhu, Tiejun; Cao, Gaoshao; Zhao, Xinbing; Zhang, Shichao

2014-04-07

Preparation of two-dimensional (2D) graphene-like materials is currently an emerging field in materials science since the discovery of single-atom-thick graphene prepared by mechanical cleavage. In this work, we proposed a new method to prepare 2D NiS, where reduced graphene oxide (rGO) was found to induce the recrystallization of NiS from nanorods to nanosheets in a hydrothermal process. The process and mechanism of recrystallization have been clarified by various characterization techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) mapping, and X-ray photoelectron spectroscopy (XPS). The characterization of ex situ NiS/rGO products by SEM and EDS mapping indicates that the recrystallization of NiS from nanorods to nanosheets is realized actually through an exfoliation process, while the characterization of in situ NiS/rGO products by SEM, TEM, and EDS mapping reveals the exfoliation process. The XPS result demonstrates that hydrothermally assisted chemical bonding occurs between NiS and rGO, which induces the exfoliation of NiS nanorods into nanosheets. The obtained NiS/rGO composite shows promising Na-storage properties.

Plasma-enhanced preparation of graphene composites with polyaniline and polypyrrole

NASA Astrophysics Data System (ADS)

Uygun Oksuz, Aysegul; Cogal, Sadik; Celik Cogal, Gamze; Uygun, Emre; Oksuz, Lutfi

2016-10-01

This study presents the preparation of graphene (GR) nanocomposites with polyaniline (PANI) and polypyrrole (PPy) through the fast, versatile and environmentally friendly process of radiofrequency (RF) -plasma polymerization. Morphological characterization of nanocomposites was performed using scanning electron microscopy (SEM) and showed that the PANI and PPy conducting polymers coated the GR surface. The surface properties of the GR nanocomposites were determined using Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) analysis. This work has been supported by Tubitak with 114M867 project number.

Direct characterization of the energy level alignments and molecular components in an organic hetero-junction by integrated photoemission spectroscopy and reflection electron energy loss spectroscopy analysis.

PubMed

Yun, Dong-Jin; Shin, Weon-Ho; Bulliard, Xavier; Park, Jong Hwan; Kim, Seyun; Chung, Jae Gwan; Kim, Yongsu; Heo, Sung; Kim, Seong Heon

2016-08-26

A novel, direct method for the characterization of the energy level alignments at bulk-heterojunction (BHJ)/electrode interfaces on the basis of electronic spectroscopy measurements is proposed. The home-made in situ photoemission system is used to perform x-ray/ultraviolet photoemission spectroscopy (XPS/UPS), reflection electron energy loss spectroscopy (REELS) and inverse photoemission spectroscopy of organic-semiconductors (OSCs) deposited onto a Au substrate. Through this analysis system, we are able to obtain the electronic structures of a boron subphthalocyanine chloride:fullerene (SubPC:C60) BHJ and those of the separate OSC/electrode structures (SubPC/Au and C60/Au). Morphology and chemical composition analyses confirm that the original SubPC and C60 electronic structures remain unchanged in the electrodes prepared. Using this technique, we ascertain that the position and area of the nearest peak to the Fermi energy (EF = 0 eV) in the UPS (REELS) spectra of SubPC:C60 BHJ provide information on the highest occupied molecular orbital level (optical band gap) and combination ratio of the materials, respectively. Thus, extracting the adjusted spectrum from the corresponding SubPC:C60 BHJ UPS (REELS) spectrum reveals its electronic structure, equivalent to that of the C60 materials. This novel analytical approach allows complete energy-level determination for each combination ratio by separating its electronic structure information from the BHJ spectrum.

Hydrothermal-reduction synthesis of manganese oxide nanomaterials for electrochemical supercapacitors.

PubMed

Zhang, Xiong; Chen, Yao; Yu, Peng; Ma, Yanwei

2010-11-01

In the present work, amorphous manganese oxide nanomaterials have been synthesized by a common hydrothermal method based on the redox reaction between MnO4(-) and Fe(2+) under an acidic condition. The synthesized MnO2 samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electrochemical studies. XRD results showed that amorphous manganese oxide phase was obtained. XPS quantitative analysis revealed that the atomic ratio of Mn to Fe was 3.5 in the MnO2 samples. TEM images showed the porous structure of the samples. Electrochemical properties of the MnO2 electrodes were studied using cyclic voltammetry and galvanostatic charge-discharge cycling in 1 M Na2SO4 aqueous electrolyte, which showed excellent pseudocapacitance properties. A specific capacitance of 192 Fg(-1) at a current density of 0.5 Ag(-1) was obtained at the potential window from -0.1 to 0.9 V (vs. SCE).

Nanostructure CdS/ZnO heterojunction configuration for photocatalytic degradation of Methylene blue

NASA Astrophysics Data System (ADS)

Velanganni, S.; Pravinraj, S.; Immanuel, P.; Thiruneelakandan, R.

2018-04-01

In the present manuscript, thin films of Zinc Oxide (ZnO) have been deposited on a FTO substrate using a simple successive ionic layer adsorption and reaction (SILAR) and chemical bath deposition (CBD) method. Cadmium Sulphide (CdS) nanoparticles are sensitized over ZnO thin films using SILAR method. The synthesized nanostructured CdS/ZnO heterojunction thin films was characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), High resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS), UV-Vis spectroscopy and Raman spectroscopy techniques. The band gap of CdS nanoparticles over ZnO nanostructure was found to be about 3.20 eV. The photocatalytic activities of the deposited CdS/ZnO thin films were evaluated by the degradation of methylene blue (MB) in an aqueous solution under sun light irradiation.

Total photoelectron yield spectroscopy of energy distribution of electronic states density at GaN surface and SiO2/GaN interface

NASA Astrophysics Data System (ADS)

Ohta, Akio; Truyen, Nguyen Xuan; Fujimura, Nobuyuki; Ikeda, Mitsuhisa; Makihara, Katsunori; Miyazaki, Seiichi

2018-06-01

The energy distribution of the electronic state density of wet-cleaned epitaxial GaN surfaces and SiO2/GaN structures has been studied by total photoelectron yield spectroscopy (PYS). By X-ray photoelectron spectroscopy (XPS) analysis, the energy band diagram for a wet-cleaned epitaxial GaN surface such as the energy level of the valence band top and electron affinity has been determined to obtain a better understanding of the measured PYS signals. The electronic state density of GaN surface with different carrier concentrations in the energy region corresponding to the GaN bandgap has been evaluated. Also, the interface defect state density of SiO2/GaN structures was also estimated by not only PYS analysis but also capacitance–voltage (C–V) characteristics. We have demonstrated that PYS analysis enables the evaluation of defect state density filled with electrons at the SiO2/GaN interface in the energy region corresponding to the GaN midgap, which is difficult to estimate by C–V measurement of MOS capacitors.

Calculation of density of states of transition metals: From bulk sample to nanocluster

NASA Astrophysics Data System (ADS)

Krasavin, Andrey V.; Borisyuk, Petr V.; Vasiliev, Oleg S.; Zhumagulov, Yaroslav V.; Kashurnikov, Vladimir A.; Kurelchuk, Uliana N.; Lebedinskii, Yuriy Yu.

2018-03-01

A technique is presented of restoring the electronic density of states of the valence band from data of X-ray photoelectron spectroscopy (XPS). The originality of the technique consists in using a stochastic procedure to solve an integral equation relating the density of states and the experimental X-ray photoelectron spectra via the broadening function. To obtain the broadening function, only the XPS spectra of the core levels are needed. The results are presented for bulk sample of gold and tungsten and nanoclusters of tantalum; the possibility of using the results to determine the density of states of low-dimensional structures, including ensembles of metal nanoclusters, is demonstrated.

Synthesis, structural and optical properties of ZnO spindle/reduced graphene oxide composites with enhanced photocatalytic activity under visible light irradiation

NASA Astrophysics Data System (ADS)

Prabhu, S.; Pudukudy, M.; Sohila, S.; Harish, S.; Navaneethan, M.; Navaneethan, D.; Ramesh, R.; Hayakawa, Y.

2018-05-01

In the present work, spindle-shaped ZnO and reduced graphene oxide sheets were successfully synthesized by a hydrothermal method and then ZnO/r-GO composite was prepared by a direct solution mixing method. Various characterization results confirmed the interior and surface decoration of spindle-shaped ZnO on the reduced graphene oxide sheets. The phase formation, crystalline structure, morphology, surface states and optical properties were characterized using Powder X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Fourier Transform Infrared Spectroscopy (FTIR) and UV-Vis spectroscopy. The X-ray diffraction analysis showed the formation of the hexagonal wurtzite crystalline structure of ZnO with high crystalline quality. The band gap of the ZnO/r-GO composite was found to be low (3.03eV) compared to the band gap of spindle shaped ZnO (3.13 eV), as calculated from optical studies. The spindle-like morphology of the single crystalline ZnO was clearly shown in the electron microscopic images. The chemical bonding and surface states of the samples were studied using XPS measurement. Moreover, a possible growth mechanism for the ZnO spindle was proposed. The catalytic activity of the as-synthesized samples was evaluated for the photodegradation of methylene blue under visible light irradiation. Among the synthesized samples, the ZnO/r-GO composite showed higher degradation efficiency of 93% and successfully reused for four consecutive run without any activity loss.

Effects of M=Si, Ga and Al for Co substitution on the electronic properties of RCo4M as probed by XPS

NASA Astrophysics Data System (ADS)

Laslo, A.; Dudric, R.; Neumann, M.; Isnard, O.; Coldea, M.; Pop, V.

2014-12-01

The electronic properties of RCo5-xMx (R=Er, Sm, Tm; M=Si, Ga, Al; x=0 and 1) compounds were investigated by X-ray photoelectron spectroscopy (XPS). The study was focused on the Co 3s exchange splitting, the valence bands and chemical shifts of the elements from the analyzed compounds. The Co 2p3/2 core-level chemical shifts were described by means of the Auger parameters and Wagner plot. The hybridization between the R 5d6s and M 3sp and 4sp states and Co 3d states leads to a partial filling of the Co 3d band and to a decrease of the Co magnetic moments in comparison with the value in pure Co metal, in good agreement with the magnetic measurements.

Acetate- and thiol-capped monodisperse ruthenium nanoparticles: XPS, XAS, and HRTEM studies.

PubMed

Chakroune, Nassira; Viau, Guillaume; Ammar, Souad; Poul, Laurence; Veautier, Delphine; Chehimi, Mohamed M; Mangeney, Claire; Villain, Françoise; Fiévet, Fernand

2005-07-19

Monodisperse ruthenium nanoparticles were prepared by reduction of RuCl3 in 1,2-propanediol. The mean particle size was controlled by appropriate choice of the reduction temperature and the acetate ion concentration. Colloidal solutions in toluene were obtained by coating the metal particles with dodecanethiol. High-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and X-ray absorption spectroscopy (XANES and EXAFS for the Ru K-absorption edge) were performed on particles of two different diameters, 2 and 4 nm, and in different environments, polyol/acetate or thiol. For particles stored in polyol/acetate XPS studies revealed superficial oxidation limited to one monolayer and a surface coating containing mostly acetate ions. Analysis of the EXAFS spectra showed both oxygen and ruthenium atoms around the ruthenium atoms with a Ru-Ru coordination number N smaller than the bulk value, as expected for fine particles. In the case of 2 nm acetate-capped particles N is consistent with particles made up of a metallic core and an oxidized monolayer. For 2 nm thiol-coated particles, a Ru-S bond was evidenced by XPS and XAS. For the 4 nm particles XANES and XPS studies showed that most of the ruthenium atoms are in the zerovalent state. Nevertheless, in both cases, when capped with thiol, the Ru-Ru coordination number inferred from EXAFS is much smaller than for particles of the same size stored in polyol. This is attributed to a structural disorganization of the particles by thiol chemisorption. HRTEM studies confirm the marked dependence of the structural properties of the ruthenium particles on their chemical environment; they show the acetate-coated particles to be single crystals, whereas the thiol-coated particles appear to be polycrystalline.

Ligand exchange synthesis of organometallic Rh nanoparticles and application in explosive sensing

NASA Astrophysics Data System (ADS)

Srivastav, Amit K.; Agrawal, Bhavesh; Swami, Bhavya; Agrawal, Yadvendra K.; Maity, Prasenjit

2017-06-01

Alkyne {phenyl acetylene (PA) and 9-ethynylphenanthrene (EPT)}-ligated Rh nanoparticles ( 1 and 2, respectively) with mean diameter of 1.5 ± 0.2 nm were synthesized via a facile and high-yield biphasic ligand exchange protocol using similar sized ethylene glycol (EG)-stabilized Rh nanoparticles as precursors (EG:Rh). The synthesized organometallic Rh nanoparticles were convincingly characterized using several spectroscopic and microscopic techniques, e.g., Fourier transform infrared spectroscopy (FTIR), proton nuclear magnetic resonance (1H NMR), optical absorption spectroscopy (UV-Vis), photoluminescence spectroscopy (PL), powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscope (TEM). We propose that the syntheses mechanism relies on catalytic acetylenic (≡C-H, carbon-hydrogen) bond breaking by EG:Rh followed by strong metal-carbon bond formation with a vinyldiene (>C═C═M) motif. The obtained 1 and 2 showed luminescence property, which arises from ligand structure through intraparticle conjugation. Electron-rich phenanthrene-ligated Rh nanoparticles ( 2) showed good sensing performance for detection of electron deficient nitro-aromatic explosive molecules (NA) in solution phase through luminescence quenching method.

Microscopic and Metallurgical Aspects of the Space Shuttle Columbia Accident Investigation and Reconstruction

NASA Technical Reports Server (NTRS)

McDaniels, Steven J.

2004-01-01

The Space Shuttle Columbia was descending for a landing at the Kennedy Space Center (KSC) on February 1, 2003. Approximately 20 minutes prior to touchdown, the Columbia began disintegrating over the western United States; the majority of debris eventually impacted in eastern Texas and western Louisiana. A monumental effort eventually recovered approximately 84,000 pieces of debris, approximately 38% of the Orbiter's original dry weight. The debris was transported to KSC, where the items were catalogued and evaluated. Critical areas of interest, such as the left and right leading edge surfaces and the underside of the ship, were placed upon a grid to aid in the reconstruction. Items of interest included metallic structures, reinforced carbon-carbon composites, and ceramic heat insulation tiles. Many of the leading edge elements had re-solidified metallic deposits spattered on them. These deposits became known as slag and were one of the main focuses of the investigation. In order to help determine the sequence of events inside the left wing during the accident, the slag's composition, layering order, and directionality of deposition were studied. A myriad of analytical tests were performed in an attempt to ascertain the compositional and depositional characteristics of selected slag deposits, including the ordering of deposited layers within each individual slag deposit harvested. Initially, Scanning Electron Microscopy and Energy Dispersive X-Ray Spectroscopy (SEM/EDX) were performed to quickly characterize the overall composition of individual slag deposits: SEM utilizes a narrowlyfocused high-energy electron beam impinging upon a specimen. The incident beam excites and liberates lower energy secondary electrons, which are detected and analyzed, providing a visual representation of the sample's surface topography. EDX also relies on an incident electron beam, except an EDX unit measures X-ray energies generated by the impinging beam. Each element generates a unique X-ray signature; the EDX detector measures these discreet energies. EDX actually penetrates approximately 2 microns into the bulk of the sample. However, random examination of various portions of slag, coupled with the semiquantitative nature of the SEM/EDX analysis, did not yield convincingly pertinent data. Therefore, X-ray dot mapping was conducted, which provided more understandable data, both in terms of slag layering and composition. An X-ray dot map is generated by performing numerous EDX scans for individual elements, then compiling the scans in a visual representation. Eventually, specimens consisting of not only the slag, but of the adjacent RCC substrate as well were cross-sectioned. X-Ray dot mapping of the materialographicallymounted and -polished cross- sections provided a visual representation of both the layering sequence and compositional characteristics of the slag. Contemporaneously, Electron Spectroscopy for Chemical Analysis/X-Ray Photoelectron Spectroscopy (ESCA/XPS) and powdered X-Ray Diffraction (XRD) were performed to further characterize the deposits and to attempt to identify what, if any, compounds were present. The ESCA/XPS analysis allowed the analyst to "sputter" into the sample with an electron gun, aiding in the identification of the layering sequence. XPS uses photons, rather than electrons, which impinge upon the surface of the sample. XPS measures the electrons emitted from within the first 5 nm of the sample's surface. The XRD measures the scatter angles of incident X-rays; the angle and intensity of scatter depend upon the crystalline structure of the pulverized sample. XRD is considered a qualitative rather than quantitative technique. ESCA/XPS revealed that the final layer to deposit was predominantly carbonaceous. XRD was successful in identifying specific compounds, such as Al 2O3, Al and/or Al3 21SiO47, mullite (3(Al2)O3 -SiO2), and nickel-aluminides. Eventually, Electron MicroProbe Analysis (EMPA) was conducted on the marialographically-prepared cross- sections of selected slag deposits. Microprobe combines SEM and Wavelength Dispersive X-Ray Spectroscopy (WDS), and, like EDX, uses a narrowly-focused high-energy electron beam impinging upon a specimen to elicit, in the case of EPMA, characteristic X-rays with specific wavelengths. This quantitative, analytical tool proved the most useful in determining depositional layering and composition of the slag deposits. This information was utilized in verifying the location of the breach in the left leading edge of the wing of the Columbia.

Influence of a cellulosic ether carrier on the structure of biphasic calcium phosphate ceramic particles in an injectable composite material.

PubMed

Dupraz, A; Nguyen, T P; Richard, M; Daculsi, G; Passuti, N

1999-04-01

An injectable composite material based on biphasic calcium phosphate (BCP) and a nonionic cellulose ether has been elaborated for use in percutaneous surgery for spine fusion. This paper reports the characterization results of this material by spectroscopic techniques including X-ray diffraction (XRD), infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) fitted with an energy dispersive X-Ray analysis system and high-resolution transmission electron microscopy (HR-TEM). From FTIR and XPS results, it was observed that the adhesion between the polymer and the ceramic might be insured by oxygen bridging developed through an ionic bonding between calcium ions and (C-O) groups of the polymer. Moreover, XPS showed attraction of Ca2+ ions in the polymer matrix, while the ceramic surface was modified in a HPO4(2-) -rich layer. These results suggest a possible dissolution/precipitation process at the interface ceramic/polymer. HR-TEM observations supported this hypothesis, showing a light contrasted fringe at the surface of the ceramic grains in the composite paste. As well, changes in the XRD spectra could indicate a small decrease in the crystal size of the BCP powder through the contact to polymer solution. In addition, SEM observation showed a decrease of the initial BCP granulometry. Aggregates of 80-200 microm seemed to be mostly dissociated in micrograins. The ceramic grains were coated with and bonded between each other by the polymer matrix, which acted as spacer in between the ceramic grains, creating a macroporous-like material structure.

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

Olivieri, Giorgia; Brown, Matthew A., E-mail: matthew.brown@mat.ethz.ch; Parry, Krista M.

Over the past decade, energy-dependent ambient pressure X-ray photoelectron spectroscopy (XPS) has emerged as a powerful analytical probe of the ion spatial distributions at the vapor (vacuum)-aqueous electrolyte interface. These experiments are often paired with complementary molecular dynamics (MD) simulations in an attempt to provide a complete description of the liquid interface. There is, however, no systematic protocol that permits a straightforward comparison of the two sets of results. XPS is an integrated technique that averages signals from multiple layers in a solution even at the lowest photoelectron kinetic energies routinely employed, whereas MD simulations provide a microscopic layer-by-layer descriptionmore » of the solution composition near the interface. Here, we use the National Institute of Standards and Technology database for the Simulation of Electron Spectra for Surface Analysis (SESSA) to quantitatively interpret atom-density profiles from MD simulations for XPS signal intensities using sodium and potassium iodide solutions as examples. We show that electron inelastic mean free paths calculated from a semi-empirical formula depend strongly on solution composition, varying by up to 30% between pure water and concentrated NaI. The XPS signal thus arises from different information depths in different solutions for a fixed photoelectron kinetic energy. XPS signal intensities are calculated using SESSA as a function of photoelectron kinetic energy (probe depth) and compared with a widely employed ad hoc method. SESSA simulations illustrate the importance of accounting for elastic-scattering events at low photoelectron kinetic energies (<300 eV) where the ad hoc method systematically underestimates the preferential enhancement of anions over cations. Finally, some technical aspects of applying SESSA to liquid interfaces are discussed.« less

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach.

PubMed

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO(2) composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO(2) nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. This journal is © The Royal Society of Chemistry 2011

Synthesis of High Valence Silver-Loaded Mesoporous Silica with Strong Antibacterial Properties

PubMed Central

Chen, Chun-Chi; Wu, Hsin-Hsien; Huang, Hsin-Yi; Liu, Chen-Wei; Chen, Yi-Ning

2016-01-01

A simple chemical method was developed for preparing high valence silver (Ag)-loaded mesoporous silica (Ag-ethylenediaminetetraacetic acid (EDTA)-SBA-15), which showed strong antibacterial activity. Ag-EDTA-SBA-15 exhibited stronger and more effective antibacterial activity than commercial Ag nanoparticles did, and it offered high stability of high valence silver in the porous matrix and long-lasting antibacterial activity. The synthesized materials were characterized using Fourier transform infrared spectroscopy, powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) analysis, and transmission electron microscopy (TEM). Ag existed in both surface complexation and Ag particles. EDTA anchored within a porous structure chelated Ag ions in higher oxidation states and prevented their agglomeration and oxidation reduction. The XRD results showed that most Ag in the Ag-EDTA-SBA-15 existed in higher oxidation states such as Ag(II) and Ag(III). However, the XPS and TEM results showed that Ag easily reduced in lower oxidation states and agglomerated as Ag particles on the exterior layer of the SBA-15. PMID:26742050

SeO2 adsorption on CaO surface: DFT and experimental study on the adsorption of multiple SeO2 molecules

NASA Astrophysics Data System (ADS)

Fan, Yaming; Zhuo, Yuqun; Li, Liangliang

2017-10-01

SeO2 adsorption mechanisms on CaO surface were firstly investigated by both density functional theory (DFT) calculations and adsorption experiments. Adsorption of multiple SeO2 on the CaO (001) surface was investigated using slab model. Based on the results of adsorption energy and surface property, a double-layer adsorption mechanisms were proposed. In experiments, the SeO2 adsorption products were prepared in a U-shaped quartz reactor at 200 °C. The surface morphology was investigated by field emission scanning electron microscopy (FE-SEM). The superficial and total SeO2 mass fractions were measured by X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma atomic emission spectroscopy (ICP-AES), respectively. The surface valence state and bulk structure are determined by XPS and X-Ray Diffraction (XRD). The experimental results are in good agreement with the DFT results. In conclusion, the fundamental SeO2 chemisorption mechanisms on CaO surface were suggested.

Synthesis of Ternary Borocarbonitrides by High Temperature Pyrolysis of Ethane 1,2-Diamineborane

PubMed Central

Leardini, Fabrice; Massimi, Lorenzo; Flores-Cuevas, Eduardo; Fernández, Jose Francisco; Ares, Jose Ramon; Betti, Maria Grazia; Mariani, Carlo

2015-01-01

Ethane 1,2-diamineborane (EDAB) is an alkyl-containing amine-borane adduct with improved hydrogen desorption properties as compared to ammonia borane. In this work, it is reported the high temperature thermolytic decomposition of EDAB. Thermolysis of EDAB has been investigated by concomitant thermogravimetry-differential thermal analysis-mass spectrometry experiments. EDAB shows up to four H2 desorption events below 1000 °C. Small fractions of CH4, C2H4 and CO/CO2 are also observed at moderate-high temperatures. The solid-state thermolysis product has been characterized by means of different structural and chemical methods, such as X-ray diffraction, Raman spectroscopy, Scanning electron microscopy, Elemental analysis, and X-ray photoelectron spectroscopy (XPS). The obtained results indicate the formation of a ternary borocarbonitride compound with a poorly-crystalline graphitic-like structure. By contrast, XPS measurements show that the surface is rich in carbon and nitrogen oxides, which is quite different to the bulk of the material. PMID:28793545

Depth profile composition studies of thin film CdS:Cu2S solar cells using XPS and AES

NASA Astrophysics Data System (ADS)

Bhide, V. G.; Salkalachen, S.; Rastogi, A. C.; Rao, C. N. R.; Hegde, M. S.

1981-09-01

Studies of the surface composition and depth profiles of thin film CdS:Cu2S solar cells based on the techniques of X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) are reported. Specimens were fabricated by the thermal deposition of polycrystalline CdS films onto silver-backed electrodes predeposited on window glass substrates, followed by texturization in hot HCl and chemical plating in a hot CuCl(I) bath for a few seconds to achieve the topotaxial growth of CuS films. The XPS and AES studies indicate the junction to be fairly diffused in the as-prepared cell, with heat treatment in air at 210 C sharpening the junction, improving the stoichiometry of the Cu2S layer and thus improving cell performance. The top copper sulfide layer is found to contain impurities such as Cd, Cl, O and C, which may be removed by mild Ar(+) ion beam etching. The presence of copper deep in the junction is invariably detected, apparently in the grain boundary region in the form of CuS or Cu(2+) trapped in the lattice. It is also noted that the nominal valence state of copper changes abruptly from Cu(+) to Cu(2+) across the junction.

New insights into micro/nanoscale combined probes (nanoAuger, μXPS) to characterize Ag/Au@SiO2 core-shell assemblies.

PubMed

Ledeuil, J B; Uhart, A; Soulé, S; Allouche, J; Dupin, J C; Martinez, H

2014-10-07

This work has examined the elemental distribution and local morphology at the nanoscale of core@shell Ag/Au@SiO2 particles. The characterization of such complex metal/insulator materials becomes more efficient when using an initial cross-section method of preparation of the core@shell nanoparticles (ion milling cross polisher). The originality of this route of preparation allows one to obtain undamaged, well-defined and planar layers of cross-cut nano-objects. Once combined with high-resolution techniques of characterization (XPS, Auger and SEM), the process appears as a powerful way to minimize charging effects and enhance the outcoming electron signal (potentially affected by the topography of the material) during analysis. SEM experiments have unambiguously revealed the hollow-morphology of the metal core, while Auger spectroscopy observations showed chemical heterogeneity within the particles (as silver and gold are randomly found in the core ring). To our knowledge, this is the first time that Auger nano probe spectroscopy has been used and successfully optimized for the study of some complex metal/inorganic interfaces at such a high degree of resolution (≈12 nm). Complementarily, XPS Au 4f and Ag 3d peaks were finally detected attesting the possibility of access to the whole chemistry of such nanostructured assemblies.

Electronic structure, charge transfer, and intrinsic luminescence of gadolinium oxide nanoparticles: Experiment and theory

NASA Astrophysics Data System (ADS)

Zatsepin, D. A.; Boukhvalov, D. W.; Zatsepin, A. F.; Kuznetsova, Yu. A.; Mashkovtsev, M. A.; Rychkov, V. N.; Shur, V. Ya.; Esin, A. A.; Kurmaev, E. Z.

2018-04-01

The cubic (c) and monoclinic (m) polymorphs of Gd2O3 were studied using the combined analysis of several materials science techniques - X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. Density functional theory (DFT) based calculations for the samples under study were performed as well. The cubic phase of gadolinium oxide (c-Gd2O3) synthesized using a precipitation method exhibits spheroidal-like nanoclusters with well-defined edges assembled from primary nanoparticles with an average size of 50 nm, whereas the monoclinic phase of gadolinium oxide (m-Gd2O3) deposited using explosive pyrolysis has a denser structure compared with natural gadolinia. This phase also has a structure composed of three-dimensional complex agglomerates without clear-edged boundaries that are ∼21 nm in size plus a cubic phase admixture of only 2 at.% composed of primary edge-boundary nanoparticles ∼15 nm in size. These atomic features appear in the electronic structure as different defects ([Gd…Osbnd OH] and [Gd…Osbnd O]) and have dissimilar contributions to the charge-transfer processes among the appropriate electronic states with ambiguous contributions in the Gd 5р - O 2s core-like levels in the valence band structures. The origin of [Gd…Osbnd OH] defects found by XPS was well-supported by PL analysis. The electronic and atomic structures of the synthesized gadolinias calculated using DFT were compared and discussed on the basis of the well-known joint OKT-van der Laan model, and good agreement was established.

Urea-assisted low temperature green synthesis of graphene nanosheets for transparent conducting film

NASA Astrophysics Data System (ADS)

Chamoli, Pankaj; Das, Malay K.; Kar, Kamal K.

2018-02-01

Present work demonstrates the fabrication of graphene nanosheet (GN) based transparent conducting film (TCF) using spray coating. Green synthesis of GN is carried out by reduction of graphene oxide (GO) using urea as green reducing agent. The reductive ability of urea with varied concentration is studied for GO at low temperature (i.e., 90 °C). As synthesized graphene nanosheets (GNs) are characterized by Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), UV-visible spectroscopy, field emission scanning electron microscopy (FESEM), atomic force microscope (AFM), and X-ray Photon spectroscopy (XPS). Raman analysis confirms that the maximum reduction of oxygen species is noticed using 30 mg/ml urea concentration at 90 °C from GO, and found Raman D to G band ratio (ID/IG) of ∼1.30. XPS analysis validates the Raman signature of removal of oxygen functional groups from GO, and obtained C/O ratio of ∼5.28. Further, transparent conducting films (TCFs) are fabricated using synthesized GNs. Thermal graphitization is carried out to enhance the optical and electrical properties of TCFs. TCF shows best performance when it is annealed at 900 °C for 1 h in vacuum, and obtained sheet resistance is ∼1.89 kΩ/□ with transmittance of ∼62.53%.

Probing the influence of the center atom coordination structure in iron phthalocyanine multi-walled carbon nanotube-based oxygen reduction reaction catalysts by X-ray absorption fine structure spectroscopy

NASA Astrophysics Data System (ADS)

Peng, Yingxiang; Li, Zhipan; Xia, Dingguo; Zheng, Lirong; Liao, Yi; Li, Kai; Zuo, Xia

2015-09-01

Three different pentacoordinate iron phthalocyanine (FePc) electrocatalysts with an axial ligand (pyridyl group, Py) anchored to multi-walled carbon nanotubes (MWCNTs) are prepared by a microwave method as high performance composite electrocatalysts (FePc-Py/MWCNTs) for the oxygen reduction reaction (ORR). For comparison, tetracoordinate FePc electrocatalysts without an axial ligand anchored to MWCNTs (FePc/MWCNTs) are assembled in the same way. Ultraviolet-visible spectrophotometry (UV-Vis), Raman spectroscopy (RS), and high-resolution transmission electron microscopy (HRTEM) are used to characterize the obtained electrocatalysts. The electrocatalytic activity of the samples is measured by linear sweep voltammetry (LSV), and the onset potential of all of the FePc-Py/MWCNTs electrocatalysts is found to be more positive than that of their FePc/MWCNTs counterparts. X-ray photoelectron spectroscopy (XPS) and X-ray absorption fine structure (XAFS) spectroscopy are employed to elucidate the relationship between molecular structure and electrocatalytic activity. XPS indicates that higher concentrations of Fe3+ and pyridine-type nitrogen play critical roles in determining the electrocatalytic ORR activity of the samples. XAFS spectroscopy reveals that the FePc-Py/MWCNTs electrocatalysts have a coordination geometry around Fe that is closer to the square pyramidal structure, a higher concentration of Fe3+, and a smaller phthalocyanine ring radius compared with those of FePc/MWCNTs.

Size and shape dependence of CO adsorption sites on sapphire supported Fe microcrystals

NASA Technical Reports Server (NTRS)

Papageorgopoulos, C.; Heinemann, K.

1985-01-01

The surface structure and stoichiometry of alumina substrates, as well as the size, growth characteristics, and shape of Fe deposits on sapphire substrates have been investigated by low energy electron diffraction (LEED), Auger electron spectroscopy, electron energy loss spectroscopy, and X-ray photoemission spectroscopy (XPS), as well as work function measurements, in conjunction with transition electron microscopy observations. The substrates used in this work were the following: (1) new, clean Al2O3; (2) same surface amorphized by Ar ion bombardment; (3) same surface regenerated by 650 C annealing; (4) amorphous alumina films on Ta slab; and (5) polycrystal alumina films, obtained by heating amorphous films to 600 C. Substrate cleaning was found to be most effective in producing a reproducible surface upon oxygen RF plasma treatment. The Fe nucleation and growth process was found to depend strongly on the type of substrate surface and deposition conditions. Ar ion bombardment under beam flooding, and subsequent annealing at 650 C was found an effective means to restore the original Al2O3 (1102) surface for renewed Fe deposition.

Attachment of Single-wall Carbon Nanotubes (SWNTs) on Platinum Surfaces by Self-Assembling Techniques

NASA Technical Reports Server (NTRS)

Rosario-Castro, Belinda I.; Cabrera, Carlos R.; Perez-Davis, Maria; Lebron, Marisabel; Meador, Michael

2003-01-01

Single-wall carbon nanotubes (SWNTs) are very interesting materials because of their morphology, electronic and mechanical properties. Its morphology (high length-to-diameter ratio) and electronic properties suggest potential application of SWNTs as anode material for lithium ion secondary batteries. The introduction of SWNTs on these types of sources systems will improve their performance, efficiency, and capacity to store energy. A purification method has been applied for the removal of iron and amorphous carbon from the nanotubes. Unpurified and purified SWNTs were characterized by transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). In order to attach carbon nanotubes on platinum electrode surfaces, a self-assembled monolayer (SAM) of 4-aminothiophenol (4-ATP) was deposited over the electrodes. The amino-terminated SAM obtained was characterized by cyclic voltammetry, X-ray photoelectron spectroscopy (XPS), and Fourier-transforms infrared (FTIR) spectroscopy. Carbon nanotubes were deposited over the amino-terminated SAM by an amide bond formed between SAM amino groups and carboxylic acid groups at the open ends of the carbon nanotubes.This deposition was characterized using Raman spectroscopy and Scanning Electron microscopy (SEM).

Characterization of the Surface Film Formed on Molten AZ91D Magnesium Alloy in Atmospheres Containing SO2

NASA Astrophysics Data System (ADS)

Wang, Xian-Fei; Xiong, Shou-Mei

2012-11-01

The surface film formed on molten AZ91D magnesium alloy in an atmosphere containing SO2 was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS). The surface film primarily contained MgO and MgS and had a network structure. MgS increased the Pilling-Bedworth ratio of the film and enhanced its protective capability. The films with a few pores at the surface consisted of two layers with an outer MgO layer and an inner layer of MgO and MgS. The film without pores at the surface also contained MgS and small amounts of MgSO4 in the outer layer. Increasing the SO2 content in the atmosphere promoted film growth and the formation of the protective film was prevented with the increased temperature.

A novel cetyltrimethyl ammonium silver bromide complex and silver bromide nanoparticles obtained by the surfactant counterion.

PubMed

Liu, Xian-Hao; Luo, Xiao-Hong; Lu, Shu-Xia; Zhang, Jing-Chang; Cao, Wei-Liang

2007-03-01

A novel cetyltrimethyl ammonium silver bromide (CTASB) complex has been prepared simply through the reaction of silver nitrate with cetyltrimethyl ammonium bromide (CTAB) in aqueous solution at room temperature by controlling the concentration of CTAB and the molar ratio of CTAB to silver nitrate in the reaction solution, in which halogen in CTAB is used as surfactant counterion. The structure and thermal behavior of cetyltrimethyl ammonium silver bromide have been investigated by using X-ray diffraction (XRD), infrared spectroscopy (IR), X-ray photoelectron spectroscopy (XPS), UV/vis spectroscopy, thermal analysis (TG-DTA), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The results show that the complex possesses a metastable layered structure. Upon heating the CTASB aqueous dispersion to above 80 degrees C, the structure change of the complex took place and CTAB-capped nanosized silver bromide particles further formed.

Tremella-like graphene-Au composites used for amperometric determination of dopamine.

PubMed

Li, Cong; Zhao, Jingyu; Yan, Xiaoyi; Gu, Yue; Liu, Weilu; Tang, Liu; Zheng, Bo; Li, Yaru; Chen, Ruixue; Zhang, Zhiquan

2015-03-21

Electrochemical detection of dopamine (DA) plays an important role in medical diagnosis. In this paper, tremella-like graphene-Au (t-GN-Au) composites were synthesized by a one-step hydrothermal method for selective detection of DA. Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy, and Fourier transform infrared (FTIR) spectroscopy were used to characterize as-prepared t-GN-Au composites. The t-GN-Au composites were directly used for the determination of DA via cyclic voltammetry (CV) and the chronoamperometry (CA) technique. CA measurement gave a wide linear range from 0.8 to 2000 μM, and the detection limit of 57 nM (S/N = 3) for DA. The mechanism and the heterogeneous electron transfer kinetics of the DA oxidation were discussed in the light of rotating disk electrode (RDE) experiments. Moreover, the modified electrode was applied to the determination of DA in human urine and serum samples.

Study of behaviors of aluminum overlayers deposited on uranium via AES, EELS, and XPS

NASA Astrophysics Data System (ADS)

Liu, Kezhao; Luo, Lizhu; Zhou, Wei; Yang, Jiangrong; Xiao, Hong; Hong, Zhanglian; Yang, Hui

2013-04-01

Aluminum overlayers on uranium were prepared by sputtering at room temperature in an ultra-high vacuum chamber. The growth mode of aluminum overlayers and behaviors of the Al/U interface reaction were studied in situ by auger electron spectroscopy, electron energy loss spectroscopy, and X-ray photoelectron spectroscopy. The results suggested that the interdiffusion took place at the Al/U interface during the initial stage of deposition. The U4f spectra of the Al/U interface showed strong correlation satellites at binding energies of 380.4 and 392.7 eV and plasma loss features at 404.2 eV, respectively. The interactions between aluminum and uranium yielded the intermetallic compound of UAlx, inducing the shift to a low binding energy for Al2p peaks. The results indicated that aluminum overlayers were formed on the uranium by sputtering in an island growth mode.

Nanoparticles of nickel oxide: growth and organization on zinc-substituted anionic clay matrix by one-pot route at room temperature

NASA Astrophysics Data System (ADS)

Carja, Gabriela; Nakajima, Akira; Dranca, Cristian; Okada, Kiyoshi

2010-10-01

A room temperature nanocarving strategy is developed for the fabrication of nanoparticles of nickel oxide on zinc-substituted anionic clay matrix (Ni/ZnLDH). It is based on the growth and organization of nanoparticles of nickel oxide which occur during the structural reconstruction of the layered structure of the anionic clay in NiSO4 aqueous solution. No organic compounds are used during the fabrication. The described material was characterized by X-ray diffraction (XRD), IR spectroscopy (FTIR), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) spectroscopy, and X-ray photoelectron spectroscopy (XPS). Results show that the nickel-clay nanoarchitecture consists of small nanoparticles of nickel oxide (average size 7 nm) deposited on the larger nanoparticles (average size 90 nm) of zinc-substituted clay. The optical properties of the new nickel-zinc formulation are studied by UV-Vis.

Interaction of acidic trace gases with ice from a surface science perspective

NASA Astrophysics Data System (ADS)

Waldner, A.; Kong, X.; Ammann, M.; Orlando, F.; Birrer, M.; Artiglia, L.; Bartels-Rausch, T.

2016-12-01

Acidic trace gases, such as HCOOH, HCl and HONO, play important roles in atmospheric chemistry. The presence of ice is known to have the capability to modify this chemistry (Neu et al. 2012). The molecular level processes of the interaction of acidic trace gases with ice are still a matter of debate and a quantification of the uptake is difficult (Dash et al. 2006, Bartels-Rausch et al. 2014, Huthwelker et al. 2006). This hampers a proper inclusion of ice as a substrate in models of various scales as for example in global chemistry climate models that would among others allow predicting large-scale effects of ice clouds. So far, direct observations of the ice surface and of the interaction with trace gases at temperatures and concentrations relevant to the environment are very limited. In this study, we take advantage of the surface and analytical sensitivity as well as the chemical selectivity of photoemission and absorption spectroscopy performed at ambient pressure using the near ambient pressure photoemission endstation (NAPP) at Swiss Light Source to overcome this limitation in environmental science (Orlando et al. 2016). Specifically, ambient pressure X-ray Photoelectron Spectroscopy (XPS) allows us to get information about chemical state and concentration depth profiles of dopants. The combination of XPS with auger electron yield Near-Edge X-ray Absorption Fine Structure (NEXAFS) enables us to locate the dopant and analyse wheather the interaction leads to enhanced surface disorder and to what extent different disorders influences the uptake of the trace gas. For the first time, this study looks directly at the interaction of HCOOH, the strongest organic acid, with ice at 2 different temperatures (233 and 253 K) relevant for environmental science by means of electron spectroscopy. XPS depth profiles indicate that the HCOOH basically remains within the topmost ice layers and O K-edge NEXAFS analysis show that the interaction ice-HCOOH does not lead to enhanced surface disorder at environmentally relevant conditions.

Thermally induced hydrosilylation at deuterium-terminated silicon nanoparticles: an investigation of the radical chain propagation mechanism.

PubMed

Holm, Jason; Roberts, Jeffrey T

2009-06-16

Isotopic labeling techniques were employed to study alkene addition to hydrogen- and deuterium-terminated silicon nanoparticles. Deuterium-terminated silicon nanoparticle synthesis is described, as is the characterization of fresh deuterium-terminated particles by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and in situ Fourier transform infrared spectroscopy (FTIR). Particles were refluxed in pure 1-dodecene and subsequently characterized by FTIR and nuclear magnetic resonance (NMR) spectroscopy. (1)H NMR results showed features consistent with dodecyl-terminated nanoparticles. Infrared absorption spectra of refluxed particles showed strong evidence of new C-D bond formation, which is consistent with a radical chain mechanism for alkene addition by hydrosilylation.

X-ray Photoelectron Spectroscopy (XPS), Rutherford Back Scattering (RBS) studies

NASA Technical Reports Server (NTRS)

Neely, W. C.; Bozak, M. J.; Williams, J. R.

1993-01-01

X-ray photoelectron spectroscopy (XPS), Rutherford Back Scattering (RBS) studies of each of sample received were completed. Since low angle X-ray could not be performed because of instrumentation problems, Auger spectrometry was employed instead. The results of these measurements for each of the samples is discussed in turn.

Compositional ratio effect on the surface characteristics of CuZn thin films

NASA Astrophysics Data System (ADS)

Choi, Ahrom; Park, Juyun; Kang, Yujin; Lee, Seokhee; Kang, Yong-Cheol

2018-05-01

CuZn thin films were fabricated by RF co-sputtering method on p-type Si(100) wafer with various RF powers applied on metallic Cu and Zn targets. This paper aimed to determine the morphological, chemical, and electrical properties of the deposited CuZn thin films by utilizing a surface profiler, atomic force microscopy (AFM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), UV photoelectron spectroscopy (UPS), and a 4-point probe. The thickness of the thin films was fixed at 200 ± 8 nm and the roughness of the thin films containing Cu was smaller than pure Zn thin films. XRD studies confirmed that the preferred phase changed, and this tendency is dependent on the ratio of Cu to Zn. AES spectra indicate that the obtained thin films consisted of Cu and Zn. The high resolution XPS spectra indicate that as the content of Cu increased, the intensities of Zn2+ decreased. The work function of CuZn thin films increased from 4.87 to 5.36 eV. The conductivity of CuZn alloy thin films was higher than pure metallic thin films.

Synthesis and characterization of an effective organic/inorganic hybrid green corrosion inhibitive complex based on zinc acetate/Urtica Dioica

NASA Astrophysics Data System (ADS)

Salehi, E.; Naderi, Reza; Ramezanzadeh, B.

2017-02-01

This study aims at synthesis and characterization of an effective corrosion inhibitive complex based on zinc acetate/Urtica Dioica (ZnA-U.D) for corrosion protection of mild steel in chloride solution. The chemical structure and morphology of the complex were characterized by Fourier transform infrared spectroscopy (FT-IR), UV-vis, thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The corrosion protection performance of the mild steel samples dipped in 3.5 wt.% NaCl solutions with and without ZnA-U.D extract was investigated by visual observations, open circuit potential (OCP) measurements, electrochemical impedance spectroscopy (EIS) and polarization test. Results revealed that the ZnA successfully chelated with organic inhibitive compounds (i.e Quercetin, Quinic acid, Caffeic acid, Hystamine and Serotonin) present in the U.D extract. The electrochemical measurements revealed the effective inhibition action of ZnA-U.D complex in the sodium chloride solution on the mild steel. The synergistic effect between Zn2+ and organic compounds present in the U.D extract resulted in protective film deposition on the steel surface, which was proved by SEM and XPS analyses.

Preparation and Characterization of Polyurethanes with Cross-Linked Siloxane in the Side Chain by Sol-Gel Reactions

PubMed Central

Zhao, Hui; Hao, Tong-Hui; Hu, Guo-Hua; Shi, Dean; Huang, Da; Jiang, Tao; Zhang, Qun-Chao

2017-01-01

A series of novel polyurethanes containing cross-linked siloxane in the side chain (SPU) were successfully synthesized through a sol-gel process. The SPU was composed of 0%–20% N-(n-butyl)-3-aminopropyltriethoxysilane (HDI-T) modified hexamethylene diisocynate homopolymer. The effects of HDI-T content on both the structure and properties of SPU were investigated by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), mechanical properties tests, gel content test, water contact angle measurement and water absorption test. FT-IR, XPS and XRD results confirmed the successful incorporation of HDI-T onto polyurethanes and the formation of Si–O–Si. The surface roughness and the Si content of SPU enhanced with the increase of HDI-T content. Both crystallization and melting temperature shifted to a lower point after the incorporation of HDI-T. The hydrophobicity, tensile strength, Young’s modulus and pencil hardness overall increased with the increasing of HDI-T content, whereas the thermal stability and the elongation at break of SPU slightly decreased. PMID:28772607

O electrolyte for bio-application

NASA Astrophysics Data System (ADS)

Naddaf, M.; Almariri, A.

2014-09-01

Porous silicon (PS) has been prepared in the dark by anodic etching of n+-type (111) silicon substrate in a HF:HCl:C2H5OH:H2O2:H2O electrolyte. The processed PS layer is characterized by means of photoluminescence (PL) spectroscopy, scanning electron microscope (SEM), water contact angle (CA) measurements, Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and micro-Raman scattering. The CA of fresh PS layer is found to be ~142°. On aging at ambient conditions, the CA decreases gently to reach ~133° after 3 month, and then it is stabilized for a prolonged time of aging. The visible PL emission from the PS layer also exhibits a good stability against aging time. The FTIR and XPS measurements and analysis show that the stable aged PS layer has rather SiO2-rich surface. The micro/nanostructure nature of the PS layer is revealed from SEM and micro-Raman results and correlated to CA results. Stable hydrophobic surface of oxidized PS layer is attractive for bio-applications. The efficiency of the produced PS layers as an entrapping template for specific immobilization of IgG2a antibody via physical absorption process is demonstrated.

Reduced graphene oxide growth on 316L stainless steel for medical applications

NASA Astrophysics Data System (ADS)

Cardenas, L.; MacLeod, J.; Lipton-Duffin, J.; Seifu, D. G.; Popescu, F.; Siaj, M.; Mantovani, D.; Rosei, F.

2014-07-01

We report a new method for the growth of reduced graphene oxide (rGO) on the 316L alloy of stainless steel (SS) and its relevance for biomedical applications. We demonstrate that electrochemical etching increases the concentration of metallic species on the surface and enables the growth of rGO. This result is supported through a combination of Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy (SEM), density functional theory (DFT) calculations and static water contact angle measurements. Raman spectroscopy identifies the G and D bands for oxidized species of graphene at 1595 cm-1 and 1350 cm-1, respectively, and gives an ID/IG ratio of 1.2, indicating a moderate degree of oxidation. XPS shows -OH and -COOH groups in the rGO stoichiometry and static contact angle measurements confirm the wettability of rGO. SEM and AFM measurements were performed on different substrates before and after coronene treatment to confirm rGO growth. Cell viability studies reveal that these rGO coatings do not have toxic effects on mammalian cells, making this material suitable for biomedical and biotechnological applications.

The green hydrothermal synthesis of nanostructured Cu2ZnSnSe4 as solar cell material and study of their structural, optical and morphological properties

NASA Astrophysics Data System (ADS)

Vanalakar, S. A.; Agawane, G. L.; Kamble, A. S.; Patil, P. S.; Kim, J. H.

2017-12-01

Cu2ZnSnSe4 (CZTSe) has attracted intensive attention as an absorber material for the thin-film solar cells due to its high absorption coefficient, direct band gap, low toxicity, and abundance of its constituent elements. In this study nanostructured CZTSe nanoparticles are prepared via green hydrothermal synthesis without using toxic solvents, organic amines, catalysts or noxious chemicals. The structural, optical, and morphological properties of CZTSe nanostructured powder were studied using X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), UV-vis absorption spectroscopy, and transmission electron microscope (TEM) techniques. Raman peaks at 170, 195, and 232 cm-1 confirm the formation of pure phase CZTSe nanostructured particles. In addition, the EDS and XPS results confirm the appropriate chemical purity of the annealed CZTSe nanoparticles. Meanwhile, the TEM analysis showed the presence of phase pure oval like CZTSe particle with size of about 80-140 nm. The UV-Vis-NIR absorption spectra analysis showed that the optical band gap of CZTSe nanostructured particles is about 1.14 eV. This band gap energy is close to the optimum value of a photovoltaic solar cell absorber material.

Relative impact of H 2 O and O 2 in the oxidation of UO 2 powders from 50 to 300 °C

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

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong

Here, we studied the reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO 2) powder at elevated temperature by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). We observed and quatified oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Relative impact of H2O and O2 in the oxidation of UO2 powders from 50 to 300 °C

NASA Astrophysics Data System (ADS)

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong; Roberts, Sarah K.; Nelson, Art J.

2017-12-01

The reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO2) powder at elevated temperature was studied by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). Oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice was observed and quantified. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Relative impact of H 2 O and O 2 in the oxidation of UO 2 powders from 50 to 300 °C

DOE PAGES

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong; ...

2017-10-04

Here, we studied the reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO 2) powder at elevated temperature by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). We observed and quatified oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Investigation of Industrial Polyurethane Foams Modified with Antimicrobial Copper Nanoparticles

PubMed Central

Sportelli, Maria Chiara; Picca, Rosaria Anna; Ronco, Roberto; Bonerba, Elisabetta; Tantillo, Giuseppina; Pollini, Mauro; Sannino, Alessandro; Valentini, Antonio; Cataldi, Tommaso R.I.; Cioffi, Nicola

2016-01-01

Antimicrobial copper nanoparticles (CuNPs) were electrosynthetized and applied to the controlled impregnation of industrial polyurethane foams used as padding in the textile production or as filters for air conditioning systems. CuNP-modified materials were investigated and characterized morphologically and spectroscopically, by means of Transmission Electron Microscopy (TEM), and X-ray Photoelectron Spectroscopy (XPS). The release of copper ions in solution was studied by Electro-Thermal Atomic Absorption Spectroscopy (ETAAS). Finally, the antimicrobial activity of freshly prepared, as well as aged samples—stored for two months—was demonstrated towards different target microorganisms. PMID:28773665

Quantitative depth profiling of Ce(3+) in Pt/CeO2 by in situ high-energy XPS in a hydrogen atmosphere.

PubMed

Kato, Shunsuke; Ammann, Markus; Huthwelker, Thomas; Paun, Cristina; Lampimäki, Markus; Lee, Ming-Tao; Rothensteiner, Matthäus; van Bokhoven, Jeroen A

2015-02-21

The redox property of ceria is a key factor in the catalytic activity of ceria-based catalysts. The oxidation state of well-defined ceria nanocubes in gas environments was analysed in situ by a novel combination of near-ambient pressure X-ray Photoelectron Spectroscopy (XPS) and high-energy XPS at a synchrotron X-ray source. In situ high-energy XPS is a promising new tool to determine the electronic structure of matter under defined conditions. The aim was to quantitatively determine the degree of cerium reduction in a nano-structured ceria-supported platinum catalyst as a function of the gas environment. To obtain a non-destructive depth profile at near-ambient pressure, in situ high-energy XPS analysis was performed by varying the kinetic energy of photoelectrons from 1 to 5 keV, and, thus, the probing depth. In ceria nanocubes doped with platinum, oxygen vacancies formed only in the uppermost layers of ceria in an atmosphere of 1 mbar hydrogen and 403 K. For pristine ceria nanocubes, no change in the cerium oxidation state in various hydrogen or oxygen atmospheres was observed as a function of probing depth. In the absence of platinum, hydrogen does not dissociate and, thus, does not lead to reduction of ceria.

Understanding of sub-band gap absorption of femtosecond-laser sulfur hyperdoped silicon using synchrotron-based techniques

PubMed Central

Limaye, Mukta V.; Chen, S. C.; Lee, C. Y.; Chen, L. Y.; Singh, Shashi B.; Shao, Y. C.; Wang, Y. F.; Hsieh, S. H.; Hsueh, H. C.; Chiou, J. W.; Chen, C. H.; Jang, L. Y.; Cheng, C. L.; Pong, W. F.; Hu, Y. F.

2015-01-01

The correlation between sub-band gap absorption and the chemical states and electronic and atomic structures of S-hyperdoped Si have been extensively studied, using synchrotron-based x-ray photoelectron spectroscopy (XPS), x-ray absorption near-edge spectroscopy (XANES), extended x-ray absorption fine structure (EXAFS), valence-band photoemission spectroscopy (VB-PES) and first-principles calculation. S 2p XPS spectra reveal that the S-hyperdoped Si with the greatest (~87%) sub-band gap absorption contains the highest concentration of S2− (monosulfide) species. Annealing S-hyperdoped Si reduces the sub-band gap absorptance and the concentration of S2− species, but significantly increases the concentration of larger S clusters [polysulfides (Sn2−, n > 2)]. The Si K-edge XANES spectra show that S hyperdoping in Si increases (decreased) the occupied (unoccupied) electronic density of states at/above the conduction-band-minimum. VB-PES spectra evidently reveal that the S-dopants not only form an impurity band deep within the band gap, giving rise to the sub-band gap absorption, but also cause the insulator-to-metal transition in S-hyperdoped Si samples. Based on the experimental results and the calculations by density functional theory, the chemical state of the S species and the formation of the S-dopant states in the band gap of Si are critical in determining the sub-band gap absorptance of hyperdoped Si samples. PMID:26098075

Efficient solar light-driven degradation of Congo red with novel Cu-loaded Fe3O4@TiO2 nanoparticles.

PubMed

Arora, Priya; Fermah, Alisha; Rajput, Jaspreet Kaur; Singh, Harminder; Badhan, Jigyasa

2017-08-01

In this work, Cu-loaded Fe 3 O 4 @TiO 2 core shell nanoparticles were prepared in a single pot by coating of TiO 2 on Fe 3 O 4 nanoparticles followed by Cu loading. X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM), thermogravimetric analysis (TGA), Brunauer-Emmett- Teller (BET), vibrating sample magnetometry (VSM), X-ray photoelectron spectroscopy (XPS), and valence band X-ray photoelectron spectroscopy (VB XPS) techniques were used for characterization of as prepared nanoparticles. Synergism between copper and titania was evaluated by studying the solar light-driven photodegradation of Congo red dye solution in the presence of Fe 3 O 4 @TiO 2 nanoparticles on one side and Cu-loaded Fe 3 O 4 @TiO 2 nanoparticles on the other side. The latter performed better than the former catalyst, indicating the enhanced activity of copper-loaded catalyst. Further photodegradation was studied by three means, i.e., under ultraviolet (UV), refluxing, and solar radiations. Cu-loaded Fe 3 O 4 @TiO 2 enhanced the degradation efficiency of Congo red dye. Thus, Cu act possibly by reducing the band gap of TiO 2 and widening the optical response of semiconductor, as a result of which solar light could be used to carry out photocatalysis. Graphical abstract Photodegradation of congo red over Cu-loaded Fe 3 O 4 @TiO 2 nanoparticles.

Multicharged Ion Promoted Desorption (MIPD) of Reaction Co-Products

DTIC Science & Technology

2015-02-13

measurements of surface modifications using mass spectrometry, Raman spectroscopy and XPS were made to 1. REPORT DATE (DD-MM-YYYY) 4. TITLE AND...desorption and ex-situ measurements of surface modifications using mass spectrometry, Raman spectroscopy and XPS were made to determine ion-induced...irradiations were made with the samples at normal incidence to the incoming beams and post-analysis of these samples was achieved using Raman spectroscopy. It

XPS and biocompatibility studies of titania film on anodized NiTi shape memory alloy.

PubMed

Chu, C L; Wang, R M; Hu, T; Yin, L H; Pu, Y P; Lin, P H; Dong, Y S; Guo, C; Chung, C Y; Yeung, K W K; Chu, Paul K

2009-01-01

A dense titania film is fabricated in situ on NiTi shape memory alloy (SMA) by anodic oxidation in a Na(2)SO(4) electrolyte. The microstructure of the titania film and its influence on the biocompatibility of NiTi SMA are investigated by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICPMS), hemolysis analysis, and platelet adhesion test. The results indicate that the titania film has a Ni-free zone near the surface and can effectively block the release of harmful Ni ions from the NiTi substrate in simulated body fluids. Moreover, the wettability, hemolysis resistance, and thromboresistance of the NiTi sample are improved by this anodic oxidation method.

Intrinsic ferromagnetism in nanocrystalline Mn-doped ZnO depending on Mn concentration.

PubMed

Subramanian, Munisamy; Tanemura, Masaki; Hihara, Takehiko; Soga, Tetsuo; Jimbo, Takashi

2011-04-01

The physical properties of Zn(1-x)Mn(x)O nanoparticles synthesized by thermal decomposition are extensively investigated by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Raman light scattering and Hysteresis measurements. XRD and XPS spectra reveal the absence of secondary phase in nanocrystalline ZnO doped with 5% or less Mn; and, later confirms that the valance state of Mn to be 2+ for all the samples. Raman spectra exhibit a peak at 660 cm(-1) which we attribute to the intrinsic lattice defects of ZnO with increasing Mn concentration. Overall, our results demonstrate that ferromagnetic properties can be realized while Mn-doped ZnO obtained in the nanocrystalline form.

Synthesis of TiN/a-Si3N4 thin film by using a Mather type dense plasma focus system

NASA Astrophysics Data System (ADS)

Hussain, T.; R., Ahmad; Khalid, N.; A. Umar, Z.; Hussnain, A.

2013-05-01

A 2.3 kJ Mather type pulsed plasma focus device was used for the synthesis of a TiN/a-Si3N4 thin film at room temperature. The film was characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The XRD pattern confirms the growth of polycrystalline TiN thin film. The XPS results indicate that the synthesized film is non-stoichiometric and contains titanium nitride, silicon nitride, and a phase of silicon oxy-nitride. The SEM and AFM results reveal that the surface of the synthesized film is quite smooth with 0.59 nm roughness (root-mean-square).

Surface Analysis of 4-Aminothiophenol Adsorption at Polycrystalline Platinum Electrodes

NASA Technical Reports Server (NTRS)

Rosario-Castro, Belinda I.; Fachini, Estevao R.; Contes, Enid J.; Perez-Davis, Marla E.; Cabrera, Carlos R.

2008-01-01

Formation of self-assembled monolayer (SAM) of 4-aminothiophenol (4-ATP) on polycrystalline platinum electrodes has been studied by surface analysis and electrochemistry techniques. The 4-ATP monolayer was characterized by cyclic voltammetry (CV), Raman spectroscopy, reflection absorption infrared (RAIR) spectroscopy, and X-ray photoelectron spectroscopy (XPS). Cyclic voltammetry (CV) experiments give an idea about the packing quality of the monolayer. RAIR and Raman spectra for 4-ATP modified platinum electrodes showed the characteristic adsorption bands for neat 4-ATP indicating the adsorption of 4-ATP molecules on platinum surface. The adsorption on platinum was also evidenced by the presence of sulfur and nitrogen peaks by XPS survey spectra of the modified platinum electrodes. High resolution XPS studies and RAIR spectrum for platinum electrodes modified with 4-ATP indicate that molecules are sulfur-bonded to the platinum surface. The formation of S-Pt bond suggests that ATP adsorption gives up an amino terminated SAM. Thickness of the monolayer was evaluated via angle-resolved XPS (AR-XPS) analyses. Derivatization of 4-ATP SAM was performed using 16-Br hexadecanoic acid.

Functionalization to control microstructural, optical, electronic and wetting properties of metal oxide surfaces

NASA Astrophysics Data System (ADS)

Singh, Jagdeep

This thesis focuses on engineering the surface chemistry of oxide surfaces in order to control their microstructural, optical, electronic and wetting properties. Several different types of experiments have been performed to tailor the properties of silicon oxide, titanium dioxide, and zinc oxide surfaces. Applications of this work include organic electronics, sensors and nanomanufacturing. Adsorption of 3-mercaptopropyltrimethoxysilane (MPS) on hydroxylated silicon oxide substrates by immersion in MPS solution or exposure to MPS vapor has been compared using X-ray photoelectron spectroscopy (XPS). To aid the interpretation, MPS has also been cryogenically condensed in ultrahigh vacuum (UHV) onto gold surfaces. Condensation of MPS vapor on gold in the absence of water does not result in MPS polymerization, as evidenced by multilayer desorption upon warming to room temperature. The C1s XPS spectrum has been used to infer the relative abundance of methoxy groups. Vapor-deposition on hydroxylated silicon oxide leads to an unpolymerized MPS monolayer consisting of molecules with two methoxy groups. UV induced hydrophilicity of titanium dioxide surfaces could possibly be used to provide a means of registration and alignment in high-rate nanomanufacturing applications or to induce transfer of nanoelements. In order to understand the nature and magnitude of intermolecular forces, force-distance curves have been measured on TiO2. Toward the goal of possibly using light to induce nanoparticle transfer, force curves have been recorded using an SiO2 colloidal probe before and after irradiating the TiO 2 surface with UV light. In order to eliminate the effects of capillary forces, the relative humidity has been kept below 1% by flowing either N 2 or N2/O2 (1:1) into the AFM chamber. In a dry nitrogen environment, no difference is observed in adhesive forces measured with and without UV exposure. Gold-coated atomic force microscope (AFM) tips functionalized with amine-, hydroxyl, carboxylic acid, and methyl-terminated alkanethiol molecules have been used to probe the adhesive forces of polystyrene and poly(acrylic acid) films in dry air (relative humidity < 0.5%). XPS and contact angle measurements confirm the quality and uniformity of similarly treated gold surfaces and the polymer films. XPS indicates that the amine-functionalized thiol films are protonated and comprised of multilayers. Toward the goal of modifying its optical properties, ZnO nanorod surfaces have been modified using 3-mercaptopropyltriethoxysilane (MPTES) and 1-propanethiol (PPT), and XPS has been used to investigate the changes occurring on the nanorods after surface modification. XPS reveals that in the case of MPTES-modified nanorods, bonding occurs via both S-Zn and Si-O-Zn bond formation. For comparison, 3-mercaptopropyltrimethoxysilane (MPTMS), dodecanethiol and methanethiol have been adsorbed on sputter-cleaned Zn-terminated ZnO (0001) in ultrahigh vacuum (UHV). In this case, XPS indicates that bonding of thiols on ZnO surfaces occurs via S-Zn bond formation. Photoluminescence spectroscopy has been used to study the effect of surface functionalization on the optical properties of the nanorods. MPTES- and PPT-functionalized nano-ZnO show an increase in intensity of the UV emission peak relative to the unfunctionalized nanorods due to reduced probability of surface dependent non-radiative processes. A decrease in the visible peak in both cases is believed to be due to passivation of surface defects. A simple method for encapsulating zinc oxide nanoparticles within an organic matrix has been discovered that consists of dispersing them in an ethanolic solution, adding an organothiol and stirring while heating. Electron microscopy, photoemission, Raman spectroscopy and thermal gray metric analyses demonstrate that partial dissolution of the oxide occurs accompanied by encapsulation within a matrix consisting of a 1:2 zinc-thiol complex. Using this methodology, it is possible to surround ZnO within diverse matrices, including fluorescent ones. (Abstract shortened by UMI.)

Activation of Magnesium Lignosulfonate and Kraft Lignin: Influence on the Properties of Phenolic Resin-Based Composites for Potential Applications in Abrasive Materials

PubMed Central

Klapiszewski, Lukasz; Jamrozik, Artur; Strzemiecka, Beata; Matykiewicz, Danuta; Voelkel, Adam; Jesionowski, Teofil

2017-01-01

Magnesium lignosulfonate and kraft lignin were activated by different oxidizing agents for use in phenolic resin composites used for the production of abrasive components. The physicochemical properties of the oxidized materials were analyzed by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), dynamic mechanical-thermal analysis (DMTA) and inverse gas chromatography (IGC). The homogeneity of the model abrasive composites containing the studied products was assessed based on observations obtained using a scanning electron microscope (SEM). FTIR and XPS analysis of the oxidized products indicated that the activation process leads mainly to the formation of carbonyl groups. The IGC technique was used to assess changes in the surface energy and the acid–base properties of the studied biopolymers. The changes in the acid–base properties suggest that more groups acting as electron donors appear on the oxidized surface of the materials. DMTA studies showed that the model composites with 5% magnesium lignosulfonate oxidized by H2O2 had the best thermomechanical properties. Based on the results it was possible to propose a hypothetical mechanism of the oxidation of the natural polymers. The use of such oxidized products may improve the thermomechanical properties of abrasive articles. PMID:28594358

Preparation of Rh/Ag bimetallic nanoparticles as effective catalyst for hydrogen generation from hydrolysis of KBH4

NASA Astrophysics Data System (ADS)

Huang, Liang; Jiao, Chengpeng; Wang, Liqiong; Huang, Zili; Liang, Feng; Liu, Simin; Wang, Yuhua; Zhang, Haijun; Zhang, Shaowei

2018-01-01

ISOBAM-104 protected Rh/Ag bimetallic nanoparticles (NPs) with average diameter less than 3.0 nm were synthesized by a co-reduction method. Ultraviolet-visible spectroscopy, transmission electron microscopy (TEM), high-resolution TEM and x-ray photoelectron spectroscopy (XPS) were employed to characterize the structure, particle size, and electronic structure of the prepared bimetallic NPs. The catalytic activities of prepared bimetallic NPs for hydrogen generation from hydrolysis of a basic KBH4 solution were evaluated in detail. The results indicated that as-prepared Rh/Ag bimetallic NPs showed a higher catalytic activity than corresponding monometallic NPs. Among all the monometallic NPs and bimetallic NPs, Rh80Ag20 bimetallic NPs exhibited the highest catalytic activity with a value of 6010 mol-H2·h-1·mol-catalyst-1 at pH = 12 and 303 K. The high catalytic activities of Rh/Ag bimetallic NPs could be attributed to presence of negatively charged Rh atoms and positively charged Ag atoms, which is supported by the results of XPS and density functional theory calculation. Based on the kinetic study, the apparent activation energy for the hydrolysis reaction of the basic KBH4 solution catalyzed by Rh80Ag20 bimetallic NPs was about 47.0 ± 3.9 kJ mol-1.

Synthesis of graphene oxide and reduced graphene oxide by needle platy natural vein graphite

NASA Astrophysics Data System (ADS)

Rathnayake, R. M. N. M.; Wijayasinghe, H. W. M. A. C.; Pitawala, H. M. T. G. A.; Yoshimura, Masamichi; Huang, Hsin-Hui

2017-01-01

Among natural graphite varieties, needle platy vein graphite (NPG) has very high purity. Therefore, it is readily used to prepare graphene oxide (GO) and reduced graphene oxide (rGO). In this study, GO and rGO were prepared using chemical oxidation and reduction process, respectively. The synthesized materials were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectroscopy. XRD studies confirmed the increase of the interlayer spacing of GO and rGO in between 3.35 to 8.66 A°. AFM studies showed the layer height of rGO to be 1.05 nm after the reduction process. TEM micrographs clearly illustrated that the prepared GO has more than 25 layers, while the rGO has only less than 15 layers. Furthermore, the effect of chemical oxidation and reduction processes on surface morphology of graphite were clearly observed in FESEM micrographs. The calculated RO/C of GO and rGO using XPS analysis are 5.37% and 1.77%, respectively. The present study revealed the successful and cost effective nature of the chemical oxidation, and the reduction processes for the production of GO and rGO out of natural vein graphite.

Graphite intercalated polyaniline composite with superior anticorrosive and hydrophobic properties, as protective coating material on steel surfaces

NASA Astrophysics Data System (ADS)

Rathnayake, R. M. N. M.; Mantilaka, M. M. M. G. P. G.; Hara, Masanori; Huang, Hsin-Hui; Wijayasinghe, H. W. M. A. C.; Yoshimura, Masamichi; Pitawala, H. M. T. G. A.

2017-07-01

Solid polymer composite systems are widely being used for potential technological applications in secondary energy sources and electrochromic devices. In this study, we synthesized and characterized a composite material composed of polyaniline (PANI) and natural needle platy (NPG) vein graphite. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), cyclic voltammetry (CV), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), micro-Raman analysis, thermogravimetric and differential thermal analysis (TGA/DTA), transmission electron microscopy (TEM) were used to study the structural and electrochemical properties of the prepared PANI/NPG graphite composite. XPS, FTIR, and micro-Raman analysis confirmed the existence of relevant functional groups and bonding in the prepared PANI/NPG composite material. The composite shows a very low corrosion rate, approximately 29 μm per year, and high hydrophobicity on steel surfaces, which helps to prevent the corrosion due to O2 penetration towards the metal surface. It indicates that the composite can be used as a high potential surface coating material to anticorrosion. The specific capacitance of PANI/NPG composite is 833.3 F g-1, which is higher than that of PANI. This synergistic electrical performance result proves the prepared PANI/NPG graphite composite as a suitable protective coating material for steel surfaces.

New quaternary thallium indium germanium selenide TlInGe2Se6: Crystal and electronic structure

NASA Astrophysics Data System (ADS)

Khyzhun, O. Y.; Parasyuk, O. V.; Tsisar, O. V.; Piskach, L. V.; Myronchuk, G. L.; Levytskyy, V. O.; Babizhetskyy, V. S.

2017-10-01

Crystal structure of a novel quaternary thallium indium germanium selenide TlInGe2Se6 was investigated by means of powder X-ray diffraction method. It was determined that the compound crystallizes in the trigonal space group R3 with the unit cell parameters a = 10.1798(2) Å, c = 9.2872(3) Å. The relationship with similar structures was discussed. The as-synthesized TlInGe2Se6 ingot was tested with X-ray photoelectron spectroscopy (XPS) and X-ray emission spectroscopy (XES). In particular, the XPS valence-band and core-level spectra were recorded for initial and Ar+ ion-bombarded surfaces of the sample under consideration. The XPS data allow for statement that the TlInGe2Se6 surface is rigid with respect to Ar+ ion-bombardment. Particularly, Ar+ ion-bombardment (3.0 keV, 5 min duration, ion current density fixed at 14 μA/cm2) did not cause substantial modifications of stoichiometry in topmost surface layers. Furthermore, comparison on a common energy scale of the XES Se Kβ2 and Ge Kβ2 bands and the XPS valence-band spectrum reveals that the principal contributions of the Se 4p and Ge 4p states occur in the upper and central portions of the valence band of TlInGe2Se6, respectively, with also their substantial contributions in other portions of the band. The bandgap energy of TlInGe2Se6 at the level of αg=103 cm-1 is equal to 2.38 eV at room temperature.

Local symmetry breaking in SnO2 nanocrystals with cobalt doping and its effect on optical properties.

PubMed

Roy, S; Joshi, Amish G; Chatterjee, S; Ghosh, Anup K

2018-06-07

X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to study the structural and morphological characteristics of cobalt doped tin(iv) oxide (Sn1-xCoxO2; 0 ≤ x ≤ 0.04) nanocrystals synthesized by a chemical co-precipitation technique. Electronic structure analysis using X-ray photoemission spectroscopy (XPS) shows the formation of tin interstitials (Sni) and reduction of oxygen vacancies (VO) in the host lattice on Co doping and that the doped Co exists in mixed valence states of +2 and +3. Using XRD, the preferential position of the Sni and doped Co in the unit cell of the nanocrystals have been estimated. Rietveld refinement of XRD data shows that samples are of single phase and variation of lattice constants follows Vegard's law. XRD and TEM measurements show that the crystallite size of the nanocrystals decrease with increase in Co doping concentration. SAED patterns confirm the monocrystalline nature of the samples. The study of the lattice dynamics using Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy shows the existence of many disorder activated forbidden optical phonon modes, along with the corresponding classical modes, signifying Co induced local symmetry breaking in the nanocrystals. UV-Vis spectroscopy shows that the optical band gap has red shifted with increase in doping concentration. The study of Urbach energy confirms the increase in disorder in the nanocrystals with Co doping. Local symmetry breaking induced UV emission along with violet, blue and green luminescence has been observed from the PL study. The spectral contribution of UV emission decreases and green luminescence increases with increase in doping. Using PL, in conjunction with Raman spectroscopy, the type of oxygen vacancy induced in the nanocrystals on Co doping has been confirmed and the position of the defect levels in the forbidden zone (w.r.t. the optical band gap) has been studied.

Antioxidation performance of poly(vinyl alcohol) modified poly(vinylidene fluoride) membranes

NASA Astrophysics Data System (ADS)

Wang, Daohui; Li, Xianfeng; Li, Qing; Liu, Zhen; Li, Nana; Huang, Qinglin; Zhang, Yufeng; Xiao, Changfa

2018-03-01

Commercial poly(vinylidene fluoride) (PVDF) membranes were modified by dip-coating and crosslinking hydrophilic poly(vinyl alcohol) (PVA) on the membrane surface. The antioxidation performance of the modified PVDF membranes was evaluated via exposing the modified membranes to sodium hypochlorite and potassium permanganate solutions for 5-30 days, respectively. The evaluation was based on the influences of the two oxidants on the permeability, rejection, and hydrophility of the modified membranes, which were characterized by water flux, ink rejection, water contact angle, x-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy, and x-ray diffraction (XRD) measurements. The XPS and water contact angle results show that the hydrophilicity of PVDF membranes was significantly improved when PVA was crosslinked on the surface of PVDF membranes. When the modified membranes had been treated with sodium hypochlorite or potassium permanganate for 30 days, the permeability and hydrophilicity were basically maintained and the rejection was slightly decreased. XPS and XRD indicated that some of PVAs coated on the membrane surface could be oxidized and peeled.

Low work function, stable thin films

DOEpatents

Dinh, Long N.; McLean, II, William; Balooch, Mehdi; Fehring, Jr., Edward J.; Schildbach, Marcus A.

2000-01-01

Generation of low work function, stable compound thin films by laser ablation. Compound thin films with low work function can be synthesized by simultaneously laser ablating silicon, for example, and thermal evaporating an alkali metal into an oxygen environment. For example, the compound thin film may be composed of Si/Cs/O. The work functions of the thin films can be varied by changing the silicon/alkali metal/oxygen ratio. Low work functions of the compound thin films deposited on silicon substrates were confirmed by ultraviolet photoelectron spectroscopy (UPS). The compound thin films are stable up to 500.degree. C. as measured by x-ray photoelectron spectroscopy (XPS). Tests have established that for certain chemical compositions and annealing temperatures of the compound thin films, negative electron affinity (NEA) was detected. The low work function, stable compound thin films can be utilized in solar cells, field emission flat panel displays, electron guns, and cold cathode electron guns.

Freeze-drying synthesis of three-dimensional porous LiFePO4 modified with well-dispersed nitrogen-doped carbon nanotubes for high-performance lithium-ion batteries

NASA Astrophysics Data System (ADS)

Tu, Xiaofeng; Zhou, Yingke; Song, Yijie

2017-04-01

The three-dimensional porous LiFePO4 modified with uniformly dispersed nitrogen-doped carbon nanotubes has been successfully prepared by a freeze-drying method. The morphology and structure of the porous composites are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), and the electrochemical performances are evaluated using the constant current charge/discharge tests, cyclic voltammetry and electrochemical impedance spectroscopy. The nitrogen-doped carbon nanotubes are uniformly dispersed inside the porous LiFePO4 to construct a superior three-dimensional conductive network, which remarkably increases the electronic conductivity and accelerates the diffusion of lithium ion. The porous composite displays high specific capacity, good rate capability and excellent cycling stability, rendering it a promising positive electrode material for high-performance lithium-ion batteries.

Composite materials obtained by the ion-plasma sputtering of metal compound coatings on polymer films

NASA Astrophysics Data System (ADS)

Khlebnikov, Nikolai; Polyakov, Evgenii; Borisov, Sergei; Barashev, Nikolai; Biramov, Emir; Maltceva, Anastasia; Vereshchagin, Artem; Khartov, Stas; Voronin, Anton

2016-01-01

In this article, the principle and examples composite materials obtained by deposition of metal compound coatings on polymer film substrates by the ion-plasma sputtering method are presented. A synergistic effect is to obtain the materials with structural properties of the polymer substrate and the surface properties of the metal deposited coatings. The technology of sputtering of TiN coatings of various thicknesses on polyethylene terephthalate films is discussed. The obtained composites are characterized by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), atomic force microscopy (AFM), and scanning tunneling microscopy (STM) is shown. The examples of application of this method, such as receiving nanocomposite track membranes and flexible transparent electrodes, are considered.

XPS studies of structure-induced radiation effects at the Si/SiO2 interface. [X ray Photoelectron Spectroscopy

NASA Technical Reports Server (NTRS)

Grunthaner, F. J.; Lewis, B. F.; Zamini, N.; Maserjian, J.; Madhukar, A.

1980-01-01

The interfacial structures of radiation hard and soft oxides grown by dry and wet processes on silicon substrates have been examined by high-resolution X-ray photoelectron spectroscopy. It is found that the primary difference in the local atomic structure at the Si/SiO2 interface is the significantly higher concentration of strained 120 deg SiO2 bonds and SiO interfacial species in soft samples. Results of in situ radiation damage experiments using low energy electrons (0-20 eV) are reported which correlate with the presence of a strained layer of SiO2 (20 A) at the interface. The results are interpreted in terms of a structural model for hole and electron trap generation by ionizing radiation.

Morphology and Chemical Composition of soot particles emitted by Wood-burning Cook-Stoves: a HRTEM, XPS and Elastic backscattering Studies.

NASA Astrophysics Data System (ADS)

Carabali-Sandoval, G. A., Sr.; Castro, T.; Peralta, O.; De la Cruz, W.; Días, J.; Amelines, O.; Rivera-Hernández, M.; Varela, A.; Muñoz-Muñoz, F.; Policroniades, R.; Murillo, G.; Moreno, E.

2014-12-01

The morphology, microstructure and the chemical composition on surface of soot particles were studied by using high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and elastic backscattering spectrometry. In order to obtain freshly soot particles emitted by home-made wood-burning cook stoves, copper grids for Transmission Electron Microscope (TEM) were placed on the last two of an 8-stages MOUDI cascade impactor. The analysis of HRTEM micrographs revealed the nanostructure and the particle size of soot particles. The XPS survey spectra show a large carbon peak around 285 eV and the oxygen signal at 533 eV. Some differences observed in the carbon/oxygen (C/O) ratio of the particles probably depend on the combustion process efficiency of each cook-stove analyzed. The C-1s XPS spectra show an asymmetric broad peak and other with low intensity that corresponds to sp2 and sp3hybridization, which were fitted with a convolution using Gaussian functions. Elastic backscattering technique allows a chemical elemental analysis of samples and confirms the presence of C, O and Si observed by XPS. Additionally, the morphological properties of soot aggregates were analyzed calculating the border-based fractal dimension (Df). Particles exhibit complex shapes with high values of Df. Also, real-time absorption (σabs) and scattering (σsct) coefficients of fine (with aerodynamic diameter < 2.5 µm) soot particles were measured. The trend in σabs and σsct indicate that the cooking process has two important combustion stages which varied in its flaming strength, being vigorous in the first stage and soft in the second one.

X-ray Photoelectron Spectroscopy study of CaV1-xMoxO3-δ

NASA Astrophysics Data System (ADS)

Belyakov, S. A.; Kuznetsov, M. V.; Shkerin, S. N.

2018-06-01

An investigation was carried out on perovskite-based derivatives of CaV1-xMoxO3-δ using X-ray Photoelectron Spectroscopy (XPS). According to the XRD pattern, the area of homogeneity covers the region from x = 0 to x = 0.6. Wide XPS-peaks of Ca, V, Mo and O are observed, signalling that elements are presented in multiple states. A model for explaining the large chemical shifts of XPS peaks due to different charging effects on different parts of the sample surface is proposed.

Growth of an Ultrathin Zirconia Film on Pt3Zr Examined by High-Resolution X-ray Photoelectron Spectroscopy, Temperature-Programmed Desorption, Scanning Tunneling Microscopy, and Density Functional Theory.

PubMed

Li, Hao; Choi, Joong-Il Jake; Mayr-Schmölzer, Wernfried; Weilach, Christian; Rameshan, Christoph; Mittendorfer, Florian; Redinger, Josef; Schmid, Michael; Rupprechter, Günther

2015-02-05

Ultrathin (∼3 Å) zirconium oxide films were grown on a single-crystalline Pt 3 Zr(0001) substrate by oxidation in 1 × 10 -7 mbar of O 2 at 673 K, followed by annealing at temperatures up to 1023 K. The ZrO 2 films are intended to serve as model supports for reforming catalysts and fuel cell anodes. The atomic and electronic structure and composition of the ZrO 2 films were determined by synchrotron-based high-resolution X-ray photoelectron spectroscopy (HR-XPS) (including depth profiling), low-energy electron diffraction (LEED), scanning tunneling microscopy (STM), and density functional theory (DFT) calculations. Oxidation mainly leads to ultrathin trilayer (O-Zr-O) films on the alloy; only a small area fraction (10-15%) is covered by ZrO 2 clusters (thickness ∼0.5-10 nm). The amount of clusters decreases with increasing annealing temperature. Temperature-programmed desorption (TPD) of CO was utilized to confirm complete coverage of the Pt 3 Zr substrate by ZrO 2 , that is, formation of a closed oxide overlayer. Experiments and DFT calculations show that the core level shifts of Zr in the trilayer ZrO 2 films are between those of metallic Zr and thick (bulklike) ZrO 2 . Therefore, the assignment of such XPS core level shifts to substoichiometric ZrO x is not necessarily correct, because these XPS signals may equally well arise from ultrathin ZrO 2 films or metal/ZrO 2 interfaces. Furthermore, our results indicate that the common approach of calculating core level shifts by DFT including final-state effects should be taken with care for thicker insulating films, clusters, and bulk insulators.

Characterization of iron surface modified by 2-mercaptobenzothiazole self-assembled monolayers

NASA Astrophysics Data System (ADS)

Feng, Yuanyuan; Chen, Shenhao; Zhang, Honglin; Li, Ping; Wu, Ling; Guo, Wenjuan

2006-12-01

A self-assembled monolayer of 2-mercaptobenzothiazole (MBT) adsorbed on the iron surface was prepared. The films were characterized by electrochemical impedance spectroscopy (EIS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared reflection spectroscopy (FT-IR) and scanning electron microscopy (SEM). Besides, the microcalorimetry method was utilized to study the self-assembled process on iron surface and the adsorption mechanism was discussed from the power-time curve. The results indicated that MBT was able to form a film spontaneously on iron surface and the presence of it could protect iron from corrosion effectively. However, the assembling time and the concentration influence the protection efficiency. Quantum chemical calculations, according to which adsorption mechanism was discussed, could explain the experimental results to some extent.

Catalyst-free growth of Al-doped SnO2 zigzag-nanobelts for low ppm detection of organic vapours

NASA Astrophysics Data System (ADS)

Sinha, Sudip Kumar; Ghosh, Saptarshi

2016-10-01

In this effort, we report on development of specific sensors dedicated for detection of two of these volatiles, namely ethanol and acetone, below the prescribed statutory limits. Single crystalline Al-doped SnO2 zigzag nanobelt structures were deposited on Si substrate by a catalyst-free thermal evaporation method. The Al-doped SnO2 zigzag nanostructures exhibit high sensitivity and repeatability together with coveted features like fast response and excellent stability. Structural attributes involving the crystal quality and morphology of Al-doped SnO2 zigzag nanobelts were analyzed using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy and transmission electron microscopy. The microscopic images revealed formation of randomly oriented 'zigzag-like' nanobelts with characteristic width between 60 nm and 200 nm and length of 50-300 μm. The Al-doping was observed to have a discerning effect in enhancing the sensitivity in comparison to the pristine nanowires by creating excess oxygen vacancies in the crystal lattice, confirmed through XPS and PL spectra.

Synthesis of linear low-density polyethylene-g-poly (acrylic acid)-co-starch/organo-montmorillonite hydrogel composite as an adsorbent for removal of Pb(ΙΙ) from aqueous solutions.

PubMed

Irani, Maryam; Ismail, Hanafi; Ahmad, Zulkifli; Fan, Maohong

2015-01-01

The purpose of this work is to remove Pb(II) from the aqueous solution using a type of hydrogel composite. A hydrogel composite consisting of waste linear low density polyethylene, acrylic acid, starch, and organo-montmorillonite was prepared through emulsion polymerization method. Fourier transform infrared spectroscopy (FTIR), Solid carbon nuclear magnetic resonance spectroscopy (CNMR)), silicon(-29) nuclear magnetic resonance spectroscopy (Si NMR)), and X-ray diffraction spectroscope ((XRD) were applied to characterize the hydrogel composite. The hydrogel composite was then employed as an adsorbent for the removal of Pb(II) from the aqueous solution. The Pb(II)-loaded hydrogel composite was characterized using Fourier transform infrared spectroscopy (FTIR)), scanning electron microscopy (SEM)), and X-ray photoelectron spectroscopy ((XPS)). From XPS results, it was found that the carboxyl and hydroxyl groups of the hydrogel composite participated in the removal of Pb(II). Kinetic studies indicated that the adsorption of Pb(II) followed the pseudo-second-order equation. It was also found that the Langmuir model described the adsorption isotherm better than the Freundlich isotherm. The maximum removal capacity of the hydrogel composite for Pb(II) ions was 430mg/g. Thus, the waste linear low-density polyethylene-g-poly (acrylic acid)-co-starch/organo-montmorillonite hydrogel composite could be a promising Pb(II) adsorbent. Copyright © 2014. Published by Elsevier B.V.

Monitoring N3 dye adsorption and desorption on TiO2 surfaces: a combined QCM-D and XPS study.

PubMed

Wayment-Steele, Hannah K; Johnson, Lewis E; Tian, Fangyuan; Dixon, Matthew C; Benz, Lauren; Johal, Malkiat S

2014-06-25

Understanding the kinetics of dye adsorption and desorption on semiconductors is crucial for optimizing the performance of dye-sensitized solar cells (DSSCs). Quartz crystal microbalance with dissipation monitoring (QCM-D) measures adsorbed mass in real time, allowing determination of binding kinetics. In this work, we characterize adsorption of the common RuBipy dye N3 to the native oxide layer of a planar, sputter-coated titanium surface, simulating the TiO2 substrate of a DSSC. We report adsorption equilibrium constants consistent with prior optical measurements of N3 adsorption. Dye binding and surface integrity were also verified by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy (XPS). We further study desorption of the dye from the native oxide layer on the QCM sensors using tetrabutylammonium hydroxide (TBAOH), a commonly used industrial desorbant. We find that using TBAOH as a desorbant does not fully regenerate the surface, though little ruthenium or nitrogen is observed by XPS after desorption, suggesting that carboxyl moieties of N3 remain bound. We demonstrate the native oxide layer of a titanium sensor as a valid and readily available planar TiO2 morphology to study dye adsorption and desorption and begin to investigate the mechanism of dye desorption in DSSCs, a system that requires further study.

"Un-annealed and Annealed Pd Ultra-Thin Film on SiC Characterized by Scanning Probe Microscopy and X-ray Photoelectron Spectroscopy"

NASA Technical Reports Server (NTRS)

Lu, W. J.; Shi, D. T.; Elshot, K.; Bryant, E.; Lafate, K.; Chen, H.; Burger, A.; Collins, W. E.

1998-01-01

Pd/SiC has been used as a hydrogen and a hydrocarbon gas sensor operated at high temperature. UHV (Ultra High Vacuum)-Scanning Tunneling Microscopy (STM), Atomic Force Microscopy (AFM) and X-ray Photoelectron Spectroscopy (XPS) techniques were applied to study the relationship between the morphology and chemical compositions for Pd ultra-thin films on SiC (less than 30 angstroms) at different annealing temperatures. Pd ultra-thin film on 6H-SiC was prepared by the RF sputtering method. The morphology from UHV-STM and AFM shows that the Pd thin film was well deposited on SiC substrate, and the Pd was partially aggregated to round shaped participates at an annealing temperature of 300 C. At 400 C, the amount of surface participates decreases, and some strap shape participates appear. From XPS, Pd2Si was formed on the surface after annealing at 300 C, and all Pd reacted with SiC to form Pd2Si after annealing at 400 C. The intensity of the XPS Pd peak decreases enormously at 400 C. The Pd film diffused into SiC, and the Schottky barrier height has almost no changes. The work shows the Pd sicilides/SiC have the same electronic properties with Pd/SiC, and explains why the Pd/SiC sensor still responds to hydrogen at high operating temperatures.

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

Farrokhzadeh, Abdolkarim; Modarresi-Alam, Ali Reza, E-mail: modaresi@chem.usb.ac.ir

Poly [(±)-2-(sec-butyl) aniline]/silica-supported perchloric acid composites were synthesized by combination of poly[(±)-2-sec-butylaniline] base (PSBA) and the silica-supported perchloric acid (SSPA) as dopant solid acid in solid-state. The X-ray photoelectron spectroscopy (XPS) and CHNS results confirm nigraniline oxidation state and complete doping for composites (about 75%) and non-complete for the PSBA·HCl salt (about 49%). The conductivity of samples was (≈0.07 S/cm) in agreement with the percent of doping obtained of the XPS analysis. Also, contact resistance was determined by circular-TLM measurement. The morphology of samples by the scanning electron microscopy (SEM) and their coating were investigated by XPS, SEM-map and energy-dispersivemore » X-ray spectroscopy (EDX). The key benefits of this work are the preparation of conductive chiral composite with the delocalized polaron structure under green chemistry and solid-state condition, the improvement of the processability by inclusion of the 2-sec-butyl group and the use of dopant solid acid (SSPA) as dopant. - Highlights: • The solid-state synthesis of the novel chiral composites of poly[(±)-2-(sec-butyl)aniline] (PSBA) and silica-supported perchloric acid (SSPA). • It takes 120 h for complete deprotonation of PSBA.HCl salt. • Use of SSPA as dopant solid acid for the first time to attain the complete doping of PSBA. • The coating of silica surface with PSBA.« less

CMC-coated Fe3O4 nanoparticles as new MRI probes for hepatocellular carcinoma

NASA Astrophysics Data System (ADS)

Sitthichai, Sudarat; Pilapong, Chalermchai; Thongtem, Titipun; Thongtem, Somchai

2015-11-01

Pure Fe3O4 nanoparticles and Fe3O4 magnetic nanoparticles (MNPs) coated with carboxymethyl cellulose (CMC) were successfully prepared by co-precipitating of FeCl2·4H2O and FeCl3·6H2O in the solutions containing ammonia at 80 °C for 3 h. Phase, morphology, particle-sized distribution, surface chemistry, and weight loss were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) including high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), thermogravimetric analysis (TGA), and Fourier transform infrared (FTIR) spectroscopy. In this research, CMC-coated Fe3O4 MNPs consisting of Fe2+ and Fe3+ ions with 543.3-mM-1 s-1 high relaxivity were detected and were able to be used for magnetic resonance imaging (MRI) application with very good contrast for targeting hepatocellular carcinoma (HCC) without any further vectorization.

Dielectric relaxation and electronic structure of double perovskite Sr{sub 2}FeSbO{sub 6}

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

Dutta, Alo; Sinha, T. P.; Shannigrahi, Santiranjan

2008-09-15

The dielectric property and the electronic structure of a double perovskite, Sr{sub 2}FeSbO{sub 6} (SFS) synthesized by solid state reaction technique are investigated. The x-ray diffraction of the sample taken at room temperature shows cubic phase. The scanning electron micrograph of the sample also confirms the formation of the single phase of the material. We have measured the capacitance and conductance of SFS in a frequency range from 50 Hz to 1 MHz and in a temperature range from 163 to 463 K. A relaxation is observed in the entire temperature range as a gradual decrease in {epsilon}{sup '}({omega}) andmore » as a broad peak in {epsilon}{sup ''}({omega}). The frequency dependent electrical data are analyzed in the framework of conductivity and electric modulus formalisms. The frequencies corresponding to the maxima of the imaginary electric modulus at various temperatures are found to obey an Arrhenius law with an activation energy of 0.74 eV. The Cole-Cole model is used to study the dielectric relaxation of SFS. The scaling behavior of imaginary part of electric modulus suggests that the relaxation describes the same mechanism at various temperatures. The frequency dependent conductivity spectra follow the universal power law. The electronic structure of the SFS is studied by x-ray photoemission spectroscopy (XPS). Its valence band consists mainly of the oxygen 2p-states hybridized with the Fe 3d-states. The XPS spectra are investigated by the first principles full potential linearized augmented plane wave method. The angular momentum projected total and partial density of states obtained from first principles calculation are used to analyze the XPS results of the sample. The calculated electronic structures of SFS are qualitatively similar to those of the XPS spectra in terms of spectral features, energy positions, and relative intensities. The electronic structure calculation reveals that the electrical properties of SFS are dominated by the interaction between transition-metal and oxygen ions.« less

Lab-based ambient pressure X-ray photoelectron spectroscopy from past to present

NASA Astrophysics Data System (ADS)

Arble, Chris; Jia, Meng; Newberg, John T.

2018-05-01

Chemical interactions which occur at a heterogeneous interface between a gas and substrate are critical in many technological and natural processes. Ambient pressure X-ray photoelectron spectroscopy (AP-XPS) is a powerful spectroscopy tool that is inherently surface sensitive, elemental and chemical specific, with the ability to probe sample surfaces in the presence of a gas phase. In this review, we discuss the evolution of lab-based AP-XPS instruments, from the first development by Siegbahn and coworkers up through modern day systems. A comprehensive overview is given of heterogeneous experiments investigated to date via lab-based AP-XPS along with the different instrumental metrics that affect the quality of sample probing. We conclude with a discussion of future directions for lab-based AP-XPS, highlighting the efficacy for this in-demand instrument to continue to expand in its ability to significantly advance our understanding of surface chemical processes under in situ conditions in a technologically multidisciplinary setting.

Structural and mechanical properties of hydroxyapatite coatings formed by ion-beam assisted deposition

NASA Astrophysics Data System (ADS)

Zykova, A.; Safonov, V.; Dudin, S.; Yakovin, S.; Donkov, N.; Ghaemi, M. H.; Szkodo, M.; Antoszkiewicz, M.; Szyfelbain, M.; Czaban, A.

2018-03-01

The ion-beam assisted deposition (IBAD) is an advanced method capable of producing crystalline coatings at low temperatures. We determined the characteristics of hydroxyapatite Ca10(PO4)6(OH)2 target and coatings formed by IBAD using X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and energy dispersive X-ray (EDX). The composition of the coatings’ cross-section and surface was close to those of the target. The XPS spectra showed that the binding energy values of Ca (2p1/2, 2p3/2), P (2p3/2), and O 1s levels are related to the hydroxyapatite phase. The coatings demonstrate an optimal H/E ratio, and a good resistance to scratch tests.

Preparation of K-doped TiO2 nanostructures by wet corrosion and their sunlight-driven photocatalytic performance

NASA Astrophysics Data System (ADS)

Shin, Eunhye; Jin, Saera; Kim, Jiyoon; Chang, Sung-Jin; Jun, Byung-Hyuk; Park, Kwang-Won; Hong, Jongin

2016-08-01

K-doped TiO2 nanowire networks were prepared by the corrosion reaction of Ti nanoparticles in an alkaline (potassium hydroxide: KOH) solution. The prepared nanostructures were characterized by scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) analysis, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, X-ray diffraction (XRD) and photoluminescence (PL) spectra. Their sunlight-driven photocatalytic activity was also investigated with differently charged dye molecules, such as methylene blue, rhodamine B and methyl orange. The adsorption of the dye molecules on the photocatalyst surface would play a critical role in their selective photodegradation under sunlight illumination.

X-ray photoelectron spectroscopy and paramagnetic resonance evidence for shock-induced intramolecular bond breaking in some energetic solids

NASA Astrophysics Data System (ADS)

Owens, F. J.; Sharma, J.

1980-03-01

Solid samples of 1,3,5, trinitro 1,3,5, triazacyclohexane (RDX), trinitrotoluene (TNT), and ammonium nitrate were subjected to shock pulses of strength and duration less than the threshold to cause detonation. The recovered shocked samples were studied by x-ray photoelectron spectroscopy (XPS) and electron paramagnetic resonance (EPR). The results of these measurements indicate that the shock pulse either broke or altered the internal bonds of the molecules of the solid. The results of the shock decomposition are compared with measurements of the uv and slow thermal decomposition of these materials using the same experimental techniques.

Optimization of process factors for self-healing vanadium-based conversion coating on AZ31 magnesium alloy

NASA Astrophysics Data System (ADS)

Li, Kun; Liu, Junyao; Lei, Ting; Xiao, Tao

2015-10-01

A self-healing vanadium-based conversion coating was prepared on AZ31 magnesium alloy. The optimum operating conditions including vanadia solution concentration, pH and treating temperature for obtaining the best corrosion protective vanadia coatings and improved localized corrosion resistance to the magnesium substrate were determined by an orthogonal experiment design. Surface morphology and composition of the resultant conversion coatings were investigated by scanning electron microscope (SEM) and X-ray photoelectron spectroscopy (XPS). The self-healing behavior of the coating was investigated by cross-cut immersion test and electrochemical impedance spectroscopy (EIS) measurements in 3.5% NaCl solution.

Sonochemical fabrication of 8-hydroxyquinoline aluminum (Alq3) nanoflowers with high electrogenerated chemiluminescence.

PubMed

Mao, Chang-Jie; Wang, Dan-Chen; Pan, Hong-Cheng; Zhu, Jun-Jie

2011-03-01

Well-defined Alq(3) nanoflowers were fabricated via a facile and fast sonochemical route. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the structure and shape of the as-prepared product. The results showed that the resulting Alq(3) was composed of nanobelts with thickness about 50 nm, average widths of 200 nm, and length up to 10 μm. The Alq(3) nanoflowers exhibited good electrogenerated chemiluminescence behavior. Copyright © 2010 Elsevier B.V. All rights reserved.

Structure and colossal dielectric permittivity of Ca2TiCrO6 ceramics

NASA Astrophysics Data System (ADS)

Yan-Qing, Tan; Meng, Yan; Yong-Mei, Hao

2013-01-01

A colossal permittivity ceramic material, Ca2TiCrO6, was successfully synthesized by the conventional solid-state reaction, and was characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), x-ray photoemission spectroscopy (XPS) and x-ray diffraction (XRD). Rietveld refinement of XRD data indicated that the material crystallized in orthorhombic structure with space group pbnm. SEM displayed Ca2TiCrO6 ceramic grains packed uniformly with the size range 5-20 µm. XPS analyses indicated that elemental chromium and titanium of the material were in mixed valence. The corresponding dielectric property was tested in the frequency range 1 kHz-1 MHz and the temperature range 213-453 K, and the ceramics exhibited a relaxation-like dielectric behaviour. Importantly, the permittivity of Ca2TiCrO6 could reach 80 000 at 298 K (100 Hz) and was maintained at 40 000 up to 398 K at 1 MHz, which could be attributed to the ion disorder and mixed valence of Cr3+/Cr6+ and Ti3+/Ti4+.

An investigation into the surface heterogeneity of nitric acid oxidized carbon fiber

NASA Astrophysics Data System (ADS)

Woodhead, Andrea L.; de Souza, Mandy L.; Church, Jeffrey S.

2017-04-01

The carbon fiber surface plays a critical role in the performance of carbon fiber composite materials and, thus it is important to have a thorough understanding of the fiber surface. A series of nitric acid treated intermediate modulus carbon fibers with increasing treatment level was prepared and characterized using a range of surface sensitive techniques including Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), X-ray Photoelectron Spectroscopy (XPS) and Raman spectroscopy. The results, which were found to be consistent with increasing treatment levels, were compared to the literature. Raman spectral mapping has been used to investigate the heterogeneity of the carbon fiber surface after nitric acid oxidation. The mapping enabled the effects of surface treatment on carbon fiber to be investigated at a spatial resolution unattainable by XPS and provided chemical structure information not provided by SEM or AFM. The highest level of treatment resulted in the most heterogeneous surface. Raman mapping, while time consuming, can provide valuable information which can lead to an enhanced understanding of the heterogeneity of the carbon fiber surface.

Tribological properties and surface chemistry of silicon carbide at temperatures to 1500 C

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.

1981-01-01

Silicon carbide surfaces were heated to 1500 C in a vacuum and analyzed at room temperature with X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). The basic unit of the surfaces was considered as a plane of a tetrahedron of either SiC4 and CSi4 composition. AES spectra were obtained from 250-1500 C, with an analysis depth of 1 nm revealed the presence of little Si and mostly graphite. XPS analysis depth was 2 nm or less, and Si was found in the second 1 nm. Sliding friction tests with single-crystal silicon carbide in contact with iron in a vacuum were characterized by a stock-slip value. The coefficient of friction increased with increasing temperature up to 400 C, then decreased with increasing temperature from 400-600 C. Reheating surfaces to 800 C after preheating them to that temperature produced no changes in AES readings. It is concluded that the maximum density of silicon and silicon-carbide is at 800 C, and the higher the sliding temperature, the more metal that is transferred.

Electrochemical synthesis and photoelectrochemical properties of grass-like nanostructured α-Fe2O3 photoanodes for use in solar water oxidation

NASA Astrophysics Data System (ADS)

Hanedar, Yesim; Demir, Umit; Oznuluer, Tuba

2016-10-01

Grass-like nanostructured α-Fe2O3 photoelectrodes were prepared for the first time through a simple cathodic electrodeposition method from an oxygenated aqueous solution of Fe3+ at room temperature without using surfactant, capping agents or any other additives. The α-Fe2O3 electrodeposits were characterized by X-ray photoelectron spectroscopy (XPS), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), X-ray diffraction (XRD), UV-vis absorption and photoelectrochemical (PEC) techniques. The SEM and XRD results indicated that the as-deposited α-Fe2O3 are composed of single crystalline nanoleaves. The formation mechanisms of α-Fe2O3 have also been proposed based on a series of cyclic voltammetric and XPS studies. This new electrochemical method is expected to be a useful technique for the fabrication of single crystalline and photoactive α-Fe2O3 nanostructures directly onto the electrode surface, which is required in most applications, such as energy conversion and storage and sensors.

Characterization of fossil remains using XRF, XPS and XAFS spectroscopies

NASA Astrophysics Data System (ADS)

Zougrou, I. M.; Katsikini, M.; Pinakidou, F.; Brzhezinskaya, M.; Papadopoulou, L.; Vlachos, E.; Tsoukala, E.; Paloura, E. C.

2016-05-01

Synchrotron radiation micro-X-Ray Fluorescence (μ-XRF), X-ray photoelectron (XPS) and X-ray Absorption Fine Structure (XAFS) spectroscopies are applied for the study of paleontological findings. More specifically the costal plate of a gigantic terrestrial turtle Titanochelon bacharidisi and a fossilized coprolite of the cave spotted hyena Crocuta crocuta spelaea are studied. Ca L 2,3-edge NEXAFS and Ca 2p XPS are applied for the identification and quantification of apatite and Ca containing minerals. XRF mapping and XAFS are employed for the study of the spatial distribution and speciation of the minerals related to the deposition environment.

XPS studies of MgO based magnetic tunnel junction structures

NASA Astrophysics Data System (ADS)

Read, John; Mather, Phil; Tan, Eileen; Buhrman, Robert

2006-03-01

The very high tunneling magnetoresistance (TMR) obtained in MgO magnetic tunnel junctions (MTJ)^(1,2) motivates the investigation of the electronic properties of the MgO barrier layer and the study of the ferromagnetic metal - MgO interface chemistry. Such large TMR values are predicted by theory due to the high degree of order apparent in the barrier and electrode materials. However, as grown ultra-thin MgO films generally contain defects that can influence electron transport properties through the creation of low energy states within the bulk MgO band-gap. We will report the results of x-ray photoelectron spectroscopy (XPS) studies of (001) textured ultra-thin MgO layers that are prepared by RF magnetron sputtering and electron beam evaporation on ordered ferromagnetic electrodes and in ordered MTJ structures with and without post growth vacuum annealing. XPS spectra for both MgO deposition techniques clearly indicate a surface oxygen species that is likely bound by defects in the oxide^(3) in half-formed junctions and improvements in MgO quality after counter electrode deposition. We will discuss our results regarding the chemical properties of the oxide and its interfaces directed towards possibly providing guidance to engineer improved MgO MTJ devices. [1] S.S.P. Parkin et. al., Nature Materials, 3, 862 (2004). [2] S. Yuasa et. al., Nature Materials, 3, 868 (2004). [3] E. Tan et. al. , Phys. Rev. B. , 71, 161401 (2005).

Orbital alignment at the internal interface of arylthiol functionalized CdSe molecular hybrids

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

Li, Zhi; Schlaf, Rudy, E-mail: schlaf@usf.edu; Mazzio, Katherine A.

Organic-inorganic nanoparticle molecular hybrid materials are interesting candidates for improving exciton separation in organic solar cells. The orbital alignment at the internal interface of cadmium selenide (ArS-CdSe) hybrid materials functionalized with covalently attached arylthiolate moieties was investigated through X-ray photoemission spectroscopy (XPS) and ultraviolet photoemission spectroscopy (UPS). A physisorbed interface between arylthiol (ArSH) ligands and CdSe nanoparticles was also investigated for comparison. This interface was created via a multi-step thin film deposition procedure in-vacuo, where the surface was characterized after each experimental step. This enabled the direct comparison of ArSH/CdSe interfaces produced via physisorption and ArS-CdSe covalently attached hybrid materials,more » which rely on a chemical reaction for their synthesis. All material depositions were performed using an electrospray deposition, which enabled the direct injection of solution-originating molecular species into the vacuum system. This method allows XPS and UPS measurements to be performed immediately after deposition without exposure to the atmosphere. Transmission electron microscopy was used to determine the morphology and particle size of the deposited materials. Ultraviolet-visible spectroscopy was used to estimate the optical band gap of the CdSe nanoparticles and the HOMO-LUMO gap of the ArSH ligands. These experiments showed that hybridization via covalent bonds results in an orbital realignment at the ArSH/CdSe interface in comparison to the physisorbed interface. The orbital alignment within the hybrid caused a favorable electron injection barrier, which likely facilitates exciton-dissociation while preventing charge-recombination.« less

Band line-up determination at p- and n-type Al/4H-SiC Schottky interfaces using photoemission spectroscopy

NASA Astrophysics Data System (ADS)

Kohlscheen, J.; Emirov, Y. N.; Beerbom, M. M.; Wolan, J. T.; Saddow, S. E.; Chung, G.; MacMillan, M. F.; Schlaf, R.

2003-09-01

The band lineup of p- and n-type 4H-SiC/Al interfaces was determined using x-ray photoemission spectroscopy (XPS). Al was deposited in situ on ex situ cleaned SiC substrates in several steps starting at 1.2 Å up to 238 Å nominal film thickness. Before growth and after each growth step, the sample surface was characterized in situ by XPS. The analysis of the spectral shifts indicated that during the initial deposition stages the Al films react with the ambient surface contamination layer present on the samples after insertion into vacuum. At higher coverage metallic Al clusters are formed. The band lineups were determined from the analysis of the core level peak shifts and the positions of the valence bands maxima (VBM) depending on the Al overlayer thickness. Shifts of the Si 2p and C 1s XPS core levels occurred to higher (lower) binding energy for the p-(n-)type substrates, which was attributed to the occurrence of band bending due to Fermi-level equilibration at the interface. The hole injection barrier at the p-type interface was determined to be 1.83±0.1 eV, while the n-type interface revealed an electron injection barrier of 0.98±0.1 eV. Due to the weak features in the SiC valence bands measured by XPS, the VBM positions were determined using the Si 2p peak positions. This procedure required the determination of the Si 2p-to-VBM binding energy difference (99.34 eV), which was obtained from additional measurements.

Fabrication of Total-Dose-Radiation-Hardened (TDRH) SOI wafer with embedded silicon nanoclusters

NASA Astrophysics Data System (ADS)

Wu, Aimin; Wang, Xi; Wei, Xing; Chen, Jing; Chen, Ming; Zhang, Zhengxuan

2009-05-01

Si ion-implantation and post annealing of silicon wafers prior to wafer bonding were used to radiation-harden the thermal oxide layer of Silicon on Insulator structures. After grinding and polishing, Total-Dose-Radiation-Hardened SOI (TDRH-SOI) wafers with several-micron-thick device layers were prepared. Electrical characterization before and after X-ray irradiation showed that the flatband voltage shift induced by irradiation was reduced by this preprocessing. Photoluminescence Spectroscopy (PL), Transmission Electron Microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) results indicated that the improvement of the total dose response of the TDRH-SOI wafer was associated with formation of Si nanoclusters in the implanted oxide layer, suggesting that these were the likely candidates for electron and proton trapping centers that reduce the positive charge buildup effect in the buried oxide.

Removal of aqueous chromium and environmental CO2 by using photocatalytic TiO2 doped with tungsten.

PubMed

Trejo-Valdez, M; Hernández-Guzmán, S R; Manriquez-Ramírez, M E; Sobral, H; Martínez-Gutiérrez, H; Torres-Torres, C

2018-05-15

Removal of hexavalent chromium was accomplished by using photocatalyst materials of TiO 2 doped with tungsten oxide, environmental air as oxygen supply and white light as irradiation source. Dichromate anions in concentration ranges of 50 to 1000 μg/L were removed by means of aqueous dispersions of TiO 2 doped with tungsten. The aqueous chromium analyses were performed by Differential Pulse Voltammetry technique. Additionally, mineralization of CO 2 gas was promoted by the photocatalysis process, as was clearly shown by Raman spectroscopy and X-ray Photoelectron Spectroscopy (XPS) analyses obtained from the TiO 2 samples recovered after photocatalytic experiments. Results of sample analyses by Scanning Electron Microscopy (SEM) and High Resolution Transmission Electron Microscopy (HRTEM) are presented and discussed. Copyright © 2018 Elsevier B.V. All rights reserved.

Enhancement of interaction of L-929 cells with functionalized graphene via COOH+ ion implantation vs. chemical method

PubMed Central

Zhao, Meng-li; Liu, Xiao-qi; Cao, Ye; Li, Xi-fei; Li, De-jun; Sun, Xue-liang; Gu, Han-qing; Wan, Rong-xin

2016-01-01

Low hydrophilicity of graphene is one of the major obstacles for biomaterials application. To create some hydrophilic groups on graphene is addressed this issue. Herein, COOH+ ion implantation modified graphene (COOH+/graphene) and COOH functionalized graphene were designed by physical ion implantation and chemical methods, respectively. The structure and surface properties of COOH+/graphene and COOH functionalized graphene were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and contact angle measurement. Compared with graphene, COOH+/graphene and COOH functionalized graphene revealed improvement of cytocompatibility, including in vitro cell viability and morphology. More importantly, COOH+/graphene exhibited better improvement effects than functionalized graphene. For instance, COOH+/graphene with 1 × 1018 ions/cm2 showed the best cell-viability, proliferation and stretching. This study demonstrated that ion implantation can better improve the cytocompatibility of the graphene. PMID:27845420

Fabrication of a temperature-responsive and recyclable MoS2 nanocatalyst through composting with poly (N-isopropylacrylamide)

NASA Astrophysics Data System (ADS)

Liu, Yan; Chen, Pengpeng; Nie, Wangyan; Zhou, Yifeng

2018-04-01

A temperature-responsive, recyclable nanocatalyst was fabricated by composting the exfoliated molybdenum disulfide (MoS2) nanosheets with poly (N-isopropylacry lamide) (PNIPAM). The structure and morphology of MoS2/PNIPAM nanocatalyst was fully characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), Thermogravimetry analysis (TGA), Scanning electron microscope (SEM) and Transmission electron microscopy (TEM). The temperature-responsive properties of the MoS2/PNIPAM nanocatalyst were confirmed by Dynamic Light Scattering (DLS) and Ultraviolet-visible ((UV-vis)) absorption spectroscopy. The catalytic activities of the MoS2/PNIPAM nanocatalyst were studied using the reduction reaction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) as the model reaction. Results showed that the catalytic activity of the MoS2/PNIPAM nanocatalyst could be regulated by temperature. Furthermore, when the temperature went higher than the low critical solution temperature (LCST) of PNIPAM, the MoS2/PNIPAM nanocatalyst tended to aggregated to form bulk materials from homogeneous suspension.

Dead biomass of Amazon yeast: A new insight into bioremediation and recovery of silver by intracellular synthesis of nanoparticles.

PubMed

Salvadori, Marcia R; Ando, Rômulo A; Nascimento, Cláudio A Oller; Corrêa, Benedito

2017-09-19

This investigation was undertaken to describe a natural process for the removal of silver and the simultaneous recovery of Ag/Ag 2 O nanoparticles by dead biomass of the yeast Rhodotorula mucilaginosa. The removal of silver ions from aqueous solution and the synthesis of Ag/Ag 2 O nanoparticles were analyzed based on physicochemical factors and equilibrium concentration, combined with transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and infrared spectroscopy (FTIR). A successful process for the synthesis of Ag/Ag 2 O nanoparticles was obtained, following the Langmuir isotherm model, showing a high biosorption capacity of silver (49.0 mg g -1 ). The nanoparticles were spherical, had an average size of 11.0 nm, were synthesized intracellularly and capped by yeast proteins. This sustainable protocol is an attractive platform for the industrial-scale production of silver nanoparticles and of a silver nanobiosorbent.

Enhanced metal loading in SBA-15-type catalysts facilitated by salt addition. Synthesis, characterization and catalytic epoxide alcoholysis activity of molybdenum incorporated porous silica

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

Budhi, Sridhar; Peeraphatdit, Chorthip; Pylypenko, Svitlana

2014-02-07

We report a novel method to increase the metal loading in SBA-15 silica matrix via direct synthesis. It was demonstrated through the synthesis and characterization of a series of molybdenum containing SBA-15 mesoporous silica catalysts prepared with and without diammonium hydrogen phosphate (DHP) as an additive. Catalysts prepared with DHP show a 2–3 times increase in incorporation of molybdenum in the silica matrix and pore size enlargement. The synthesized catalysts were characterized using nitrogen sorption, X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma–optical emission spectroscopy (ICP–OES). Themore » catalytic activity of catalysts prepared with DHP for alcoholysis of epoxides was superior than the catalyst prepared without DHP. Alcoholysis of epoxides was demonstrated for a range of alcohols and epoxides under ambient conditions in as little as 30 min with high selectivity.« less

Synthesis, optical properties and efficient photocatalytic activity of CdO/ZnO hybrid nanocomposite

NASA Astrophysics Data System (ADS)

Reddy, Ch Venkata; Babu, B.; Shim, Jaesool

2018-01-01

Pure CdO, ZnO and CdO/ZnO hybrid nanocomposite photocatalyst were synthesized using simple co-precipitation technique and studied in detail. The synthesized photocatalysts were characterized using several measurements such as X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), surface analysis (BET), diffuse reflectance UV-vis spectroscopy, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, FT-IR, TG-DTA and photoluminescence (PL). The XRD results revealed that the hexagonal and cubic crystal structure of CdO and ZnO nanoparticles. The optical response for the composite showed the presence of separate absorption signature for CdO and ZnO in the visible region at about 510 nm and 360 nm respectively. The CdO/ZnO hybrid nanocomposite photocatalyst exhibited enhanced photocatalytic degradation activity compared to pristine CdO and ZnO. The enhanced photocatalytic activity may be due to the higher specific surface area and significantly reduced the electron-hole recombination rate.

The preparation and cathodoluminescence of ZnS nanowires grown by chemical vapor deposition

NASA Astrophysics Data System (ADS)

Huang, Meng-Wen; Cheng, Yin-Wei; Pan, Ko-Ying; Chang, Chen-Chuan; Shieu, F. S.; Shih, Han C.

2012-11-01

Single crystal ZnS nanowires were successfully synthesized in large quantities on Si (1 0 0) substrates by simple thermal chemical vapor deposition without using any catalyst. The morphology, composition, and crystal structure were characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and cathodoluminescence (CL) spectroscopy. SEM observations show that the nanowires have diameters about 20-50 nm and lengths up to several tens of micrometers. XRD and TEM results confirmed that the nanowires exhibited both wurtzite and zinc blende structures with growth directions aligned along [0 0 0 2] and [1 1 1], respectively. The CL spectrum revealed emission bands in the UV and blue regions. The blue emissions at 449 and ˜581 nm were attributed to surface states and impurity-related defects of the nanowires, respectively. The perfect crystal structure of the nanowires indicates their potential applications in nanotechnology and in the fabrication of nanodevices.

Iron Oxide Nanoparticles Employed as Seeds for the Induction of Microcrystalline Diamond Synthesis

PubMed Central

2008-01-01

Iron nanoparticles were employed to induce the synthesis of diamond on molybdenum, silicon, and quartz substrates. Diamond films were grown using conventional conditions for diamond synthesis by hot filament chemical vapor deposition, except that dispersed iron oxide nanoparticles replaced the seeding. X-ray diffraction, visible, and ultraviolet Raman Spectroscopy, energy-filtered transmission electron microscopy , electron energy-loss spectroscopy, and X-ray photoelectron spectroscopy (XPS) were employed to study the carbon bonding nature of the films and to analyze the carbon clustering around the seed nanoparticles leading to diamond synthesis. The results indicate that iron oxide nanoparticles lose the O atoms, becoming thus active C traps that induce the formation of a dense region of trigonally and tetrahedrally bonded carbon around them with the ensuing precipitation of diamond-type bonds that develop into microcrystalline diamond films under chemical vapor deposition conditions. This approach to diamond induction can be combined with dip pen nanolithography for the selective deposition of diamond and diamond patterning while avoiding surface damage associated to diamond-seeding methods.

Low Temperature Ohmic Contact Formation of Ni2Si on N-type 4H-SiC and 6H-SiC

NASA Technical Reports Server (NTRS)

Elsamadicy, A. M.; Ila, D.; Zimmerman, R.; Muntele, C.; Evelyn, L.; Muntele, I.; Poker, D. B.; Hensley, D.; Hirvonen, J. K.; Demaree, J. D.;

Mesomeric Effects of Graphene Modified with Diazonium Salts: Substituent Type and Position Influence its Properties.

PubMed

Bouša, Daniel; Jankovský, Ondřej; Sedmidubský, David; Luxa, Jan; Šturala, Jiří; Pumera, Martin; Sofer, Zdeněk

2015-12-01

In the last decade, graphene and graphene derivatives have become some of the most intensively studied materials. Tuning of the electronic and electrochemical properties of graphene is of paramount importance. In this study, six diazonium-modified graphenes containing different functional groups according to the diazonium salt precursor were investigated. These diazonium moieties have a strong mesomeric (resonance) effect and act as either electron-donating or -withdrawing species. Different graphene precursors, such as thermally and chemically reduced graphenes were studied. All the products were characterized in detail by elemental combustion analysis, FTIR spectroscopy, Raman spectroscopy, high-resolution X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry. Resistivity and zeta potential measurements were consistent with theoretical (DFT) calculations. The results show that chemical modification of graphene by diazotation strongly influences its properties, creating a huge application potential in microelectronics, energy storage and conversion devices, and electrocatalysis. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of trace metals in TSP and PM2.5 materials collected in the Metropolitan Area of Monterrey, Mexico: A characterization study by XPS, ICP-AES and SEM-EDS

NASA Astrophysics Data System (ADS)

González, Lucy T.; Longoria Rodríguez, F. E.; Sánchez-Domínguez, M.; Cavazos, Aleyda; Leyva-Porras, C.; Silva-Vidaurri, L. G.; Askar, Karim Acuña; Kharissov, B. I.; Villarreal Chiu, J. F.; Alfaro Barbosa, J. M.

2017-11-01

The concentration levels of trace metals of toxicological importance were evaluated in the total suspended particles (TSP) and particulate matter smaller than 2.5 μm (PM2.5) collected in the Metropolitan Area of Monterrey (MAM) in Mexico. Samples were characterized by inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy with an energy-dispersive spectroscopy system (SEM-EDS). In addition, the data were statistically treated by the methodology of Pearson Correlation (PC) and Principal Components Analysis (PCA) to identify the possible emitting sources. Surface analysis of the particulate matter (PM) by XPS revealed that the most abundant elements were Ca, Al, Na, Zn, Cu and Mg. The deconvolution of the Ca2p, Zn2p and Cu2p signals showed that the main contributors were CaCO3, ZnO and Cu/Cu2O, respectively. The bulk analysis of the PM by ICP-AES showed Fe, Cu and Zn as the most abundant elements. Fe-rich particles presented two different morphologies: the prismatic particles were associated with a natural origin, while the spherical particles with anthropogenic sources. The Zn and Cu were predominantly observed in the sampling stations with high vehicular traffic, and the emitting sources were associated with the burning of fuels from automobiles and the wear of the tires and brakes. The highest concentration of Pb was detected in the sampling station located near the industrial zones, and its cause was associated with the ceramic and glass industries, the burning of fuel oil in power plants and the production of lead-based batteries for automobiles.

Assessing the oxidation states and structural stability of the Ce analogue of brannerite

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

Aluri, Esther Rani; Bachiu, Lisa M.; Grosvenor, Andrew P.

2017-07-04

The Ce-containing analogue of brannerite (ie, UTi2O6) was previously considered to be stoichiometric (ie, CeTi2O6); however, it has recently been determined that the material is O deficient. This oxygen-deficient material has been suggested to be charged balanced by the presence of a minor concentration of Ce3+ or by the A-site being cation deficient with the Ce oxidation state being 4+. A variety of Ti-containing oxides (including brannerite) have been investigated as potential nuclear wasteforms, and it is necessary to understand the electronic structure of a proposed nuclear wasteform material as well as how the structure responds to radiation from incorporatedmore » waste elements. The radiation resistance of a material can be simulated by ion implantation. The objective of this study was to confirm the Ce oxidation state in the cation- and oxygen-deficient material (ie, Ce0.94Ti2O6 - δ) and to determine how radiation damage affects this material. X-ray photoelectron spectroscopy (XPS) and X-ray absorption near-edge spectroscopy were used to study Ce0.94Ti2O6 - δ before and after being implanted with 2 MeV Au- ions. Analysis of the Ce 3d XPS spectra from the as-synthesized samples by using a previously developed fitting method has unequivocally shown that Ce adopts both 4+ (major) and 3+ (minor) oxidation states, which was confirmed by examination of magnetic susceptibility data. Analysis of XPS and X-ray absorption near-edge spectroscopy spectra from ion-implanted materials showed that both Ce and Ti were reduced because of radiation damage and that the local coordination environments of the cations are greatly affected by radiation damage.« less

Facile fabrication of BiVO4 nanofilms with controlled pore size and their photoelectrochemical performances.

PubMed

Feng, Chenchen; Jiao, Zhengbo; Li, Shaopeng; Zhang, Yan; Bi, Yingpu

2015-12-28

We demonstrate a facile method for the rational fabrication of pore-size controlled nanoporous BiVO(4) photoanodes, and confirmed that the optimum pore-size distributions could effectively absorb visible light through light diffraction and confinement functions. Furthermore, in situ X-ray photoelectron spectroscopy (XPS) reveals more efficient photoexcited electron-hole separation than conventional particle films, induced by light confinement and rapid charge transfer in the inter-crossed worm-like structures.

Pyrolytic synthesis and characterization of N-doped carbon nanoflakes for electrochemical applications

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

Savilov, S.V., E-mail: savilov@chem.msu.ru; N.S. Kurnakov Institute of General and Inorganic Chemistry Of Russian Academy of Sciences, Leninsky avenue, 31, Moscow 119991; Arkhipova, E.A.

2015-09-15

Highlights: • Carbon nanoflakes doped with nitrogen were produced by a pyrolytic technique. • Quarternary, pyrrolic and pyridinic types of nitrogen are confirmed by XPS. • Nitrogen content depends on precursor used and temperature processed. • Specific surface area values decrease with increasing of synthesis duration. • N-doped carbon nanoflakes may be suitable for electrochemical applications. - Abstract: Nitrogen doped carbon nanoflakes, which are very important for many electrochemical applications, were synthesized by pyrolysis of nitrogen containing organic compounds over metal oxide template. Acetonitrile, pyridine and butylamine, which are of different volatility were tested as N-containing precursors. Morphology, structure andmore » chemical composition of the as-synthesized materials were investigated by scanning electron microscopy (SEM), high resolution transmission electron microscopy (TEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). It was found that materials are highly defective and consist of a few malformed graphene layers. X-ray photoelectron spectra reflect the dominant graphitic and pyridinic N-bonding configuration. It was also noted that specific surface area depends on the duration and temperature of the reaction. Increase in duration and temperature led to decrease of the specific surface area from 1000 to 160 m{sup 2}/g, 1170 to 210 m{sup 2}/g and 1180 to 480 m{sup 2}/g for acetonitrile, butylamine and pyridine precursors, respectively.« less

X-Ray Photoelectron Spectroscopy and Ultrahigh Vacuum Contactless Capacitance-Voltage Characterization of Novel Oxide-Free InP Passivation Process Using a Silicon Surface Quantum Well

NASA Astrophysics Data System (ADS)

Takahashi, Hiroshi; Hashizume, Tamotsu; Hasegawa, Hideki

1999-02-01

In order to understand and optimize a novel oxide-free InP passivation process using a silicon surface quantum well, a detailed in situ X-ray photoelectron spectroscopy (XPS) and ultrahigh vacuum (UHV) contactless capacitance-voltage (C-V) study of the interface was carried out. Calculation of quantum levels in the silicon quantum well was performed on the basis of the band lineup of the strained Si3N4/Si/InP interface and the result indicated that the interface should become free of gap states when the silicon layer thickness is below 5 Å. Experimentally, such a delicate Si3N4/Si/InP structure was realized by partial nitridation of a molecular beam epitaxially (MBE) grown pseudomorphic silicon layer using an electron cyclotron resonance (ECR) N2 plasma. The progress of nitridation was investigated in detail by angle-resolved XPS. A newly developed UHV contactless C-V method realized in situ characterization of surface electronic properties of InP at each processing step for passivation. It was found that the interface state density decreased substantially into the 1010 cm-2 eV-1 range by optimizing the nitridation process of the silicon layer. It was concluded that both the surface bond termination and state removal by quantum confinement are responsible for the NSS reduction.

Anatomy of a Visible Light Activated Photocatalyst for Water Splitting

DOE PAGES

Phivilay, Somphonh Peter; Roberts, Charles; Gamalski, Andrew; ...

2018-06-08

The supported mixed oxide (Rh 2-yCr yO 3)/(Ga 1-xZn x)(N 1-xO x) photocatalyst, highly active for splitting of H 2O, was extensively characterized for its bulk and surface properties with the objective of developing fundamental structure-photoactivity relationships. Raman and UV-vis spectroscopy revealed that the molecular and electronic structures, respectively, of the oxynitride (Ga 1-xZn x)(N 1-xO x) support are not perturbed by the deposition of the (Rh 2-yCr yO 3) NPs. Photoluminescence (PL) spectroscopy, however, showed that the oxynitride (Ga 1-xZn x)(N 1-xO x) support is the source of excited electrons/holes and the (Rh 2-yCr yO 3) NPs greatly reducemore » the undesirable recombination of photoexcited electron/holes by acting as efficient electron traps as well as increase the lifetimes of the excitons. High Resolution-XPS and High Sensitivity-LEIS surface analyses reveal that the surfaces of the (Rh 2-yCr yO 3) NPs consist of Rh +3 and Cr +3 mixed oxide species. In Situ AP-XPS help to reveal that the Rh+3 and surface N atoms are involved in water splitting. Dispersed RhOx species on the (Ga 1-xZn x)(N 1-xO x) support and on CrO x NPs were found to be the photocatalytic active sites for H 2 generation and N and Zn sites from the (Ga 1-xZn x)(N 1-xO x) support are the photocatalytic active site for O 2 generation. The current investigation establishes the fundamental structure-photoactivity relationships of these visible light activated photocatalysts.« less

Anatomy of a Visible Light Activated Photocatalyst for Water Splitting

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

Phivilay, Somphonh Peter; Roberts, Charles; Gamalski, Andrew

The supported mixed oxide (Rh 2-yCr yO 3)/(Ga 1-xZn x)(N 1-xO x) photocatalyst, highly active for splitting of H 2O, was extensively characterized for its bulk and surface properties with the objective of developing fundamental structure-photoactivity relationships. Raman and UV-vis spectroscopy revealed that the molecular and electronic structures, respectively, of the oxynitride (Ga 1-xZn x)(N 1-xO x) support are not perturbed by the deposition of the (Rh 2-yCr yO 3) NPs. Photoluminescence (PL) spectroscopy, however, showed that the oxynitride (Ga 1-xZn x)(N 1-xO x) support is the source of excited electrons/holes and the (Rh 2-yCr yO 3) NPs greatly reducemore » the undesirable recombination of photoexcited electron/holes by acting as efficient electron traps as well as increase the lifetimes of the excitons. High Resolution-XPS and High Sensitivity-LEIS surface analyses reveal that the surfaces of the (Rh 2-yCr yO 3) NPs consist of Rh +3 and Cr +3 mixed oxide species. In Situ AP-XPS help to reveal that the Rh+3 and surface N atoms are involved in water splitting. Dispersed RhOx species on the (Ga 1-xZn x)(N 1-xO x) support and on CrO x NPs were found to be the photocatalytic active sites for H 2 generation and N and Zn sites from the (Ga 1-xZn x)(N 1-xO x) support are the photocatalytic active site for O 2 generation. The current investigation establishes the fundamental structure-photoactivity relationships of these visible light activated photocatalysts.« less

Alkali reduction of graphene oxide in molten halide salts: production of corrugated graphene derivatives for high-performance supercapacitors.

PubMed

Abdelkader, Amr M; Vallés, Cristina; Cooper, Adam J; Kinloch, Ian A; Dryfe, Robert A W

2014-11-25

Herein we present a green and facile approach to the successful reduction of graphene oxide (GO) materials using molten halide flux at 370 °C. GO materials have been synthesized using a modified Hummers method and subsequently reduced for periods of up to 8 h. Reduced GO (rGO) flakes have been characterized using X-ray-diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR), all indicating a significantly reduced amount of oxygen-containing functionalities on the rGO materials. Furthermore, impressive electrical conductivities and electrochemical capacitances have been measured for the rGO flakes, which, along with the morphology determined from scanning electron microscopy, highlight the role of surface corrugation in these rGO materials.

Synergistic effect of tartaric acid with 2,6-diaminopyridine on the corrosion inhibition of mild steel in 0.5 M HCl

PubMed Central

Qiang, Yujie; Guo, Lei; Zhang, Shengtao; Li, Wenpo; Yu, Shanshan; Tan, Jianhong

2016-01-01

The inhibitive ability of 2,6-diaminopyridine, tartaric acid and their synergistic effect towards mild steel corrosion in 0.5 M HCl solution was evaluated at various concentrations using potentiodynamic polarization measurements, electrochemical impedance spectroscopy (EIS), and weight loss experiments. Corresponding surfaces of mild steel were examined by atomic force microscope (AFM), field emission scanning electron microscope (FE-SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS) analysis. The experimental results are in good agreement and reveal a favorable synergistic effect of 2,6-diaminopyridine with tartaric acid, which could protect mild steel from corrosion effectively. Besides, quantum chemical calculations and Monte Carlo simulation were used to clarify the inhibition mechanism of the synergistic effect. PMID:27628901

Surface spectroscopy studies of the oxidation behavior of uranium

NASA Astrophysics Data System (ADS)

Bloch, J.; Atzmony, U.; Dariel, M. P.; Mintz, M. H.; Shamir, N.

1982-02-01

Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS) techniques were utilized to study the oxidation behavior of clean uranium surfaces, at very low pressures of various atmospheres (UHV, H 2, O 2, and CO 2), at room temperature. Both for O 2 and CO 2, a precursor chemisorbed oxygen species has been identified at the very initial stage of the oxidation reaction. This chemisorbed oxygen transforms to the oxide form at a rate which depends on the pressure of the oxidizing atmosphere. Residual gaseous carbon compounds which are present even under UHV conditions result in the simultaneous formation of surface carbide which accompanies the initial stage of oxidation. This carbide however decomposes later as oxidation proceeds. Adventitious hydrocarbon adsorption occurs on the formed oxide layer.

A facile and green preparation of reduced graphene oxide using Eucalyptus leaf extract

NASA Astrophysics Data System (ADS)

Li, Chengyang; Zhuang, Zechao; Jin, Xiaoying; Chen, Zuliang

2017-11-01

In this paper, a green and facile synthesis of reduced graphene oxide (GO) by Eucalyptus leaf extract (EL-RGO) was investigated, which was characterized with ultraviolet-visible spectroscopy (UV), Raman spectroscopy, X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and Thermal gravimetric analysis (TG). Eucalyptus leaf extract also play both reducing and capping stabilizing agents prepared EL-RGO as shown a good stability and electrochemical properties. This approach could provide an alternative method to prepare EL-RGO in large-scale production. Moreover, the good electrochemical property and biocompatibility can be used in various applications. In addition, the merit of this study is that both the oxidized products and the reducing agents are environmental friendly by green reduction.

Surface analysis of 316 stainless steel treated with cold atmospheric plasma

NASA Astrophysics Data System (ADS)

Williams, David F.; Kellar, Ewen J. C.; Jesson, David A.; Watts, John F.

2017-05-01

The surface of 316 stainless steel has been modified using cold atmospheric plasma (CAP) to increase the surface free energy (by cleaning the and chemically activating the surface)IN preparation for subsequent processes such as painting, coating or adhesive bonding. The analyses carried out, on CAP treated 316 stainless steel surfaces, includes X-ray photoelectron spectroscopy (XPS), imaging XPS (iXPS), and surface free energy (SFE) analysis using contact angle measurements. The CAP treatment is shown to increase the SFE of as-received 316 stainless steel from ∼39 mJ m-1 to >72 mJ m-1 after a short exposure to the plasma torch. This was found to correlate to a reduction in adventitious carbon, as determined by XPS analysis of the surface. The reduction from ∼90 at% to ∼30% and ∼39 at%, after being plasma treated for 5 min and 15 s respectively, shows that the process is relatively quick at changing the surface. It is suggested that the mechanism that causes the increase in surface free energy is chain scission of the hydrocarbon contamination triggered by free electrons in the plasma plume followed by chemical functionalisation of the metal oxide surface and some of the remaining carbon contamination layer.

Combined UHV/high-pressure catalysis setup for depth-resolved near-surface spectroscopic characterization and catalytic testing of model catalysts

NASA Astrophysics Data System (ADS)

Mayr, Lukas; Rameshan, Raffael; Klötzer, Bernhard; Penner, Simon; Rameshan, Christoph

2014-05-01

An ultra-high vacuum (UHV) setup for "real" and "inverse" model catalyst preparation, depth-resolved near-surface spectroscopic characterization, and quantification of catalytic activity and selectivity under technologically relevant conditions is described. Due to the all-quartz reactor attached directly to the UHV-chamber, transfer of the catalyst for in situ testing without intermediate contact to the ambient is possible. The design of the UHV-compatible re-circulating batch reactor setup allows the study of reaction kinetics under close to technically relevant catalytic conditions up to 1273 K without contact to metallic surfaces except those of the catalyst itself. With the attached differentially pumped exchangeable evaporators and the quartz-microbalance thickness monitoring equipment, a reproducible, versatile, and standardised sample preparation is possible. For three-dimensional near-surface sample characterization, the system is equipped with a hemispherical analyser for X-ray photoelectron spectroscopy (XPS), electron-beam or X-ray-excited Auger-electron spectroscopy, and low-energy ion scattering measurements. Due the dedicated geometry of the X-ray gun (54.7°, "magic angle") and the rotatable sample holder, depth analysis by angle-resolved XPS measurements can be performed. Thus, by the combination of characterisation methods with different information depths, a detailed three-dimensional picture of the electronic and geometric structure of the model catalyst can be obtained. To demonstrate the capability of the described system, comparative results for depth-resolved sample characterization and catalytic testing in methanol steam reforming on PdGa and PdZn near-surface intermetallic phases are shown.

An XPS study on the impact of relative humidity on the aging of UO 2 powders

DOE PAGES

Donald, Scott B.; Dai, Zurong R.; Davisson, M. Lee; ...

2017-02-10

High resolution x-ray photoemission spectroscopy (XPS) was used to characterize the chemical speciation of high purity uranium dioxide (UO 2) powder samples following aging for periods of up to one year under controlled conditions with relative humidity ranging from 34% to 98%. A systematic shift to higher uranium oxidation states, and thus an increase in the mean uranium valence, was found to directly correlate with the dose of water received (i.e. the product of exposure time and relative humidity). Exposure duration was found to have a greater impact on sample aging than relative humidity. Lastly, the sample aged at 98%more » relative humidity was found to have unique structural differences for exposure time beyond 180 days when observed by scanning electron microscopy (SEM).« less

An XPS study on the impact of relative humidity on the aging of UO 2 powders

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

Donald, Scott B.; Dai, Zurong R.; Davisson, M. Lee

High resolution x-ray photoemission spectroscopy (XPS) was used to characterize the chemical speciation of high purity uranium dioxide (UO 2) powder samples following aging for periods of up to one year under controlled conditions with relative humidity ranging from 34% to 98%. A systematic shift to higher uranium oxidation states, and thus an increase in the mean uranium valence, was found to directly correlate with the dose of water received (i.e. the product of exposure time and relative humidity). Exposure duration was found to have a greater impact on sample aging than relative humidity. Lastly, the sample aged at 98%more » relative humidity was found to have unique structural differences for exposure time beyond 180 days when observed by scanning electron microscopy (SEM).« less

Electrochemical and XPS study of LiFePO4 cathode nanocomposite with PPy/PEG conductive network

NASA Astrophysics Data System (ADS)

Fedorková, A.; Oriňáková, R.; Oriňák, A.; Kupková, M.; Wiemhöfer, H.-D.; Audinot, J. N.; Guillot, J.

2012-08-01

High performance PPy/PEG-LiFePO4 nanocomposites as cathode materials were synthesized by solvothermal method and simple chemical oxidative polymerization of pyrrole (Py) monomer on the surface of LiFePO4 particles. The samples were characterized by scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectrometry (XPS) and charge-discharge tests. PPyPEG hybrid layers decrease particle to particle contact resistance while the impedance measurements confirmed that the coating of PPy-PEG significantly decreases the charge transfer resistance of the electrode material. The initial discharge capacities of this sample at C/5 and 1C are 150 and 128 mAh/g, respectively. The results show that PPy/PEGLiFePO4 composites are more effective than bare LiFePO4 as cathode material.

Elemental content of enamel and dentin after bleaching of teeth (a comparative study between laser-induced breakdown spectroscopy and x-ray photoelectron spectroscopy)

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

Imam, H.; Ahmed, Doaa; Eldakrouri, Ashraf

2013-06-21

The elemental content of the superficial and inner enamel as well as that of dentin was analyzed using laser-induced breakdown spectroscopy (LIBS) and x-ray photoelectron spectroscopy (XPS) of bleached and unbleached tooth specimens. It is thus clear from the spectral analysis using both the LIBS and XPS technique that elemental changes (though insignificant within the scopes of this study) of variable intensities do occur on the surface of the enamel and extend deeper to reach dentin. The results of the LIBS revealed a slight reduction in the calcium levels in the bleached compared to the control specimens in all themore » different bleaching groups and in both enamel and dentin. The good correlation found between the LIBS and XPS results demonstrates the possibility of LIBS technique for detection of minor loss in calcium and phosphorus in enamel and dentin.« less

Synthesis and characterization of blue fluorescent surface modified nano-graphene oxide flakes as a pH-sensitive drug delivery system

NASA Astrophysics Data System (ADS)

Hashemi, Hamed; Namazi, Hassan

2018-07-01

A new blue fluorescent surface modified graphene oxide (GO) by 6-(5-bromothiophen-2-yl) benzo[c][1,2,5]selenadiazole-5-carboxylic acid (TB) denoted as (GO-TB) was synthesized. The obtained hybrid was characterized by Scanning Electron Microscope (SEM/EDS); Brunauer-Emmett-Teller (BET); X-Ray Diffraction Spectroscopy (XRD); X-Ray Photoelectron Spectroscopy (XPS); UV-Vis Absorption Spectroscopy, and Fourier Transformed Infrared Spectroscopy (FTIR). The synthesized TB moiety displayed orange emission around 590 nm, while GO-TB exhibited a blue photoluminescence around 431 and 159 nm blue shift of photoluminescence. Doxorubicin immobilized on the hybrid surface up to 93%, and the release behavior in three different pHs was investigated. The release profile indicated a pH-dependent liberation with Fickian diffusion mechanism. The cytotoxicity of the hybrid was studied and the IC50 value for the hybrid was 5.16 µg/ml.

Generation of low work function, stable compound thin films by laser ablation

DOEpatents

Dinh, Long N.; McLean, II, William; Balooch, Mehdi; Fehring, Jr., Edward J.; Schildbach, Marcus A.

2001-01-01

Generation of low work function, stable compound thin films by laser ablation. Compound thin films with low work function can be synthesized by simultaneously laser ablating silicon, for example, and thermal evaporating an alkali metal into an oxygen environment. For example, the compound thin film may be composed of Si/Cs/O. The work functions of the thin films can be varied by changing the silicon/alkali metal/oxygen ratio. Low work functions of the compound thin films deposited on silicon substrates were confirmed by ultraviolet photoelectron spectroscopy (UPS). The compound thin films are stable up to 500.degree. C. as measured by x-ray photoelectron spectroscopy (XPS). Tests have established that for certain chemical compositions and annealing temperatures of the compound thin films, negative electron affinity (NEA) was detected. The low work function, stable compound thin films can be utilized in solar cells, field emission flat panel displays, electron guns, and cold cathode electron guns.

Synthesis and characterization of Ag@polycarbazole coaxial nanocables and their enhanced dispersion behavior

NASA Astrophysics Data System (ADS)

Zahoor, Ahmad; Teng, Qiu; Wang, Haiqiao; Choudhry, M. A.; Li, Xiaoyu

2011-06-01

Ag@polycarbazole coaxial nanocables (CNCs) have been successfully fabricated by the oxidative polymerization of carbazole over Ag nanowires (NWs) in acetonitrile. The morphology of Ag NWs and CNCs was studied by employing a transmission electron microscope (TEM) and a scanning electron microscope (SEM), which showed them to be a monodisperse material. The thickness of the polymer sheath was found to be 5 nm to 8 nm by observation under a high-resolution transmission electron microscope (HR-TEM). Energy dispersive X-ray spectroscopy (EDS), FT-IR and Raman measurements were used to characterize the polymer sheath, which demonstrated it to be a carbon material in polycarbazole form. X-ray photoelectron spectroscopy (XPS) was used for an interfacial study, which revealed that Ag surface atoms remained intact during polymer growth. In the end, zeta potential showed that the dispersion stability of Ag NWs increased due to polymer encapsulation, which is significant to obtain a particular alignment for anisotropic measurement of electrical conductivity.

Topochemical conversion of a dense metal–organic framework from a crystalline insulator to an amorphous semiconductor† †Electronic supplementary information (ESI) available: PXRD, impedance, TGA, IR, XPS, PDF, ESR, and CIF files. CCDC 1018776–1018778. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c4sc03295k Click here for additional data file.

PubMed Central

Hamoudi, H.; Suga, T.; Bennett, T. D.; Cairns, A. B.

2015-01-01

The topochemical conversion of a dense, insulating metal–organic framework (MOF) into a semiconducting amorphous MOF is described. Treatment of single crystals of copper(i) chloride trithiocyanurate, CuICl(ttcH3) (ttcH3 = trithiocyanuric acid), 1, in aqueous ammonia solution yields monoliths of amorphous CuI 1.8(ttc)0.6(ttcH3)0.4, 3. The treatment changes the transparent orange crystals of 1 into shiny black monoliths of 3 with retention of morphology, and moreover increases the electrical conductivity from insulating to semiconducting (conductivity of 3 ranges from 4.2 × 10–11 S cm–1 at 20 °C to 7.6 × 10–9 S cm–1 at 140 °C; activation energy = 0.59 eV; optical band gap = 0.6 eV). The structure and properties of the amorphous conductor are fully characterized by AC impedance spectroscopy, X-ray photoelectron spectroscopy, X-ray pair distribution function analysis, infrared spectroscopy, diffuse reflectance spectroscopy, electron spin resonance spectroscopy, elemental analysis, thermogravimetric analysis, and theoretical calculations. PMID:29560235

Thickness measurement of a thin hetero-oxide film with an interfacial oxide layer by X-ray photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Kim, Kyung Joong; Lee, Seung Mi; Jang, Jong Shik; Moret, Mona

2012-02-01

The general equation Tove = L cos θ ln(Rexp/R0 + 1) for the thickness measurement of thin oxide films by X-ray photoelectron spectroscopy (XPS) was applied to a HfO2/SiO2/Si(1 0 0) as a thin hetero-oxide film system with an interfacial oxide layer. The contribution of the thick interfacial SiO2 layer to the thickness of the HfO2 overlayer was counterbalanced by multiplying the ratio between the intensity of Si4+ from a thick SiO2 film and that of Si0 from a Si(1 0 0) substrate to the intensity of Si4+ from the HfO2/SiO2/Si(1 0 0) film. With this approximation, the thickness levels of the HfO2 overlayers showed a small standard deviation of 0.03 nm in a series of HfO2 (2 nm)/SiO2 (2-6 nm)/Si(1 0 0) films. Mutual calibration with XPS and transmission electron microscopy (TEM) was used to verify the thickness of HfO2 overlayers in a series of HfO2 (1-4 nm)/SiO2 (3 nm)/Si(1 0 0) films. From the linear relation between the thickness values derived from XPS and TEM, the effective attenuation length of the photoelectrons and the thickness of the HfO2 overlayer could be determined.

The surface characterization and passive behavior of Type 316L stainless steel in H2S-containing conditions

NASA Astrophysics Data System (ADS)

Wang, Zhu; Zhang, Lei; Tang, Xian; Zhang, Ziru; Lu, Minxu

2017-11-01

The protectiveness and characterization of passive films formed at various potentials in H2S-containing environments were studied using electrochemical measurements and surface analysis method. The corrosion resistance of 316L in H2S-containing environment decreases with the applied potential. The Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS) results indicate that Ni participates in the film formation, which results in the corresponding enrichment in the passive film. The oxidization degree analysis indicates that metallic elements are present in the passive film. Sulfide ions are significantly favored in the passive film at higher potentials, which is responsible for the breakdown of passive film.

Low temperature synthesis and characterization of carbonated hydroxyapatite nanocrystals

NASA Astrophysics Data System (ADS)

Anwar, Aneela; Asghar, Muhammad Nadeem; Kanwal, Qudsia; Kazmi, Mohsin; Sadiqa, Ayesha

2016-08-01

Carbonate substituted hydroxyapatite (CHA) nanorods were synthesized via coprecipitation method from aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate (with urea as carbonate ion source) in the presence of ammonium hydroxide solution at 70 °C at the conditions of pH 11. The obtained powders were physically characterized using transmission electron microscopy (TEM), X-ray powder diffraction analysis (XRD), and FTIR and Raman spectroscopy. The particle size was evaluated by Dynamic light scattering (DLS). The chemical structural analysis of as prepared sample was performed using X-ray photoelectron spectroscopy (XPS). After ageing for 12 h, and heat treatment at 1000 °C for 1 h, the product was obtained as highly crystalline nanorods of CHA.

Fracture surface analysis in composite and titanium bonding: Part 1: Titanium bonding

NASA Technical Reports Server (NTRS)

Sanderson, K. A.; Wightman, J. P.

1985-01-01

Fractured lap shear Ti 6-4 adherends bonded with polyphenyquinoxaline (PPQ) and polysulfone were analyzed. The effects of adherend pretreatment, stress level, thermal aging, anodizing voltage, and modified adhesive of Ti 6-4 adherend bonded with PPQ on lap shear strength were studied. The effect of adherend pretreatment on lap shear strength was investigated for PS samples. Results of scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) used to study the surface topography and surface composition are also discussed.

Applications of High Throughput (Combinatorial) Methodologies to Electronic, Magnetic, Optical, and Energy-Related Materials

DTIC Science & Technology

2013-06-17

of the films without having to fabricate capacitors. In addition, the use of X - ray diffraction (XRD) analysis enabled Chikyow et al.40 to identify an...effects of Al doping and annealing on the thermal stabil- ity of the Y2O3/Si gate stack were studied by X - ray photoemission spectroscopy (XPS) and X - ray ...the major diffraction features in the phase distribution. For a given structural phase, the X - ray peak intensity allows one to track the compositional

Microcontact Printing Patterning of an HOPG Surface by an Inverse Electron Demand Diels-Alder Reaction.

PubMed

Zhu, Jun; Hiltz, Jonathan; Tefashe, Ushula M; Mauzeroll, Janine; Lennox, R Bruce

2018-06-21

The chemical modification of an sp 2 hybridized carbon surface in a controllable manner is very challenging but also crucial for many applications. An inverse electron demand Diels-Alder (IEDDA) reaction using microcontact printing technique is introduced to spatially control the modification of a highly ordered pyrolytic graphite (HOPG) surface under ambient conditions. The covalent modification was characterized by Raman spectroscopy, XPS, and SECM. Tetrazine derivatives can effectively react with an HOPG surface and with microcontact printing methods resulting in spatially patterned surfaces being produced with micrometer-scale resolution. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Novel band gap-tunable K-Na co-doped graphitic carbon nitride prepared by molten salt method

NASA Astrophysics Data System (ADS)

Zhao, Jiannan; Ma, Lin; Wang, Haoying; Zhao, Yanfeng; Zhang, Jian; Hu, Shaozheng

2015-03-01

Novel band gap-tunable K-Na co-doped graphitic carbon nitride was prepared by molten salt method using melamine, KCl, and NaCl as precursor. X-ray diffraction (XRD), N2 adsorption, Scanning electron microscope (SEM), UV-vis spectroscopy, Photoluminescence (PL), and X-ray photoelectron spectroscopy (XPS) were used to characterize the prepared catalysts. The CB and VB potentials of graphitic carbon nitride could be tuned from -1.09 and +1.55 eV to -0.29 and +2.25 eV by controlling the weight ratio of eutectic salts to melamine. Besides, ions doping inhibited the crystal growth of graphitic carbon nitride, enhanced the surface area, and increased the separation rate of photogenerated electrons and holes. The visible-light-driven Rhodamine B (RhB) photodegradation and mineralization performances were significantly improved after K-Na co-doping.

Nickel oxide nanoparticles film produced by dead biomass of filamentous fungus

PubMed Central

Salvadori, Marcia Regina; Nascimento, Cláudio Augusto Oller; Corrêa, Benedito

2014-01-01

The synthesis of nickel oxide nanoparticles in film form using dead biomass of the filamentous fungus Aspergillus aculeatus as reducing agent represents an environmentally friendly nanotechnological innovation. The optimal conditions and the capacity of dead biomass to uptake and produce nanoparticles were evaluated by analyzing the biosorption of nickel by the fungus. The structural characteristics of the film-forming nickel oxide nanoparticles were analyzed by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and atomic force microscopy (AFM). These techniques showed that the nickel oxide nanoparticles had a size of about 5.89 nm and were involved in a protein matrix which probably permitted their organization in film form. The production and uptake of nickel oxide nanoparticles organized in film form by dead fungal biomass bring us closer to sustainable strategies for the biosynthesis of metal oxide nanoparticles. PMID:25228324

Beryllium Interactions in Molten Salts

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

G. S. Smolik; M. F. Simpson; P. J. Pinhero

Molten flibe (2LiF·BeF2) is a candidate as a cooling and tritium breeding media for future fusion power plants. Neutron interactions with the salt will produce tritium and release excess free fluorine ions. Beryllium metal has been demonstrated as an effective redox control agent to prevent free fluorine, or HF species, from reacting with structural metal components. The extent and rate of beryllium solubility in a pot design experiments to suppress continuously supplied hydrogen fluoride gas has been measured and modeled[ ]. This paper presents evidence of beryllium loss from specimens, a dependence of the loss upon bi-metal coupling, i.e., galvanicmore » effect, and the partitioning of the beryllium to the salt and container materials. Various posttest investigative methods, viz., scanning electron microscopy (SEM), Auger electron spectroscopy (AES) and x-ray photoelectron spectroscopy (XPS) were used to explore this behavior.« less

Theoretical modeling of the uranium 4f XPS for U(VI) and U(IV) oxides

NASA Astrophysics Data System (ADS)

Bagus, Paul S.; Nelin, Connie J.; Ilton, Eugene S.

2013-12-01

A rigorous study is presented of the physical processes related to X-Ray photoelectron spectroscopy, XPS, in the 4f level of U oxides, which, as well as being of physical interest in themselves, are representative of XPS in heavy metal oxides. In particular, we present compelling evidence for a new view of the screening of core-holes that extends prior understandings. Our analysis of the screening focuses on the covalent mixing of high lying U and O orbitals as opposed to the, more common, use of orbitals that are nominally pure U or pure O. It is shown that this covalent mixing is quite different for the initial and final, core-hole, configurations and that this difference is directly related to the XPS satellite intensity. Furthermore, we show that the high-lying U d orbitals as well as the U(5f) orbital may both contribute to the core-hole screening, in contrast with previous work that has only considered screening through the U(5f) shell. The role of modifying the U-O interaction by changing the U-O distance has been investigated and an unexpected correlation between U-O distance and XPS satellite intensity has been discovered. The role of flourite and octahedral crystal structures for U(IV) oxides has been examined and relationships established between XPS features and the covalent interactions in the different structures. The physical views of XPS satellites as arising from shake processes or as arising from ligand to metal charge transfers are contrasted; our analysis provides strong support that shake processes give a more fundamental physical understanding than charge transfer. Our theoretical studies are based on rigorous, strictly ab initio determinations of the electronic structure of embedded cluster models of U oxides with formal U(VI) and U(IV) oxidation states. Our results provide a foundation that makes it possible to establish quantitative relationships between features of the XPS spectra and materials properties.

Hydrothermal synthesis of highly crystalline RuS{sub 2} nanoparticles as cathodic catalysts in the methanol fuel cell and hydrochloric acid electrolysis

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

Li, Yanjuan; College of Material Science and Engineering, Key Laboratory of Automobile Materials of Ministry of Education, Jilin University, 2699 Qianjin Street, Changchun 130012; Li, Nan, E-mail: lin@jlu.edu.cn

2015-05-15

Highlights: • Highly crystalline RuS{sub 2} nanoparticles have been first synthesized by a “one-step” hydrothermal method. • The product presents a pure cubic phase of stoichiometric ratio RuS{sub 2} with average particle size of 14.8 nm. • RuS{sub 2} nanoparticles were used as cathodic catalysts in methanol fuel cell and hydrochloric acid electrolysis. • The catalyst outperforms commercial Pt/C in methanol tolerance and stability towards Cl{sup −}. - Abstract: Highly crystalline ruthenium sulfide (RuS{sub 2}) nanoparticles have been first synthesized by a “one-step” hydrothermal method at 400 °C, using ruthenium chloride and thiourea as reactants. The products were characterized bymore » powder X-ray diffraction (XRD), scanning electron microscopy/energy disperse spectroscopy (SEM/EDS), thermo gravimetric-differential thermal analyze (TG-DTA), transmission electron microscopy equipped with selected area electron diffraction (TEM/SAED). Fourier transform infrared spectra (IR), and X-ray photoelectron spectroscopy (XPS). XRD result illustrates that the highly crystalline product presents a pure cubic phase of stoichiometric ratio RuS{sub 2} and the average particle size is 14.8 nm. SEM and TEM images display the products have irregular shape of 6–25 nm. XPS analyst indicates that the sulfur exists in the form of S{sub 2}{sup 2−}. Cyclic voltammetry (CV), rotating disk electrode (RDE), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) measurements are conducted to evaluate the electrocatalytic activity and stability of the highly crystalline RuS{sub 2} nanoparticles in oxygen reduction reaction (ORR) for methanol fuel cell and hydrochloric acid electrolysis. The results illustrate that RuS{sub 2} is active towards oxygen reduction reaction. Although the activity of RuS{sub 2} is lower than that of Pt/C, the RuS{sub 2} catalyst outperforms commercial Pt/C in methanol tolerance and stability towards Cl{sup −}.« less

The crystallization behavior of amorphous Ge2Sb2Te5 films induced by a multi-pulsed nanosecond laser

NASA Astrophysics Data System (ADS)

Fan, T.; Liu, F. R.; Li, W. Q.; Guo, J. C.; Wang, Y. H.; Sun, N. X.; Liu, F.

2017-09-01

In this paper, accumulated crystallization of amorphous Ge2Sb2Te5 (a-GST) films induced by a multi-pulsed nanosecond (ns) excimer laser was investigated by x-ray diffraction (XRD), atomic force microscopy, field-emission scanning electron microscopy, x-ray photoelectron spectroscopy (XPS) and a spectrophotometer. XRD analyses revealed that detectable crystallization was firstly observed in the preferred orientation (200), followed by the orientations (220) and (111) after two pulses. Optical contrast, determined by crystallinity as well as surface roughness, was found to retain a linear relation within the first three pulses. A layered growth mechanism from the top surface to the interior of a-GST films was used to explain the crystallization behavior induced by the multi-pulse ns laser. XPS analyses for bond rearrangement and electronic structure further suggested that the crystallization process was performed by generating new bonds of Ge-Te and Sb-Te after laser irradiations. This paper presents the potential of multi-level devices and tunable thermal emitters based on controllable crystallization of phase-change materials.

Chemistry of MOS-LSI radiation hardening

NASA Technical Reports Server (NTRS)

Grunthaner, P.

1985-01-01

The objective of this task was to obtain chemical information on MOS test samples. Toward this end, high resolution X-ray photoemission spectroscopy (XPS) has been the primary techniques used to characterize the chemistry and structure of the SiO2/Si interface for a variety of MOS structures with differing degrees of susceptibility to damage by ionizing radiation. The major accomplishments of this program are: (1) the identification of a structurally distinct region of SiO2 in the near-interfacial region of thermal SiO2 on Si; (2) the identification in the near-interfacial region of SiO2 structural differences between radiation hard and soft gate oxides; (3) the direct observation of radiation-induced damage sites in thermal SiO2 with XPS using in situ electron stress; (4) the correlation of suboxide state distributions at the SiO2/Si interface with processing parameters and radiation susceptibility; (5) the development of a chemical mechanism for radiation-induced interface state generation in SiO2/Si structures; and (6) the development benign chemical profiling techniques which permit the investigation of oxide/semiconductor structures using surface sensitive electron spectroscopic techniques.

Low toxic maghemite nanoparticles for theranostic applications.

PubMed

Kuchma, Elena A; Zolotukhin, Peter V; Belanova, Anna A; Soldatov, Mikhail A; Lastovina, Tatiana A; Kubrin, Stanislav P; Nikolsky, Anatoliy V; Mirmikova, Lidia I; Soldatov, Alexander V

2017-01-01

Iron oxide nanoparticles have numerous and versatile biological properties, ranging from direct and immediate biochemical effects to prolonged influences on tissues. Most applications have strict requirements with respect to the chemical and physical properties of such agents. Therefore, developing rational design methods of synthesis of iron oxide nanoparticles remains of vital importance in nanobiomedicine. Low toxic superparamagnetic iron oxide nanoparticles (SPIONs) for theranostic applications in oncology having spherical shape and maghemite structure were produced using the fast microwave synthesis technique and were fully characterized by several complementary methods (transmission electron microscopy [TEM], X-ray diffraction [XRD], dynamic light scattering [DLS], X-ray photoelectron spectroscopy [XPS], X-ray absorption near edge structure [XANES], Mossbauer spectroscopy, and HeLa cells toxicity testing). TEM showed that the majority of the obtained nanoparticles were almost spherical and did not exceed 20 nm in diameter. The averaged DLS hydrodynamic size was found to be ~33 nm, while that of nanocrystallites estimated by XRD waŝ16 nm. Both XRD and XPS studies evidenced the maghemite (γ-Fe 2 O 3 ) atomic and electronic structure of the synthesized nanoparticles. The XANES data analysis demonstrated the structure of the nanoparticles being similar to that of macroscopic maghemite. The Mossbauer spectroscopy revealed the γ-Fe 2 O 3 phase of the nanoparticles and vibration magnetometry study showed that reactive oxygen species in HeLa cells are generated both in the cytoplasm and the nucleus. Quasispherical Fe 3+ SPIONs having the maghemite structure with the average size of 16 nm obtained by using the fast microwave synthesis technique are expected to be of great value for theranostic applications in oncology and multimodal anticancer therapy.

Low toxic maghemite nanoparticles for theranostic applications

PubMed Central

Zolotukhin, Peter V; Belanova, Anna A; Soldatov, Mikhail A; Lastovina, Tatiana A; Kubrin, Stanislav P; Nikolsky, Anatoliy V; Mirmikova, Lidia I

2017-01-01

Background Iron oxide nanoparticles have numerous and versatile biological properties, ranging from direct and immediate biochemical effects to prolonged influences on tissues. Most applications have strict requirements with respect to the chemical and physical properties of such agents. Therefore, developing rational design methods of synthesis of iron oxide nanoparticles remains of vital importance in nanobiomedicine. Methods Low toxic superparamagnetic iron oxide nanoparticles (SPIONs) for theranostic applications in oncology having spherical shape and maghemite structure were produced using the fast microwave synthesis technique and were fully characterized by several complementary methods (transmission electron microscopy [TEM], X-ray diffraction [XRD], dynamic light scattering [DLS], X-ray photoelectron spectroscopy [XPS], X-ray absorption near edge structure [XANES], Mossbauer spectroscopy, and HeLa cells toxicity testing). Results TEM showed that the majority of the obtained nanoparticles were almost spherical and did not exceed 20 nm in diameter. The averaged DLS hydrodynamic size was found to be ~33 nm, while that of nanocrystallites estimated by XRD waŝ16 nm. Both XRD and XPS studies evidenced the maghemite (γ-Fe2O3) atomic and electronic structure of the synthesized nanoparticles. The XANES data analysis demonstrated the structure of the nanoparticles being similar to that of macroscopic maghemite. The Mossbauer spectroscopy revealed the γ-Fe2O3 phase of the nanoparticles and vibration magnetometry study showed that reactive oxygen species in HeLa cells are generated both in the cytoplasm and the nucleus. Conclusion Quasispherical Fe3+ SPIONs having the maghemite structure with the average size of 16 nm obtained by using the fast microwave synthesis technique are expected to be of great value for theranostic applications in oncology and multimodal anticancer therapy. PMID:28919740

Arsenic(V) removal from groundwater using nano scale zero-valent iron as a colloidal reactive barrier material.

PubMed

Kanel, Sushil Raj; Greneche, Jean-Mark; Choi, Heechul

2006-03-15

The removal of As(V), one of the most poisonous groundwater pollutants, by synthetic nanoscale zero-valent iron (NZVI) was studied. Batch experiments were performed to investigate the influence of pH, adsorption kinetics, sorption mechanism, and anionic effects. Field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Mossbauer spectroscopy were used to characterize the particle size, surface morphology, and corrosion layer formation on pristine NZVI and As(V)-treated NZVI. The HR-TEM study of pristine NZVI showed a core-shell-like structure, where more than 90% of the nanoparticles were under 30 nm in diameter. Mössbauer spectroscopy further confirmed its structure in which 19% were in zero-valent state with a coat of 81% iron oxides. The XRD results showed that As(V)-treated NZVI was gradually converted into magnetite/maghemite corrosion products over 90 days. The XPS study confirmed that 25% As(V) was reduced to As(III) by NZVI after 90 days. As(V) adsorption kinetics were rapid and occurred within minutes following a pseudo-first-order rate expression with observed reaction rate constants (Kobs) of 0.02-0.71 min(-1) at various NZVI concentrations. Laser light scattering analysis confirmed that NZVI-As(V) forms an inner-sphere surface complexation. The effects of competing anions revealed that HCO3-, H4SiO4(0), and H2PO4(2-) are potential interfering agents in the As(V) adsorption reaction. Our results suggest that NZVI is a suitable candidate for As(V) remediation.

Enhanced photocatalytic performance of RGO/Ag nanocomposites produced via a facile microwave irradiation for the degradation of Rhodamine B in aqueous solution

NASA Astrophysics Data System (ADS)

Divya, K. S.; Chandran, Akash; Reethu, V. N.; Mathew, Suresh

2018-06-01

A series of RGO/Ag nanocomposites with different weight addition ratios of graphene oxide (GO) have been successfully prepared in situ through the simultaneous reduction of GO and AgNO3 via a facile microwave irradiation. X-ray diffraction analysis, Fourier Transform Infrared Spectroscopy, UV-vis diffuse reflectance spectra, Scanning electron microscopy, Photoluminescence spectra, Raman spectra, Atomic Force Microscopy, X-ray photoelectron spectroscopy (XPS) and Transmission electron microscopy are employed to determine the properties of the samples. It is found that RGO/Ag nanocomposites with a proper weight addition ratios of GO exhibit higher photocatalytic activity toward liquid phase photodegradation of Rhodamine B under visible light irradiation. The improved photoactivity of RGO/Ag nanocomposites can be ascribed to the integrative synergestic effect of enhanced adsorption capacity, the prolonged lifetime of photogenerated electron-hole pairs and effective interfacial hybridization between RGO and Ag nanoparticles. This study also shows that graphene sheets act as electronic conductive channels to efficiently separate charge carriers from Ag nanoparticles.

Fabrication of meso-porous BiOI sensitized zirconia nanoparticles with enhanced photocatalytic activity under simulated solar light irradiation

NASA Astrophysics Data System (ADS)

Vignesh, K.; Suganthi, A.; Min, Bong-Ki; Kang, Misook

2015-01-01

In this present work, BiOI sensitized zirconia (BiOI-ZrO2) nanoparticles were fabricated using a precipitation-deposition method. The physicochemical characteristics of BiOI/ZrO2 were studied through X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), BET-surface area, X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (UV-vis-DRS) and photoluminescence (PL) spectroscopy techniques. The absorption maximum of ZrO2 was shifted to the visible region after sensitization with BiOI. BET-surface area results inferred that the prepared hetero-junctions were meso-porous in nature. The photocatalytic activity of BiOI-ZrO2 for the degradation of methyl violet (MV) dye under simulated solar light irradiation was investigated in detail. 3% BiOI-ZrO2 exhibited the highest photocatalytic performance (98% of MV degradation) when compared with ZrO2 and BiOI. The enhancement in the photocatalytic activity of BiOI-ZrO2 is ascribed to the sensitization effect of BiOI, suppression of electron-hole recombination and the formation of p-n hetero-junction.

Structural, optical, electrochemical and photovoltaic studies of spider web like Silver Indium Diselenide Quantum dots synthesized by ligand mediated colloidal sol-gel approach

NASA Astrophysics Data System (ADS)

Adhikari, Tham; Pathak, Dinesh; Wagner, Tomas; Jambor, Roman; Jabeen, Uzma; Aamir, Muhammad; Nunzi, Jean-Michel

2017-11-01

Silver indium diselenide quantum dots were successively synthesized by colloidal sol-gel method by chelating with organic ligand oleylamine (OLA). The particle size was studied by transmission electron microscopy (TEM) and the size was found about 10 nm. X-ray diffraction (XRD) was used to study crystalline structure of the nanocrystals. The grain size and morphology were further studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The elemental composition was studied by X-ray photon electron spectroscopy (XPS) and energy dispersive x-ray spectroscopy (EDAX). The capping property of OLA in nanocrystal was also demonstrated by Fourier Transform Infrared spectroscopy (FTIR). The band gap was calculated from both cyclic voltammetry and optical absorption and suggest quantum confinement. The solution processed bilayer thin film solar cells were fabricated with n-type Zinc oxide using doctor blading/spin coating method and their photovoltaic performance was studied. The best device sintered at 450 °C showed an efficiency 0.75% with current density of 4.54 mAcm-2, open-circuit voltage 0.44 V and fill factor 39.4%.

Surfactant-mediated growth of cobalt on magnesium oxide(111)

NASA Astrophysics Data System (ADS)

Johnson-Steigelman, Harry Trevor

Monolayer films of Co have been deposited using an electrostatic electron-beam evaporator on single-crystal MgO(111)-( 3x3 ) R 30° and MgO(111)-(1x1) substrates held at room temperature (RT), with subsequent annealing of temperatures 400°C to 800°C. These films have been characterized using low-energy electron diffraction (LEED), x-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM). Upon RT deposition of Co, the LEED pattern of the substrate disappears and the XPS signal of MgO features reduce in intensity. After short anneals of 400°C, the LEED pattern returns and the MgO features increase in intensity. AFM images suggest that islanding has occurred at the surface. This conclusion is supported by the behavior of thicker films of Co on MgO(111), which showed pronounced changes in the MgO related XPS features. The behavior of the Mg 2p and O 1s features were analyzed and compared to previously reported reconstructions of the MgO(111)-(1x1) and MgO(111)-( 3x3 ) R 30° surfaces. Ag was examined as a potential surfactant to aid in the growth of smooth Co films. Ag was deposited onto MgO(111)-( 3x3 ) R 30° substrates and investigated using XPS, LEED, and AFM. It was found that Ag formed islands upon annealing. Despite the fact that Ag formed islands, it was found that the presence of Ag did have a surfactant effect upon the thin-film growth of Co on Ag/MgO(111)-( 3x3 ) R 30° substrates with 1-2 ML of Ag. Co islands were still present, but much more smooth than islands formed without the Ag surfactant. XPS peak intensity changes and AFM suggest strongly that Ag floated to the top of these samples at temperatures above 400°C. The Co growth mode appears to be Volmer-Weber island growth, as seen in AFM.

Conduction band offset at GeO{sub 2}/Ge interface determined by internal photoemission and charge-corrected x-ray photoelectron spectroscopies

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

Zhang, W. F.; Nishimula, T.; Nagashio, K.

2013-03-11

We report a consistent conduction band offset (CBO) at a GeO{sub 2}/Ge interface determined by internal photoemission spectroscopy (IPE) and charge-corrected X-ray photoelectron spectroscopy (XPS). IPE results showed that the CBO value was larger than 1.5 eV irrespective of metal electrode and substrate type variance, while an accurate determination of valence band offset (VBO) by XPS requires a careful correction of differential charging phenomena. The VBO value was determined to be 3.60 {+-} 0.2 eV by XPS after charge correction, thus yielding a CBO (1.60 {+-} 0.2 eV) in excellent agreement with the IPE results. Such a large CBO (>1.5more » eV) confirmed here is promising in terms of using GeO{sub 2} as a potential passivation layer for future Ge-based scaled CMOS devices.« less

Identification of the silver state in the framework of Ag-containing zeolite by XRD, FTIR, photoluminescence, 109Ag NMR, EPR, DR UV-vis, TEM and XPS investigations.

PubMed

Popovych, Nataliia; Kyriienko, Pavlo; Soloviev, Sergiy; Baran, Rafal; Millot, Yannick; Dzwigaj, Stanislaw

2016-10-26

Silver has been identified in the framework of Ag x SiBEA zeolites (where x = 3-6 Ag wt%) by the combined use of XRD, 109 Ag MAS NMR, FTIR, diffuse reflectance UV-visible, EPR and XPS spectroscopy. The incorporation of Ag ions into the framework of SiBEA zeolite has been evidenced by XRD. The consumption of OH groups as a result of their reaction with the silver precursor has been monitored by FTIR and photoluminescence spectroscopy. The changes in the silver state as a function of Ag content and thermal and hydrogen treatment at 573 K have been identified by 109 Ag MAS NMR, EPR, DR UV-visible, TEM and XPS investigations. The acidity of AgSiBEA has been investigated by FTIR spectroscopy of adsorbed CO and pyridine used as probe molecules.

Study of fission-product segregation in used CANDU fuel by X-ray photoelectron spectroscopy (XPS) II

NASA Astrophysics Data System (ADS)

Hocking, William H.; Duclos, A. Michael; Johnson, Lawrence H.

1994-03-01

A thorough investigation of the grain-boundary chemistry of used CANDU fuel from one intact element has been conducted by X-ray photoelectron spectroscopy (XPS). Selected findings from more extensive XPS measurements on other used CANDU fuels exposed to storage conditions are included for comparison. Cesium, rubidium, tellurium and barium have been commonly observed, often reaching high degrees of surface enrichment, although their relative abundances can vary widely with a complex dependence on the fuel irradiation history. Lower concentrations of cadmium, molybdenum, strontium and iodine have also been occasionally detected. Except for iodine, chemical-shift data are indicative of oxidized species, possibly uranates. Segregation at monolayer-level coverages has been demonstrated by sequential XPS analysis and argon-ion sputtering. Calculations based on an idealized thin-film model are consistent with the depth profiles. The interpretation of these results is discussed in the context of previous studies, especially on LWR fuels.

Effect of sulfate ions on the crystallization and photocatalytic activity of TiO2/diatomite composite photocatalyst

NASA Astrophysics Data System (ADS)

Zhang, Jinjun; Wang, Xiaoyan; Wang, Jimei; Wang, Jing; Ji, Zhijiang

2016-01-01

TiO2 nanoparticles were immobilized on diatomite by hydrolysis-deposition method using titanium tetrachloride as precursor. The effect of sulfate ions on the crystallization and photocatalytic activity of TiO2/diatomite composite photocatalyst was characterized by TG-DSC, XRD, BET surface area, SEM, FT-IR spectroscopy, XPS and UV-vis diffuse reflectance spectra. The results indicate that addition of a small amount of sulfate ions promotes the formation of anatase phase and inhibits the transformation from anatase to rutile. On the other hand, sulfate ions immobilized on the surface of TiO2/diatomite have strong affinity for electrons, capturing the photo-generated electrons, which hinders the recombination of electrons and holes.

Surface studies of praseodymium by electron spectroscopies

NASA Astrophysics Data System (ADS)

Krawczyk, Mirosław; Pisarek, Marcin; Lisowski, Wojciech; Jablonski, Aleksander

2016-12-01

Electron transport properties in praseodymium (Pr) foil samples were studied by elastic-peak electron spectroscopy (EPES). Prior to EPES measurements, the Pr sample surface was pre-sputtered by Ar ions with ion energy of 2-3 keV. After such treatment, the Pr sample still contained about 10 at.% of residual oxygen in the surface region, as detected by X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) analyses. The inelastic mean free path (IMFP), characterizing electron transport within this region (4 nm-thick), was evaluated from EPES using both Ni and Au standards as a function of energy in the range of 0.5-2 keV. Experimental IMFPs, λ, were approximated by the simple function λ = kEp, where E is energy (in eV), and k = 0.1549 and p = 0.7047 were the fitted parameters. These values were compared with IMFPs for the praseodymium surface in which the presence of oxygen was tentatively neglected, and also with IMFPs resulting from the TPP-2M predictive equation for bulk praseodymium. We found that the measured IMFP values to be only slightly affected by neglect of oxygen in calculations. The fitted function applied here was consistent with the energy dependence of the EPES-measured IMFPs. Additionally, the measured IMFPs were found to be from 2% to 4.2% larger than the predicted IMFPs for praseodymium in the energy range of 500-1000 eV. For electron energies of 1500 eV and 2000 eV, there was an inverse correlation between these values, and then the resulting deviations of -0.4% and -2.7%, respectively, were calculated.

Covalent binding of cyclohexene, 1,3-cyclohexadiene and 1,4-cyclohexadiene on Si(1 1 1)-7 × 7

NASA Astrophysics Data System (ADS)

Tao, Feng; Wang, Zhong Hai; Xu, Guo Qin

2003-05-01

The adsorption reactions and binding configurations of cyclohexene, 1,3-cyclohexadiene and 1,4-cyclohexadiene on Si(1 1 1)-7 × 7 were studied using high-resolution electron energy loss spectroscopy (HREELS), ultraviolet photoelectron spectroscopy (UPS), X-ray photoelectron spectroscopy (XPS) and DFT calculation. The covalent attachments of these unsaturated hydrocarbons to Si(1 1 1)-7 × 7 through the formation of Si-C linkages are clearly demonstrated by the observation of the Si-C stretching mode at 450-500 cm -1 in their HREELS spectra. For chemisorbed cyclohexene, the involvement of π CC in binding is further supported by the absence of CC stretching modes and the disappearance of the π CC photoemission. The chemisorption of both 1,3-cyclohexadiene and 1,4-cyclohexadiene leads to the formation of cyclohexene-like intermediates through di-σ bonding. The existence of one π CC bond in their chemisorbed states is confirmed by the observation of the CC and (sp 2)CH stretching modes and the UPS and XPS results. DFT calculations show that [4 + 2]-like cycloaddition is thermodynamically preferred for 1,3-cyclohexadiene on Si(1 1 1)-7 × 7, but a [2 + 2]-like reaction mechanism is proposed for the covalent attachment of cyclohexene and 1,4-cyclohexadiene.

Effect of Vinylene Carbonate and Fluoroethylene Carbonate on SEI Formation on Graphitic Anodes in Li-Ion Batteries

DOE PAGES

Nie, Mengyun; Demeaux, Julien; Young, Benjamin T.; ...

2015-07-23

Binder free (BF) graphite electrodes were utilized to investigate the effect of electrolyte additives fluoroethylene carbonate (FEC) and vinylene carbonate (VC) on the structure of the solid electrolyte interface (SEI). The structure of the SEI has been investigated via ex-situ surface analysis including X-ray Photoelectron spectroscopy (XPS), Hard XPS (HAXPES), Infrared spectroscopy (IR) and transmission electron microscopy (TEM). The components of the SEI have been further investigated via nuclear magnetic resonance (NMR) spectroscopy of D2O extractions. The SEI generated on the BF-graphite anode with a standard electrolyte (1.2 M LiPF6 in ethylene carbonate (EC) / ethyl methyl carbonate (EMC), 3/7more » (v/v)) is composed primarily of lithium alkyl carbonates (LAC) and LiF. Incorporation of VC (3% wt) results in the generation of a thinner SEI composed of Li2CO3, poly(VC), LAC, and LiF. Incorporation of VC inhibits the generation of LAC and LiF. Incorporation of FEC (3% wt) also results in the generation of a thinner SEI composed of Li2CO3, poly(FEC), LAC, and LiF. The concentration of poly(FEC) is lower than the concentration of poly(VC) and the generation of LAC is inhibited in the presence of FEC. The SEI appears to be a homogeneous film for all electrolytes investigated.« less

Effect of modification substrate on the microstructure of hydroxyapatite coating

NASA Astrophysics Data System (ADS)

Realpe-Jaramillo, J.; Morales-Morales, J. A.; González-Sánchez, J. A.; Cabanzo, R.; Mejía-Ospino, E.; Rodríguez-Pereira, J.

2017-01-01

Bioactive hydroxyapatite (HA) coatings were fabricated by a precipitation, sol-gel and dip-coating method. The effects of the aging time and the base used to adjust pH and substrate materials on the phases and microstructures of HA coatings were studied by field emission scanning electron microscopy FESEM, energy dispersive spectroscopy EDS, X-ray photoelectron spectroscopy XPS, and the vibrations of the phosphate groups were determined by Raman spectroscopy. The results showed that all the films were composed of the phases of TiO2 and HA. With coated titanium substrate with TiO2, the crystallinity of the HA coating increases, the structure became more compact and the Ca/P ratio increased because of the loss of P in the films. The addition of sodium hydroxide (adjusting the pH level to about 10) can increase the HA content in the coating. XPS and EDS results for steel substrate and titanium showed poor calcium content as obtained with a Ca/P ratio of 1.38 and 1.58, respectively, composition is similar to that of natural apatite. However, spectroscopic results suggest the presence of a mixture of hydroxyapatite and octacalcium phosphate. The different substrate materials have a high influence on the microstructure of the separated double films. However, hydroxyapatite nanopowders coatings were obtained using a simple method, with potential biomedical applications.

Effects of the carrier concentration on polarity determination in Ga-doped ZnO films by hard x-ray photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Song, Huaping; Makino, Hisao; Kobata, Masaaki; Nomoto, Junichi; Kobayashi, Keisuke; Yamamoto, Tetsuya

2018-03-01

Core level (CL) and valence band (VB) spectra of heavily Ga-doped ZnO (GZO) films with carrier concentrations (Ne) ranging from 1.8 × 1020 to 1.0 × 1021 cm-3 were measured by high-resolution Al Kα (hν = 1486.6 eV) x-ray photoelectron spectroscopy (XPS) and Cr Kα (hν = 5414.7 eV) hard x-ray photoelectron spectroscopy (HAXPES). The CL spectra of the GZO films measured by XPS had little dependence on Ne. In contrast, clear differences in asymmetric broadening were observed in the HAXPES spectra owing to the large probing depth. The asymmetry in the Zn 2p3/2 and O 1s HAXPES spectra is mainly attributed to the energy loss of the conduction electron plasmon caused by the high Ne of the GZO films. Similar asymmetry was also observed in the VB spectra of these GZO films. It was found that such asymmetry plays a crucial role in the determination of crystal polarity. With increasing Ne, the intensity of the sub-peak at a binding energy Eb of about 5 eV in the VB spectrum decreased and the sub-peak became indistinguishable. We clarified the limitation of the criterion using the sub-peak and proposed an alternative method for polarity determination.

Architecture-dependent surface chemistry for Pt monolayers on carbon-supported Au.

PubMed

Cheng, Shuang; Rettew, Robert E; Sauerbrey, Marc; Alamgir, Faisal M

2011-10-01

Pt monolayers were grown by surface-limited redox replacement (SLRR) on two types of Au nanostructures. The Au nanostructures were fabricated electrochemically on carbon fiber paper (CFP) by either potentiostatic deposition (PSD) or potential square wave deposition (PSWD). The morphology of the Au/CFP heterostructures, examined using scanning electron microscopy (SEM), was found to depend on the type of Au growth method employed. The properties of the Pt deposit, as studied using X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and cyclic voltammetry (CV), were found to depend strongly on the morphology of the support. Specifically, it was found that smaller Au morphologies led to a higher degree of cationicity in the resulting Pt deposit, with Pt(4+) and Pt(2+) species being identified using XPS and XAS. For fuel-cell catalysts, the resistance of ultrathin catalyst deposits to surface area loss through dissolution, poisoning, and agglomeration is critical. This study shows that an equivalent of two monolayers (ML) is the low-loading limit of Pt on Au. At 1 ML or below, the Pt film decreases in activity and durability very rapidly due to presence of cationic Pt. © 2011 American Chemical Society

Atomic layer deposition of ruthenium surface-coating on porous platinum catalysts for high-performance direct ethanol solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Jeong, Heon Jae; Kim, Jun Woo; Jang, Dong Young; Shim, Joon Hyung

2015-09-01

Pt-Ru bi-metallic catalysts are synthesized by atomic layer deposition (ALD) of Ru surface-coating on sputtered Pt mesh. The catalysts are evaluated in direct ethanol solid oxide fuel cells (DESOFCs) in the temperature range of 300-500 °C. Island-growth of the ALD Ru coating is confirmed by transmission electron microscopy and X-ray photoelectron spectroscopy (XPS) analyses. The performance of the DESOFCs is evaluated based on the current-voltage output and electrochemical impedance spectroscopy. Genuine reduction of the polarization impedance, and enhanced power output with improved surface kinetics are achieved with the optimized ALD Ru surface-coating compared to bare Pt. The chemical composition of the Pt/ALD Ru electrode surface after fuel cell operation is analyzed via XPS. Enhanced cell performance is clearly achieved, attributed to the effective Pt/ALD Ru bi-metallic catalysis, including oxidation of Cdbnd O by Ru, and de-protonation of ethanol and cleavage of C-C bonds by Pt, as supported by surface morphology analysis which confirms formation of a large amount of carbon on bare Pt after the ethanol-fuel-cell test.

Controlled synthesis, characterization and photoluminescence property of olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3}

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

Zhang, Youjin, E-mail: zyj@ustc.edu.cn; Zheng, Ao; Yang, Xiaozhi

2012-09-15

Highlights: ► The olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3} was gained with EDTA assisted hydrothermal method. ► The product was characterized by XRD, XPS, FTIR, FESEM, and PL. ► The possible formation mechanism for olive-like α-Nd{sub 2}(MoO{sub 4}){sub 3} was proposed. ► The PL in visible region of the olive-like α-Nd{sub 2}(MoO{sub 4}){sub 3} was studied. -- Abstract: The olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3} was obtained by a convenient and facile complex agent assisted hydrothermal method. The product was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectroscopy, field-emission scanning electron microscopy (FESEM) andmore » photoluminescence (PL). The possible formation mechanism of the olive-like α-Nd{sub 2}(MoO{sub 4}){sub 3} was proposed. The photoluminescence property in visible region of the olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3} was studied.« less

X-Ray Photoelectron Spectroscopy and Tribology Studies of Annealed Fullerene-like WS2 Nanoparticles

NASA Astrophysics Data System (ADS)

Kopnov, F.; Tenne, R.; Späth, B.; Jägermann, W.; Cohen, H.; Feldman, Y.; Zak, A.; Moshkovich, A.; Rapoport, L.

The temporal chemical changes occurring at the surface of fullerene-like (IF) nanoparticles of WS2 were investigated using X-ray photo-electron spectroscopy (XPS) and compared to those of bulk powder (2H) of the same material. It is possible to follow the long term (surface oxidation and carbonization) occurring at defects on the outermost surface (0001) layer of the fullerene-like nanoparticles. Similar but perhaps more distinctive changes are observed on the prismatic (hk0) surfaces of the 2H powder. Vacuum annealing is shown to remove most of these changes and bring the surface close to its stoichiometric composition. In accordance with previous measurements, further evidence is obtained for the existence of water molecules which are entrapped in the hollow core and interstitial defects of the fullerene-like nanoparticles during the synthesis. They are also shown to be removed by the vacuum annealing process. Chemically resolved electrical measurements (CREM) in the XPS show that the vacuum annealed IF samples become more intrinsic. Finally, tribological measurements show that the vacuum annealed IF samples perform better as an additive to oil than the non-annealed IF samples and the bulk (2H) platelets powder.

Oxygen accumulation on metal surfaces investigated by XPS, AES and LEIS, an issue for sputter depth profiling under UHV conditions

NASA Astrophysics Data System (ADS)

Steinberger, R.; Celedón, C. E.; Bruckner, B.; Roth, D.; Duchoslav, J.; Arndt, M.; Kürnsteiner, P.; Steck, T.; Faderl, J.; Riener, C. K.; Angeli, G.; Bauer, P.; Stifter, D.

2017-07-01

Depth profiling using surface sensitive analysis methods in combination with sputter ion etching is a common procedure for thorough material investigations, where clean surfaces free of any contamination are essential. Hence, surface analytic studies are mostly performed under ultra-high vacuum (UHV) conditions, but the cleanness of such UHV environments is usually overrated. Consequently, the current study highlights the in principle known impact of the residual gas on metal surfaces (Fe, Mg, Al, Cr and Zn) for various surface analytics methods, like X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and low-energy ion scattering (LEIS). The investigations with modern, state-of-the-art equipment showed different behaviors for the metal surfaces in UHV during acquisition: (i) no impact for Zn, even after long time, (ii) solely adsorption of oxygen for Fe, slight and slow changes for Cr and (iii) adsorption accompanied by oxide formation for Al and Mg. The efficiency of different counter measures was tested and the acquired knowledge was finally used for ZnMgAl coated steel to obtain accurate depth profiles, which exhibited before serious artifacts when data acquisition was performed in an inconsiderate way.

Polyamidoamine dendrimers-assisted electrodeposition of gold-platinum bimetallic nanoflowers.

PubMed

Qian, Lei; Yang, Xiurong

2006-08-24

Novel Au-Pt bimetallic flower nanostructures fabricated on a polyamidoamine dendrimers-modified surface by electrodeposition are reported. These polyamidoamine dendrimers were stable, and they assisted the formation of Au-Pt bimetallic nanoflowers during the electrodeposition process. These nanoflowers were characterized by field-emitted scanning electron microscopy (FE-SEM), energy-dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction, and electrochemical methods. FE-SEM images showed that the bimetallic nanoflower included two parts: the "light" and the "pale" part. The two parts consisted of many small bimetallic nanoparticles, which was attributed to the progressive nucleation process. Moreover, the "light" part contained more bimetallic nanoparticles. The morphologies of bimetallic nanoflowers depended on the electrodeposition time and potential and the layer number of assembled dendrimers. The average size of nanoflowers increased with the increase in electrodeposition time. The layer number of assembled dendrimers obviously affected the size and morphologies of the "pale" parts of deposited nanoflowers. EDS and XPS indicated that the content of Au element was higher than that of Pt element in the nanoflowers. The bimetallic nanoflowers-modified electrode had electrochemical properties similar to those of bare gold and platinum electrodes. It also exhibited significant electrocatalytic activities toward oxygen reduction.

Palladium nanoparticle deposition via precipitation: a new method to functionalize macroporous silicon

PubMed Central

Scheen, Gilles; Bassu, Margherita; Douchamps, Antoine; Zhang, Chao; Debliquy, Marc; Francis, Laurent A

2014-01-01

We present an original two-step method for the deposition via precipitation of Pd nanoparticles into macroporous silicon. The method consists in immersing a macroporous silicon sample in a PdCl2/DMSO solution and then in annealing the sample at a high temperature. The impact of composition and concentration of the solution and annealing time on the nanoparticle characteristics is investigated. This method is compared to electroless plating, which is a standard method for the deposition of Pd nanoparticles. Scanning electron microscopy and computerized image processing are used to evaluate size, shape, surface density and deposition homogeneity of the Pd nanoparticles on the pore walls. Energy-dispersive x-ray spectroscopy (EDX) and x-ray photoelectron spectroscopy (XPS) analyses are used to evaluate the composition of the deposited nanoparticles. In contrast to electroless plating, the proposed method leads to homogeneously distributed Pd nanoparticles along the macropores depth with a surface density that increases proportionally with the PdCl2 concentration. Moreover EDX and XPS analysis showed that the nanoparticles are composed of Pd in its metallic state, while nanoparticles deposited by electroless plating are composed of both metallic Pd and PdOx. PMID:27877732

The polymeric nanofilm of triazinedithiolsilane fabricated by self-assembled technique on copper surface. Part 2: Characterization of composition and morphology

NASA Astrophysics Data System (ADS)

Wang, Yabin; Liu, Zhong; Huang, Yudong; Qi, Yutai

2015-11-01

In the first part, a novel design route for metal protection against corrosion was proposed, and a class of triazinedithiolsilane compounds was conceived as protector for copper. The protective capability of the polymeric nanofilm, fabricated by self-assembling one representative (abbreviated as TESPA) of triazinedithiolsilane compounds onto copper surface, has been investigated and evaluated by electrochemical tests. The results show that the polymeric nanofilm significantly inhibits copper corrosion. This study, on the one hand, concentrates on the chemical composition of the TESPA polymeric nanofilm by means of X-ray photoelectron spectroscopy (XPS). The XPS results reveal that the chemical bonds between copper and TESPA monomers, three dimensional disulfide units and siloxane networks are responsible for the satisfactory protection of TESPA polymeric nanofilm against copper corrosion. On the other hand, scanning electron microscope (SEM) and energy-dispersive spectroscopy (EDS) are utilized to reveal the morphology and the uniformity of the TESPA polymeric nanofilm. The SEM-EDS results demonstrate that the copper surfaces are uniformly covered with TESPA self-assembled monolayer and the polymeric nanofilm. The TESPA-covered copper surfaces turn out to be smoother than that of the bare copper surface.

Structural characterization of oxidized titanium surfaces

NASA Astrophysics Data System (ADS)

Jobin, M.; Taborelli, M.; Descouts, P.

1995-05-01

Oxidized titanium surfaces resulting from various processes have been structurally characterized by means of scanning force microscopy, x-ray photoemission spectroscopy (XPS), x-ray diffraction, and electron energy-loss spectroscopy (EELS) with losses in the 0-100 eV range. It has been found that the surface morphology has a granular structure for electropolished titanium and for titanium evaporated on mica at low substrate temperature (570 K), but changes to flat terraces for the films evaporated at higher temperature (770 K). Angular-dependent XPS has revealed the presence of a Ti2O3 suboxide at the Ti/TiO2 interface for electropolished titanium. Dry oxidation has been performed at 770 and 970 K on both weakly and highly crystallized evaporated titanium films oriented along (0001). In the case of underlying crystallized metallic titanium, the resulting TiO2 films are crystallized with the anatase (004) orientation for oxidation at 770 K and with rutile (200) orientation for oxidation at 970 K. EELS spectra interpreted in terms of the molecular orbitals of a (TiO6)8- cluster show that the local octahedral environment of titanium atoms is preserved on native oxides, even if these oxides are not crystallized.

Failure Mechanisms of the Protective Coatings for the Hot Stamping Applications

NASA Astrophysics Data System (ADS)

Zhao, Chen

In the present study, four different nitriding techniques were carried on the ductile irons NAAMS-D6510 and cast steels NAAMS-S0050A, which are widely used stamping die materials; duplex treatments (PVD CrN coating+nitriding) were carried on H13 steels, which are common inserts for the hot stamping dies. Inclined impact-sliding wear tests were performed on the nitriding cases under simulated stamping conditions. Surface profilometer, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) were used to investigate the wear and failure mechanisms of the protective coatings. It was found that the nitrided ductile iron samples performed better than the nitrided cast steel specimens. High temperature inclined impact-sliding wear tests were carried out on the CrN coatings. It was found that the coating performed better at elevated temperature. XPS analysis indicated the top surface layer (about 3-4nm) of the coating was oxidized at 400 °C and formed a Cr2O3 protective film. The in-situ formation of the thin Cr2O3 protective layer likely led to the change of wear mechanisms from severe adhesive failure to mild abrasive wear.

Stoichiometry dependence of potential screening at La ( 1 - δ ) Al ( 1 + δ ) O 3 / SrTiO 3 interfaces

DOE PAGES

Weiland, Conan; Sterbinsky, George E.; Rumaiz, Abdul K.; ...

2015-04-03

Hard x-ray photoelectron spectroscopy (HAXPES) and variable kinetic energy x-ray photoelectron spectroscopy (VKE-XPS) analyses have been performed on ten-unit-cell-thick La (1-δ)Al (1+δ)O₃ films, with La:Al ratios of 1.1, 1.0, and 0.9, deposited on SrTiO₃. Only Al-rich films are known to have a conductive interface. VKE-XPS, coupled with maximum entropy analysis, shows significant differences in the compositional depth profile among the Al-rich, La-rich, and stoichiometric films: significant La enrichment at the interface is observed in the La-rich and stoichiometric films, while the Al-rich film shows little to no intermixing. Additionally, the La-rich and stoichiometric films show a high concentration of Almore » at the surface, which is not observed in the Al-rich film. HAXPES valence band (VB) analysis shows a broadening of the VB for the Al-rich sample relative to the stoichiometric and La-rich samples. This broadening is consistent with an electric field across the Al-rich film. These results are consistent with a defect-driven electronic reconstruction.« less

Flame retardancy and thermal behavior of intumescent flame-retardant EVA composites with an efficient triazine-based charring agent

NASA Astrophysics Data System (ADS)

Xu, Bo; Ma, Wen; Wu, Xiao; Qian, Lijun; Jiang, Shan

2018-04-01

Intumescent flame retardant (IFR) EVA composites were prepared based on a hyperbranched triazine charring-foaming agent (HTCFA) and ammonium polyphosphate (APP). The synergistic effect of HTCFA and APP on the flame retardancy and thermal behavior of the composites were investigated through flammability tests, cone calorimeter measurements, thermogravimetric analysis (TGA) including evolved gas analysis (TG-IR) and residue analysis (Fourier transform infrared (FTIR), laser Raman spectroscopy (LRS), x-ray Photoelectron Spectroscopy (XPS) and scanning electron microscopy (SEM)). The flammability test results showed HTCFA/APP (1/3) system presented the best synergistic effect in flame-retardant EVA composites with the highest LOI value and UL-94 V-0 rating. As for cone calorimeter results, IFR changed the combustion behavior of EVA and resulted in remarkable decrease of flammability and smoke product. TGA results showed the synergistic effect between APP and HTCFA could strengthen the char-forming ability of composites. TG-IR results indicated the melt viscosities and gas release with increasing temperature were well-correlated for EVA/IFR composite. The residue analysis results from SEM, LRS, FT-IR and XPS revealed IFR promoted forming more compact graphitic char layer, connected by rich P–O–C and P–N structures.

Full membrane spanning self-assembled monolayers as model systems for UHV-based studies of cell-penetrating peptides

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

Franz, Johannes; Graham, Daniel J.; Schmüser, Lars

2015-03-01

Biophysical studies of the interaction of peptides with model membranes provide a simple yet effective approach to understand the transport of peptides and peptide based drug carriers across the cell membrane. Therein, the authors discuss the use of self-assembled monolayers fabricated from the full membrane-spanning thiol (FMST) 3-((14-((4'-((5-methyl-1-phenyl-35-(phytanyl)oxy-6,9,12,15,18,21,24,27,30,33,37-undecaoxa-2,3-dithiahenpentacontan-51-yl)oxy)-[1,1'-biphenyl]-4-yl)oxy)tetradecyl)oxy)-2-(phytanyl)oxy glycerol for ultrahigh vacuum (UHV) based experiments. UHV-based methods such as electron spectroscopy and mass spectrometry can provide important information about how peptides bind and interact with membranes, especially with the hydrophobic core of a lipid bilayer. Moreover, near-edge x-ray absorption fine structure spectra and x-ray photoelectron spectroscopy (XPS) data showed thatmore » FMST forms UHV-stable and ordered films on gold. XPS and time of flight secondary ion mass spectrometry depth profiles indicated that a proline-rich amphipathic cell-penetrating peptide, known as sweet arrow peptide is located at the outer perimeter of the model membrane.« less

Staircase polymetalsilicon nanocomplexes - Polymetalphenyl siloxanes: Structure and properties

NASA Astrophysics Data System (ADS)

Shapkin, N. P.; Balanov, M. I.; Razov, V. I.; Gardionov, S. V.; Mayorov, V. Yu; Tokar, E. A.; Papynov, E. K.; Korochentsev, V. V.; Leont'ev, L. B.; Slobodyuk, A. B.; Modin, E. B.

2018-03-01

Polyphenyl siloxanes containing chromium, iron, and aluminum in the backbone chain have been synthesized. The structure of the obtained staircase nano-metal complexes has been studied by the methods of XRD analysis and IR, 29Si and 27Al NMR, and XPS spectroscopy and scanning electron microscopy. Physical-chemical characteristics of these compounds have been investigated by the positron annihilation spectroscopy (PAS) and low-temperature nitrogen adsorption. The data of X-ray diffraction analysis (XRD) enabled us to calculate the size and volume of coherent scattering regions (CSR) and the cross-section area of the polymer chains. By means of the PAS method, the specific volumes of positron (Ve+) and positronium (Vps) "traps" have been calculated. The data of 29Si NMR spectroscopy have shown the presence of T2 and T3 fragments in the structure. As was shown on the basis of the data of 27Al NMR and XPS spectroscopy, tetrahedral (66%) and octahedral surroundings of the metal atom were realized in the backbone chain. The obtained data were used to describe a spatial layered structure of phenyl siloxanes containing trivalent metals. The electron microscopy of nanocomplexes revealed the presence of spherical particles, whose size changes in cases of chromium, iron, and aluminum. Using the data of low-temperature nitrogen adsorption, it was assumed that the specific surface area was filled with a layer of compacted spherical particles, whereas the layer thickness was determined, in its turn, by the specific polarizing potential (SPP) calculated as a ratio of the polarizing potential (PP) to the volume of voids between coherent scattering regions. Similar dependence is observed between the layer thickness and the specific polarizing potential calculated as a ratio of the polarizing potential to the positronium "trap" volume. A direct dependence between the thickness of the spherical particles layer and the specific polarizing potential has been demonstrated. The assumption on a fractal structure of spherical particles was made. Tribotechnical properties of the motor oil with metal siloxane additives have been studied.

Surface characterization of polydimethylsiloxane treated pharmaceutical glass containers by X-ray-excited photo- and Auger electron spectroscopy.

PubMed

Mundry, T; Surmann, P; Schurreit, T

2000-12-01

The siliconization of pharmaceutical glass containers is an industrially frequently applied procedure. It is done by spreading an aqueous silicone oil emulsion film on the inner surface and successive heat curing treatment at temperatures above 300 degrees C for 10-30 min. It was often proposed that a covalent bonding of PDMS to the glass or branching of the linear PDMS occurs during heat treatment. The present study was performed for a detailed investigation of the glass and silicone (polydimethylsiloxane = PDMS) chemical state before and after heat-curing treatment and analysis of the bond nature. Combined X-ray excited photoelectron (XPS) and Auger electron spectroscopy as well as angle resolved XPS-measurements were used for analysis of the glass samples. The silicon surface atoms of the borosilicate container glass were transformed to a quartz-like compound whereas the former linear PDMS had a branched, two-dimensional structure after the heat curing treatment. It was concluded that the branching indicates the formation of new siloxane bonds to the glass surface via hydroxyl groups. Further evidence for the presence of bonded PDMS at the glass surface can be found in the valence band spectra of the siliconized and untreated samples. However, this bond could not be detected directly due to its very similar nature to the siloxane bonds of the glass matrix and the organosilicon backbone of PDMS. Due to the high variation of data from the siliconized samples it was concluded, that the silicone film is not homogeneous. Previously raised theories of reactions during heat-curing glass siliconization are supported by the XPS data of this investigation. Yet, the postulation of fixing or baking the silicone on the glass surface is only partially true since the bonded layer is very thin and most of the silicone originally on the surface after heat curing can be removed by suitable solvents. This fraction can therefore still interact with drug products being in contact to the siliconized container wall.

Visible-light-driven Bi 2 O 3 /WO 3 composites with enhanced photocatalytic activity

DOE PAGES

Adhikari, Shiba P.; Dean, Hunter; Hood, Zachary D.; ...

2015-10-19

Semiconductor heterojunctions (composites) have been shown to be effective photocatalytic materials to overcome the drawbacks of low photocatalytic efficiency that results from electron–hole recombination and narrow photo-response range. We prepared a novel visible-light-driven Bi 2O 3/WO 3 composite photocatalyst by hydrothermal synthesis. The composite was characterized by scanning transmission electron microscopy (STEM), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), Brunauer–Emmett–Teller (BET) surface area, Raman spectroscopy, photoluminescence spectroscopy (PL) and electrochemical impedance spectroscopy (EIS) to better understand the structures, compositions, morphologies and optical properties. Bi 2O 3/WO 3 heterojunction was found to exhibit significantly higher photocatalyticmore » activity towards the decomposition of Rhodamine B (RhB) and 4-nitroaniline (4-NA) under visible light irradiation compared to that of Bi 2O 3 and WO 3. A tentative mechanism for the enhanced photocatalytic activity of the heterostructured composite is discussed based on observed activity, band position calculations, photoluminescence, and electrochemical impedance data. Our study provides a new strategy for the design of composite materials with enhanced visible light photocatalytic performance.« less

X-ray photoelectron spectroscopic and morphologic studies of Ru nanoparticles deposited onto highly oriented pyrolytic graphite

NASA Astrophysics Data System (ADS)

Bavand, R.; Yelon, A.; Sacher, E.

2015-11-01

Ruthenium nanoparticles (Ru NPs) function as effective catalysts in specific reactions, such as methanation and Fischer-Tropsch syntheses. It is our purpose to physicochemically characterize their surfaces, at which catalysis occurs, by surface-sensitive X-ray photoelectron spectroscopy (XPS), using the symmetric peak component anaylsis technique developed in our laboratory to reveal previously hidden components. Ru NPs were deposited by evaporation (0.25-1.5 nm nominal deposition range) onto highly oriented pyrolytic graphite (HOPG). In addition to their surfaces being characterized by XPS, an indication of morphology was obtained from transmission electron microscopy (TEM). Our use of symmetric peak component XPS analysis has revealed detailed information on a previously unidentified surface oxide initially formed, as well as on the valence electronic structure and its variation with NP size, information that is of potential importance in the use of these NPs in catalysis. Each of the several Ru core XPS spectra characterized (3d, 3p and 3s) was found to be composed of three symmetric components. Together with two metal oxide O1s components, these give evidence of a rather complex, previously unidentified oxide that is initially formed. The Ru valence band (4d and 5s) spectra clearly demonstrate a loss of metallicity, a simultaneous increase of the Kubo gap, and an abrupt transfer in valence electron density from the 4d to the 5s orbitals (known as electron spill-over), as the NP size decreases below 0.5 nm. TEM photomicrographs, as a function of deposition rate, show that, at a rate that gives insufficient time for the NP condensation energy to dissipate, the initially well-separated NPs are capable of diffusing laterally and aggregating. This indicates weak NP bonding to the HOPG substrate. Carbide is formed, at both high and low deposition rates, at Ru deposition thicknesses greater than 0.25 nm, its formation explained by Ru NPs reacting with residual hydrocarbon vapor, under the influence of the heat of condensation released on Ru deposition, and not by Ru reacting with the HOPG substrate.

Improved electron transfer and plasmonic effect in dye-sensitized solar cells with bi-functional Nb-doped TiO2/Ag ternary nanostructures.

PubMed

Park, Jung Tae; Chi, Won Seok; Jeon, Harim; Kim, Jong Hak

2014-03-07

TiO2 nanoparticles are surface-modified via atom transfer radical polymerization (ATRP) with a hydrophilic poly(oxyethylene)methacrylate (POEM), which can coordinate to the Ag precursor, i.e. silver trifluoromethanesulfonate (AgCF3SO3). Following the reduction of Ag ions, a Nb2O5 doping process and calcination at 450 °C, bi-functional Nb-doped TiO2/Ag ternary nanostructures are generated. The resulting nanostructures are characterized by energy-filtering transmission electron microscopy (EF-TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and UV-visible spectroscopy. The dye-sensitized solar cell (DSSC) based on the Nb-doped TiO2/Ag nanostructure photoanode with a polymerized ionic liquid (PIL) as the solid polymer electrolyte shows an overall energy conversion efficiency (η) of 6.9%, which is much higher than those of neat TiO2 (4.7%) and Nb-doped TiO2 (5.4%). The enhancement of η is mostly due to the increase of current density, attributed to the improved electron transfer properties including electron injection, collection, and plasmonic effects without the negative effects of charge recombination or problems with corrosion. These properties are supported by intensity modulated photocurrent/voltage spectroscopy (IMPS/IMVS) and incident photon-to-electron conversion efficiency (IPCE) measurements.

On the origin of an unusual dependence of (bio)chemical reactivity of ferric hydroxides on nanoparticle size.

PubMed

Chernyshova, I V; Ponnurangam, S; Somasundaran, P

2010-11-14

Application of in situ UV-Vis absorption spectroscopy and ex situ X-ray photoelectron spectroscopy (XPS) makes it possible to resolve the controversies about the electronic properties of hematite (α-Fe(2)O(3)) nanoparticles (NPs) and, on this basis, to rationalize the unusual dependence of aquatic (bio)chemistry of these NPs on NP size. 2-Line ferrihydrite (FH) is also included in the study as the end polymorph of the size-driven phase transformation of hematite NPs in aqueous media. It is shown that the absorption edge of all NPs studied is due to the direct O 2p-Fe 3d charge transfer (CT) process, while a manifold of weak bands superimposed onto two main p-d CT bands is attributed to the d-d ligand field transitions. The band gap decreases from 2.95 to 2.18 eV with increasing NP size from 7 nm to 120 nm. This effect is attributed to restoration of hematite lattice structure, which ultimately results in an increase in the O 2p-Fe 3d hybridization, stabilization of the valence band, and delocalization of valence electrons, as confirmed by XPS. Finally, we show that the optical effects such as the Mie resonance significantly distort absorption spectra of hematite NPs larger than ∼120 nm. Possible impacts of these findings on (photo)catalytic and biochemical properties of ferric (hydr)oxide NPs are discussed.

Characterisation of the surface topography, tomography and chemistry of fretting corrosion product found on retrieved polished femoral stems.

PubMed

Bryant, M; Ward, M; Farrar, R; Freeman, R; Brummitt, K; Nolan, J; Neville, A

2014-04-01

This study presents the characterisation of the surface topography, tomography and chemistry of fretting corrosion product found on retrieved polished femoral stems. Scanning Electron Microscopy (SEM), X-ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM) and Fourier Transform Infrared Spectroscopy (FI-IR) were utilised in order to assess the surface morphology of retrieved Metal-on-Metal Total Hip Replacements and surface chemistry of the films found on the surface. Gross slip, plastic deformation and directionality of the surface were extensively seen on the proximal surfaces of the retrievals. A more corrosive phenomenon was observed in the distal regions of the stem, demonstrating a seemingly intergranular attack. Tribochemical reactions were seen to occur within the stem-cement interfaces with tribofilms being observed on the femoral stem and counterpart PMMA bone cement. XPS, TEM-EDX and FT-IR analyses demonstrated that the films present in the stem surfaces were a complex mixture of chromium oxide and amorphous organic material. A comparison between current experimental and clinical literature has been conducted and findings from this study demonstrate that the formation and chemistry of films are drastically influenced by the type of wear or degradation mechanism. Films formed in the stem-cement interface are thought to further influence the biological environment outside the stem-cement interface due to the formation of Cr and O rich films within the interface whilst Co is free to migrate away. © 2013 Elsevier Ltd. All rights reserved.

The effect of gradient boracic polyanion-doping on structure, morphology, and cycling performance of Ni-rich LiNi0.8Co0.15Al0.05O2 cathode material

NASA Astrophysics Data System (ADS)

Chen, Tao; Li, Xiang; Wang, Hao; Yan, Xinxiu; Wang, Lei; Deng, Bangwei; Ge, Wujie; Qu, Meizhen

2018-01-01

A gradient boracic polyanion-doping method is applied to Ni-rich LiNi0.8Co0.15Al0.05O2 (NCA) cathode material in this study to suppress the capacity/potential fade during charge-discharge cycling. Scanning electron microscope (SEM) results show that all samples present spherical morphology and the secondary particle size increases with increasing boron content. X-ray diffraction (XRD), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) results demonstrate that boracic polyanions are successfully introduced into the bulk material and more enriched in the outer layer. XPS analysis further reveals that the valence state of Ni3+ is partly reduced to Ni2+ at the surface due to the incorporation of boracic polyanions. From the electrochemical measurements, B0.015-NCA electrode exhibits excellent cycling performance, even at high potential and elevated temperature. Moreover, the SEM images illustrate the presence of cracks and a thick SEI layer on pristine particles after 100 cycles at high temperature, while the B0.015-NCA particles show an intact structure and thin SEI layer. Electrochemical impedance spectroscopy confirms that the boracic polyanion doping could hinder the impedance increase during cycling at elevated temperature. These results clearly indicate that the gradient boracic polyanion-doping contributes to the remarkable enhancement of structure stability and cycling performance of NCA.

Treatment for GaSb surfaces using a sulphur blended (NH4)2S/(NH4)2SO4 solution

NASA Astrophysics Data System (ADS)

Murape, D. M.; Eassa, N.; Neethling, J. H.; Betz, R.; Coetsee, E.; Swart, H. C.; Botha, J. R.; Venter, A.

2012-07-01

A sulphur based chemical, [(NH4)2S/(NH4)2SO4] to which S has been added, not previously reported for the treatment of (1 0 0) n-GaSb surfaces, is introduced and benchmarked against the commonly used passivants Na2S·9H2O and (NH4)2S. The surfaces of the treated material were studied by scanning electron microscopy (SEM), Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). It has been found that the native oxides present on the GaSb surface are more effectively removed when treated with ([(NH4)2S/(NH4)2SO4] + S) than with (NH4)2S or Na2S·9H2O, as evidenced by the ratio of the O506 eV to Sb457 eV AES peaks. XPS results reveal that Sb2S3/Sb2S5 "replaces" Sb2O3/Sb2O5, suggesting that sulphur atoms substitute oxygen atoms in Sb2O3/Sb2O5 to form Sbsbnd S. It seems sulphurization only partially removes Ga2O3. Treatment with ([(NH4)2S/(NH4)2SO4] + S) also results in a noteworthy improvement in the current-voltage (I-V) characteristics of Au/n-GaSb Schottky contacts compared to those fabricated on as-received material.

Hierarchically porous carbon/polyaniline hybrid for use in supercapacitors.

PubMed

Joo, Min Jae; Yun, Young Soo; Jin, Hyoung-Joon

2014-12-01

A hierarchically porous carbon (HPC)/polyaniline (PANI) hybrid electrode was prepared by the polymerization of PANI on the surface of the HPC via rapid-mixing polymerization. The surface morphologies and chemical composition of the HPC/PANI hybrid electrode were characterized using transmission electron microscopy and X-ray photoelectron spectroscopy (XPS), respectively. The surface morphologies and XPS results for the HPC, PANI and HPC/PANI hybrids indicate that PANI is coated on the surface of HPC in the HPC/PANI hybrids which have two different nitrogen groups as a benzenoid amine (-NH-) peak and positively charged nitrogen (N+) peak. The electrochemical performances of the HPC/PANI hybrids were analyzed by performing cyclic voltammetry and galvanostatic charge-discharge tests. The HPC/PANI hybrids showed a better specific capacitance (222 F/g) than HPC (111 F/g) because of effect of pseudocapacitor behavior. In addition, good cycle stabilities were maintained over 1000 cycles.

Observing Graphene Grow: Catalyst–Graphene Interactions during Scalable Graphene Growth on Polycrystalline Copper

PubMed Central

2013-01-01

Complementary in situ X-ray photoelectron spectroscopy (XPS), X-ray diffractometry, and environmental scanning electron microscopy are used to fingerprint the entire graphene chemical vapor deposition process on technologically important polycrystalline Cu catalysts to address the current lack of understanding of the underlying fundamental growth mechanisms and catalyst interactions. Graphene forms directly on metallic Cu during the high-temperature hydrocarbon exposure, whereby an upshift in the binding energies of the corresponding C1s XPS core level signatures is indicative of coupling between the Cu catalyst and the growing graphene. Minor carbon uptake into Cu can under certain conditions manifest itself as carbon precipitation upon cooling. Postgrowth, ambient air exposure even at room temperature decouples the graphene from Cu by (reversible) oxygen intercalation. The importance of these dynamic interactions is discussed for graphene growth, processing, and device integration. PMID:24041311

Composition measurement of epitaxial Sc x Ga1-x N films

NASA Astrophysics Data System (ADS)

Tsui, H. C. L.; Goff, L. E.; Barradas, N. P.; Alves, E.; Pereira, S.; Palgrave, R. G.; Davies, R. J.; Beere, H. E.; Farrer, I.; Ritchie, D. A.; Moram, M. A.

2016-06-01

Four different methods for measuring the compositions of epitaxial Sc x Ga1-x N films were assessed and compared to determine which was the most reliable and accurate. The compositions of epitaxial Sc x Ga1-x N films with 0 ≤ x ≤ 0.26 were measured directly using Rutherford backscattering (RBS) and x-ray photoelectron spectroscopy (XPS), and indirectly using c lattice parameter measurements from x-ray diffraction and c/a ratio measurements from electron diffraction patterns. RBS measurements were taken as a standard reference. XPS was found to underestimate the Sc content, whereas c lattice parameter and c/a ratio were not reliable for composition determination due to the unknown degree of strain relaxation in the film. However, the Sc flux used during growth was found to relate linearly with x and could be used to estimate the Sc content.

Thickness Influence on In Vitro Biocompatibility of Titanium Nitride Thin Films Synthesized by Pulsed Laser Deposition

PubMed Central

Duta, Liviu; Stan, George E.; Popa, Adrian C.; Husanu, Marius A.; Moga, Sorin; Socol, Marcela; Zgura, Irina; Miculescu, Florin; Urzica, Iuliana; Popescu, Andrei C.; Mihailescu, Ion N.

2016-01-01

We report a study on the biocompatibility vs. thickness in the case of titanium nitride (TiN) films synthesized on 410 medical grade stainless steel substrates by pulsed laser deposition. The films were grown in a nitrogen atmosphere, and their in vitro cytotoxicity was assessed according to ISO 10993-5 [1]. Extensive physical-chemical analyses have been carried out on the deposited structures with various thicknesses in order to explain the differences in biological behavior: profilometry, scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction and surface energy measurements. XPS revealed the presence of titanium oxynitride beside TiN in amounts that vary with the film thickness. The cytocompatibility of films seems to be influenced by their TiN surface content. The thinner films seem to be more suitable for medical applications, due to the combined high values of bonding strength and superior cytocompatibility. PMID:28787846

Structure of mono- and bimetallic heterogeneous catalysts based on noble metals obtained by means of fluid technology and metal-vapor synthesis

NASA Astrophysics Data System (ADS)

Said-Galiev, E. E.; Vasil'kov, A. Yu.; Nikolaev, A. Yu.; Lisitsyn, A. I.; Naumkin, A. V.; Volkov, I. O.; Abramchuk, S. S.; Lependina, O. L.; Khokhlov, A. R.; Shtykova, E. V.; Dembo, K. A.; Erkey, C.

2012-10-01

Monometallic nanocomposites are obtained with the use of supercritical carbon dioxide (fluid technique) and metal-vapor synthesis (MVS), while bimetallic nanocomposites of Pt and Au noble metals and γ-Al2O3 oxide matrix are synthesized by a combination of these two methods. The structures, concentrations, and chemical states of metal atoms in composites are studied by means of small-angle X-ray scattering (SAXS), transparent electron microscopy (TEM), X-ray fluorescent analysis (XFA), and X-ray photoelectron spectroscopy (XPS). The neutral state of metal atoms in clusters is shown by XPS and their size distribution is found according to SAXS; as is shown, it is determined by the pore sizes of the oxide matrices and lies in the range of 1 to 50 nm. The obtained composites manifest themselves as effective catalysts in the oxidation of CO to CO2.

Nitridation of silicon by nitrogen neutral beam

NASA Astrophysics Data System (ADS)

Hara, Yasuhiro; Shimizu, Tomohiro; Shingubara, Shoso

2016-02-01

Silicon nitridation was investigated at room temperature using a nitrogen neutral beam (NB) extracted at acceleration voltages of less than 100 V. X-ray photoelectron spectroscopy (XPS) analysis confirmed the formation of a Si3N4 layer on a Si (1 0 0) substrate when the acceleration voltage was higher than 20 V. The XPS depth profile indicated that nitrogen diffused to a depth of 36 nm for acceleration voltages of 60 V and higher. The thickness of the silicon nitrided layer increased with the acceleration voltages from 20 V to 60 V. Cross-sectional transmission electron microscopy (TEM) analysis indicated a Si3N4 layer thickness of 3.1 nm was obtained at an acceleration voltage of 100 V. Moreover, it was proved that the nitrided silicon layer formed by the nitrogen NB at room temperature was effective as the passivation film in the wet etching process.

Adsorption and reaction of propene on Ni(100)

NASA Astrophysics Data System (ADS)

Kleyna, R.; Borgmann, D.; Wedler, G.

1998-05-01

Photoelectron spectroscopy (UPS, XPS) and thermal desorption techniques were used to study the chemisorption and decomposition reactions of propene on Ni(100). Propene is molecularly adsorbed at temperatures below 150 K. At saturation coverage the TD spectrum shows two propene desorption peaks at 155 and 225 K and three hydrogen desorption peaks at 300, 330 and 380 K with a shoulder at 420 K. No other desorbing species could be detected. The amount of desorption of propene was determined by XPS to be 20% of the saturation coverage. The electronic structure of adsorbed propene and the chemical nature of its decomposition products were deduced from UP and XP spectra taken at saturation coverage. Adsorption at low temperatures results in a π-bonded species which is stable up to 150 K. At temperatures above 150 K the UP spectra point to a σ-bonded species which decomposes further at temperatures above 260 K.

Self-repairing vanadium-zirconium composite conversion coating for aluminum alloys

NASA Astrophysics Data System (ADS)

Zhong, Xin; Wu, Xiaosong; Jia, Yuyu; Liu, Yali

2013-09-01

In this paper, new self-repairing vanadium-zirconium composite conversion coating was prepared and investigated by Electrochemical impedance spectra (EIS), Scanning electron microscope (SEM) and X-ray photoelectron spectroscopy (XPS), respectively. EIS results showed that V-Zr conversion coating with hydrogen peroxide modified (VZO) revealed an increasing corrosion resistance in corrosive media which meant a certain self-repairing effect. SEM comparison photos also disclosed that VZO treated with scratches was gradually ameliorated from the initial cracked configuration to fewer cracks and more fillers through an immersion of 3.5% NaCl solution. XPS results demonstrated that the content of vanadium on VZO increased and zirconium declined when immersed in the corrosive solution. This explained further that the self-repairing ability could be related to vanadium. From the above results, we inferred possible structures of VZO and proposed that self-repairing effect was achieved through a hydrolysis condensation polymerization process of vanadate in the localized corrosion area.

Study of mesoporous CdS-quantum-dot-sensitized TiO2 films by using X-ray photoelectron spectroscopy and AFM

PubMed Central

Wojcieszak, Robert; Raj, Gijo

2014-01-01

Summary CdS quantum dots were grown on mesoporous TiO2 films by successive ionic layer adsorption and reaction processes in order to obtain CdS particles of various sizes. AFM analysis shows that the growth of the CdS particles is a two-step process. The first step is the formation of new crystallites at each deposition cycle. In the next step the pre-deposited crystallites grow to form larger aggregates. Special attention is paid to the estimation of the CdS particle size by X-ray photoelectron spectroscopy (XPS). Among the classical methods of characterization the XPS model is described in detail. In order to make an attempt to validate the XPS model, the results are compared to those obtained from AFM analysis and to the evolution of the band gap energy of the CdS nanoparticles as obtained by UV–vis spectroscopy. The results showed that XPS technique is a powerful tool in the estimation of the CdS particle size. In conjunction with these results, a very good correlation has been found between the number of deposition cycles and the particle size. PMID:24605274

Utilization of visible to NIR light energy by Yb+3, Er+3 and Tm+3 doped BiVO4 for the photocatalytic degradation of methylene blue

NASA Astrophysics Data System (ADS)

Regmi, Chhabilal; Kshetri, Yuwaraj K.; Ray, Schindra Kumar; Pandey, Ramesh Prasad; Lee, Soo Wohn

2017-01-01

Lanthanide-doped BiVO4 semiconductors with efficient photocatalytic activities over a broad range of the solar light spectrum have been synthesized by the microwave hydrothermal method using ethylenediaminetetraacetic acid (EDTA). The structural, morphological, and optical properties of the as-synthesized samples were evaluated by Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-ray powder diffraction (XRD), Raman spectroscopy, FT-IR spectroscopy, UV-vis diffuse reflectance spectroscopy (DRS), and photoluminescence spectroscopy (PL). The chemical compositions were analyzed by X-ray photoelectron spectroscopy (XPS). The toxicity of the samples was measured using Mus musculus skin melanoma cells (B16-F10 (ATCC® CRL-6475™)) and were found to be nontoxic for human cells. The photocatalytic efficiency of the prepared samples was evaluated by methylene blue (MB) degradation. The best photocatalytic activity was shown by BiVO4 with 6:3:3 mol percentage of Yb+3:Er+3:Tm+3 in all solar light spectrum. The synthesized samples possess low band gap energy and a hollow structure suitable for the better photocatalytic activity. The observed NIR photoactivity supports that the upconversion mechanism is involved in the overall photocatalytic process. Therefore, this approach provides a better alternative upconversion material for integral solar light absorption.

Large-scale synthesis of coiled-like shaped carbon nanotubes using bi-metal catalyst

NASA Astrophysics Data System (ADS)

Krishna, Vemula Mohana; Somanathan, T.; Manikandan, E.; Umar, Ahmad; Maaza, M.

2018-02-01

Carbon nanomaterials (CNMs), especially carbon nanotubes (CNTs) with coiled structure exhibit scientifically fascinating. They may be projected as an innovative preference to future technological materials. Coiled carbon nanotubes (c-CNTs) on a large-scale were successfully synthesized with the help of bi-metal substituted α-alumina nanoparticles catalyst via chemical vapor deposition (CVD) technique. Highly spring-like carbon nanostructures were observed by field emission scanning electron microscope (FESEM) examination. Furthermore, the obtained material has high purity, which correlates the X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDX) analysis. Raman spectroscopy reveals that the carbon multi layers are well graphitized and crystalline, even if they have defects in its structure due to coiled morphology. High-resolution transmission electron microscope (HRTEM) describes internal structure and dia of the product. Ultimately, results support the activity of bi-metal impregnated α-alumina nanoparticles catalyst to determine the high yield, graphitization and internal structure of the material. We have also studied the purified c-CNTs magnetic properties at room temperature and will be an added advantage in several applications.

Theoretical studies on the structural and spectra properties of two C74 fullerenes and the chlorinated species C74Cl10

NASA Astrophysics Data System (ADS)

Zheng, Mei; Song, Xitong; Li, Xiaoqi; Qi, Jiayuan

2018-07-01

The geometrical/electronic structures, X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine structure spectroscopy of two especially C74 fullerenes (D3h-C74 and C1-C74) and the chlorinated species C1-C74Cl10, which are newly isolated in the experiment, have been calculated by means of the density functional theory (DFT) method. Effective changes in the electronic structure and simulated X-ray spectra have been observed after chlorination. Strong isomer dependence has been found in both spectra, thus the 'fingerprints' in the spectra can be employed as a tool to identify the isomers. The ultraviolet-visible (UV-vis) absorption spectrum of C1-C74Cl10 has been performed by using the time-dependent DFT method. The generated UV-vis spectrum coincides with the previous experimental counterpart. The results of this work can provide useful information especially for isomer identification and further study on fullerenes by means of the aforementioned spectroscopy techniques.

Synthesis of Fluorinated Graphene/CoAl-Layered Double Hydroxide Composites as Electrode Materials for Supercapacitors.

PubMed

Peng, Weijun; Li, Hongqiang; Song, Shaoxian

2017-02-15

CoAl-layered double hydroxide/fluorinated graphene (CoAl-LDH/FGN) composites were fabricated via a two-step hydrothermal method. The synthesized CoAl-LDH/FGN composites have been characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and electrochemical measurements. The results indicated that the fluorinated carbon with various configuration forms were grafted onto the framework of graphene, and the C-F bond configuration and fluorine content could be tuned by the fluorination time. Most of semi-ionic C-F bonds were formed at an appropriate fluorination time and, then, converted into fluorine rich surface groups (such as CF 2 , CF 3 , etc.) which were electrochemically inactive as the fluorination time prolonged. Moreover, the CoAl-LDH/FGN composites prepared at the optimal fluorination time exhibited the highest specific capacitance (1222 F/g at 1 A/g), the best rate capability, and the most stable capacitance retention, which offered great promise as electrode materials for supercapacitors.

Introduction of oxygen vacancies and fluorine into TiO{sub 2} nanoparticles by co-milling with PTFE

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

Senna, Mamoru, E-mail: senna@applc.keio.ac.jp; Sepelak, Vladimir; Shi, Jianmin

2012-03-15

Solid-state processes of introducing oxygen vacancies and transference of fluorine to n-TiO{sub 2} nanoparticles by co-milling with poly(tetrafluoroethylene) (PTFE) powder were examined by diffuse reflectance spectroscopy (DRS) of UV, visual, near- and mid-IR regions, thermal analyses (TG-DTA), energy-dispersive X-ray spectroscopy (EDXS), X-ray photoelectron spectroscopy (XPS), high-resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD). The broad absorption peak at around 8800 cm{sup -1} (1140 nm) was attributed to the change in the electronic states, viz. electrons trapped at the oxygen vacancies (Vo) and d-d transitions of titanium ions. Incorporation of fluorine into n-TiO{sub 2} was concentrated at the near surfacemore » region and amounted to ca. 40 at% of the total fluorine in PTFE, after co-milling for 3 h, as confirmed by the F1s XPS spectrum. The overall atomic ratio, F/Ti, determined by EDXS was 0.294. By combining these analytical results, a mechanism of the present solid state processes at the boundary between PTFE and n-TiO{sub 2} was proposed. The entire process is triggered by the partial oxidative decomposition of PTFE. This is accompanied by the abstraction of oxygen atoms from the n-TiO{sub 2} lattices. Loss of the oxygen atoms results in the formation of the diverse states of locally distorted coordination units of titania, i.e. TiO{sub 6-n}Vo{sub n}, located at the near surface region. This leads subsequent partial ligand exchange between F and O, to incorporate fluorine preferentially to the near surface region of n-TiO{sub 2} particles, where local non-crystalline states predominate. - Graphical abstract: Scheme of the reaction processes: (a) pristine mixture, (b) oxygen abstraction from TiO{sub 2} and (c) fluorine migration from PTFE to TiO{sub 2}. Highlights: Transfer of fluorine from PTFE to n-TiO{sub 2} in a dry solid state process was confirmed. Black-Right-Pointing-Pointer 40% of F in PTFE was incorporated to the near surface region of n-TiO{sub 2} nanoparticles. Black-Right-Pointing-Pointer The transfer process is triggered by the oxidative decomposition of PTFE. Black-Right-Pointing-Pointer Fluorine incorporation is mediated by the formation of oxygen vacancies. Black-Right-Pointing-Pointer The sequential mechanisms are verified by XPS, EDXS, HRTEM, TG and DRS.« less

Facile solvothermal synthesis of cube-like Ag@AgCl: a highly efficient visible light photocatalyst

NASA Astrophysics Data System (ADS)

Han, Lei; Wang, Ping; Zhu, Chengzhou; Zhai, Yueming; Dong, Shaojun

2011-07-01

In this paper, a stable and highly efficient plasmonic photocatalyst, Ag@AgCl, with cube-like morphology, has been successfully prepared via a simple hydrothermal method. Using methylene dichloride as chlorine source in the synthesis can efficiently control the morphology of Ag@AgCl, due to the low release rate of chloride ions. Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectra were used to characterize the obtained product. The photocatalytic activity of the obtained product was evaluated by the photodegradation of methyl orange (MO) under visible light irradiation, and it was found, interestingly, that Ag@AgCl exhibits high visible light photocatalytic activity and good stability.In this paper, a stable and highly efficient plasmonic photocatalyst, Ag@AgCl, with cube-like morphology, has been successfully prepared via a simple hydrothermal method. Using methylene dichloride as chlorine source in the synthesis can efficiently control the morphology of Ag@AgCl, due to the low release rate of chloride ions. Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectra were used to characterize the obtained product. The photocatalytic activity of the obtained product was evaluated by the photodegradation of methyl orange (MO) under visible light irradiation, and it was found, interestingly, that Ag@AgCl exhibits high visible light photocatalytic activity and good stability. Electronic supplementary information (ESI) available: SEM images of the AgCl samples synthesized by changing the addition amount of PVP and AgNO3. See DOI: 10.1039/c1nr10247h

The synthesis of Ag/polypyrrole coaxial nanocables via ion adsorption method using different oxidants

NASA Astrophysics Data System (ADS)

Qiu, Teng; Xie, Huxiao; Zhang, Jiangru; Zahoor, Amad; Li, Xiaoyu

2011-03-01

Ag/polypyrrole (PPy) coaxial nanocables (NCs) were synthesized by an ion adsorption method. In this method, the pre-made Ag nanowires (NWs) were dispersed in the aqueous solution of copper acetate (Cu(Ac)2), and the Cu2+ ions adsorbed onto the surface of Ag NWs can oxidize pyrrole monomers to polymerize into uniform PPy sheath outside Ag NWs after the Cu(Ac)2-treated Ag NWs were re-dispersed in the aqueous solution of pyrrole. The morphology of NCs was characterized by transmission electron microscope (TEM) and scanning electron microscope (SEM). The relationship between the thickness of polymer sheath and the concentration of Cu(Ac)2 was established. As Cu(Ac)2 which served as the oxidant can also be replaced by AgNO3 in this synthesis, the differences on the structure of polymer sheath caused by different oxidants were studied by surface-enhanced Raman scattering (SERS), high-resolution transmission electron microscope (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS). Comparing with the characterization results of Ag/PPy NCs synthesized using AgNO3 as the oxidant which indicates the random arrangement of PPy chains at the interface between polymer sheath and Ag NWs, PPy chain oxidized by Cu2+ tends to show a relatively ordered conformation at the interface with the pyrrole rings identically taking the plane vertical to the surface of Ag NWs. In addition, although the main part of the polymer sheath was composed of PPy whatever kind of oxidant was used, the sheath of the NCs oxidized by Cu2+ is typical for the existence of Cu(I)-pyrrole coordinate structures with strong Cu(I)-N bond signal shown in XPS characterization.

Gold/silver core-shell 20 nm nanoparticles extracted from citrate solution examined by XPS

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

Engelhard, Mark H.; Smith, Jordan N.; Baer, Donald R.

Silver nanoparticles of many types are widely used in consumer and medical products. The surface chemistry of particles and the coatings that form during synthesis or use in many types of media can significantly impact the behaviors of particles including dissolution, transformation and biological or environmental impact. Consequently it is useful to be able to extract information about the thickness of surface coatings and other attributes of nanoparticles produced in a variety of ways. It has been demonstrated that X-ray Photoelectron Spectroscopy (XPS) can be reliably used to determine the thickness of organic and other nanoparticles coatings and shells. However,more » care is required to produce reliable and consistent information. Here we report the XPS spectra from gold/silver core-shell nanoparticles of nominal size 20 nm removed from a citrate saturated solution after one and two washing cycles. The Simulation of Electron Spectra for Surface Analysis (SESSA) program had been used to model peak amplitudes to obtain information on citrate coatings that remain after washing and demonstrate the presence of the gold core. This data is provided so that others can compare use of SESSA or other modeling approaches to quantify the nature of coatings to those already published and to explore the impacts particle non-uniformities on XPS signals from core-shell nanoparticles.« less

Effective reduction of p-nitrophenol by silver nanoparticle loaded on magnetic Fe3O4/ATO nano-composite

NASA Astrophysics Data System (ADS)

Karki, Hem Prakash; Ojha, Devi Prashad; Joshi, Mahesh Kumar; Kim, Han Joo

2018-03-01

A silver loaded hematite (Fe3O4) and antimony doped tin oxide (ATO) magnetic nano-composite (Ag-Fe3O4/ATO) was successfully synthesized by in situ one pot green and facile hydrothermal process. The formation of nano-composite, its structure, morphology, and stability were characterized by field emission scanning electron microscopy (FE-SEM), high resolution transmission electron microscopy (HRTEM), electron diffraction spectroscopy (EDS), elemental mapping by high resolution scanning transmission electron microscopy (STEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infra-red spectroscopy (FTIR). UV-vis spectroscopy was used to monitor the catalytic reduction of p-nitrophenol (PNP) into p-aminophenol (PAP) in presence of Ag-Fe3O4/ATO nano-composite with excess of sodium borohydride (NaBH4). The pseudo-first order kinetic equation could describe the reduction of p-nitrophenol with excess of NaBH4. For the first time, ATO surface was used for hydrothermal growth of silver and iron oxide magnetic nanoparticles. The in situ growth of these nanoparticles provided an effective bonding of components of the nano-composite over the surface of ATO nanoparticles. This nano-composite exhibited easy synthesis, high stability, cost effective and rapid separation using external magnet. The excellent catalytic and anti-bacterial activity of as-synthesized silver nano-composite makes it potential nano-catalyst for waste water treatment as well as biomedical application.

Synthesis and Characterization of the Nano-TiO2 Visible Light Photocatalysts: Vanadium Surface Doping Modification

NASA Astrophysics Data System (ADS)

Wang, Xia; Li, Zongbao; Jia, Lichao; Xing, Xiaobo

2018-05-01

A simple strategy to greatly increase the photocatalytic ability of nanocrystalline anatase has been put forward to fabricate efficient TiO2-based photocatalysts under visible irradiation. By surface modification with V ion, samples with different ratios were synthesized by using an incipient wetness impregnation method. The as-prepared specimens were characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and UV-vis diffuse reflectance spectroscopy. The photocatalytic activities were evaluated by using methylene blue degradations. Meanwhile, the optimized loading structure and electronic structures were calculated by using the density function theory (DFT). This work should provide a practical route to reasonably design and synthesize high-performance TiO2-based nanostructured photocatalysts.

Sputter deposition of indium tin oxide onto zinc pthalocyanine: Chemical and electronic properties of the interface studied by photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Gassmann, Jürgen; Brötz, Joachim; Klein, Andreas

2012-02-01

The interface chemistry and the energy band alignment at the interface formed during sputter deposition of transparent conducting indium tin oxide (ITO) onto the organic semiconductor zinc phtalocyanine (ZnPc), which is important for inverted, transparent, and stacked organic light emitting diodes, is studied by in situ photoelectron spectroscopy (XPS and UPS). ITO was sputtered at room temperature and a low power density with a face to face arrangement of the target and substrate. With these deposition conditions, no chemical reaction and a low barrier height for charge injection at this interface are observed. The barrier height is comparable to those observed for the reverse deposition sequence, which also confirms the absence of sputter damage.

Protective Performance of Polyaniline-Sulfosalicylic Acid/Epoxy Coating for 5083 Aluminum

PubMed Central

Liu, Suyun; Liu, Li; Meng, Fandi; Li, Ying; Wang, Fuhui

2018-01-01

Epoxy coatings incorporating different content of sulfosalicylic acid doped polyaniline (PANI-SSA) have been investigated for corrosion protection of 5083 aluminum alloy in 3.5% NaCl solution. The performance of the coatings is studied using a combination of electrochemical impedance spectroscopy (EIS), open circuit potential (OCP), gravimetric tests, adhesion tests, scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The results demonstrate that the content of PANI-SSA not only affects the coating compactness and the transportation of aggressive medium, but also has a significant influence on the-based aluminum. The coating with 2 wt. % PANI-SSA exhibits the best corrosion inhibition due to its good protective properties and the formation of a complete PANI-SSA induced oxide layer. PMID:29438304

Electrocatalytic oxidation of hydrazine and hydroxylamine by graphene oxide-Pd nanoparticle-modified glassy carbon electrode.

PubMed

Lee, Eunhee; Kim, Daekun; You, Jung-Min; Kim, Seul Ki; Yun, Mira; Jeon, Seungwon

2012-12-01

Pd nanoparticle catalysts supported by thiolated graphene oxide (tGO) on a glassy carbon electrode (GCE), and denoted as tGO-Pd/GCE, are used in this study for the electrochemical determination of hydroxylamine and hydrazine. The physicochemical properties of tGO-Pd were characterized by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and electrochemical impedance spectroscopy (EIS). They showed strong catalytic activity toward the oxidation of hydroxylamine and hydrazine. Cyclic voltammetry (CV) and amperometry were used to characterize the sensors' performances. The detection limits of hydroxylamine and hydrazine by tGO-Pd/GCE were 0.31 and 0.25 microM (s/n = 3), respectively. The sensors' sensitivity, selectivity, and stability were also investigated.

Investigation on the effect of collagen and vitamins on biomimetic hydroxyapatite coating formation on titanium surfaces.

PubMed

Ciobanu, Gabriela; Ciobanu, Octavian

2013-04-01

This study uses an in vitro experimental approach to investigate the roles of collagen and vitamins in regulating the deposition of hydroxyapatite layer on the pure titanium surface. Titanium implants were coated with a hydroxyapatite layer under biomimetic conditions by using a supersaturated calcification solution (SCS), modified by adding vitamins A and D3, and collagen. The hydroxyapatite deposits on titanium were investigated by means of scanning electron microscopy (SEM) coupled with X-ray analysis (EDX), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy. The results obtained have shown that hydroxyapatite coatings were produced in vitro under vitamins and collagen influence. Copyright © 2012 Elsevier B.V. All rights reserved.

A novel and expeditious method to fabricate superhydrophobic metal carboxylate surface

NASA Astrophysics Data System (ADS)

Li, Feng; Geng, Xingguo; Chen, Zhi; Zhao, Lei

2012-01-01

This article has presented a novel method to fabricate superhydrophobic metal carboxylate surface on substrates like copper, ferrum, etc. This method markedly shortened the fabrication time to less than one second. The superhydrophobic effect is even better that the contact angle (CA) is 170±1° and the sliding angle (SA) <2°. Scanning electron microscopy (SEM) images showed micro-nano flower-like structures. Fourier transform infrared (FTIR) spectroscopy and X-ray photoelectron spectroscopy (XPS) confirmed that the flower-like structures are composed of Cu[CH3(CH2)12COO]2. The ethanol solution containing fatty acid and metal salt plays a key role in this method. This method has tremendous potentials in industrial production of superhydrophobic materials.

The decisive effect of interface states on the photocatalytic activity of the silver(I) oxide/titanium dioxide heterojunction.

PubMed

Lei, Yanqiang; Lu, Xiaoqing

2017-04-15

A one-step hydrothermal method was adopted to synthesize the Ag 2 O/TiO 2 nanoheterojunction. Its photocatalytic activity was evaluated by degrading methylene blue (MB) aqueous solution under UV and visible light. The MB degradation results showed that the Ag 2 O/TiO 2 nanoheterojunction enhances the photocatalytic activity under UV irradiation rather than visible light. X-ray photoelectron spectroscopy (XPS) was performed to detect the electronic structure at the interface of Ag 2 O and TiO 2 . The XPS results confirmed that the electronic band structure of the nanoheterojunction was determined by the interface states between the Ag 2 O and TiO 2 interface. Thus, the photocatalytic enhancement mechanism can be ascribed to the creation of an additional potential barrier in the conduction band between Ag 2 O and TiO 2 , which facilitates the transport of holes from TiO 2 to Ag 2 O but inhibits the flow of electrons in the reverse direction unless sufficient potential energy is provided to overcome the additional barrier. Our results have provided a new insight on the role of interface states between the p-n nanojunction in the photocatalytic activity. Copyright © 2017 Elsevier Inc. All rights reserved.

Surface study of graphene ink for fine solid lines printed on BOPP Substrate in micro-flexographic printing using XPS analysis technique

NASA Astrophysics Data System (ADS)

Hassan, S.; Yusof, M. S.; Embong, Z.; Ding, S.; Maksud, M. I.

2018-01-01

Micro-flexographic printing is a combination of flexography and micro-contact printing technique. It is a new printing method for fine solid lines printing purpose. Graphene material has been used as depositing agent or printing ink in other printing technique like inkjet printing. This graphene ink is printed on biaxially oriented polypropylene (BOPP) by using Micro-flexographic printing technique. The choose of graphene as a printing ink is due to its wide application in producing electronic and micro-electronic devices such as Radio-frequency identification (RFID) and printed circuit board. The graphene printed on the surface of BOPP substrate was analyzed using X-Ray Photoelectron Spectroscopy (XPS). The positions for each synthetic component in the narrow scan are referred to the electron binding energy (eV). This research is focused on two narrow scan regions which are C 1s and O 1s. Further discussion of the narrow scan spectrum will be explained in detail. From the narrow scan analysis, it is proposed that from the surface adhesive properties of graphene, it is suitable as an alternative printing ink medium for Micro-flexographic printing technique in printing multiple fine solid lines at micro to nano scale feature.

Nitrogen-doped graphene aerogel-supported spinel CoMn2O4 nanoparticles as an efficient catalyst for oxygen reduction reaction

NASA Astrophysics Data System (ADS)

Liu, Yisi; Li, Jie; Li, Wenzhang; Li, Yaomin; Chen, Qiyuan; Zhan, Faqi

2015-12-01

Spinel CoMn2O4 (CMO) nanoparticles grown on three-dimensional (3D) nitrogen-doped graphene areogel (NGA) is prepared by a facile two-step hydrothermal method. The NGA not only possesses the intrinsic property of graphene, but also has abundant pore conformations for supporting spinel metal oxide nanoparticles, thus would be suitable as a good electrocatalysts' support for oxygen reduction reaction (ORR). The structure, morphology, porous properties, and chemical composition of CMO/NGA are investigated by X-ray diffraction (XRD) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, nitrogen adsorption-desorption measurements, and X-ray photoelectron spectroscopy (XPS). The electrocatalytic activity of catalysts is discussed by cyclic voltammograms (CV), electrochemical impedance spectroscopy (EIS), and rotating disk electrode (RDE) measurements in O2-saturated 0.1 M KOH electrolyte. The CMO/NGA hybrid exhibits more positive onset potential and half-wave potential, faster charge transfer than that of CMO and NGA, and its electrocatalytic performance is comparable with the commercial 20 wt.% Pt/C. Furthermore, it mainly favors a direct 4e- reaction pathway, and has excellent ethanol tolerance and high durability, which is attributed to the unique 3D crumpled porous nanostructure of NGA with large specific area and fast electron transport, and the synergic covalent coupling between the CoMn2O4 nanoparticles and NGA.

Study of the electronic structure of electron accepting cyano-films: TCNQversusTCNE.

PubMed

Capitán, Maria J; Álvarez, Jesús; Navio, Cristina

2018-04-18

In this article, we perform systematic research on the electronic structure of two closely related organic electron acceptor molecules (TCNQ and TCNE), which are of technological interest due to their outstanding electronic properties. These studies have been performed from the experimental point of view by the use electron spectroscopies (XPS and UPS) and supported theoretically by the use of ab-initio DFT calculations. The cross-check between both molecules allows us to identify the characteristic electronic features of each part of the molecules and their contribution to the final electronic structure. We can describe the nature of the band gap of these materials, and we relate this with the appearance of the shake-up features in the core level spectra. A band bending and energy gap reduction of the aforementioned electronic structure in contact with a metal surface are seen in the experimental results as well in the theoretical calculations. This behavior implies that the TCNQ thin film accepts electrons from the metal substrate becoming a Schottky n-junction.

Oxidation of MnO(100) and NaMnO2 formation: Characterization of Mn2+ and Mn3+ surfaces via XPS and water TPD

NASA Astrophysics Data System (ADS)

Feng, Xu; Cox, David F.

2018-09-01

The oxidation of clean and Na precovered MnO(100) has been investigated by X-ray photoelectron spectroscopy (XPS), low energy electron diffraction (LEED) and temperature programmed desorption (TPD) of adsorbed water. XPS results indicate that Mn3O4-like and Mn2O3-like surfaces can be formed by various oxidation treatments of clean and nearly-stoichiometric MnO(100), while a NaMnO2-like surface can be produced by the oxidation of MnO(100) pre-covered with multilayers of metallic Na. Water TPD results indicate that water adsorption/desorption is sensitive to the available oxidation states of surface Mn cations, and can be used to distinguish between surfaces exposing Mn2+and Mn3+ cations, or a combination of these oxidation states. Carbon dioxide and water TPD results from the NaMnO2-like surface indicate that pre-adsorbed water blocks the uptake of CO2, while water displaces pre-adsorbed CO2. No indication of a strong reactive interaction is observed between CO2, water and the NaMnO2-like surface under the conditions of our study.

Experimental design and analysis of activators regenerated by electron transfer-atom transfer radical polymerization experimental conditions for grafting sodium styrene sulfonate from titanium substrates.

PubMed

Foster, Rami N; Johansson, Patrik K; Tom, Nicole R; Koelsch, Patrick; Castner, David G

2015-09-01

A 2 4 factorial design was used to optimize the activators regenerated by electron transfer-atom transfer radical polymerization (ARGET-ATRP) grafting of sodium styrene sulfonate (NaSS) films from trichlorosilane/10-undecen-1-yl 2-bromo-2-methylpropionate (ester ClSi) functionalized titanium substrates. The process variables explored were: (1) ATRP initiator surface functionalization reaction time; (2) grafting reaction time; (3) CuBr 2 concentration; and (4) reducing agent (vitamin C) concentration. All samples were characterized using x-ray photoelectron spectroscopy (XPS). Two statistical methods were used to analyze the results: (1) analysis of variance with [Formula: see text], using average [Formula: see text] XPS atomic percent as the response; and (2) principal component analysis using a peak list compiled from all the XPS composition results. Through this analysis combined with follow-up studies, the following conclusions are reached: (1) ATRP-initiator surface functionalization reaction times have no discernable effect on NaSS film quality; (2) minimum (≤24 h for this system) grafting reaction times should be used on titanium substrates since NaSS film quality decreased and variability increased with increasing reaction times; (3) minimum (≤0.5 mg cm -2 for this system) CuBr 2 concentrations should be used to graft thicker NaSS films; and (4) no deleterious effects were detected with increasing vitamin C concentration.

Solid-State Spun Fibers from 1 mm Long Carbon Nanotube Forests Synthesized by Water-Assisted Chemical Vapor Deposition

NASA Technical Reports Server (NTRS)

Zhang, Shanju; Zhu, Lingbo; Minus, Marilyn L.; Chae, han Gi; Jagannathan, Sudhakar; Wong, Ching-Ping; Kowalik, Janusz; Roberson, Luke B.; Kumar, Satish

2007-01-01

In this work, we report continuous carbon nanotube fibers dry-drawn directly from water-assisted CVD grown forests with millimeter scale length. As-drawn nanotube fibers exist as aerogel and can be transformed into more compact fibers through twisting or densification with a volatile liquid. Nanotube fibers are characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Raman microscopy and wide-angle X-ray diffraction (WAXD). Mechanical behavior and electrical conductivity of the post-treated nanotube fibers are investigated.

The effect of bulk/surface defects ratio change on the photocatalysis of TiO2 nanosheet film

NASA Astrophysics Data System (ADS)

Wang, Fangfang; Ge, Wenna; Shen, Tong; Ye, Bangjiao; Fu, Zhengping; Lu, Yalin

2017-07-01

The photocatalysis behavior of TiO2 nanosheet array films was studied, in which the ratio of bulk/surface defects were adjusted by annealing at different temperature. Combining positron annihilation spectroscopy, EPR and XPS, we concluded that the bulk defects belonged to Ti3+ related vacancy defects. The results show that the separation efficiency of photogenerated electrons and holes could be significantly improved by optimizing the bulk/surface defects ratio of TiO2 nanosheet films, and in turn enhancing the photocatalysis behaviors.

Growth and characterization of a-axis oriented Cr-doped AlN films by DC magnetron sputtering

NASA Astrophysics Data System (ADS)

Panda, Padmalochan; Ramaseshan, R.; Krishna, Nanda Gopala; Dash, S.

2016-05-01

Wurtzite type Cr-doped AlN thin films were grown on Si (100) substrates using DC reactive magnetron sputtering with a function of N2 concentration (15 to 25%). Evolution of crystal structure of these films was studied by GIXRD where a-axis preferred orientation was observed. The electronic binding energy and concentration of Cr in these films were estimated by X-ray photoemission spectroscopy (XPS). We have observed indentation hardness (HIT) of around 28.2 GPa for a nitrogen concentration of 25%.

Growth and characterization of a-axis oriented Cr-doped AlN films by DC magnetron sputtering

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

Panda, Padmalochan; Ramaseshan, R., E-mail: seshan@igcar.gov.in; Dash, S.

2016-05-23

Wurtzite type Cr-doped AlN thin films were grown on Si (100) substrates using DC reactive magnetron sputtering with a function of N{sub 2} concentration (15 to 25%). Evolution of crystal structure of these films was studied by GIXRD where a-axis preferred orientation was observed. The electronic binding energy and concentration of Cr in these films were estimated by X-ray photoemission spectroscopy (XPS). We have observed indentation hardness (H{sub IT}) of around 28.2 GPa for a nitrogen concentration of 25%.

Sulfonated reduced graphene oxide as a highly efficient catalyst for direct amidation of carboxylic acids with amines using ultrasonic irradiation.

PubMed

Mirza-Aghayan, Maryam; Tavana, Mahdieh Molaee; Boukherroub, Rabah

2016-03-01

Sulfonated reduced graphene oxide nanosheets (rGO-SO3H) were prepared by grafting sulfonic acid-containing aryl radicals onto chemically reduced graphene oxide (rGO) under sonochemical conditions. rGO-SO3H catalyst was characterized by Fourier-transform infrared (FT-IR) spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and X-ray photoelectron spectroscopy (XPS). rGO-SO3H catalyst was successfully applied as a reusable solid acid catalyst for the direct amidation of carboxylic acids with amines into the corresponding amides under ultrasonic irradiation. The direct sonochemical amidation of carboxylic acid takes place under mild conditions affording in good to high yields (56-95%) the corresponding amides in short reaction times. Copyright © 2015 Elsevier B.V. All rights reserved.

Extracellular biosynthesis of gadolinium oxide (Gd2O3) nanoparticles, their biodistribution and bioconjugation with the chemically modified anticancer drug taxol

PubMed Central

Khan, Shadab Ali; Gambhir, Sanjay

2014-01-01

Summary As a part of our programme to develop nanobioconjugates for the treatment of cancer, we first synthesized extracellular, protein-capped, highly stable and well-dispersed gadolinium oxide (Gd2O3) nanoparticles by using thermophilic fungus Humicola sp. The biodistribution of the nanoparticles in rats was checked by radiolabelling with Tc-99m. Finally, these nanoparticles were bioconjugated with the chemically modified anticancer drug taxol with the aim of characterizing the role of this bioconjugate in the treatment of cancer. The biosynthesized Gd2O3 nanoparticles were characterized by UV–vis spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoemission spectroscopy (XPS). The Gd2O3–taxol bioconjugate was confirmed by UV–vis spectroscopy and fluorescence microscopy and was purified by using high performance liquid chromatography (HPLC). PMID:24778946

Structural model of homogeneous As–S glasses derived from Raman spectroscopy and high-resolution XPS

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

Golovchak, R.; Shpotyuk, O.; Mccloy, J. S.

2010-11-28

The structure of homogeneous bulk As x S 100- x (25 ≤ x ≤ 42) glasses, prepared by the conventional rocking–melting–quenching method, was investigated using high-resolution X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. It is shown that the main building blocks of their glass networks are regular AsS 3/2 pyramids and sulfur chains. In the S-rich domain, the existence of quasi-tetrahedral (QT) S = As(S 1/2) 3 units is deduced from XPS data, but with a concentration not exceeding ~3–5% of total atomic sites. Therefore, QT units do not appear as primary building blocks of the glass backbone in thesemore » materials, and an optimally-constrained network may not be an appropriate description for glasses when x < 40. Finally, it is shown that, in contrast to Se-based glasses, the ‘chain-crossing’ model is only partially applicable to sulfide glasses.« less

Hydrolysis condensation reactions of titanium alkoxides in thin films: A study of the steric hindrance effect by X-ray photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Barlier, Vincent; Bounor-Legaré, Véronique; Boiteux, Gisèle; Davenas, Joël; Léonard, Didier

2008-06-01

An original approach based on X-ray photoelectron spectroscopy (XPS) is proposed to study the influence of the surrounding humidity on the hydrolysis-condensation reactions of five titanium alkoxides in thin films. More precisely, the influence of the nature of the ligands (propoxide, butoxide, isopropoxide, phenoxide, and 9H-carbazole-9-yl-ethyl-oxy) on the reaction rate was evidenced. The reaction advancement was evaluated by comparing XPS chemical compositions to theoretical compositions calculated for all the possible rates. XPS chemical environment information allowed validating the reliability of this approach through the evaluation of the condensation state. In both approaches, the influence of the steric hindrance on the reactivity of titanium alkoxides was highlighted to be similar to what has been previously observed in solution. Theses results corroborate the validity of our XPS approach to determine titanium alkoxide hydrolysis-condensation reactions in the specific application of thin films.

A preliminary view on adsorption of organics on ice at temperatures close to melting point

NASA Astrophysics Data System (ADS)

Kong, Xiangrui; Waldner, Astrid; Orlando, Fabrizio; Artiglia, Luca; Ammann, Markus; Bartels-Rausch, Thorsten

2016-04-01

Ice and snow play active roles in the water cycle, the energy budget of the Earth, and environmental chemistry in the atmosphere and cryosphere. The uptake of trace gases from the atmosphere may induce changes in the structure of the surface layer of ice crystals and has important consequences for atmospheric chemistry and the climate system. However, a molecular-level understanding of trace gas adsorption on ice is still missing, and also little is known about the impurity-induced ice-surface disorder in the context of environmental relevance. It is a general challenge to apply highly sensitive experimental approaches to ambient air conditions, e.g. studies of volatile surfaces, because of the strict requirements of vacuum experimental conditions. In this study, we employed synchrotron-based X-ray Photoelectron Spectroscopy (XPS) and partial electron yield Near Edge X-ray Absorption Fine Structure (NEXAFS) in a state-of-the-art Near-Ambient Pressure Photoelectron (NAPP) spectroscopy end station. The NAPP enables to utilize the surface sensitive experimental methods, XPS and NEXAFS with electron detection, on volatile surfaces, i.e. ice at temperatures approaching zero degree Celsius. XPS and NEXAFS provide unique information of hydrogen bonding network, surface concentration of organic adsorbates, depth profile of dopants in the ice, and acid-base dissociation on the surfaces. For instance, a few carboxylic acids, e.g. acetic acid and formic acid, have been recently studied by XPS and NEXAFS in NAPP. Amines are a group of nitrogen-containing basic organics with atmospheric relevance. Only few studies have been focused on amines, and atmospheric models rarely take account of them due to the limitation of knowledge. Several amines have been found to play active roles in the processes of aerosol formation, e.g. dimethylamine (DMA), trimethylamine (TMA) and 1-propanamine. In this study, we will focus on one of these three amines after pre-tests, and perform core-level spectroscopies to reveal the behaviour of adsorption and dissociation on ice. Additionally, pure ice and amine doped ice will be compared for their surface structure change at different temperatures, which will indicate the differences of surface disordering caused by different factors. For instance, we will have a chance to know better if impurities will cause local disordering, i.e. forming hydration shell, which challenges the traditional picture of a homogenous disordered doped ice surface. The findings of this study could not only improve our understanding of how acidic organics adsorb to ice, and of their chemical properties on ice, but also have potentials to know better the behaviour of pure ice at temperatures approaching to the melting point.

AgBr/MgBi2O6 heterostructured composites with highly efficient visible-light-driven photocatalytic activity

NASA Astrophysics Data System (ADS)

Zhong, Liansheng; Hu, Chaohao; Zhuang, Jing; Zhong, Yan; Wang, Dianhui; Zhou, Huaiying

2018-06-01

AgBr/MgBi2O6 heterostructured photocatalysts were synthesized by the deposition-precipitation method. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), photoluminescence (PL), and UV-Visible diffuse reflectance spectroscopy (UV-Vis DRS) were employed to examine the phase structure, morphology and optical properties of the as-prepared samples. The photocatalytic activity was investigated by decomposing methylene blue (MB) solution under visible light irradiation (λ > 420 nm). AgBr/MgBi2O6 composites exhibited significantly enhanced visible-light-driven photocatalytic properties in comparison with pure MgBi2O6 and AgBr. When the molar ratio of AgBr to MgBi2O6 was 3:1, the composite catalyst showed the optimal photocatalytic activity and excellent stability. The enhanced photocatalytic activity of AgBr/MgBi2O6 composites was attributed to the formation of p-n heterojunction between AgBr and MgBi2O6, thereby resulting in the effective separation and transfer of photogenerated electrons-hole pairs.

Green synthesis of soya bean sprouts-mediated superparamagnetic Fe 3O 4 nanoparticles

NASA Astrophysics Data System (ADS)

Cai, Yan; Shen, Yuhua; Xie, Anjian; Li, Shikuo; Wang, Xiufang

2010-10-01

Superparamagnetic Fe 3O 4 nanoparticles were first synthesized via soya bean sprouts (SBS) templates under ambient temperature and normal atmosphere. The reaction process was simple, eco-friendly, and convenient to handle. The morphology and crystalline phase of the nanoparticles were determined from scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and X-ray diffraction (XRD) spectra. The effect of SBS template on the formation of Fe 3O 4 nanoparticles was investigated using X-ray photoemission spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FT-IR). The results indicate that spherical Fe 3O 4 nanoparticles with an average diameter of 8 nm simultaneously formed on the epidermal surface and the interior stem wall of SBS. The SBS are responsible for size and morphology control during the whole formation of Fe 3O 4 nanoparticles. In addition, the superconducting quantum interference device (SQUID) results indicate the products are superparamagnetic at room temperature, with blocking temperature ( TB) of 150 K and saturation magnetization of 37.1 emu/g.

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.

Facile fabrication of CuO-Pb2O3 nanophotocatalyst for efficient degradation of Rose Bengal dye under visible light irradiation

NASA Astrophysics Data System (ADS)

Kamaraj, Eswaran; Somasundaram, Sivaraman; Balasubramani, Kavitha; Eswaran, Muthu Prema; Muthuramalingam, Rajarajan; Park, Sanghyuk

2018-03-01

A p-type CuO/n-type Pb2O3 heterojunction photocatalyst was prepared by a simple wet chemical process and the photocatalytic ability was evaluated for the degradation of Rose Bengal (RB) under visible light irradiation. Synthesized nanocatalysts were characterized by X-ray diffraction (XRD), UV-vis diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Energy-dispersive X-ray spectroscopy (EDS), Brunauer-Emmett-Teller (BET) surface area analysis, and X-ray photoelectron spectroscopy (XPS). The p-n heterojunction of CuO-Pb2O3 nanostructures can promote the light absorption capability of photocatalyst and charge separation of electron-hole pairs. Photodegradation assays showed that the addition of CuO effectively enhanced the photocatalytic activity of CuO-Pb2O3 under visible light irradiation (λmax > 420 nm). Compared with pure Pb2O3 and CuO, the CuO-Pb2O3 exhibited significantly enhanced photocatalytic degradation activity. The reaction rate constant of CuO-Pb2O3 is 0.092 min-1, which is much higher than those of CuO (0.073 min-1) and Pb2O3 (0.045 min-1).

NEXAFS and XPS characterization of molecular oxygen adsorbed on Ni(100) at 80 K

NASA Astrophysics Data System (ADS)

Kim, C. M.; Jeong, H. S.; Kim, E. H.

2000-07-01

X-ray photoelectron spectroscopy (XPS), thermal desorption spectroscopy (TDS) and near edge extended X-ray absorption fine structure (NEXAFS) have been combined to investigate the adsorption of oxygen on Ni(100) at 80 K. Three O(1s) XPS features were observed at 530.0, 531.1 and 534.7 eV when the Ni(100) surface was exposed to 600 L of oxygen at 80 K. They are assigned as O 2-, O 1- and molecular oxygen species, respectively. The presence of molecular oxygen has been confirmed by TDS and NEXAFS. Molecular O 2 on Ni(100) is oriented perpendicular to the surface, and the OO bond length is estimated to be 1.24 Å, based on the NEXAFS σ ∗ resonance energy.

Facile preparation of dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil for application as a SERS-substrate

NASA Astrophysics Data System (ADS)

Yi, Zao; Tan, Xiulan; Niu, Gao; Xu, Xibin; Li, Xibo; Ye, Xin; Luo, Jiangshan; Luo, Binchi; Wu, Weidong; Tang, Yongjian; Yi, Yougen

2012-05-01

Dendritic Ag-Pd bimetallic nanostructures have been synthesized on the surface of Cu foil via a multi-stage galvanic replacement reaction (MGRR) of Ag dendrites in a Na2PdCl4 solution. After five stages of replacement reaction, one obtained structures with protruding Ag-Pd flakes; these will mature into many porous structures with a few Ag atoms that are left over dendrites. The dendritic Ag-Pd bimetallic nanostructures were characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray (EDX), selected area electron diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). The morphology of the products strongly depended on the stage of galvanic replacement reaction and reaction temperature. The morphology and composition-dependent surface-enhanced Raman scattering (SERS) of the as-synthesized Ag-Pd bimetallic nanostructures were investigated. The effectiveness of these dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil as substrates toward SERS detection was evaluated by using rhodamine 6G (R6G) as a probe molecule. The results indicate that as-synthesized dendritic Ag-Pd bimetallic nanostructures are good candidates for SERS spectroscopy.

Surface-and bulk-properties of EPDM rubber modified by electron beam irradiation

NASA Astrophysics Data System (ADS)

Majumder, Papiya Sen; Bhowmick, Anil K.

1999-01-01

Electron beam initiated grafting of trimethylol propane triacrylate (TMPTA) onto ethylene propylene diene monomer (EPDM) has been carried out over a wide range of irradiation doses (0-200 kGy) using a fixed concentration (10%) of TMPTA. The samples have been both surface and bulk modified. Infrared (IR) studies indicate increased peak absorbances at 1730, 1260, 1120 and 1019 cm -1 upto 50 kGy and hence increased CO and C-O-C concentrations. The results are further supported by X-ray photoelectron spectroscopy (XPS) studies. The surface energy of EPDM increases from 46.5 to 60.7 mJ/m 2 on irradiation of the surface modified samples to 50 kGy dose, due to increased contribution of γSAB and γS(-). The results have been explained with the help of IR and XPS data. The values of tensile strength of the surface modified samples have not changed very significantly, while the moduli values have increased at the cost of the elongation at break. DMTA studies have shown changes in Tg and tan δmax on modification of the surface. The surface morphology of the modified and irradiated samples reveals acrylate flow marks at high magnification.

Selective Binding, Self-Assembly and Nanopatterning of the Creutz-Taube Ion on Surfaces

PubMed Central

Wang, Yuliang; Lieberman, Marya; Hang, Qingling; Bernstein, Gary

2009-01-01

The surface attachment properties of the Creutz-Taube ion, i.e., [(NH3)5Ru(pyrazine)Ru(NH3)5]5+, on both hydrophilic and hydrophobic types of surfaces were investigated using X-ray photoelectron spectroscopy (XPS). The results indicated that the Creutz-Taube ions only bound to hydrophilic surfaces, such as SiO2 and –OH terminated organic SAMs on gold substrates. No attachment of the ions on hydrophobic surfaces such as –CH3 terminated organic SAMs and poly(methylmethacrylate) (PMMA) thin films covered gold or SiO2 substrates was observed. Further ellipsometric, atomic force microscopy (AFM) and time-dependent XPS studies suggested that the attached cations could form an inorganic analog of the self-assembled monolayer on SiO2 substrate with a “lying-down” orientation. The strong electrostatic interaction between the highly charged cations and the anionic SiO2 surface was believed to account for these observations. Based on its selective binding property, patterning of wide (∼200 nm) and narrow (∼35 nm) lines of the Creutz-Taube ions on SiO2 surface were demonstrated through PMMA electron resist masks written by electron beam lithography (EBL). PMID:19333420

Effects of K and Pt promoters on the performance of cobalt catalyst supported on CNTs

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

Zabidi, Noor Asmawati Mohd, E-mail: noorasmawati-mzabidi@petronas.com.my; Ali, Sardar, E-mail: alikhan-635@yahoo.com; Subbarao, Duvvuri, E-mail: duvvuri-subbarao@petronas.com.my

2014-10-24

This paper presents a comparative study on the effects of incorporation of potassium (K) and platinum (Pt) as promoters on the physicochemical properties of cobalt catalyst. The catalyst was prepared by a wet impregnation method on a CNTs support. Samples were characterized using transmission electron microscopy (TEM), H{sub 2}-temperature-programmed reduction (TPR) and X-ray photoelectron spectroscopy (XPS) techniques. Fischer-Tropsch Synthesis (FTS) was carried out in a fixed-bed microreactor at 543 K and 1 atm, with H{sub 2}/CO = 2v/v and space velocity, SV of 12 L/g.h for 5 hours. The K-promoted and Pt-promoted Co catalysts have different physicochemical properties and catalytic performances comparedmore » to that of the un-promoted Co catalyst. XPS analysis revealed that K and Pt promoters induced electronic modifications as exhibited by the shifts in the Co binding energies. Incorporation of 0.06 wt% K and 0.06 wt% Pt in Co/CNTs catalyst resulted in an increase in the CO conversion and C{sub 5+} selectivity and a decrease in methane selectivity. Potassium was found to be a better promoter for Co/CNTs catalyst compared to platinum.« less

Effects of K and Pt promoters on the performance of cobalt catalyst supported on CNTs

NASA Astrophysics Data System (ADS)

Zabidi, Noor Asmawati Mohd; Ali, Sardar; Subbarao, Duvvuri

2014-10-01

This paper presents a comparative study on the effects of incorporation of potassium (K) and platinum (Pt) as promoters on the physicochemical properties of cobalt catalyst. The catalyst was prepared by a wet impregnation method on a CNTs support. Samples were characterized using transmission electron microscopy (TEM), H2-temperature-programmed reduction (TPR) and X-ray photoelectron spectroscopy (XPS) techniques. Fischer-Tropsch Synthesis (FTS) was carried out in a fixed-bed microreactor at 543 K and 1 atm, with H2/ CO = 2v / v and space velocity, SV of 12 L/g.h for 5 hours. The K-promoted and Pt-promoted Co catalysts have different physicochemical properties and catalytic performances compared to that of the un-promoted Co catalyst. XPS analysis revealed that K and Pt promoters induced electronic modifications as exhibited by the shifts in the Co binding energies. Incorporation of 0.06 wt% K and 0.06 wt% Pt in Co/CNTs catalyst resulted in an increase in the CO conversion and C5+ selectivity and a decrease in methane selectivity. Potassium was found to be a better promoter for Co/CNTs catalyst compared to platinum.

Surface characterization of graphene based materials

NASA Astrophysics Data System (ADS)

Pisarek, M.; Holdynski, M.; Krawczyk, M.; Nowakowski, R.; Roguska, A.; Malolepszy, A.; Stobinski, L.; Jablonski, A.

2016-12-01

In the present study, two kind of samples were used: (i) a monolayer graphene film with a thickness of 0.345 nm deposited by the CVD method on Cu foil, (ii) graphene flakes obtained by modified Hummers method and followed by reduction of graphene oxide. The inelastic mean free path (IMFP), characterizing electron transport in graphene/Cu sample and reduced graphene oxide material, which determines the sampling depth of XPS and AES were evaluated from relative Elastic Peak Electron Spectroscopy (EPES) measurements with the Au standard in the energy range 0.5-2 keV. The measured IMFPs were compared with IMFPs resulting from experimental optical data published in the literature for the graphite sample. The EPES IMFP values at 0.5 and 1.5 keV was practically identical to that calculated from optical data for graphite (less than 4% deviation). For energies 1 and 2 keV, the EPES IMFPs for rGO were deviated up to 14% from IMFPs calculated using the optical data by Tanuma et al. [1]. Before EPES measurements all samples were characterized by various techniques like: FE-SEM, AFM, XPS, AES and REELS to visualize the surface morphology/topography and identify the chemical composition.

Core-level spectra and molecular deformation in adsorption: V-shaped pentacene on Al(001)

PubMed Central

Lin, He; Brivio, Gian Paolo; Floreano, Luca; Fratesi, Guido

2015-01-01

Summary By first-principle simulations we study the effects of molecular deformation on the electronic and spectroscopic properties as it occurs for pentacene adsorbed on the most stable site of Al(001). The rationale for the particular V-shaped deformed structure is discussed and understood. The molecule–surface bond is made evident by mapping the charge redistribution. Upon X-ray photoelectron spectroscopy (XPS) from the molecule, the bond with the surface is destabilized by the electron density rearrangement to screen the core hole. This destabilization depends on the ionized carbon atom, inducing a narrowing of the XPS spectrum with respect to the molecules adsorbed hypothetically undistorted, in full agreement to experiments. When looking instead at the near-edge X-ray absorption fine structure (NEXAFS) spectra, individual contributions from the non-equivalent C atoms provide evidence of the molecular orbital filling, hybridization, and interchange induced by distortion. The alteration of the C–C bond lengths due to the V-shaped bending decreases by a factor of two the azimuthal dichroism of NEXAFS spectra, i.e., the energy splitting of the sigma resonances measured along the two in-plane molecular axes. PMID:26734516

Limitations of using Raman microscopy for the analysis of high-content-carbon-filled ethylene propylene diene monomer rubber.

PubMed

Ghanbari-Siahkali, Afshin; Almdal, Kristoffer; Kingshott, Peter

2003-12-01

The effects of laser irradiation on changes to the surface chemistry and structure of a commercially available ethylene propylene diene monomer (EPDM) rubber sample after Raman microscopy analysis was investigated. The Raman measurements were carried out with different levels of laser power on the sample, ranging from 4.55 mW to 0.09 mW. The surface of the EPDM was analyzed before and after laser exposure using X-ray photoelectron spectroscopy (XPS) and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy. The techniques have surface probe depths of approximately < or = 10 nm and 1 microm, respectively. Both sets of analysis show that ingredients of the blended EPDM rubber "bloom" to the surface as a result of local heating that takes place due to the absorption of laser by carbon black during the Raman analysis. Scanning electron microscopy (SEM) analysis was also performed on the Raman analyzed areas to visually illustrate the effects created due to laser light exposure (i.e., burning marks). The change in surface chemistry also occurs in regions a few millimeters from the exposed sites, indicating that the effect is quite long range. However, this phenomenon has no major influence, as far as XPS or ATR-FTIR results disclose, on the backbone structure of the rubber sample. The results indicate that precautions should be taken when analyzing complex blended polymer samples using Raman spectroscopy.

Oxygen vacancy induced phase formation and room temperature ferromagnetism in undoped and Co-doped TiO2 thin films

NASA Astrophysics Data System (ADS)

Mohanty, P.; Mishra, N. C.; Choudhary, R. J.; Banerjee, A.; Shripathi, T.; Lalla, N. P.; Annapoorni, S.; Rath, Chandana

2012-08-01

TiO2 and Co-doped TiO2 (CTO) thin films deposited at various oxygen partial pressures by pulsed laser deposition exhibit room temperature ferromagnetism (RTFM) independent of their phase. Films deposited at 0.1 mTorr oxygen partial pressure show a complete rutile phase confirmed from glancing angle x-ray diffraction and Raman spectroscopy. At the highest oxygen partial pressure, i.e. 300 mTorr, although the TiO2 film shows a complete anatase phase, a small peak corresponding to the rutile phase along with the anatase phase is identified in the case of CTO film. An increase in O to Ti/(Ti+Co) ratio with increase in oxygen partial pressure is observed from Rutherford backscattering spectroscopy. It is revealed from x-ray photoelectron spectroscopy (XPS) that oxygen vacancies are found to be higher in the CTO film than TiO2, while the valency of cobalt remains in the +2 state. Therefore, the CTO film deposited at 300 mTorr does not show a complete anatase phase unlike the TiO2 film deposited at the same partial pressure. We conclude that RTFM in both films is not due to impurities/contaminants, as confirmed from XPS depth profiling and cross-sectional transmission electron microscopy (TEM), but due to oxygen vacancies. The magnitude of moment, however, depends not only on the phase of TiO2 but also on the crystallinity of the films.

Structural and electrochemical analysis of chemically synthesized microcubic architectured lead selenide thin films

NASA Astrophysics Data System (ADS)

Bhat, T. S.; Shinde, A. V.; Devan, R. S.; Teli, A. M.; Ma, Y. R.; Kim, J. H.; Patil, P. S.

2018-01-01

The present work deals with the synthesis of lead selenide (PbSe) thin films by simple and cost-effective chemical bath deposition method with variation in deposition time. The structural, morphological, and electrochemical properties of as-deposited thin films were examined using characterization techniques such as X-ray diffraction spectroscopy (XRD), field-emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy. XRD reveals formation of rock salt phase cubic structured PbSe. FE-SEM images show the formation of microcubic structured morphology. The existence of the PbSe is confirmed from the XPS analysis. On the other hand, CV curves show four reaction peaks corresponding to oxidation [PbSe and Pb(OH)2] and reduction (PbO2 and Pb(OH)2) at the surface of PbSe thin films. The PbSe:2 sample deposited for 80 min. shows maximum specific capacitance of 454 ± 5 F g- 1 obtained at 0.25 mA cm- 2 current density. The maximum energy density of 69 Wh kg- 1 was showed by PbSe:2 electrode with a power density of 1077 W kg- 1. Furthermore, electrochemical impedance studies of PbSe:2 thin film show 80 ± 3% cycling stability even after 500 CV cycles. Such results show the importance of microcubic structured PbSe thin film as an anode in supercapacitor devices.

Vectorial method used to monitor an evolving system: Titanium oxide thin films under UV illumination

NASA Astrophysics Data System (ADS)

Béchu, Solène; Humbert, Bernard; Fernandez, Vincent; Fairley, Neal; Richard-Plouet, Mireille

2018-07-01

Under in situ UV illumination, some materials present evolution of their opto-electronic properties that can be monitored by spectroscopy. We present here a mathematical method which can be applied to spectroscopic measurements when an evolving set of data is recorded: the vectorial method. The investigations and quantifications are performed by Infrared spectroscopy and XPS on organic-inorganic thin films prepared by sol-gel. The inorganic part of these hybrid thin films contains Ti oxide-network based whereas the organic part is composed of N,N-dimethylformamide and its hydrolysis products. Under UV illumination, those films exhibit intermediate bandgap behavior due to the photoreduction of Ti(IV) in Ti(III). The role of the solvent in the thin film is underlined during the process of photoreduction together with an understanding of the condensation of the Ti oxide-based network, as these evolutions are critical for the opto-electronic properties of those thin films.

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.

Fabrication of hierarchical core-shell polydopamine@MgAl-LDHs composites for the efficient enrichment of radionuclides

NASA Astrophysics Data System (ADS)

Zhu, Kairuo; Lu, Songhua; Gao, Yang; Zhang, Rui; Tan, Xiaoli; Chen, Changlun

2017-02-01

Novel hierarchical core/shell structured polydopamine@MgAl-layered double hydroxides (PDA@MgAl-LDHs) composites involving MgAl-layered double hydroxide shells and PDA cores were fabricated thought one-pot coprecipitation assembly and methodically characterized by X-ray diffraction, Fourier transformed infrared spectroscopy, scanning/transmission electron microscopy, selected area electron diffraction, elemental mapping, thermogravimetric analysis and X-ray photoelectron spectroscopy technologies. U(VI) and Eu(III) sorption experiments showed that the PDA@MgAl-LDHs exhibited higher sorption ability with a maximum sorption capacity of 142.86 and 76.02 mg/g at 298 K and pH 4.5, respectively. More importantly, according to XPS analyses, U(VI) and Eu(III) were sorbed on PDA@MgAl-LDHs via oxygen-containing functional groups, and the chemical affinity of U(VI) by oxygen-containing functional groups is higher than that of Eu(III). These observations show great expectations in the enrichment of radionuclides from aquatic environments by PDA@MgAl-LDHs.

Jingle-bell-shaped ferrite hollow sphere with a noble metal core: Simple synthesis and their magnetic and antibacterial properties

NASA Astrophysics Data System (ADS)

Li, Siheng; Wang, Enbo; Tian, Chungui; Mao, Baodong; Kang, Zhenhui; Li, Qiuyu; Sun, Guoying

2008-07-01

In this paper, a simple strategy is developed for rational fabrication of a class of jingle-bell-shaped hollow structured nanomaterials marked as Ag@ MFe 2O 4 ( M=Ni, Co, Mg, Zn), consisting of ferrite hollow shells and metal nanoparticle cores, using highly uniform colloidal Ag@C microspheres as template. The final composites were obtained by direct adsorption of metal cations Fe 3+ and M 2+ on the surface of the Ag@C spheres followed by calcination process to remove the middle carbon shell and transform the metal ions into pure phase ferrites. The as-prepared composites were characterized by X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray analysis (EDX), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis spectroscopy and SQUID magnetometer. The results showed that the composites possess the magnetic property of the ferrite shell and the optical together with antibacterial property of the Ag core.

Green chemistry approach for the synthesis of ZnO-carbon dots nanocomposites with good photocatalytic properties under visible light.

PubMed

Bozetine, Hakima; Wang, Qi; Barras, Alexandre; Li, Musen; Hadjersi, Toufik; Szunerits, Sabine; Boukherroub, Rabah

2016-03-01

We report on a simple and one-pot synthetic method to produce ZnO/carbon quantum dots (ZnO/CQDs) nanocomposites. The morphological features and chemical composition of the nanocomposites were characterized using X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analyses (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The optical properties of the nanocomposites were examined using UV-visible (UV-vis) spectrophotometry. The photocatalytic activity of the ZnO/CQDs was evaluated for the degradation of a model organic pollutant, rhodamine B, under visible light irradiation at room temperature. The highly efficient photodegradation capability of the nanocomposite was demonstrated by comparison with ZnO particles, prepared using identical experimental conditions. Overall, the present approach adheres to green chemistry principles and the nanocomposite holds promise for the development of remarkably efficient catalytic systems. Copyright © 2015 Elsevier Inc. All rights reserved.

Single-step process to improve the mechanical properties of carbon nanotube yarn.

PubMed

Evora, Maria Cecilia; Lu, Xinyi; Hiremath, Nitilaksha; Kang, Nam-Goo; Hong, Kunlun; Uribe, Roberto; Bhat, Gajanan; Mays, Jimmy

2018-01-01

Carbon nanotube (CNT) yarns exhibit low tensile strength compared to conventional high-performance carbon fibers due to the facile sliding of CNTs past one another. Electron beam (e-beam) irradiation was employed for in a single-step surface modification of CNTs to improve the mechanical properties of this material. To this end, CNT yarns were simultaneously functionalized and crosslinked using acrylic acid (AA) and acrylonitrile (AN) in an e-beam irradiation process. The chemical modification of CNT yarns was confirmed by X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and scanning electron microscopy (SEM). The best improvement in mechanical properties was achieved on a sample treated with an aqueous solution of AA and subsequent irradiation. CNT yarn treatment with AA enhanced the strength (444.5 ± 68.4 MPa) by more than 75% and the modulus (21.5 ± 0.6 GPa) by more than 144% as compared to untreated CNT yarn (strength 251 ± 26.5 MPa and modulus 8.8 ± 1.2 GPa).

Single-step process to improve the mechanical properties of carbon nanotube yarn

PubMed Central

Lu, Xinyi; Hiremath, Nitilaksha; Kang, Nam-Goo; Hong, Kunlun; Uribe, Roberto; Bhat, Gajanan; Mays, Jimmy

2018-01-01

Carbon nanotube (CNT) yarns exhibit low tensile strength compared to conventional high-performance carbon fibers due to the facile sliding of CNTs past one another. Electron beam (e-beam) irradiation was employed for in a single-step surface modification of CNTs to improve the mechanical properties of this material. To this end, CNT yarns were simultaneously functionalized and crosslinked using acrylic acid (AA) and acrylonitrile (AN) in an e-beam irradiation process. The chemical modification of CNT yarns was confirmed by X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and scanning electron microscopy (SEM). The best improvement in mechanical properties was achieved on a sample treated with an aqueous solution of AA and subsequent irradiation. CNT yarn treatment with AA enhanced the strength (444.5 ± 68.4 MPa) by more than 75% and the modulus (21.5 ± 0.6 GPa) by more than 144% as compared to untreated CNT yarn (strength 251 ± 26.5 MPa and modulus 8.8 ± 1.2 GPa). PMID:29527431

Summary: Update to ASTM Guide E 1523 to Charge Control and Charge Referencing Techniques in X-ray Photoelectron Spectroscopy

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

Baer, Donald R.

2005-04-22

An updated version of the ASTM guide E1523 to the methods to charge control and charge referencing techniques in x-ray photoelectron spectroscopy has been released by ASTM. The guide is meant to acquaint x-ray photoelectron spectroscopy (XPS) users with the various charge control and charge referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens. The current guide has been expanded to include new references as well as recommendations for reporting information on charge control and charge referencing. The previous version of the document had been published in 1997.

The Gaussian-Lorentzian Sum, Product, and Convolution (Voigt) functions in the context of peak fitting X-ray photoelectron spectroscopy (XPS) narrow scans

NASA Astrophysics Data System (ADS)

Jain, Varun; Biesinger, Mark C.; Linford, Matthew R.

2018-07-01

X-ray photoelectron spectroscopy (XPS) is arguably the most important vacuum technique for surface chemical analysis, and peak fitting is an indispensable part of XPS data analysis. Functions that have been widely explored and used in XPS peak fitting include the Gaussian, Lorentzian, Gaussian-Lorentzian sum (GLS), Gaussian-Lorentzian product (GLP), and Voigt functions, where the Voigt function is a convolution of a Gaussian and a Lorentzian function. In this article we discuss these functions from a graphical perspective. Arguments based on convolution and the Central Limit Theorem are made to justify the use of functions that are intermediate between pure Gaussians and pure Lorentzians in XPS peak fitting. Mathematical forms for the GLS and GLP functions are presented with a mixing parameter m. Plots are shown for GLS and GLP functions with mixing parameters ranging from 0 to 1. There are fundamental differences between the GLS and GLP functions. The GLS function better follows the 'wings' of the Lorentzian, while these 'wings' are suppressed in the GLP. That is, these two functions are not interchangeable. The GLS and GLP functions are compared to the Voigt function, where the GLS is shown to be a decent approximation of it. Practically, both the GLS and the GLP functions can be useful for XPS peak fitting. Examples of the uses of these functions are provided herein.

Ti-Nb thin films deposited by magnetron sputtering on stainless steel

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

Gonzalez, E. David; Niemeyer, Terlize C.; Afonso, Conrado R. M.

2016-03-15

Thin films of Ti-Nb alloys were deposited on AISI 316L stainless steel substrate by magnetron sputtering, and the structure, composition, morphology, and microstructure of the films were analyzed by means of x-ray diffraction (XRD), (scanning) transmission electron microscopy (TEM) coupled with energy-dispersive x-ray spectroscopy, atomic force microscopy (AFM), and x-ray photoelectron spectroscopy (XPS). Thin films of four compositions were produced: Ti{sub 85}Nb{sub 15} (Ti-26 wt. % Nb), Ti{sub 80}Nb{sub 20} (Ti-33 wt. % Nb), Ti{sub 70}Nb{sub 30} (Ti-45 wt. % Nb), and Ti{sub 60}Nb{sub 40} (Ti-56 wt. % Nb). Structural characterization by XRD indicated that only the β phase was present in the thinmore » films and that the increase in the Nb content modified the alloy film texture. These changes in the film texture, also detected by TEM analysis, were attributed to different growth modes related to the Nb content in the alloy films. The mean grain sizes measured by AFM increased with the Nb amount (from 197 to 222 nm). XPS analysis showed a predominance of oxidized Ti and Nb on the film surfaces and an enrichment of Ti.« less

S2p core level spectroscopy of short chain oligothiophenes

NASA Astrophysics Data System (ADS)

Baseggio, O.; Toffoli, D.; Stener, M.; Fronzoni, G.; de Simone, M.; Grazioli, C.; Coreno, M.; Guarnaccio, A.; Santagata, A.; D'Auria, M.

2017-12-01

The Near-Edge X-ray-Absorption Fine-Structure (NEXAFS) and X-ray Photoemission Spectroscopy (XPS) of short-chain oligothiophenes (thiophene, 2,2'-bithiophene, and 2,2':5',2″-terthiophene) in the gas phase have been measured in the sulfur L2,3-edge region. The assignment of the spectral features is based on the relativistic two-component zeroth-order regular approximation time dependent density functional theory approach. The calculations allow us to estimate both the contribution of the spin-orbit splitting and of the molecular-field splitting to the sulfur binding energies and give results in good agreement with the experimental measurements. The deconvolution of the calculated S2p NEXAFS spectra into the two manifolds of excited states converging to the LIII and LII edges facilitates the attribution of the spectral structures. The main S2p NEXAFS features are preserved along the series both as concerns the energy positions and the nature of the transitions. This behaviour suggests that the electronic and geometrical environment of the sulfur atom in the three oligomers is relatively unaffected by the increasing chain length. This trend is also observed in the XPS spectra. The relatively simple structure of S2p NEXAFS spectra along the series reflects the localized nature of the virtual states involved in the core excitation process.

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

Zehtab Yazdi, Alireza; Roberts, Edward P.L.; Sundararaj, Uttandaraman, E-mail: u.sundararaj@ucalgary.ca

Highlights: • MWCNTs synthesized and electrochemically oxidized to study the formation of GNR • HRTEM, Raman and XPS confirmed no successful unzipping occurred after oxidation • Electrochemical oxidation very unlikely facilitate formation of intercalated MWCNTs - Abstract: Multiwalled carbon nanotubes (MWCNTs) with different geometrical characteristics and chemical doping have been synthesized and electrochemically oxidized to study the possibility of unzipping, and creating graphene nanoribbon (GNR) nanostructures. Modified glassy carbon electrodes of the MWCNTs have been tested in an aqueous electrolyte via anodic scans in a wide range of potentials, followed by keeping at the maximum potential for different times. Themore » microstructural features, structural defects, and functional groups and their elements have been then studied using high resolution transmission electron microscopy (HRTEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS), respectively. All results have confirmed that no successful unzipping occurs in the MWCNTs after electrochemical oxidation, even for the nitrogen-doped MWCNTs (CN{sub x}-MWCNTs) with reactive nitrogen groups and defective bamboo structures. In contrast to the report by Shinde et al. (J. Am. Chem. Soc. 2011, 133, 4168–4171), it has been concluded that the electrochemical oxidation in aqueous electrolytes is very unlikely to facilitate sufficient incorporation of the intercalated molecules among the walls of the MWCNTs. These molecules are, however, responsible for unzipping of MWCNTs.« less

Use of high L.E.T. radiation to improve adhesion of metals to polytetrafluoroethylene

NASA Technical Reports Server (NTRS)

Wheeler, D. R.; Pepper, S. V.

1982-01-01

MgK alpha X-rays (1254 eV) and 2 keV electrons irradiate the surface of polytetrafluoro ethylene (PTFE). The damage is confined to a few tenths of a micron below the surface, and the doses exceed 10 to the eight power rad. X-ray Photoelectron Spectroscopy (XPS) of the irradiated surfaces and mass spectroscopy of the gaseous products of irradiation indicate that the damaged layer is crosslinked or branched PTFE. After either type of irradiation, the surface has enhanced affinity for metals and a lower contact angle with hexadecane. Tape pull tests show that evaporated Ni and Au films adhere better to the irradiated surface. XPS shows the Ni interacts chemically with PTFE forming NiF2 and possibly NiC. However, the gold adhesion and contact angle results indicate that the interaction is, at least in part, chemically nonspecific. Decreased contact angles on FEP Teflon crystallized against gold were attributed to either the presence of a polar oxygen layer or increased physical forces due to greater density. In the case of irradiated PTFE, no oxygen on the surface was observed. The crosslinked structure might, however, have a greater density, thus accounting for the observed increase in adhesion and wettability.

Band alignment of 2D WS2/HfO2 interfaces from x-ray photoelectron spectroscopy and first-principles calculations

NASA Astrophysics Data System (ADS)

Zhu, H. L.; Zhou, C. J.; Tang, B. S.; Yang, W. F.; Chai, J. W.; Tay, W. L.; Gong, H.; Pan, J. S.; Zou, W. D.; Wang, S. J.; Chi, D. Z.

2018-04-01

We report on the growth of two-dimensional (2D) WS2 on high-k HfO2/Si substrates by reactive sputtering deposition. Raman, x-ray photoelectron spectroscopy (XPS), and high-resolution transmission electron microscopy characterizations indicate that the 2D WS2 layers exhibit high-quality crystallinity and exact stoichiometry. Through high-resolution XPS valence spectra, we find a type I alignment at the interface of monolayer WS2/HfO2 with a valence band offset (VBO) of 1.95 eV and a conduction band offset (CBO) of 1.57 eV. The VBO and CBO are also found to increase up to 2.24 eV and 2.09 eV, respectively, with increasing WS2 layers. This is consistent with the results obtained from our first-principles calculations. Our theoretical calculations reveal that the remarkable splitting and shift of the W 5 d z 2 orbital originating from interlayer orbital coupling in thicker WS2 films induce a reduction of its bandgap, leading to an increase in both the VBO and CBO. This observation can be attributed to the asymmetric splitting at different high symmetric k-points caused by the interlayer orbital coupling.

Polarity determination of polar and semipolar (112¯2) InN and GaN layers by valence band photoemission spectroscopy

NASA Astrophysics Data System (ADS)

Skuridina, D.; Dinh, D. V.; Lacroix, B.; Ruterana, P.; Hoffmann, M.; Sitar, Z.; Pristovsek, M.; Kneissl, M.; Vogt, P.

2013-11-01

We demonstrate that the polarity of polar (0001), (0001¯) and semipolar (112¯2) InN and GaN thin layers can be determined by valence band X-ray photoemission spectroscopy (XPS). The polarity of the layers has been confirmed by wet etching and convergent beam electron diffraction. Unlike these two techniques, XPS is a non-destructive method and unaffected by surface oxidation or roughness. Different intensities of the valence band states in spectra recorded by using AlKα X-ray radiation are observed for N-polar and group-III-polar layers. The highest intensity of the valence band state at ≈3.5 eV for InN and ≈5.2 eV for GaN correlates with the group-III polarity, while the highest intensity at ≈6.7 eV for InN and ≈9.5 eV for GaN correlates with the N-polarity. The difference between the peaks for the group-III- and N-polar orientations was found to be statistically significant at the 0.05 significance level. The polarity of semipolar (112¯2) InN and GaN layers can be determined by recording valence band photoelectrons emitted along the [000 ± 1] direction.

Reaction of methyl formate with VC(1 0 0) and TiC(1 0 0) surfaces

NASA Astrophysics Data System (ADS)

Frantz, Peter; Kim, Hyun I.; Didziulis, Stephen V.; Li, Shuang; Chen, Zhiying; Perry, Scott S.

2005-12-01

The chemistry of the (1 0 0) surface of the tribologically important materials vanadium carbide (VC) and titanium carbide (TiC) with methyl formate (CH 3OCHO) has been studied with X-ray photoelectron spectroscopy (XPS), high resolution electron energy loss spectroscopy (HREELS), and temperature programmed desorption (TPD). The molecule reacts with each surface at temperatures below 150 K, although the extent of reaction is greater on the TiC surface. XPS and HREELS results indicate that the first step in this chemistry is the cleavage of the CH 3O-CHO bond, generating surface methoxy groups (CH 3O-) and either carbon monoxide on VC or a formyl (CHO) group on TiC. The methoxy group reacts further on both surfaces via pathways expected based on previous methanol adsorption studies, primarily decomposing through a formyl intermediate on VC to generate formaldehyde and evolving methanol on TiC. The formyl group formed directly from methyl formate on TiC enables the production and evolution of formaldehyde, and also appears to break down further to the elements. These results indicate a propensity for these carbides to react with esters, leading potentially to the beneficial formation of friction lowering surface films or the deleterious degradation of ester-based lubricants.

A sulfur segregation study of PWA 1480, NiCrAl, and NiAl alloys

NASA Technical Reports Server (NTRS)

Jayne, D. T.; Smialek, J. L.

1993-01-01

Some nickel based superalloys show reduced oxidation resistance from the lack of an adherent oxide layer during high temperature cyclic oxidation. The segregation of sulfur to the oxide-metal interface is believed to effect oxide adhesion, since low sulfur alloys exhibit enhanced adhesion. X ray Photoelectron Spectroscopy (XPS) was combined with an in situ sample heater to measure sulfur segregation in NiCrAl, PWA 1480, and NiAl alloys. The polished samples with a 1.5 to 2.5 nm (native) oxide were heated from 650 to 1100 C with hold times up to 6 hr. The sulfur concentration was plotted as a function of temperature versus time at temperature. One NiCrAl sulfur study was performed on the same casting used by Browning to establish a base line between previous Auger Electron Spectroscopy (AES) results and the XPS results of this study. Sulfur surface segregation was similar for PWA 1480 and NiCrAl and reached a maximum of 30 at% at 800 to 850 C. Above 900 C the sulfur surface concentration decreased to about 3 at% at 1100 C. These results are contrasted to the minimal segregation observed for low sulfur hydrogen annealed materials which exhibit improved scale adhesion.

Bioaccumulation characterization of uranium by a novel Streptomyces sporoverrucosus dwc-3.

PubMed

Li, Xiaolong; Ding, Congcong; Liao, Jiali; Du, Liang; Sun, Qun; Yang, Jijun; Yang, Yuanyou; Zhang, Dong; Tang, Jun; Liu, Ning

2016-03-01

The biosorption mechanisms of uranium on an aerobic bacterial strain Streptomyces sporoverrucosus dwc-3, isolated from a potential disposal site for (ultra-)low uraniferous radioactive waste in Southwest China, were evaluated by using transmission electron microscopy (TEM), energy dispersive X-ray (EDX) analysis, Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), proton induced X-ray emission (PIXE) and enhanced proton backscattering spectrometry (EPBS). Approximately 60% of total uranium at an initial concentration of 10mg/L uranium nitrate solution could be absorbed on 100mg S. sporoverrucosus dwc-3 with an adsorption capacity of more than 3.0mg/g (wet weight) after 12hr at room temperature at pH3.0. The dynamic biosorption process of S. sporoverrucosus dwc-3 for uranyl ions was well described by a pseudo second-order model. S. sporoverrucosus dwc-3 could accumulate uranium on cell walls and within the cell, as revealed by SEM and TEM analysis as well as EDX spectra. XPS and FT-IR analysis further suggested that the absorbed uranium was bound to amino, phosphate and carboxyl groups of the cells. Additionally, PIXE and EPBS results confirmed that ion exchange also contributed to the adsorption process of uranium. Copyright © 2015. Published by Elsevier B.V.

Biomolecule-controlled hydrothermal synthesis of C-N-S-tridoped TiO2 nanocrystalline photocatalysts for NO removal under simulated solar light irradiation.

PubMed

Wang, Yawen; Huang, Yu; Ho, Wingkei; Zhang, Lizhi; Zou, Zhigang; Lee, Shuncheng

2009-09-30

In this study, C-N-S-tridoped titanium dioxide (TiO(2)) nanocrystals were synthesized by using a facile hydrothermal method in the presence of a biomolecule l-cysteine. This biomolecule could not only serve as the common source for the carbon, sulfur and nitrogen tridoping, but also could control the final crystal phases and morphology. The resulting materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption and UV-vis diffuse reflectance spectroscopy. XPS analysis revealed that S was incorporated into the lattice of TiO(2) through substituting oxygen atoms, N might coexist in the forms of N-Ti-O and Ti-O-N in tridoped TiO(2) and most C could form a mixed layer of carbonate species deposited on the surface of TiO(2) nanoparticles. The photocatalytic activities of the samples were tested on the removal of NO at typical indoor air level in a flow system under simulated solar light irradiation. The tridoped TiO(2) samples showed much higher removal efficiency than commercial P25 and the undoped counterpart photocatalyst. The enhanced visible light photocatalytic activity of C-N-S-tridoped TiO(2) nanocrystals was explained on the basis of characterizations. The possible formation process of the monodispersed C-N-S-tridoped anatase TiO(2) nanocrystals was also proposed. This study provides a new method to prepare visible light active TiO(2) photocatalyst.

A novel hydroxyl epoxy phosphate monomer enhancing the anticorrosive performance of waterborne Graphene/Epoxy coatings

NASA Astrophysics Data System (ADS)

Ding, Jiheng; Rahman, Obaid ur; Peng, Wanjun; Dou, Huimin; Yu, Haibin

2018-01-01

Herein, we report the synthesis of a novel hydroxyl epoxy phosphate monomer (PGHEP) as an efficient dispersant for graphene to enhance the compatibility of the graphene in epoxy resin. Raman spectroscopy, Ultraviolet-visible spectroscopy (UV-vis) and X-ray photoelectron spectroscopy (XPS) studies were confirmed the π-π interactions between PGHEP and graphene. Well-dispersed states of PGHEP functionalized graphene (G) sheets in water were analyzed by transmission electron microscopy (TEM), atomic force microscopy (AFM) and scanning electron microscopy (SEM). Further, microstructure of prepared G/waterborne epoxy coatings containing 0.5-1.0 wt.% of PGHEP functionalized G sheets were also observed with the help of SEM and TEM. The PGHEP functionalized G sheets dispersed composite coatings displayed enhanced corrosion resistance compared with pure epoxy resin, these coatings have higher contact angle, lower water absorption as evident from the results of electrochemical impedance spectroscopy (EIS) and salt spray tests. The superior corrosion protection performances of G/epoxy coatings were mainly attributed to the formed passive film from uniformly dispersed PGHEP functionalized G sheets which act as physical barrier on the steel surface. Therefore, this work provides a novel bio-based efficient dispersant for G sheets and an important method for preparing G/waterborne epoxy coatings with superior corrosion resistance properties.

Fluorescent Gold Nanoclusters for Selective Detection of Dopamine in Cerebrospinal fluid

PubMed Central

Govindaraju, Saravanan; Ankireddy, Seshadri Reddy; Viswanath, Buddolla; Kim, Jongsung; Yun, Kyusik

2017-01-01

Since the last two decades, protein conjugated fluorescent gold nanoclusters (NCs) owe much attention in the field of medical and nanobiotechnology due to their excellent photo stability characteristics. In this paper, we reported stable, nontoxic and red fluorescent emission BSA-Au NCs for selective detection of L-dopamine (DA) in cerebrospinal fluid (CSF). The evolution was probed by various instrumental techniques such as UV-vis spectroscopy, High resolution transmission electron microscopy (HTEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), photoluminescence spectroscopy (PL). The synthesised BSA-Au NCs were showing 4–6 nm with high fluorescent ~8% Quantum yield (QY). The fluorescence intensity of BSA-Au NCs was quenched upon the addition of various concentrations of DA via an electron transfer mechanism. The decrease in BSA-Au NCs fluorescence intensity made it possible to determine DA in PBS buffer and the spiked DA in CSF in the linear range from 0 to 10 nM with the limit of detection (LOD) 0.622 and 0.830 nM respectively. Best of our knowledge, as-prepared BSA-Au NCs will gain possible strategy and good platform for biosensor, drug discovery, and rapid disease diagnosis such as Parkinson’s and Alzheimer diseases. PMID:28067307

Non-covalently anchored multi-walled carbon nanotubes with hexa-decafluorinated zinc phthalocyanine as ppb level chemiresistive chlorine sensor

NASA Astrophysics Data System (ADS)

Sharma, Anshul Kumar; Mahajan, Aman; Bedi, R. K.; Kumar, Subodh; Debnath, A. K.; Aswal, D. K.

2018-01-01

A cost effective solution assembly method has been explored for preparing zinc(II)1,2,3,4,8,9,10,11,15,16,17,18,22,23,24,25-hexa-decafluoro-29H,31H-phthalocyanine/multi-walled carbon nanotubes (F16ZnPc/MWCNTs-COOH) hybrid. Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE-SEM) investigations confirm the non-covalent anchoring of F16ZnPc onto MWCNTs-COOH through п-п stacking interactions. Further, a highly sensitive and selective chemiresistive Cl2 sensor has been fabricated using F16ZnPc/MWCNTs-COOH hybrid. The response of sensor is found to be 21.28% for 2 ppm of Cl2 with a response time of 14 s and theoretical detection limit of the sensor is found down to 0.06 ppb. The improved Cl2 sensing characteristics of hybrid are found to be originated from the synergetic interaction between F16ZnPc and MWCNTs-COOH. The underlying mechanism for improved gas sensing performance of F16ZnPc/MWCNTs-COOH sensor towards Cl2 has been explained using Raman, X-ray photoelectron spectroscopy (XPS) and electrochemical impedance spectroscopy (EIS) studies.

Mesoporous coaxial titanium nitride-vanadium nitride fibers of core-shell structures for high-performance supercapacitors.

PubMed

Zhou, Xinhong; Shang, Chaoqun; Gu, Lin; Dong, Shanmu; Chen, Xiao; Han, Pengxian; Li, Lanfeng; Yao, Jianhua; Liu, Zhihong; Xu, Hongxia; Zhu, Yuwei; Cui, Guanglei

2011-08-01

In this study, titanium nitride-vanadium nitride fibers of core-shell structures were prepared by the coaxial electrospinning, and subsequently annealed in the ammonia for supercapacitor applications. These core-shell (TiN-VN) fibers incorporated mesoporous structure into high electronic conducting transition nitride hybrids, which combined higher specific capacitance of VN and better rate capability of TiN. These hybrids exhibited higher specific capacitance (2 mV s(-1), 247.5 F g(-1)) and better rate capability (50 mV s(-1), 160.8 F g(-1)), which promise a good candidate for high-performance supercapacitors. It was also revealed by electrochemical impedance spectroscopy (EIS) and X-ray photoelectron spectroscopy (XPS) characterization that the minor capacitance fade originated from the surface oxidation of VN and TiN.

Mechanical properties of tantalum-based ceramic coatings for biomedical applications

NASA Astrophysics Data System (ADS)

Donkov, N.; Walkowicz, J.; Zavaleyev, V.; Zykova, A.; Safonov, V.; Dudin, S.; Yakovin, S.

2018-03-01

The properties were studied of Ta, Ta2O5 and Ta/Ta2O5 coatings deposited by reactive magnetron sputtering on stainless steel (AISI 316) substrates. The compositional, structural and morphological parameters of the coatings were investigated by means of X-ray photoemission spectroscopy (XPS), energy dispersive X-ray (EDX) spectroscopy, and scanning electron microscopy (SEM). The roughness parameters, adhesion strength, hardness, elastic modulus, and H/E ratio were evaluated by standard techniques. The hardness parameters of the Ta2O5 and Ta/Ta2O5 coatings increased in comparison with pure Ta films, while the relatively low Young’s modulus was related to high elastic recovery and high resistance to cracking. The tantalum-based coatings possessed good biomechanical parameters for advanced implant and stent applications.

Removal of Carmine from Aqueous Solution by Carbonated Hydroxyapatite Nanorods

PubMed Central

Liu, Guanxiong; Xue, Caibao; Zhu, Peizhi

2017-01-01

In this study, carbonated hydroxyapatite (CHA) nanorods were prepared by a novel hydrothermal method. The crystallinity and chemical structure of synthesized CHA nanorods was characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS), respectively. Carmine was selected as representative organic dyes to study the adsorption capacities of CHA nanorods. Mechanistic studies of carmine adsorption by CHA nanorods show that the adsorption processes both follow the pseudo-second-order kinetic model and fit the Langmuir isotherm model well. The CHA nanorods exhibited a high adsorption capacity of 85.51 mg/g for carmine at room-temperature. The experimental results prove that CHA nanorods can be promising absorbents for removing organic dye pollutants in wastewater from paper and textile plants. PMID:28587250

In situ reduction of antibacterial silver ions to metallic silver nanoparticles on bioactive glasses functionalized with polyphenols

NASA Astrophysics Data System (ADS)

Ferraris, S.; Miola, M.; Cochis, A.; Azzimonti, B.; Rimondini, L.; Prenesti, E.; Vernè, E.

2017-02-01

The realization of surfaces with antibacterial properties due to silver nanoparticles loaded through a green approach is a promising research challenge of the biomaterial field. In this research work, two bioactive glasses have been doubly surface functionalized with polyphenols (gallic acid or natural polyphenols extracted from red grape skins and green tea leaves) and silver nanoparticles deposited by in situ reduction from a silver nitrate aqueous solution. The presence of biomolecules - showing reducing ability to directly obtain in situ metallic silver - and silver nanoparticles was investigated by means of UV-vis spectroscopy, X-Ray Photoelectron Spectroscopy (XPS) and Field Emission Scanning Electron Microscopy (FESEM). The antibacterial activity of the modified surfaces was tested against a multidrug resistant Staphylococcus aureus bacterial strain.

One-pot catalytic conversion of cellulose into polyols with Pt/CNTs catalysts.

PubMed

Yang, Li; Yan, Xiaopei; Wang, Qiwu; Wang, Qiong; Xia, Haian

2015-03-02

A series of Pt nanoparticles supported on carbon nanotubes (CNTs) were synthesized using the incipient-wetness impregnation method. These catalysts were characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy, and transmission electron microscope (TEM) techniques. The characterization results indicate that the Pt nanoparticles were highly dispersed on the surface of the CNTs, and the mean size was less than 5 nm. These catalysts were utilized to convert cellulose to hexitol, ethylene glycerol (EG), and 1,2-propylene glycol (1,2-PG) under low H2 pressure. The total yields were as high as 71.4% for EG and 1,2-PG using 1Pt/CNTs as the catalyst in the hydrolytic hydrogenation of cellulose under mild reaction conditions. Copyright © 2014 Elsevier Ltd. All rights reserved.

Azobenzene-based supramolecular polymers for processing MWCNTs.

PubMed

Maggini, Laura; Marangoni, Tomas; Georges, Benoit; Malicka, Joanna M; Yoosaf, K; Minoia, Andrea; Lazzaroni, Roberto; Armaroli, Nicola; Bonifazi, Davide

2013-01-21

Photothermally responsive supramolecular polymers containing azobenzene units have been synthesised and employed as dispersants for multi-walled carbon nanotubes (MWCNTs) in organic solvents. Upon triggering the trans-cis isomerisation of the supramolecular polymer intermolecular interactions between MWCNTs and the polymer are established, reversibly affecting the suspensions of the MWCNTs, either favouring it (by heating, i.e. cis→trans isomerisation) or inducing the CNTs' precipitation (upon irradiation, trans→cis isomerisation). Taking advantage of the chromophoric properties of the molecular subunits, the solubilisation/precipitation processes have been monitored by UV-Vis absorption spectroscopy. The structural properties of the resulting MWCNT-polymer hybrid materials have been thoroughly investigated via thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and atomic force microscopy (AFM) and modelled with molecular dynamics simulations.

Facile synthesis of mesoporous spinel NiCo2O4 nanostructures as highly efficient electrocatalysts for urea electro-oxidation

NASA Astrophysics Data System (ADS)

Ding, Rui; Qi, Li; Jia, Mingjun; Wang, Hongyu

2014-01-01

Mesoporous spinel nickel cobaltite (NiCo2O4) nanostructures were synthesized via a facile chemical deposition method coupled with a simple post-annealing process. The physicochemical properties were characterized via X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS) and nitrogen sorption measurements. The electrocatalytic performances were investigated by cyclic voltammetry (CV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) tests. The obtained NiCo2O4 materials exhibit typical agglomerate mesoporous nanostructures with a large surface area (190.1 m2 g-1) and high mesopore volume (0.943 cm3 g-1). Remarkably, the NiCo2O4 shows much higher catalytic activity, lower overpotential, better stability and greater tolerance towards urea electro-oxidation compared to those of cobalt oxide (Co3O4) synthesized by the same procedure. The NiCo2O4 electrode delivers a current density of 136 mA cm-2 mg-1 at 0.7 V (vs. Hg/HgO) in 1 M KOH and 0.33 M urea electrolytes accompanied with a desirable stability. The impressive electrocatalytic activity is largely ascribed to the high intrinsic electronic conductivity, superior mesoporous nanostructures and rich surface Ni active species of the NiCo2O4 materials, which can largely boost the interfacial electroactive sites and charge transfer rates for urea electro-oxidation, indicating promising applications in future wastewater remediation, hydrogen production and fuel cells.Mesoporous spinel nickel cobaltite (NiCo2O4) nanostructures were synthesized via a facile chemical deposition method coupled with a simple post-annealing process. The physicochemical properties were characterized via X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS) and nitrogen sorption measurements. The electrocatalytic performances were investigated by cyclic voltammetry (CV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) tests. The obtained NiCo2O4 materials exhibit typical agglomerate mesoporous nanostructures with a large surface area (190.1 m2 g-1) and high mesopore volume (0.943 cm3 g-1). Remarkably, the NiCo2O4 shows much higher catalytic activity, lower overpotential, better stability and greater tolerance towards urea electro-oxidation compared to those of cobalt oxide (Co3O4) synthesized by the same procedure. The NiCo2O4 electrode delivers a current density of 136 mA cm-2 mg-1 at 0.7 V (vs. Hg/HgO) in 1 M KOH and 0.33 M urea electrolytes accompanied with a desirable stability. The impressive electrocatalytic activity is largely ascribed to the high intrinsic electronic conductivity, superior mesoporous nanostructures and rich surface Ni active species of the NiCo2O4 materials, which can largely boost the interfacial electroactive sites and charge transfer rates for urea electro-oxidation, indicating promising applications in future wastewater remediation, hydrogen production and fuel cells. Electronic supplementary information (ESI) available: XRD patterns of NO and CO; XRD patterns and XPS profiles of CO; SEM images of CO; BET plots of CO; XPS quantitative analysis of NCO; a comparison of N2 sorption data between NCO and CO; the fitted values of impedimetric parameters of NCO and CO electrodes. See DOI: 10.1039/c3nr05359h

Cobalt terephthalate MOF-templated synthesis of porous nano-crystalline Co3O4 by the new indirect solid state thermolysis as cathode material of asymmetric supercapacitor

NASA Astrophysics Data System (ADS)

Bigdeli, Hadise; Moradi, Morteza; Hajati, Shaaker; Kiani, Mohammad Ali; Toth, Jozsef

2017-10-01

In this work, two different types of Co3O4 nano-crystals were synthesized by (i) conventional direct solid state thermolysis of cobalt terephthalate metal-organic framework (MOF-71) and (ii) new indirect solid state thermolysis of Co(OH)2 derived by alkaline aqueous treatment of MOF-71. The products were then characterized by X-ray diffraction technique (XRD), Fourier transforms infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Reflection electron energy loss spectroscopy (REELS), Brunauer, Emmett, and Teller (BET), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) techniques. By REELS analysis the energy band gap of MOF-71 was determined to be 3.7 eV. Further, electrochemical performance of each Co3O4 nanostructure was studied by the cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS) in a three-electrode system in KOH electrolyte. An asymmetric supercapacitor was fabricated using indirect Co3O4 nanoparticles as cathode and electrochemically reduced graphene oxide as anode, and the electrochemical properties were studied and showed a high energy density of 13.51 Wh kg-1 along with a power density of 9775 W kg-1 and good cycling stability with capacitance retention rate of 85% after 2000 cycles.

Attenuation of encrustation by self-assembled inorganic fullerene-like nanoparticles

NASA Astrophysics Data System (ADS)

Ron, Racheli; Zbaida, David; Kafka, Ilan Z.; Rosentsveig, Rita; Leibovitch, Ilan; Tenne, Reshef

2014-04-01

Ureteral stents and urethral catheters are commonly used medical devices for maintaining urinary flow. However, long-term placement (>30 days) of these devices in the urinary tracts is limited by the development of encrustation, a phenomenon that holds a prevalence of 50% within this patient population, resulting in a great deal of morbidity to the patients. Here we report the influence of surface coating of an all-silicone catheter with rhenium-doped fullerene-like molybdenum disulfide (Re:IF-MoS2) nanoparticles on the growth and attachment of in vitro encrustation stones. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD) analyses indicated a remarkable attenuation in encrustation occupation on the Re:IF-MoS2-coated catheter surfaces compared to neat catheters. The doped nanoparticles displayed a unique tendency to self-assemble into mosaic-like arrangements, modifying the surface to be encrustation-repellent. The mechanism of encrustation retardation on the surface coated catheters is discussed in some detail. The ramification of these results for the clogging of other body indwelling devices is briefly discussed.Ureteral stents and urethral catheters are commonly used medical devices for maintaining urinary flow. However, long-term placement (>30 days) of these devices in the urinary tracts is limited by the development of encrustation, a phenomenon that holds a prevalence of 50% within this patient population, resulting in a great deal of morbidity to the patients. Here we report the influence of surface coating of an all-silicone catheter with rhenium-doped fullerene-like molybdenum disulfide (Re:IF-MoS2) nanoparticles on the growth and attachment of in vitro encrustation stones. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD) analyses indicated a remarkable attenuation in encrustation occupation on the Re:IF-MoS2-coated catheter surfaces compared to neat catheters. The doped nanoparticles displayed a unique tendency to self-assemble into mosaic-like arrangements, modifying the surface to be encrustation-repellent. The mechanism of encrustation retardation on the surface coated catheters is discussed in some detail. The ramification of these results for the clogging of other body indwelling devices is briefly discussed. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr06231g

Fabrication and characterization of sub-micron scale hall devices from 2-dimensional electron gas at the heterostrutcure of GaAs/AlGaAs

NASA Astrophysics Data System (ADS)

Keswani, Neeti; Nakajima, Yoshikata; Chauhan, Neha; Kumar, Sakthi; Ohno, H.; Das, Pintu

2018-05-01

In this work, we report the fabrication and transport properties of sub-micron Hall devices to be used for nanomagnetic studies. Hall bars were fabricated using electron-beam lithography followed by wet etching of GaAs/AlGaAs heterostructures containing two-dimensional electron gas (2-DEG). Metallization using multiple metallic layers were used to achieve ohmic contacts with the 2-DEG which is about 240 nm below the surface. Detailed characterization of the metallic layers using X-ray Photoelectron Spectroscopy (XPS) demonstrate the role of alloy formation and diffusion to form ohmic contacts with the 2-DEG. Electronic transport measurements show the metallic character of the 2-DEG. Hall effect and magnetoresistance were measured to estimate the carrier mobility of 4.2×104 cm2/V-s at 5 K in dark.

Observation of positive and small electron affinity of Si-doped AlN films grown by metalorganic chemical vapor deposition on n-type 6H-SiC

NASA Astrophysics Data System (ADS)

Feng, Liang; Ping, Chen; De-Gang, Zhao; De-Sheng, Jiang; Zhi-Juan, Zhao; Zong-Shun, Liu; Jian-Jun, Zhu; Jing, Yang; Wei, Liu; Xiao-Guang, He; Xiao-Jing, Li; Xiang, Li; Shuang-Tao, Liu; Hui, Yang; Li-Qun, Zhang; Jian-Ping, Liu; Yuan-Tao, Zhang; Guo-Tong, Du

2016-05-01

We have investigated the electron affinity of Si-doped AlN films (N Si = 1.0 × 1018-1.0 × 1019 cm-3) with thicknesses of 50, 200, and 400 nm, synthesized by metalorganic chemical vapor deposition (MOCVD) under low pressure on the n-type (001)6H-SiC substrates. The positive and small electron affinity of AlN films was observed through the ultraviolet photoelectron spectroscopy (UPS) analysis, where an increase in electron affinity appears with the thickness of AlN films increasing, i.e., 0.36 eV for the 50-nm-thick one, 0.58 eV for the 200-nm-thick one, and 0.97 eV for the 400-nm-thick one. Accompanying the x-ray photoelectron spectroscopy (XPS) analysis on the surface contaminations, it suggests that the difference of electron affinity between our three samples may result from the discrepancy of surface impurity contaminations. Project supported by the National Natural Science Foundation of China (Grant Nos. 61574135, 61574134, 61474142, 61474110, 61377020, 61376089, 61223005, and 61321063), the One Hundred Person Project of the Chinese Academy of Sciences, and the Basic Research Project of Jiangsu Province, China (Grant No. BK20130362).

A poly-epoxy surface explored by Hartree-Fock ΔSCF simulations of C1s XPS spectra

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

Gavrielides, A.; Duguet, T., E-mail: thomas.duguet@ensiacet.fr, E-mail: Paul.Bagus@unt.edu; Esvan, J.

Whereas poly-epoxy polymers represent a class of materials with a wide range of applications, the structural disorder makes them difficult to model. In the present work, we use good experimental model samples in the sense that they are pure, fully polymerized, flat and smooth, defect-free, and suitable for ultrahigh vacuum x-ray photoelectron spectroscopy, XPS, experiments. In parallel, we perform Hartree-Fock, HF, calculations of the binding energies, BEs, of the C1s electrons in a model molecule composed of the two constituents of the poly-epoxy sample. These C1s BEs were determined using the HF ΔSCF method, which is known to yield accuratemore » values, especially for the shifts of the BEs, ΔBEs. We demonstrate the benefits of combining rigorous theory with careful XPS measurements in order to obtain correct assignments of the C1s XPS spectra of the polymer sample. Both the relative binding energies—by the ΔSCF method—and relative intensities—in the sudden approximation, SA, are calculated. It results in an excellent match with the experimental spectra. We are able to identify 9 different chemical environments under the C1s peak, where an exclusively experimental work would have found only 3 contributions. In addition, we observe that some contributions are localized at discrete binding energies, whereas others allow a much wider range because of the variation of their second neighbor bound polarization. Therefore, HF-ΔSCF simulations significantly increase the spectral resolution of XPS and thus offer a new avenue for the exploration of the surface of polymers.« less

Electronic structure of α-SrB4O7: experiment and theory

NASA Astrophysics Data System (ADS)

Atuchin, V. V.; Kesler, V. G.; Zaitsev, A. I.; Molokeev, M. S.; Aleksandrovsky, A. S.; Kuzubov, A. A.; Ignatova, N. Y.

2013-02-01

The investigation of valence band structure and electronic parameters of constituent element core levels of α-SrB4O7 has been carried out with x-ray photoemission spectroscopy. Optical-quality crystal α-SrB4O7 has been grown by the Czochralski method. Detailed photoemission spectra of the element core levels have been recorded from the powder sample under excitation by nonmonochromatic Al Kα radiation (1486.6 eV). The band structure of α-SrB4O7 has been calculated by ab initio methods and compared to XPS measurements. It has been found that the band structure of α-SrB4O7 is weakly dependent on the Sr-related states.

Electronic structure of layered titanate Nd 2Ti 2O 7

NASA Astrophysics Data System (ADS)

Atuchin, V. V.; Gavrilova, T. A.; Grivel, J.-C.; Kesler, V. G.

2008-10-01

The electronic structure of the binary titanate Nd 2Ti 2O 7 has been studied by X-ray photoelectron spectroscopy (XPS). Spectral features of the valence band and all constituent element core levels have been considered. The Auger parameters of titanium and oxygen in Nd 2Ti 2O 7 are determined as αTi = 873.5 and αO = 1042.2 eV. Chemical bonding effects have been discussed with the binding energies differences ΔTi = (BE O 1s - BE Ti 2p 3/2) = 71.5 eV and ΔNd = (BE Nd 3d 5/2 - BE O 1s) = 452.5 eV as key parameters in comparison with those in other titanium- and neodymium-bearing oxides.

Structural, morphological and electronic properties of pulsed laser grown Eu2O3 thin films

NASA Astrophysics Data System (ADS)

Kumar, Sandeep; Prakash, Ram; Choudhary, R. J.; Phase, D. M.

2018-05-01

Herein, we report the growth, structural, morphological and electronic properties of Europium sesquioxide (Eu2O3) thin films on Si [1 0 0] substrate using pulsed laser deposition technique. The films were deposited at ˜750 °C substrate temperature while the oxygen partial pressure (OPP) was varied (vacuum,˜1 mTorr, ˜10 mTorr and ˜300 mTorr). X-ray diffraction results confirm the single phase cubic structure of the film grown at ˜300 mTorr. The XRD results are also supported by the Raman's spectroscopy results. Eu-3d XPS core level spectra confirms the dominant contributions from the "3+" states of Eu in the film.

Structural and Electrochemical Characteristics of Ca-Doped “Flower-like” Li 4Ti 5O 12 Motifs as High-Rate Anode Materials for Lithium-Ion Batteries

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

Wang, Lei; Zhang, Yiman; Guo, Haoyue

Doped motifs offer an intriguing structural pathway toward improving conductivity for battery applications. Specifically, Ca-doped, three-dimensional “flower-like” Li 4–xCa xTi 5O 12 (“x” = 0, 0.1, 0.15, and 0.2) micrometer-scale spheres have been successfully prepared for the first time using a simple and reproducible hydrothermal reaction followed by a short calcination process. The products were experimentally characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) mapping, inductively coupled plasma optical emission spectrometry (ICP-OES), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and galvanostatic charge–discharge testing. Calcium dopantmore » ions were shown to be uniformly distributed within the LTO structure without altering the underlying “flower-like” morphology. The largest lattice expansion and the highest Ti 3+ ratios were noted with XRD and XPS, respectively, whereas increased charge transfer conductivity and decreased Li +-ion diffusion coefficients were displayed in EIS for the Li 4–xCa xTi 5O 12 (“x” = 0.2) sample. The “x” = 0.2 sample yielded a higher rate capability, an excellent reversibility, and a superior cycling stability, delivering 151 and 143 mAh/g under discharge rates of 20C and 40C at cycles 60 and 70, respectively. In addition, a high cycling stability was demonstrated with a capacity retention of 92% after 300 cycles at a very high discharge rate of 20C. In addition, first-principles calculations based on density functional theory (DFT) were conducted with the goal of further elucidating and understanding the nature of the doping mechanism in this study. The DFT calculations not only determined the structure of the Ca-doped Li 4Ti 5O 12, which was found to be in accordance with the experimentally measured XPD pattern, but also yielded valuable insights into the doping-induced effect on both the atomic and electronic structures of Li 4Ti 5O 12.« less

Structural and Electrochemical Characteristics of Ca-Doped “Flower-like” Li 4Ti 5O 12 Motifs as High-Rate Anode Materials for Lithium-Ion Batteries

DOE PAGES

Wang, Lei; Zhang, Yiman; Guo, Haoyue; ...

2018-01-22

Doped motifs offer an intriguing structural pathway toward improving conductivity for battery applications. Specifically, Ca-doped, three-dimensional “flower-like” Li 4–xCa xTi 5O 12 (“x” = 0, 0.1, 0.15, and 0.2) micrometer-scale spheres have been successfully prepared for the first time using a simple and reproducible hydrothermal reaction followed by a short calcination process. The products were experimentally characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) mapping, inductively coupled plasma optical emission spectrometry (ICP-OES), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and galvanostatic charge–discharge testing. Calcium dopantmore » ions were shown to be uniformly distributed within the LTO structure without altering the underlying “flower-like” morphology. The largest lattice expansion and the highest Ti 3+ ratios were noted with XRD and XPS, respectively, whereas increased charge transfer conductivity and decreased Li +-ion diffusion coefficients were displayed in EIS for the Li 4–xCa xTi 5O 12 (“x” = 0.2) sample. The “x” = 0.2 sample yielded a higher rate capability, an excellent reversibility, and a superior cycling stability, delivering 151 and 143 mAh/g under discharge rates of 20C and 40C at cycles 60 and 70, respectively. In addition, a high cycling stability was demonstrated with a capacity retention of 92% after 300 cycles at a very high discharge rate of 20C. In addition, first-principles calculations based on density functional theory (DFT) were conducted with the goal of further elucidating and understanding the nature of the doping mechanism in this study. The DFT calculations not only determined the structure of the Ca-doped Li 4Ti 5O 12, which was found to be in accordance with the experimentally measured XPD pattern, but also yielded valuable insights into the doping-induced effect on both the atomic and electronic structures of Li 4Ti 5O 12.« less

A first-principles core-level XPS study on the boron impurities in germanium crystal

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

Yamauchi, Jun; Yoshimoto, Yoshihide; Suwa, Yuji

2013-12-04

We systematically investigated the x-ray photoelectron spectroscopy (XPS) core-level shifts and formation energies of boron defects in germanium crystals and compared the results to those in silicon crystals. Both for XPS core-level shifts and formation energies, relationship between defects in Si and Ge is roughly linear. From the similarity in the formation energy, it is expected that the exotic clusters like icosahedral B12 exist in Ge as well as in Si.

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

Ding, Laura; Harvey, Stephen P.; Teeter, Glenn

We demonstrate the potential of X-ray photoelectron spectroscopy (XPS) to characterize new carrier-selective contacts (CSC) for solar cell application. We show that XPS not only provides information about the surface chemical properties of the CSC material, but that operando XPS, i.e. under light bias condition, can also directly measure the photovoltage that develops at the CSC/absorber interface, revealing device relevant information without the need of assembling a full solar cell. We present the application of the technique to molybdenum oxide hole-selective contact films on a crystalline silicon absorber.

Morphological investigation of nanostructured CoMo catalysts

NASA Astrophysics Data System (ADS)

Pawelec, B.; Castaño, P.; Zepeda, T. A.

2008-04-01

This work reports the morphological investigation of nanostructured sulfided CoMo catalysts by means of high-resolution transmission electron microscopy (HRTEM). The catalysts were supported on Ti-modified hexagonal mesoporous silica (HMS-Ti) and P-modified HMS-Ti (P/HMS-Ti) materials. The oxide precursors were characterized by specific surface area (S BET), temperature-programmed reduction (TPR), diffuse reflectance infrared Fourier transform spectroscopy in the OH region (DRIFTS-OH) and X-ray photoelectron spectroscopy (XPS) in order to elucidate the influence of the impregnation sequence (successive vs. simultaneous) and the effect of P-incorporation into HMS-Ti material on the morphology of calcined CoMo catalysts. Both TPR and XPS measurements indicate that the catalysts prepared by successive impregnation possess well-dispersed MoO 3 and CoO phases, whereas their counterparts prepared by simultaneous impregnation additionally possess the CoMoO 4 phase. For all sulfided catalysts, the presence of MoS 2 phase with particle size in the range 3.3-4.4 nm was confirmed by HRTEM. Catalytic activity was evaluated in the reaction of hydrodesulfurization (HDS) of dibenzothiophene (DBT) carried out in a flow reactor at 593 K and hydrogen pressure of 5.5 MPa. P-incorporation into the HMS-Ti material led to an overall increase in HDS activity and the hydrogenation ability of the sulfided catalysts. All catalysts proved to be stable during 10 h time-on-stream (TOS) operation. The activity of sulfide catalysts in the target reaction depends linearly on the surface exposure of Co species in the oxide precursors, as determined by XPS, and on the morphology of the sulfide form of catalysts (surface density of MoS 2 particles and their sizes) as determined by HRTEM.

Oxygen vacancy effect on photoluminescence of KNb3O8 nanosheets

NASA Astrophysics Data System (ADS)

Li, Rui; Liu, Liying; Ming, Bangming; Ji, Yuhang; Wang, Ruzhi

2018-05-01

Fungus-like potassium niobate (KNb3O8) nanosheets have been synthesized on indium-doped tin oxide (ITO) glass substrates by a simple and environmental friendly two-step hydrothermal process. The prepared samples have been characterized by using X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), High Resolution Transmission Electron Microscope (HRTEM), Fourier Transform Infra-Red Spectroscopy (FTIR), Raman Spectroscopy and X-ray Photoelectron Spectroscopy (XPS). Furthermore, the photoluminescence (PL) of KNb3O8 nanosheets have been systematically studied. The results showed that the PL spectrum is between 300 and 645 nm with a 325 nm light excitation, which is divided into some sub-peaks. It is different from the perfect KNb3O8 nanosheets whose PL emission peaks located at near 433 nm. It should be originated from the effect of the oxygen (O) vacancies in the KNb3O8 nanosheets, which the PLs peaks can be found at about 490 nm and 530 nm by different position of O vacancy. The experimental results are in accordance with the first-principles calculations. Our results may present a feasible clue to estimate the defect position in KNb3O8 by the shape analysis of its spectrum of PLs.

Understanding the effects of Cr doping in rutile TiO2 by DFT calculations and X-ray spectroscopy.

PubMed

Vásquez, G Cristian; Maestre, David; Cremades, Ana; Ramírez-Castellanos, Julio; Magnano, Elena; Nappini, Silvia; Karazhanov, Smagul Zh

2018-06-07

The effects of Cr on local environment and electronic structure of rutile TiO 2 are studied combining theoretical and experimental approaches. Neutral and negatively charged substitutional Cr impurities Cr Ti 0 and Cr Ti 1- as well as Cr-oxygen vacancy complex 2Cr Ti  + V O are studied by the density functional theory (DFT) within the generalized gradient approximation (GGA) of Perdew-Burke-Ernzerhof (PBE) functional. Experimental results based on X-Ray absorption spectroscopy (XAS) and X-Ray photoelectron spectroscopy (XPS) performed on Cr doped TiO 2 at the Synchrotron facility were compared to the theoretical results. It is shown that the electrons of the oxygen vacancy tend to be localized at the t 2g states of the Cr ions in order to reach the stable oxidation state of Cr 3+ . Effects of Cr on crystal field (CF) and structural distortions in the rutile TiO 2 cell were analyzed by the DFT calculations and XAS spectra revealing that the CF and tetragonal distortions in TiO 2 are very sensitive to the concentration of Cr.

Interfaces in heterogeneous catalytic reactions: Ambient pressure XPS as a tool to unravel surface chemistry

DOE PAGES

Palomino, Robert M.; Hamlyn, Rebecca; Liu, Zongyuan; ...

2017-04-27

In this paper we provide a summary of the recent development of ambient pressure X-ray photoelectron spectroscopy (AP-XPS) and its application to catalytic surface chemistry. The methodology as well as significant advantages and challenges associated with this novel technique are described. Details about specific examples of using AP-XPS to probe surface chemistry under working reaction conditions for a number of reactions are explained: CO oxidation, water-gas shift (WGS), CO 2 hydrogenation, dry reforming of methane (DRM) and ethanol steam reforming (ESR). In conclusion, we discuss insights into the future development of the AP-XPS technique and its applications.

Interfaces in heterogeneous catalytic reactions: Ambient pressure XPS as a tool to unravel surface chemistry

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

Palomino, Robert M.; Hamlyn, Rebecca; Liu, Zongyuan

In this paper we provide a summary of the recent development of ambient pressure X-ray photoelectron spectroscopy (AP-XPS) and its application to catalytic surface chemistry. The methodology as well as significant advantages and challenges associated with this novel technique are described. Details about specific examples of using AP-XPS to probe surface chemistry under working reaction conditions for a number of reactions are explained: CO oxidation, water-gas shift (WGS), CO 2 hydrogenation, dry reforming of methane (DRM) and ethanol steam reforming (ESR). In conclusion, we discuss insights into the future development of the AP-XPS technique and its applications.

Insights into structure and dynamics of (Mn,Fe)Ox-promoted Rh nanoparticles.

PubMed

Dimitrakopoulou, Maria; Huang, Xing; Kröhnert, Jutta; Teschner, Detre; Praetz, Sebastian; Schlesiger, Christopher; Malzer, Wolfgang; Janke, Christiane; Schwab, Ekkehard; Rosowski, Frank; Kaiser, Harry; Schunk, Stephan; Schlögl, Robert; Trunschke, Annette

2018-05-29

The mutual interaction between Rh nanoparticles and manganese/iron oxide promoters in silica-supported Rh catalysts for the hydrogenation of CO to higher alcohols was analyzed by applying a combination of integral techniques including temperature-programmed reduction (TPR), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS) and Fourier transform infrared (FTIR) spectroscopy with local analysis by using high angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) in combination with energy dispersive X-ray spectroscopy (EDX). The promoted catalysts show reduced CO adsorption capacity as evidenced through FTIR spectroscopy, which is attributed to a perforated core-shell structure of the Rh nano-particles in accordance with the microstructural analysis from electron microscopy. Iron and manganese occur in low formal oxidation states between 2+ and zero in the reduced catalysts as shown by using TPR and XAS. Infrared spectroscopy measured in diffuse reflectance at reaction temperature and pressure indicates that partial coverage of the Rh particles is maintained at reaction temperature under operation and that the remaining accessible metal adsorption sites might be catalytically less relevant because the hydrogenation of adsorbed carbonyl species at 523 K and 30 bar hydrogen essentially failed. It is concluded that Rh0 is poisoned due to the adsorption of CO under the reaction conditions of CO hydrogenation. The active sites are associated either with a (Mn,Fe)Ox (x < 0.25) phase or species at the interface between Rh and its co-catalyst (Mn,Fe)Ox.

Tribochemistry of contact interfaces of nanocrystalline molybdenum carbide films

NASA Astrophysics Data System (ADS)

Kumar, D. Dinesh; Kumar, N.; Panda, Kalpataru; Kamalan Kirubaharan, A. M.; Kuppusami, P.

2018-07-01

Transition metal carbides (TMC) are known for their improved tribological properties and are sensitive to the tribo-atmospheric environment. Nanocrystalline molybdenum carbide (MoC) thin films were deposited by DC magnetron sputtering technique using reactive CH4 gas. The friction and wear resistance properties of MoC thin films were significantly improved in humid-atmospheric condition as compared to high-vacuum tribo-condition. A comprehensive chemical analysis of deformed contact interfaces was carried out by X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDX) and Raman spectroscopy. XPS and Raman spectroscopy showed the formation of stable molybdenum-oxide (MoO), molybdenum carbide (MoC) and amorphous carbon (a-C) tribo-phases. Moreover, during the sliding in humid-atmospheric condition, these phases were extensively deposited on the sliding steel ball counter body which significantly protected against undesirable friction and wear.

Evidence of room temperature ferromagnetism in argon/oxygen annealed TiO2 thin films deposited by electron beam evaporation technique

NASA Astrophysics Data System (ADS)

Mohanty, P.; Kabiraj, D.; Mandal, R. K.; Kulriya, P. K.; Sinha, A. S. K.; Rath, Chandana

2014-04-01

TiO2 thin films deposited by electron beam evaporation technique annealed in either O2 or Ar atmosphere showed ferromagnetism at room temperature. The pristine amorphous film demonstrates anatase phase after annealing under Ar/O2 atmosphere. While the pristine film shows a super-paramagnetic behavior, both O2 and Ar annealed films display hysteresis at 300 K. X-ray photo emission spectroscopy (XPS), Raman spectroscopy, Rutherford's backscattering spectroscopy (RBS), cross-sectional transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS) were used to refute the possible role of impurities/contaminants in magnetic properties of the films. The saturation magnetization of the O2 annealed film is found to be higher than the Ar annealed one. It is revealed from shifting of O 1s and Ti 2p core level spectra as well as from the enhancement of high binding energy component of O 1s spectra that the higher magnetic moment is associated with higher oxygen vacancies. In addition, O2 annealed film demonstrates better crystallinity, uniform deposition and smoother surface than that of the Ar annealed one from glancing angle X-ray diffraction (GAXRD) and atomic force microscopy (AFM). We conclude that although ferromagnetism is due to oxygen vacancies, the higher magnetization in O2 annealed film could be due to crystallinity, which has been observed earlier in Co doped TiO2 film deposited by pulsed laser deposition (Mohanty et al., 2012 [10]).

As-Received, Ozone Cleaned and Ar+ Sputtered Surfaces of Hafnium Oxide Grown by Atomic Layer Deposition and Studied by XPS

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

Engelhard, Mark H.; Herman, Jacob A.; Wallace, Robert

2012-06-27

In this study, X-ray photoelectron spectroscopy (XPS) characterization was performed on 47 nm thick hafnium oxide (HfO{sub 2}) films grown by atomic layer deposition using TEMA-Hf/H{sub 2}O at 250 C substrate temperature. HfO{sub 2} is currently being studied as a possible replacement for Silicon Oxide (SiO{sub 2}) as a gate dielectric in electronics transistors. XPS spectra were collected on a Physical Electronics Quantum 2000 Scanning ESCA Microprobe using a monochromatic Al K{sub a} X-ray (1486.7 eV) excitation source. The sample was analyzed under the following conditions: as received, after UV irradiation for five minutes, and after sputter cleaning with 2more » kV Ar{sup +} ions for 180 seconds. Survey scans showed carbon, oxygen, and hafnium as the major species in the film, while the only minor species of argon and carbide was detected after sputtering. Adventitious carbon initially composed approximately 18.6 AT% of the surface, but after UV cleaning it was reduced to 2.4 AT%. This demonstrated that that the majority of carbon was due to adventitious carbon. However, after 2 kV Ar{sup +} sputtering there was still only trace amounts of carbon at {approx}1 AT%, Some of this trace carbon is now in the form of a carbide due to the interaction with Ar{sup +} used for sputter cleaning. Furthermore, the stoiciometric ratio of oxygen and hafnium is consistent with a high quality HfO{sub 2} film.« less

Electronic structure and optical properties of defect chalcopyrite HgGa2Se4

NASA Astrophysics Data System (ADS)

Gabrelian, B. V.; Lavrentyev, A. A.; Vu, Tuan V.; Parasyuk, O. V.; Khyzhun, O. Y.

2018-01-01

We report on studies from an experimental and theoretical viewpoint of the electronic structure of mercury digallium selenide, HgGa2Se4, a very promising optoelectronic material. In particular, the method of X-ray photoelectron spectroscopy (XPS) was used to evaluate binding energies of the constituent element core electrons and the shape of the valence band for pristine and Ar+-ion bombarded surfaces of HgGa2Se4 single crystal. First principles band-structure calculations were performed in the present work using the augmented plane wave + local orbitals (APW+lo). These calculations indicate that the Se 4p states are the main contributors at the top and in the upper portion of the valence band with slightly smaller contributions of the Ga 4p states in the upper portion of the band as well. Further, the central portion of the valence band is determined mainly by contributions of the Ga 4s states, and the Hg 5d states are the principal contributors to the bottom of the valence band. These theoretical data are in fair agreement when matching on a common energy scale of the X-ray emission bands giving information on the energy distribution of the Se 4p and Ga 4p states and the XPS valence-band spectrum of the HgGa2Se4 crystal. The principal optical constants are elucidated from the DFT calculations.

Characterization of Ar/N2/H2 middle-pressure RF discharge and application of the afterglow region for nitridation of GaAs

NASA Astrophysics Data System (ADS)

Raud, J.; Jõgi, I.; Matisen, L.; Navrátil, Z.; Talviste, R.; Trunec, D.; Aarik, J.

2017-12-01

This work characterizes the production and destruction of nitrogen and hydrogen atoms in RF capacitively coupled middle-pressure discharge in argon/nitrogen/hydrogen mixtures. Input power, electron concentration, electric field strength and mean electron energy were determined on the basis of electrical measurements. Gas temperature and concentration of Ar atoms in 1s states were determined from spectral measurements. On the basis of experimentally determined plasma characteristics, main production and loss mechanisms of H and N atoms were discussed. The plasma produced radicals were applied for the nitridation and oxide reduction of gallium arsenide in the afterglow region of discharge. After plasma treatment the GaAs samples were analyzed using x-ray photoelectron spectroscopy (XPS) technique. Successful nitridation of GaAs sample was obtained in the case of Ar/5% N2 discharge. In this gas mixture the N atoms were generated via dissociative recombination of N2+ created by charge transfer from Ar+. The treatment in Ar/5% N2/1% H2 mixture resulted in the reduction of oxide signals in the XPS spectra. Negligible formation of GaN in the latter mixture was connected with reduced concentration of N atoms, which was, in turn, due to less efficient mechanism of N atom production (electron impact dissociation of N2 molecules) and additional loss channel in reaction with H2.

XPS Study of Oxide/GaAs and SiO2/Si Interfaces

NASA Technical Reports Server (NTRS)

Grunthaner, F. J.; Grunthaner, P. J.; Vasquez, R. P.; Lewis, B. F.; Maserjian, J.; Madhukar, A.

1982-01-01

Concepts developed in study of SiO2/Si interface applied to analysis of native oxide/GaAs interface. High-resolution X-ray photoelectron spectroscopy (XPS) has been combined with precise chemical-profiling technique and resolution-enhancement methods to study stoichiometry of transitional layer. Results are presented in report now available.

Atomic force measurements of 16-mercaptohexadecanoic acid and its salt with CH 3, OH, and CONHCH 3 functionalized self-assembled monolayers

NASA Astrophysics Data System (ADS)

Morales-Cruz, Angel L.; Tremont, Rolando; Martínez, Ramón; Romañach, Rodolfo; Cabrera, Carlos R.

2005-03-01

Chemical and mechanical properties of different compounds can be elucidated by measuring fundamental forces such as adhesion, attraction and repulsion, between modified surfaces by means of atomic force microscopy (AFM) in force mode calibration. This work presents a combination of AFM, self-assembled monolayers (SAMs), and crystallization techniques to study the forces of interaction between excipients and active ingredients used in pharmaceutical formulations. SAMs of 16-mercaptohexadecanoate, which represent magnesium stereate, were used to modify the probe tip, whereas CH3-, OH- and CONHCH3-functional SAMs were formed on a gold-coated mica substrate, and used as examples of the surfaces of lactose and theophylline. The crystals of lactose and theophylline were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The modification of gold surfaces with 16-mercaptohexadecanoate, 10-mercapto-1-decanol (OH-functional SAM), 1-decanethiol (CH3-functional) and N-methyl-11-mercaptoundecanamide (CONHCH3-functional SAM) was studied by X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and Fourier transform-infrared spectroscopy (FT-IR) in specular reflectance mode. XPS and AES results of the modified surfaces showed the presence of sulfur binding, and kinetic energies that correspond to the presence of 10-mercapto-1-decanol, 1-decanethiol, N-methyl-11-mercaptoundecanamide and the salt of 16-mercaptohexadecanoic acid. The absorption bands in the IR spectra further confirm the modification of the gold-coated substrates with these compounds. Force versus distance measurements were performed between the modified tip and the modified gold-coated mica substrates. The mean adhesion forces between the COO-Ca2+ functionalized tip and the CH3-, OH-, and CONHCH3-modified substrates were determined to be 4.5, 8.9 and 6.3 nN, respectively. The magnitude of the adhesion force (ion-dipole) interaction between the modified tip and substrate decreases in the following order: COO-Ca2+/OH > COO-Ca2+/CONHCH3 > COO-Ca2+/CH3.

XPS and 31P NMR inquiry of Eu3+-induced structural modification in SnO-containing phosphate glass

NASA Astrophysics Data System (ADS)

Jiménez, José A.; Fachini, Esteban Rosim; Zhao, Chunqing

2018-07-01

The influence of Eu3+ doping on the structural properties of SnO-containing phosphate glass has been investigated by X-ray photoelectron spectroscopy (XPS) and 31P nuclear magnetic resonance (NMR) spectroscopy. Oxygen 1s XPS data indicates that the Eu3+ doping results in a higher concentration of non-bridging oxygens in the glass matrix, whereas 31P NMR shows an increase in the terminal phosphate chain tetrahedral units, i.e. the amount of Q1 sites with only one bridging oxygen. Accordingly, both techniques agree with a depolymerization effect induced by the Eu3+ ions. Further, XPS reveals that together with the Eu3+ doping, the presence of Sn4+ is supported while the presence of Eu2+ is also indicated. The structural changes are then indicated to be a consequence of redox chemistry between Sn2+ and Eu3+ promoting a transition of tin from Sn2+ with a role as network former to Sn4+ acting as network modifier in the glass system.

X-ray photoelectron spectroscopy on 1-peso and 2-pesos of the Argentine Republic

NASA Astrophysics Data System (ADS)

Gard, Faramarz S.; Duffo, Gustavo; Bergamasco, Pablo; Forlerer, Elena

2018-04-01

Relative concentrations of nickel and copper at the surface of the ring and centre parts of 1-peso and 2-pesos Argentine coins have been studied by means of X-ray photoemission spectroscopy (XPS). It has been observed Ni-enrichment at the surface of the ring (silvery) part of a 1-peso, minted in 1994, whereas the XPS data reveals lack of nickel at the surface of the centre (silvery) part of a 2-pesos, minted in 2016. This discrepancy is explained by analyzing the XPS peaks of oxygen and carbon, and is suggested to be related to the contamination layer on the surface of the coins. The XPS analysis of the golden parts of the coins, namely the centre part of the 1-peso and the ring part of the 2-pesos coins were inconclusive, due to the small amount of the Ni (nominally %2) used in those parts. The possible oxidations states of the metals at the surface of the untreated and treated coins with the artificial human sweat were also identified.

Study on the surface sulfidization behavior of smithsonite at high temperature

NASA Astrophysics Data System (ADS)

Lv, Jin-fang; Tong, Xiong; Zheng, Yong-xing; Xie, Xian; Wang, Cong-bing

2018-04-01

Surface sulfidization behavior of smithsonite at high temperature was investigated by X-ray powder diffractometer (XRD) along with thermodynamic calculation, X-ray photoelectron spectroscopy (XPS) and electron probe microanalysis (EPMA). The XRD and thermodynamic analyses indicated that the smithsonite was decomposed into zincite at high temperatures. After introducing a small amount of pyrite, artificial sulfides were formed at surface of the obtained zincite. The XPS analyses revealed that the sulfide species including zinc sulfide and zinc disulfide were generated at the zincite surface. The EPMA analyses demonstrated that the film of sulfides was unevenly distributed at the zincite surface. The average concentration of elemental sulfur at the sample surface increased with increasing of pyrite dosage. A suitable mole ratio of FeS2 to ZnCO3 for the surface thermal modification was determined to be about 0.3. These findings can provide theoretical support for improving the process during which the zinc recovery from refractory zinc oxide ores is achieved by xanthate flotation.

Interfacial microanalysis of rubber tyre-cord adhesion and the influence of cobalt

NASA Astrophysics Data System (ADS)

Fulton, W. Stephen; Smith, Graham C.; Titchener, Keith J.

2004-01-01

The effect of cobalt-containing adhesion promoters on the structure and morphology of rubber-brass and rubber-tyre-cord interfaces before and after ageing has been investigated by X-ray photoelectron spectroscopy (XPS) depth profiling, glancing incidence X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effect the cobalt adhesion promoters had upon the interface morphology as they suppressed the growth of crystalline dendrites normally associated with the ageing process was imaged in TEM using samples prepared by the focused ion beam (FIB) milling technique. XPS depth profiling through the interfaces revealed that different types of adhesion promoter influenced the amount and distribution of cobalt ions in the bonding layer. XRD demonstrated the influence that cobalt had upon the structure of the interface and subsequent crystallinity, with a lesser degree of crystallinity being associated with better adhesion performance. From the results a model for the effect of the Co chemistry of the adhesion promotor has been developed.

Surface analysis of graphite fiber reinforced polyimide composites

NASA Technical Reports Server (NTRS)

Messick, D. L.; Progar, D. J.; Wightman, J. P.

1983-01-01

Several techniques have been used to establish the effect of different surface pretreatments on graphite-polyimide composites. Composites were prepared from Celion 6000 graphite fibers and the polyimide LARC-160. Pretreatments included mechanical abrasion, chemical etching and light irradiation. Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) were used in the analysis. Contact angle of five different liquids of varying surface tensions were measured on the composites. SEM results showed polymer-rich peaks and polymer-poor valleys conforming to the pattern of the release cloth used durng fabrication. Mechanically treated and light irradiated samples showed varying degrees of polymer peak removal, with some degradation down to the graphite fibers. Minimal changes in surface topography were observed on concentrations of surface fluorine even after pretreatment. The light irradiation pretreatment was most effective at reducing surface fluorine concentrations whereas chemical pretreatment was the least effective. Critical surface tensions correlated directly with the surface fluorine to carbon ratios as calculated from XPS.

X-ray photoelectron spectroscopic analysis of rice kernels and flours: Measurement of surface chemical composition.

PubMed

Nawaz, Malik A; Gaiani, Claire; Fukai, Shu; Bhandari, Bhesh

2016-12-01

The objectives of this study were to evaluate the ability of X-ray photoelectron spectroscopy (XPS) to differentiate rice macromolecules and to calculate the surface composition of rice kernels and flours. The uncooked kernels and flours surface composition of the two selected rice varieties, Thadokkham-11 (TDK11) and Doongara (DG) demonstrated an over-expression of lipids and proteins and an under-expression of starch compared to the bulk composition. The results of the study showed that XPS was able to differentiate rice polysaccharides (mainly starch), proteins and lipids in uncooked rice kernels and flours. Nevertheless, it was unable to distinguish components in cooked rice samples possibly due to complex interactions between gelatinized starch, denatured proteins and lipids. High resolution imaging methods (Scanning Electron Microscopy and Confocal Laser Scanning Microscopy) were employed to obtain complementary information about the properties and location of starch, proteins and lipids in rice kernels and flours. Copyright © 2016. Published by Elsevier Ltd.

[Characteristics of hydroxyapatite/PMMA nanocomposites for provisional restoration and its biocompatibility with human gingival fibroblasts].

PubMed

Zhang, Jing-chao; Mo, An-chun; Li, Ji-dong; Wang, Xue-jiang; Li, Yu-bao

2014-05-01

To formulate hydroxyapatite (HA)/polymethyl methacrylate (PMMA) composites with improved cytocompatibility for provisional restoration. Nanocomposites with 20 wt%, 30 wt%, 40 wt%, and 50 wt% HA/PMMA (H/P) were developed and examined using X-ray photoelectron spectroscopy (XPS) and scanning electron microscope (SEM). Human gingival fibroblasts were cultured on those HA/PMMA discs and investigated by fluorescent staining on 24 h and MTT assay at 1 d, 3 d, 5 d and 7 d. Chemical integration of HA/PMMA interface was confirmed by XPS. Typical fusiform cells with adhesion spots were detected on 40 wt% and 50 wt% H/P discs. MTT results showed insignificant differences in cell growth between 40 wt% H/P and pure titanium (Ti, P > 0.05), while the other H/P discs showed significantly lower cell growth than pure Ti (P < 0.05). 40 wt% H/P might be a promising candidate for provisional dental implant restoration and for esthetic gingival contour.

Portable total reflection x-ray fluorescence analysis in the identification of unknown laboratory hazards

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

Liu, Ying, E-mail: liu.ying.48r@st.kyoto-u.ac.jp; Imashuku, Susumu; Sasaki, Nobuharu

In this study, a portable total reflection x-ray fluorescence (TXRF) spectrometer was used to analyze unknown laboratory hazards that precipitated on exterior surfaces of cooling pipes and fume hood pipes in chemical laboratories. With the aim to examine the accuracy of TXRF analysis for the determination of elemental composition, analytical results were compared with those of wavelength-dispersive x-ray fluorescence spectrometry, scanning electron microscope and energy-dispersive x-ray spectrometry, energy-dispersive x-ray fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry, x-ray diffraction spectrometry (XRD), and x-ray photoelectron spectroscopy (XPS). Detailed comparison of data confirmed that the TXRF method itself was not sufficient tomore » determine all the elements (Z > 11) contained in the samples. In addition, results suggest that XRD should be combined with XPS in order to accurately determine compound composition. This study demonstrates that at least two analytical methods should be used in order to analyze the composition of unknown real samples.« less

Improved flotation performance of hematite fines using citric acid as a dispersant

NASA Astrophysics Data System (ADS)

Luo, Xi-mei; Yin, Wan-zhong; Sun, Chuan-yao; Wang, Nai-ling; Ma, Ying-qiang; Wang, Yun-fan

2016-10-01

In this study, citric acid was used as a dispersant to improve the flotation performance of hematite fines. The effect and mechanism of citric acid on the reverse flotation of hematite fines were investigated by flotation tests, sedimentation experiments, scanning electron microscopy (SEM), zeta-potential measurements, and X-ray photoelectron spectroscopy (XPS). The results of SEM analysis and flotation tests reveal that a strong heterocoagulation in the form of slime coating or coagulation in hematite fine slurry affects the beneficiation of hematite ores by froth flotation. The addition of a small amount of citric acid (less than 300 g/t) favorably affects the reverse flotation of hematite fines by improving particle dispersion. The results of sedimentation experiments, zeta-potential measurements, and XPS measurements demonstrate that citric acid adsorbs onto hematite and quartz surfaces via hydrogen bonding, thereby reducing the zeta potentials of mineral surfaces, strengthening the electrical double-layer repulsion between mineral particles, and dispersing the pulp particles.

High performance SONOS flash memory with in-situ silicon nanocrystals embedded in silicon nitride charge trapping layer

NASA Astrophysics Data System (ADS)

Lim, Jae-Gab; Yang, Seung-Dong; Yun, Ho-Jin; Jung, Jun-Kyo; Park, Jung-Hyun; Lim, Chan; Cho, Gyu-seok; Park, Seong-gye; Huh, Chul; Lee, Hi-Deok; Lee, Ga-Won

2018-02-01

In this paper, SONOS-type flash memory device with highly improved charge-trapping efficiency is suggested by using silicon nanocrystals (Si-NCs) embedded in silicon nitride (SiNX) charge trapping layer. The Si-NCs were in-situ grown by PECVD without additional post annealing process. The fabricated device shows high program/erase speed and retention property which is suitable for multi-level cell (MLC) application. Excellent performance and reliability for MLC are demonstrated with large memory window of ∼8.5 V and superior retention characteristics of 7% charge loss for 10 years. High resolution transmission electron microscopy image confirms the Si-NC formation and the size is around 1-2 nm which can be verified again in X-ray photoelectron spectroscopy (XPS) where pure Si bonds increase. Besides, XPS analysis implies that more nitrogen atoms make stable bonds at the regular lattice point. Photoluminescence spectra results also illustrate that Si-NCs formation in SiNx is an effective method to form deep trap states.

Preparation, Characterization and Intracellular Imaging of 2,4-Dichlorophenoxyacetic Acid Conjugated Gold Nanorods.

PubMed

Jia, Jin-Liang; Jin, Xiao-Yong; Liu, Qing-Le; Liang, Wen-Long; Lin, Miao-Shan; Xu, Han-Hong

2016-05-01

Visualizing the biodistribution of pesticides inside living cells is great importance for enhancing targeting of pesticides. Here we reported for the first time that gold nanorods (Au NRs) with size of 39.4 nm x 11.3 nm could be used as a fluorescent tracer to examine the distribution of a typical herbicide, 2,4-dichlorophenoxyacetic acid (2,4-D), in tobacco bright yellow 2 (BY-2) cells. The nanostructures of hybrid materials were analyzed by using Raman spectra and X-ray photoelectron spectroscopy (XPS), including spectra assignments and electronic property. These data revealed 2,4-D has successfully conjugated MP-Au NRs according to Raman and XPS. The biodistribution of the conjugates inside BY-2 cells was directly examined at 12 and 24 h by the two-photon microscopy. The intensity of two-photon luminescence (TPL) inside cells demonstrated that the conjugates could be localized and excluded by BY-2 cells. Thus, this labeling approach opens up new avenues to the facile and efficient labeling of pesticides.

Perspective: Chemical reactions in ionic liquids monitored through the gas (vacuum)/liquid interface.

PubMed

Maier, F; Niedermaier, I; Steinrück, H-P

2017-05-07

This perspective analyzes the potential of X-ray photoelectron spectroscopy under ultrahigh vacuum (UHV) conditions to follow chemical reactions in ionic liquids in situ. Traditionally, only reactions occurring on solid surfaces were investigated by X-ray photoelectron spectroscopy (XPS) in situ. This was due to the high vapor pressures of common liquids or solvents, which are not compatible with the required UHV conditions. It was only recently realized that the situation is very different when studying reactions in Ionic Liquids (ILs), which have an inherently low vapor pressure, and first studies have been performed within the last years. Compared to classical spectroscopy techniques used to monitor chemical reactions, the advantage of XPS is that through the analysis of their core levels all relevant elements can be quantified and their chemical state can be analyzed under well-defined (ultraclean) conditions. In this perspective, we cover six very different reactions which occur in the IL, with the IL, or at an IL/support interface, demonstrating the outstanding potential of in situ XPS to gain insights into liquid phase reactions in the near-surface region.

Metal ion interaction with phosphorylated tyrosine analogue monolayers on gold.

PubMed

Petoral, Rodrigo M; Björefors, Fredrik; Uvdal, Kajsa

2006-11-23

Phosphorylated tyrosine analogue molecules (pTyr-PT) were assembled onto gold substrates, and the resulting monolayers were used for metal ion interaction studies. The monolayers were characterized by X-ray photoelectron spectroscopy (XPS), infrared reflection-absorption spectroscopy (IRAS), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS), both prior to and after exposure to metal ions. XPS verified the elemental composition of the molecular adsorbate and the presence of metal ions coordinated to the phosphate groups. Both the angle-dependent XPS and IRAS results were consistent with the change in the structural orientation of the pTyr-PT monolayer upon exposure to metal ions. The differential capacitance of the monolayers upon coordination of the metal ions was evaluated using EIS. These metal ions were found to significantly change the capacitance of the pTyr-PT monolayers in contrast to the nonphosphorylated tyrosine analogue (TPT). CV results showed reduced electrochemical blocking capabilities of the phosphorylated analogue monolayer when exposed to metal ions, supporting the change in the structure of the monolayer observed by XPS and IRAS. The largest change in the structure and interfacial capacitance was observed for aluminum ions, compared to calcium, magnesium, and chromium ions. This type of monolayer shows an excellent capability to coordinate metal ions and has a high potential for use as sensing layers in biochip applications to monitor the presence of metal ions.

XPS Protocol for the Characterization of Pristine and Functionalized Single Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Sosa, E. D.; Allada, R.; Huffman, C. B.; Arepalli, S.

2009-01-01

Recent interest in developing new applications for carbon nanotubes (CNT) has fueled the need to use accurate macroscopic and nanoscopic techniques to characterize and understand their chemistry. X-ray photoelectron spectroscopy (XPS) has proved to be a useful analytical tool for nanoscale surface characterization of materials including carbon nanotubes. Recent nanotechnology research at NASA Johnson Space Center (NASA-JSC) helped to establish a characterization protocol for quality assessment for single wall carbon nanotubes (SWCNTs). Here, a review of some of the major factors of the XPS technique that can influence the quality of analytical data, suggestions for methods to maximize the quality of data obtained by XPS, and the development of a protocol for XPS characterization as a complementary technique for analyzing the purity and surface characteristics of SWCNTs is presented. The XPS protocol is then applied to a number of experiments including impurity analysis and the study of chemical modifications for SWCNTs.

Doping concentration dependence of microstructure and magnetic behaviours in Co-doped TiO2 nanorods

PubMed Central

2014-01-01

Co-doped titanium dioxide (TiO2) nanorods with different doping concentrations were fabricated by a molten salt method. It is found that the morphology of TiO2 changes from nanorods to nanoparticles with increasing doping concentration. The mechanism for the structure and phase evolution is investigated in detail. Undoped TiO2 nanorods show strong ferromagnetism at room temperature, whereas incorporating of Co deteriorates the ferromagnetic ordering. X-ray photoelectron spectroscopy (XPS) and electron spin resonance (ESR) results demonstrate that the ferromagnetism is associated with Ti vacancy. PMID:25593558

Self-standing crystalline TiO2 nanotubes/CNTs heterojunction membrane: synthesis and characterization.

PubMed

Hesabi, Zohreh R; Allam, Nageh K; Dahmen, Klaus; Garmestani, Hamid; A El-Sayed, Mostafa

2011-04-01

In the present study, we report for the first time synthesis of TiO(2) nanotubes/CNTs heterojunction membrane. Chemical vapor deposition (CVD) of CNTs at 650 °C in a mixture of H(2)/He atmosphere led to in situ detachment of the anodically fabricated TiO(2) nanotube layers from the Ti substrate underneath. Morphological and structural evolution of TiO(2) nanotubes after CNTs deposition were investigated by field- emission scanning electron microscopy (FESEM), glancing angle X-ray diffraction (GAXRD), and X-ray photoelectron spectroscopy (XPS) analyses. © 2011 American Chemical Society

Jellyfish-like few-layer graphene nanoflakes: Synthesis, oxidation, and hydrothermal N-doping

NASA Astrophysics Data System (ADS)

Chernyak, Sergei A.; Podgornova, Angelina M.; Arkhipova, Ekaterina A.; Novotortsev, Roman O.; Egorova, Tolganay B.; Ivanov, Anton S.; Maslakov, Konstantin I.; Savilov, Serguei V.; Lunin, Valery V.

2018-05-01

Few-layer graphene nanoflakes with the bent edges, diameter of 15-40 nm and thickness of 6-7 graphene layers have been synthesized using MgO-templated CVD growth. Their oxidation by nitric acid led to the high oxygen content of 18 at.%, a third of which was attributed to carboxylic groups. Oxidized nanoflakes were post-doped by nitrogen groups using hydrothermal treatment at 220 °C with ammonia and urea water solutions resulting in corresponding nitrogen content of 7 and 5 at.%. Synthesized and treated materials were characterized by XPS, Raman spectroscopy and electron microscopy.

Interfacial chemical reactions between MoS2 lubricants and bearing materials

NASA Technical Reports Server (NTRS)

Zabinski, J. S.; Tatarchuk, B. J.

1989-01-01

XPS and conversion-electron Moessbauer spectroscopy (CEMS) were used to examine iron that was deposited on the basal plane of MoS2 single crystals and subjected to vacuum annealing, oxidizing, and reducing environments. Iron either intercalated into the MoS2 structure or formed oriented iron sulfides, depending on the level of excess S in the MoS2 structure. CEMS data demonstrated that iron sulfide crystal structures preferentially aligned with respect to the MoS2 basal plane, and that alignment (and potentially adhesion) could be varied by appropriate high-temperature annealing procedures.

In situ supported MnOx-CeOx on carbon nanotubes for the low-temperature selective catalytic reduction of NO with NH3

NASA Astrophysics Data System (ADS)

Zhang, Dengsong; Zhang, Lei; Shi, Liyi; Fang, Cheng; Li, Hongrui; Gao, Ruihua; Huang, Lei; Zhang, Jianping

2013-01-01

The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ prepared catalyst exhibited the highest activity and the most extensive operating-temperature window, compared to the catalysts prepared by impregnation or mechanically mixed methods. The XRD and TEM results indicated that the manganese oxide and cerium oxide species had a good dispersion on the CNT surface. The XPS results demonstrated that the higher atomic concentration of Mn existed on the surface of CNTs and the more chemisorbed oxygen species exist. The H2-TPR results suggested that there was a strong interaction between the manganese oxide and cerium oxide on the surface of CNTs. The NH3-TPD results demonstrated that the catalysts presented a larger acid amount and stronger acid strength. In addition, the obtained catalysts exhibited much higher SO2-tolerance and improved the water-resistance as compared to that prepared by impregnation or mechanically mixed methods.The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ prepared catalyst exhibited the highest activity and the most extensive operating-temperature window, compared to the catalysts prepared by impregnation or mechanically mixed methods. The XRD and TEM results indicated that the manganese oxide and cerium oxide species had a good dispersion on the CNT surface. The XPS results demonstrated that the higher atomic concentration of Mn existed on the surface of CNTs and the more chemisorbed oxygen species exist. The H2-TPR results suggested that there was a strong interaction between the manganese oxide and cerium oxide on the surface of CNTs. The NH3-TPD results demonstrated that the catalysts presented a larger acid amount and stronger acid strength. In addition, the obtained catalysts exhibited much higher SO2-tolerance and improved the water-resistance as compared to that prepared by impregnation or mechanically mixed methods. Electronic supplementary information (ESI) available: SEM images and EDS analysis, TEM images, and XPS spectrum of samples. See DOI: 10.1039/c2nr33006g

CCQM Pilot Study CCQM-P140: Quantitative surface analysis of multi-element alloy films

NASA Astrophysics Data System (ADS)

Kim, Kyung Joong; Jang, Jong Shik; Kim, An Soon; Suh, Jung Ki; Chung, Yong-Duck; Hodoroaba, Vasile-Dan; Wirth, Thomas; Unger, Wolfgang; Kang, Hee Jae; Popov, Oleg; Popov, Inna; Kuselman, Ilya; Lee, Yeon Hee; Sykes, David E.; Wang, Meiling; Wang, Hai; Ogiwara, Toshiya; Nishio, Mitsuaki; Tanuma, Shigeo; Simons, David; Szakal, Christopher; Osborn, William; Terauchi, Shinya; Ito, Mika; Kurokawa, Akira; Fujimoto, Toshiyuki; Jordaan, Werner; Jeong, Chil Seong; Havelund, Rasmus; Spencer, Steve; Shard, Alex; Streeck, Cornelia; Beckhoff, Burkhard; Eicke, Axel; Terborg, Ralf

2015-01-01

A pilot study for a quantitative surface analysis of multi-element alloy films has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The aim of this pilot study is to evaluate a protocol for a key comparison to demonstrate the equivalence of measures by National Metrology Institutes (NMIs) and Designated Institutes (DI) for the mole fractions of multi-element alloy films. A Cu(In,Ga)Se2 (CIGS) film with non-uniform depth distribution was chosen as a representative multi-element alloy film. The mole fractions of the reference and the test CIGS films were certified by isotope dilution—inductively coupled plasma/mass spectrometry. A total number counting (TNC) method was used as a method to determine the signal intensities of the constituent elements acquired in SIMS, XPS and AES depth profiling. TNC method is comparable with the certification process because the certified mole fractions are the average values of the films. The mole fractions of the CIGS films were measured by Secondary Ion Mass Spectrometry (SIMS), Auger Electron Spectroscopy (AES), X-ray Photoelectron Spectroscopy (XPS), X-Ray Fluorescence (XRF) Analysis and Electron Probe Micro Analysis (EPMA) with Energy Dispersive X-ray Spectrometry (EDX). Fifteen laboratories from eight NMIs, one DI, and six non-NMIs participated in this pilot study. The average mole fractions of the reported data showed relative standard deviations from 5.5 % to 6.8 % and average relative expanded uncertainties in the range from 4.52 % to 4.86 % for the four test CIGS specimens. These values are smaller than those in the key comparison CCQM-K67 for the measurement of mole fractions of Fe-Ni alloy films. As one result it can be stated that SIMS, XPS and AES protocols relying on the quantification of CIGS films using the TNC method are mature to be used in a CCQM key comparison. Main text. To reach the main text of this paper, click on Final Report. The final report has been peer-reviewed and approved for publication by CCQM.

Structural, optical and electronic properties of K2Ba(NO3)4 crystal

NASA Astrophysics Data System (ADS)

Isaenko, L. I.; Korzhneva, K. E.; Goryainov, S. V.; Goloshumova, A. A.; Sheludyakova, L. A.; Bekenev, V. L.; Khyzhun, O. Y.

2018-02-01

Nitrate crystals reveal nonlinear optical properties and could be considered as converters of laser radiation in the short-wave region. The conditions for obtaining and basic properties of K2Ba(NO3)4 double nitrate crystals were investigated. Crystal growth was implemented by slow cooling in the temperature range of 72-49 °C and low rate evaporation. The structural analysis of K2Ba(NO3)4 formation on the basis of two mixed simple nitrate structures is discussed. The main groups of oscillations in K2Ba(NO3)4 crystal were revealed using Raman and IR spectroscopy, and the table of vibrations for this compound was compiled. The electronic structure of K2Ba(NO3)4 was elucidated in the present work from both experimental and theoretical viewpoints. In particular, X-ray photoelectron spectroscopy (XPS) was employed in the present work to measure binding energies of the atoms constituting the titled compound and its XPS valence-band spectrum for both pristine and Ar+ ion-bombarded surfaces. Further, total and partial densities of states of constituent atoms of K2Ba(NO3)4 have been calculated. The calculations reveal that the O 2p states dominate in the total valence-band region of K2Ba(NO3)4 except of its bottom, where K 3p and Ba 5p states are the principal contributors, while the bottom of the conduction band is composed mainly of the unoccupied O 2p states, with somewhat smaller contributions of the N 2p∗ states as well. With respect to the occupation of the valence band by the O 2p states, the present band-structure calculations are confirmed by comparison on a common energy scale of the XPS valence-band spectrum and the X-ray emission O Kα band for the K2Ba(NO3)4 crystal under study. Furthermore, the present calculations indicate that the K2Ba(NO3)4 compound is a direct-gap material.

High resolution X-ray photoelectron spectroscopy of styrene oxide adsorption and reaction on Ag(1 1 1)

NASA Astrophysics Data System (ADS)

Piao, H.; Enever, M. C. N.; Adib, K.; Hrbek, J.; Barteau, M. A.

2004-11-01

Synchrotron-based X-ray photoelectron spectroscopy (XPS) has been used to investigate the adsorption and reaction of styrene oxide on Ag(1 1 1). When adsorption is carried out at 250 K or above, ring opening of styrene oxide forms a stable surface oxametallacycle intermediate which eventually reacts at 485 K to regenerate styrene oxide. High resolution XPS is capable of distinguishing the oxametallacycle from molecularly adsorbed and condensed styrene oxide on the basis of different C1s peak separations. The observed separations are well accounted for by the results of DFT calculations.

Novel Z-scheme BiOBr/reduced graphene oxide/protonated g-C3N4 photocatalyst: Synthesis, characterization, visible light photocatalytic activity and mechanism

NASA Astrophysics Data System (ADS)

Bao, Yongchao; Chen, Kezheng

2018-04-01

The novel BiOBr/reduced graphene oxide/protonated g-C3N4 (BiOBr/RGO/pg-C3N4) composites were successfully synthesized by using a facile solvothermal synthesis method. The structure, morphology, optical and electronic properties were explored by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectroscopy (DRS), and photoelectrochemical measurement. The photocatalytic activities of as-synthesized samples were evaluated by the degradation of Rhodamine B (Rh B) and tetracycline hydrochloride (TC) aqueous solution under visible light irradiation (λ > 420nm). Compared with BiOBr, protonated g-C3N4 (pg-C3N4), BiOBr/pg-C3N4 and RGO/pg-C3N4, BiOBr/RGO/pg-C3N4 composites exhibited higher photocatalytic activity. The total organic carbon (TOC) removal ratios of Rh B and TC over 10% BiOBr/RGO/pg-C3N4 were 88% and 59%, respectively. The excellent photcatalytic performance was investigated by photoluminescence spectroscopy (PL), the radical quenching and electron spin resonance experiments. A Z-scheme charge transfer mechanism was proposed, in which RGO acted as an electron transfer mediator. It was worth pointing out that the closely contacted two-dimensional interface among the BiOBr, the RGO and pg-C3N4 promoted the separation and transfer of photo-generated charge carriers, and thus enhanced the photocatalytic efficiency.

Platinized tin oxide catalysts for CO2 lasers: Effects of pretreatment

NASA Technical Reports Server (NTRS)

Gardner, Steven D.; Hoflund, Gar B.; Schryer, David R.; Upchurch, Billy T.

1990-01-01

Platinized tin oxide surfaces used for low-temperature CO oxidation in CO2 lasers have been characterized before and after reduction in CO at 125 and 250 C using ion scattering spectroscopy (ISS) and X ray photoelectron spectroscopy (XPS). XPS indicates that the Pt is present initially as PtO2. Reduction at 125 C converts the PtO2 to Pt(OH)2 while reduction at 250 C converts the PtO2 to metallic Pt. ISS shows that the Pt in the outermost atomic layer of the catalyst is mostly covered by substrate species during the 250 C reduction. Both the ISS and XPS results are consistent with Pt/Sn alloy formation. The surface dehydration and migration of substrate species over surface Pt and Sn appear to explain why a CO pretreatment at 250 C produces inferior CO oxidation activities compared to a 125 C pretreatment.

Platinized tin oxide catalysts for CO2 lasers - Effects of pretreatment

NASA Technical Reports Server (NTRS)

Gardner, Steven D.; Hoflund, Gar B.; Schryer, David R.; Upchurch, Billy T.

1989-01-01

Platinized tin oxide surfaces used for low-temperature CO oxidation in CO2 lasers have been characterized before and after reduction in CO at 125 and 250 C using ion scattering spectroscopy (ISS) and X-ray photoelectron spectroscopy (XPS). XPS indicates that the Pt is present initially as Pto2. Reduction at 125 C converts the PtO2 to Pt(OH)2 while reduction at 250 C converts the PtO2 to metallic Pt. ISS shows that the Pt in the outermost atomic layer of the catalyst is mostly covered by substrate species during the 250 C reduction. Both the ISS and XPS results are consistent with Pt/Sn alloy formation. The surface dehydration and migration of substrate species over surface Pt and Sn appear to explain why a CO pretreatment at 250 C produces inferior CO oxidation activities compared to a 125 C pretreatment.

Interface properties between a low band gap conjugated polymer and a calcium metal electrode.

PubMed

Zhang, Wei; Pan, Xiao; Feng, Xuefei; Wang, Chia-Hsin; Yang, Yaw-Wen; Ju, Huanxin; Zhu, Junfa

2016-04-14

Interfaces between metal electrodes and π-conjugated polymers play an important role in the organic optoelectronic devices. In this paper, the molecular orientation of the pristine poly[(9,9-dioctylfluorenyl-2,7-diyl)-alt-5,5-(4',7'-di-2-thienyl-2',1',3'-benzothiadiazole)] (APFO3) films, chemical reactions and the electronic structure during the interface formation of Ca/APFO3 have been investigated in detail using synchrotron radiation photoemission spectroscopy (SRPES), X-ray photoemission spectroscopy (XPS) and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. It is shown that the APFO3 film has a high degree of orientational ordering with its aromatic ring tilted at an angle of 43° from the substrate, and the 9,9-dioctyl fluorene unit (F8) is almost in the same plane as the benzothiazole unit (BT). Upon vapor-deposition of Ca onto APFO3 at room temperature, Ca dopes electrons into APFO3 and induces the downward band bending of APFO3. Moreover, Ca can diffuse into the APFO3 subsurface and react with N, S and C atoms of APFO3. Finally, the barrier of electron injection at the Ca/APFO3 interface is derived by the energy level alignment diagram. These results enable us to gain comprehensive insights into APFO3 and will facilitate the reasonable design of high performance devices based on APFO3.

Enhanced sunlight-driven photocatalytic performance of Bi-doped CdMoO4 benefited from efficient separation of photogenerated charge pairs

NASA Astrophysics Data System (ADS)

Huang, Jiao; Liu, Huanhuan; Zhong, Junbo; Yang, Qi; Chen, Jiufu; Li, Jianzhang; Ma, Dongmei; duan, Ran

2018-06-01

In this paper, to further boost the photocatalytic performance of CdMoO4, Bi3+ was successfully doped into CdMoO4 by a facile microwave hydrothermal method. The Bi-doped CdMoO4 photocatalysts prepared were characterized by Brunauer-Emmett-Teller (BET) method, X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), electron spin-resonance (ESR) and surface photovoltage spectroscopy (SPS). The results exhibit that doping Bi3+ into CdMoO4 remarkably boosts the separation rate of photoinduced charge pairs and the specific surface area, decrease the crystal size, narrows the band gap of the CdMoO4 and induces the binding energy shift of Cd, all these advantageous factors result in the promoted photocatalytic performance of CdMoO4. Using rhodamine B (RhB) as model toxic pollutant, the photocatalytic activities of the photocatalysts were evaluated under a 500 W Xe lamp irradiation. When the molar ratio of Bi/Cd is 0.2%, Bi-CdMoO4 prepared displays the best photocatalytic performance, the photocatalytic performance of the 0.2% sample is more than twice of that of the reference CdMoO4.

Influence of gold additives on the stability and phase transformation of titanate nanostructures.

PubMed

Pusztai, P; Puskás, R; Varga, E; Erdőhelyi, A; Kukovecz, Á; Kónya, Z; Kiss, J

2014-12-28

Gold nanoparticles were prepared and characterized on protonated (H-form) titanate nanotubes (TiONTs) and nanowires (TiONWs). The chemical nature and morphology of gold particles were monitored by X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, X-ray diffraction (XRD) and high resolution electron microscopy (HRTEM). The optical properties of Au-containing titanate nanowires were explored by means of ultraviolet-visible diffuse reflectance spectroscopy. The size distribution and homogeneity of gold particles depend on the reduction mode from the corresponding gold salt to metal particles. Smaller clusters (3-8 nm) were obtained with the NaBH4 reactant at 293 K than with molecular hydrogen reduction. An unexpectedly high binding energy gold state was found by XPS in gold-loaded titanate nanostructures. This state was absent from the spectra of gold-loaded TiO2(110). A likely explanation for this phenomenon, supported also by the characteristic decrease of band gap energy from 3.10 eV to 2.74 eV with increasing Au content, is that depending on the metal loading and titanate structure, Au is stabilized on titanate nanowires partially in positively charged gold form by ion exchange and also as Au clusters. Our important new finding is that the thermal annealing behavior of Au-loaded titanate nanotubes and nanowires is different. The former lose their tubular morphology and are readily transformed into anatase even at a very low temperature of 473 K. On the other hand, gold stabilizes the layered structure of titanate nanowires up to 873 K.

Facile synthesis of bismuth oxyhalide nanosheet films with distinct conduction type and photo-induced charge carrier behavior

NASA Astrophysics Data System (ADS)

Jia, Huimin; He, Weiwei; Zhang, Beibei; Yao, Lei; Yang, Xiaokai; Zheng, Zhi

2018-05-01

A modified successive ionic layer adsorption and reaction (SILAR) method was developed to fabricate 2D ordered BiOX (X = CI, Br, I) nanosheet array films on FTO substrates at room temperature. The formation of BiOX films were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), UV-vis absorption spectroscopy, and X-ray photoelectron spectroscopy (XPS). The semiconductor surface states determine the type of semiconductor. Although BiOCI, BiOBr and BiOI belong to the bismuth oxyhalide semiconductor family and possess similar crystal and electronic structures, they show different conductivity types due to their respective surface states. Mott-Schottky curve results demonstrate that the BiOCl and BiOI nanosheet arrays display n-type semiconductor properties, while the BiOBr films exhibit p-type semiconductor properties. Assisted by surface photovoltage (SPV) and transient photovoltage (TPV) techniques, the photoinduced charge transfer dynamics on the surface/interface of the BiOX/FTO nanosheet films were systematically and comparatively investigated. As revealed by the results, both the separation and transfer dynamics of the photo-induced carrier are influenced by film thickness.

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

Changes of electronic properties of p-GaN(0 0 0 1) surface after low-energy N+-ion bombardment

NASA Astrophysics Data System (ADS)

Grodzicki, M.; Mazur, P.; Ciszewski, A.

2018-05-01

The p-GaN(0 0 0 1) crystal with a relatively low acceptor concentration of 5 × 1016 cm-3 is used in these studies, which are carried out in situ under ultrahigh vacuum (UHV) by ultraviolet photoelectron spectroscopy (UPS), X-ray photoelectron spectroscopy (XPS) and low-energy electron diffraction (LEED). The p-GaN(0 0 0 1)-(1 × 1) surface is achieved by thermal cleaning. N+-ion bombardment by a 200 eV ion beam changes the surface stoichiometry, enriches it with nitrogen, and disorders it. Such modified surface layer inverts its semiconducting character from p- into n-type. The electron affinity for the already cleaned p-GaN surface and that just after bombardment shows a shift from 2.2 eV to 3.2 eV, as well as an increase of band bending at the vacuum/surface interface from 1.4 eV to 2.5 eV. Proper post-bombardment heating of the sample restores the initial atomic order of the modified layer, leaving its n-type semiconducting character unchanged. The results of the measurements are discussed based on two types of surface states concepts.

High-efficiency and conveniently recyclable photo-catalysts for dye degradation based on urchin-like CuO microparticle/polymer hybrid composites

NASA Astrophysics Data System (ADS)

Liu, Xiong; Cheng, Yuming; Li, Xuefeng; Dong, Jinfeng

2018-05-01

In this work, we developed a new type of photo-catalysts composed of the urchin-like cupric oxide (CuO) microparticle and polyvinylidene fluoride (PVDF) hybrid composites by the convenient organic-inorganic hybrid strategy, which show high-efficiency and conveniently recyclable for dye degradation including methylene blue (MB), Congo red (CR), and malachite green (MG) by visible light irradiation. The micro-structural characteristics of urchin-like CuO microparticles are crucial and dominant over the photo-degrading efficiency of hybrid catalyst because of their highly exposed {0 0 2} facet and larger specific surface area. Simultaneously, the intrinsic porous framework of PVDF membrane not only remains the excellent photo-catalytic activity of urchin-like CuO microparticles but also facilitates the enrichment of dyes on the membrane, and thereby synergistically contributing to the photo-catalytic efficiency. The microstructures of both urchin-like CuO microparticles and hybrid catalysts are systematically characterized by various techniques including scanning electron microscopy (SEM), transmission electron microscope (TEM), high-resolution transmission electron microscope (HRTEM), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), and nitrogen adsorption/desorption isotherms, which evidently support the mentioned mechanism.

Ultrafast Carrier dynamics of InxGa1-xN nanostructures grown directly on Si(111)

NASA Astrophysics Data System (ADS)

Kumar, Praveen; Devi, Pooja; Rodriguez⁠, P. E. D. S.; Kumar, Manish; Shivling, V. D.; Noetzel, Richard; Sharma, Chhavi; Sinha, R. K.; Kumar, Mahesh

2018-05-01

We show a flux dependence changes in structural, optical and electronic properties of InxGa1-xN nanostructures (NSs) namely nanocolumns (NCs), nanoflakes (NFs) and nanowall network (NWN) grown directly on Si(111) surface. Field emission scanning electron microscopy (FESEM) images were recorded to see morphological changes from NFs to NCs and NWNc etc, while high-resolution X-ray diffraction (HRXRD) ω-2θ scans were used to determine In incorporation. The maximum In incorporation was observed to be 20, 33 and 38% for the sharp transition from NFs to NCs and NWNs, respectively. The charge carrier dynamics of these grown NSs were probed using Ultrafast Femtosecond Transient Absorption Spectroscopy (UFTAS) with excitation at 350 nm pump wavelength. The UFTAS studies show the comparative charge carriers dynamics of the NWS, NCs and NFs. The charge carrier studies show a higher lifetime in NWNs as compare to NCs and NFs. Further, to examine electronic structure and level of degeneracy of these NSs, core-level and valence band spectra were analyzed by X-ray photoelectron spectroscopy (XPS), which manifest the upward band bending ranging from 0.2 eV to 0.4 eV.

X-ray Photoelectron Spectroscopy of Pyridinium-Based Ionic Liquids: Comparison to Imidazolium- and Pyrrolidinium-Based Analogues.

PubMed

Men, Shuang; Mitchell, Daniel S; Lovelock, Kevin R J; Licence, Peter

2015-07-20

We investigate eight 1-alkylpyridinium-based ionic liquids of the form [Cn Py][A] by using X-ray photoelectron spectroscopy (XPS). The electronic environment of each element of the ionic liquids is analyzed. In particular, a reliable fitting model is developed for the C 1s region that applies to each of the ionic liquids. This model allows the accurate charge correction of binding energies and the determination of reliable and reproducible binding energies for each ionic liquid. Shake-up/off phenomena are determinedfor both C 1s and N 1s spectra. The electronic interaction between cations and anions is investigated for both simple ionic liquids and an example of an ionic-liquid mixture; the effect of the anion on the electronic environment of the cation is also explored. Throughout the study, a detailed comparison is made between [C8 Py][A] and analogues including 1-octyl-1-methylpyrrolidinium- ([C8 C1 Pyrr][A]), and 1-octyl-3-methylimidazolium- ([C8 C1 Im][A]) based samples, where X is common to all ionic liquids. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

X‐ray Photoelectron Spectroscopy of Pyridinium‐Based Ionic Liquids: Comparison to Imidazolium‐ and Pyrrolidinium‐Based Analogues

PubMed Central

Mitchell, Daniel S.; Lovelock, Kevin R. J.

2015-01-01

Abstract We investigate eight 1‐alkylpyridinium‐based ionic liquids of the form [CnPy][A] by using X‐ray photoelectron spectroscopy (XPS). The electronic environment of each element of the ionic liquids is analyzed. In particular, a reliable fitting model is developed for the C 1s region that applies to each of the ionic liquids. This model allows the accurate charge correction of binding energies and the determination of reliable and reproducible binding energies for each ionic liquid. Shake‐up/off phenomena are determinedfor both C 1s and N 1s spectra. The electronic interaction between cations and anions is investigated for both simple ionic liquids and an example of an ionic‐liquid mixture; the effect of the anion on the electronic environment of the cation is also explored. Throughout the study, a detailed comparison is made between [C8Py][A] and analogues including 1‐octyl‐1‐methylpyrrolidinium‐ ([C8C1Pyrr][A]), and 1‐octyl‐3‐methylimidazolium‐ ([C8C1Im][A]) based samples, where X is common to all ionic liquids. PMID:25952131

XPS characterization of silver exchanged ETS-10 and mordenite molecular sieves.

PubMed

Anson, A; Maham, Y; Lin, C C H; Kuznicki, T M; Kuznicki, S M

2009-05-01

Silver exchanged molecular sieves ETS-10 (Ag-ETS-10) and mordenite (Ag-mordenite) were dehydrated under vacuum at temperatures between 100 degrees C-350 degrees C. Changes in the state of the silver were studied using X-ray photoelectron spectroscopy (XPS). Silver cations in titanosilicate Ag-ETS-10 are fully reduced to Ag(0) at temperatures as low as 150 degrees C. The characteristic features of the XPS spectrum of silver in this Ag-ETS-10 species correspond to only metallic silver. The signal for metallic silver is not observed in the XPS spectrum of aluminosilicate Ag-mordenite, indicating that silver cations are not reduced, even after heating to 350 degrees C.

Van der Waals Epitaxy of GaSe/Graphene Heterostructure: Electronic and Interfacial Properties.

PubMed

Ben Aziza, Zeineb; Henck, Hugo; Pierucci, Debora; Silly, Mathieu G; Lhuillier, Emmanuel; Patriarche, Gilles; Sirotti, Fausto; Eddrief, Mahmoud; Ouerghi, Abdelkarim

2016-10-07

Stacking two-dimensional materials in so-called van der Waals (vdW) heterostructures, like the combination of GaSe and graphene, provides the ability to obtain hybrid systems which are suitable to design optoelectronic devices. Here, we report the structural and electronic properties of the direct growth of multilayered GaSe by Molecular beam Epitaxy (MBE) on graphene. Reflection high-energy electron diffraction (RHEED) images exhibited sharp streaky features indicative of high quality GaSe layer produced via a vdW epitaxy. Micro-Raman spectroscopy showed that, after the vdW hetero-interface formation, the Raman signature of pristine graphene is preserved. However, the GaSe film tuned the charge density of graphene layer by shifting the Dirac point by about 80 meV toward lower binding energies, attesting an electron transfer from graphene to GaSe. Angle-resolved photoemission spectroscopy (ARPES) measurements showed that the maximum of the valence band of few layers of GaSe are located at the Γ point at a binding energy of about -0.73 eV relatively to the Fermi level (p-type doping). From the ARPES measurements, a hole effective mass defined along the ΓM direction and equal to about m*/m0 = -1.1 was determined. By coupling the ARPES data with high resolution X-ray photoemission spectroscopy (HR-XPS) measurements, the Schottky interface barrier height was estimated to be 1.2 eV. These findings allow deeper understanding of the interlayer interactions and the electronic structure of GaSe/graphene vdW heterostructure.

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.

Analysis of Black Bearing Balls from a Space Shuttle Body Flap Actuator

NASA Technical Reports Server (NTRS)

Sovinski, Marjorie F.; Street, Kenneth W.

2005-01-01

A significantly deteriorated ball bearing mechanism from a body flap actuator on Space Shuttle OV-103 was disassembled and the balls submitted for analysis in conjunction with Return to Flight activities. The OV-103 balls, referred to as the "black balls", were subjected to X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FT-IR) and Raman micro spectroscopy, surface profilometry, and optical and electron microscopy. The spectroscopic results in combination with microscopy analysis allowed a determination of the lubricant degradation pathway. The chemical attack mechanism does not adequately explain the unique visual appearance of the black balls. Numerous efforts have unsuccessfully focused on duplication of the phenomena causing this unique surface structure and appearance of the black balls. Further detail will be presented supporting these conclusions along with plausible explanations of the unique black appearance to the balls.

Self assembled monolayers of octadecyltrichlorosilane for dielectric materials

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

Kumar, Vijay, E-mail: cirivijaypilani@gmail.com; Mechanical Engineering Department, Birla Institute of Technology and Science-Pilani; Puri, Paridhi

2016-04-13

Treatment of surfaces to change the interaction of fluids with them is a critical step in constructing useful microfluidics devices, especially those used in biological applications. Selective modification of inorganic materials such as Si, SiO{sub 2} and Si{sub 3}N{sub 4} is of great interest in research and technology. We evaluated the chemical formation of OTS self-assembled monolayers on silicon substrates with different dielectric materials. Our investigations were focused on surface modification of formerly used common dielectric materials SiO{sub 2}, Si{sub 3}N{sub 4} and a-poly. The improvement of wetting behaviour and quality of monolayer films were characterized using Atomic force microscope,more » Scanning electron microscope, Contact angle goniometer, Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) monolayer deposited oxide surface.« less