Enhanced nitrogen selectivity for nitrate reduction on Cu-nZVI by TiO2 photocatalysts under UV irradiation

NASA Astrophysics Data System (ADS)

Krasae, Nalinee; Wantala, Kitirote

2016-09-01

The aims of this work were to study the effect of Cu-nZVI with and without TiO2 on nitrate reduction and to study the pathway of nitrate reduction utilizing to nitrogen gas. The chemical and physical properties of Cu-nZVI and Cu-nZVI/TiO2 such as specific surface area, crystalline phase, oxidation state of Cu and Fe and morphology were determined by N2 adsorption-desorption Brunauer-Emmett-Teller (BET) analytical technique, X-ray diffraction (XRD), X-ray Absorption Near Edge Structure (XANES) technique and Transmittance Electron Microscopy (TEM). The full factorial design (FFD) was used in this experiment for the effect of Cu-nZVI with and without TiO2, where the initial solution pH was varied at 4, 5.5, and 7 and initial nitrate concentration was varied at 50, 75, and 100 ppm. Finally, the pathway of nitrate reduction was examined to calculate the nitrogen gas selectivity. The specific area of Cu-nZVI and Cu-nZVI/TiO2 was found to be about 4 and 36 m2/g, respectively. The XRD pattern of Fe0 in Cu-nZVI was found at 45° (2θ), whereas Cu-nZVI/TiO2 cannot be observed. TEM images can confirm the position of the core and the shell of nZVI for Fe0 and ferric oxide. Cu-nZVI/TiO2 proved to have higher activity in nitrogen reduction performance than that without TiO2 and nitrate can be completely degraded in both of solution pH of 4 and 7 in 75 ppm of initial nitrate concentration. It can be highlighted that the nitrogen gas selectivity of Cu-nZVI/TiO2 greater than 82% was found at an initial solution pH of 4 and 7. The main effects of Cu-nZVI with and without TiO2 and the initial nitrate concentration on nitrate reduction were significant. The interaction between solution pH and initial nitrate concentration and the interaction of all effects at a reaction time of 15 min on nitrate reduction were also significant.

Heteropolyhedral silver compounds containing the polydentate ligand N,N,O-E-[6-(hydroxyimino)ethyl]-1,3,7-trimethyllumazine. Preparation, spectral and XRD structural study and AIM calculations.

PubMed

Jiménez-Pulido, Sonia B; Hueso-Ureña, Francisco; Fernández-Liencres, M Paz; Fernández-Gómez, Manuel; Moreno-Carretero, Miguel N

2013-01-14

The oxime derived from 6-acetyl-1,3,7-trimethyllumazine (1) ((E-6-(hydroxyimino)ethyl)-1,3,7-trimethylpteridine-2,4(1H,3H)-dione, DLMAceMox) has been prepared and its molecular and crystal structure determined from spectral and XRD data. The oxime ligand was reacted with silver nitrate, perchlorate, thiocyanate, trifluoromethylsulfonate and tetrafluoroborate to give complexes with formulas [Ag(2)(DLMAceMox)(2)(NO(3))(2)](n) (2), [Ag(2)(DLMAceMox)(2)(ClO(4))(2)](n) (3), [Ag(2)(DLMAceMox)(2)(SCN)(2)] (4), [Ag(2)(DLMAceMox)(2)(CF(3)SO(3))(2)(CH(3)CH(2)OH)]·CH(3)CH(2)OH (5) and [Ag(DLMAceMox)(2)]BF(4) (6). Single-crystal XRD studies show that the asymmetrical residual unit of complexes 2, 3 and 5 contains two quite different but connected silver centers (Ag1-Ag2, 2.9-3.2 Å). In addition to this, the Ag1 ion displays coordination with the N5 and O4 atoms from both lumazine moieties and a ligand (nitrato, perchlorato or ethanol) bridging to another disilver unit. The Ag2 ion is coordinated to the N61 oxime nitrogens, a monodentate and a (O,O)-bridging nitrato/perchlorato or two monodentate O-trifluoromethylsulfonato anions. The coordination polyhedra can be best described as a strongly distorted octahedron (around Ag1) and a square-based pyramid (around Ag2). The Ag-N and Ag-O bond lengths range between 2.22-2.41 and 2.40-2.67 Å, respectively. Although the structure of 4 cannot be resolved by XRD, it is likely to be similar to those described for 2, 3 and 5, containing Ag-Ag units with S-thiocyanato terminal ligands. Finally, the structure of the tetrafluoroborate compound 6 is mononuclear with a strongly distorted tetrahedral AgN(4) core (Ag-N, 2.27-2.43 Å). Always, the different Ag-N distances found clearly point to the more basic character of the oxime N61 nitrogen atom when compared with the pyrazine N5 one. A topological analysis of the electron density within the framework provided by the quantum theory of atoms in molecules (QTAIM) using DFT(M06L) levels of

Evaluation of AlGaN/GaN high electron mobility transistors grown on ZrTi buffer layers with sapphire substrates

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

Ren, Fan; Pearton, Stephen J.; Ahn, Shihyun

Here, AlGaN/GaN high electron mobility transistors (HEMTs) have been grown on sapphire substrates, using ZrTi buffer layers to provide in-plane lattice-matching to hexagonal GaN. X-ray diffraction (XRD) as well as cross-section transmission electron microscopy (TEM) were used to assess the quality of the HEMT structure. The XRD 2θ scans showed full-width-at-half-maximum values of 0.16°, 0.07°, and 0.08° for ZrTi alloy, GaN buffer layer, and the entire HEMT structure, respectively. TEM studies of the GaN buffer layer and the AlN/ZrTi/AlN stack showed the importance of growing thin AlN buffer layers on the ZrTi layer prior to growth of the GaN buffermore » layer. The density of threading dislocations in the GaN channel layer of the HEMT structure was estimated to be in the 10 8 cm –2 range. The HEMT device exhibited a saturation drain current density of 820 mA/mm, and the channel of the fabricated HEMTs could be well modulated. A cutoff frequency (f T) of 8.9 GHz and a maximum frequency of oscillation (f max) of 17.3 GHz were achieved for HEMTs with gate dimensions of 1 × 200 μm.« less

Evaluation of AlGaN/GaN high electron mobility transistors grown on ZrTi buffer layers with sapphire substrates

DOE PAGES

Ren, Fan; Pearton, Stephen J.; Ahn, Shihyun; ...

2016-09-21

Here, AlGaN/GaN high electron mobility transistors (HEMTs) have been grown on sapphire substrates, using ZrTi buffer layers to provide in-plane lattice-matching to hexagonal GaN. X-ray diffraction (XRD) as well as cross-section transmission electron microscopy (TEM) were used to assess the quality of the HEMT structure. The XRD 2θ scans showed full-width-at-half-maximum values of 0.16°, 0.07°, and 0.08° for ZrTi alloy, GaN buffer layer, and the entire HEMT structure, respectively. TEM studies of the GaN buffer layer and the AlN/ZrTi/AlN stack showed the importance of growing thin AlN buffer layers on the ZrTi layer prior to growth of the GaN buffermore » layer. The density of threading dislocations in the GaN channel layer of the HEMT structure was estimated to be in the 10 8 cm –2 range. The HEMT device exhibited a saturation drain current density of 820 mA/mm, and the channel of the fabricated HEMTs could be well modulated. A cutoff frequency (f T) of 8.9 GHz and a maximum frequency of oscillation (f max) of 17.3 GHz were achieved for HEMTs with gate dimensions of 1 × 200 μm.« less

TEM study of the (SbS){sub 1+δ}(NbS{sub 2}){sub n}, (n=1, 2, 3; δ~1.14, 1.20) misfit layer phases

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

Gómez-Herrero, A., E-mail: adriangh@pdi.ucm.es; Landa-Cánovas, A.R.; Otero-Díaz, L.C.

In the Sb–Nb–S system four new misfit layer phases have been found and carefully investigated via Transmission Electron Microscopy (TEM). Their structures are of composite modulated structure type with stoichiometries that can be formulated as (SbS){sub 1+δ}(NbS{sub 2}){sub n}; for n=1, δ~1.14 and 1.19; for n=2, δ~1.18 and for n=3, δ~1.19. Selected Area Electron Diffraction (SAED) patterns show an almost commensurate fit between the pseudo-tetragonal (SbS) and the pseudo-orthohexagonal (NbS{sub 2}){sub n} subcells along the misfit direction a, with 3(SbS)≈5(NbS{sub 2}), being b the same for both sub-lattices and c the stacking direction. For n=1, a commensurate phase with 4a{submore » SbS}=7a{sub NbS2} has also been observed. In addition to the characteristic misfit and associated modulation of the two sub-structures, a second modulation is also present which appears to be primarily associated with the (SbS) sub-structure of both the n=1 and n=2 phases. High Resolution Transmission Electron Microscopy (HRTEM) images show ordered stacking sequences between the (SbS) and (NbS{sub 2}){sub n} lamellae for each of the four phases, however, disordered intergrowths were also occasionally found. Most of the crystals showed different kinds of twinning defects on quite a fine scale. Many crystals showed curled up edges. In some cases the lamellar crystals were entirely folded giving rise to similar diffraction patterns as found for cylindrical crystals. - Graphical abstract: Idealized structure models of the first three members of the homologous series (SbS){sub 1+δ}(NbS{sub 2}){sub n}. - Highlights: • Transmission Electron Microscopy study of misfit layer sulfides (SbS){sub 1+δ}(NbS{sub 2}){sub n}. • The structures consist of a (SbS) layer interleaved between n (NbS{sub 2}) layers. • Two different members n=1, one n=2 and one n=3 have been studied. • Twinning, intergrowths and different modulations in the (SbS) substructure.« less

2D Inversion of Transient Electromagnetic Method (TEM)

NASA Astrophysics Data System (ADS)

Bortolozo, Cassiano Antonio; Luís Porsani, Jorge; Acácio Monteiro dos Santos, Fernando

2017-04-01

A new methodology was developed for 2D inversion of Transient Electromagnetic Method (TEM). The methodology consists in the elaboration of a set of routines in Matlab code for modeling and inversion of TEM data and the determination of the most efficient field array for the problem. In this research, the 2D TEM modeling uses the finite differences discretization. To solve the inversion problem, were applied an algorithm based on Marquardt technique, also known as Ridge Regression. The algorithm is stable and efficient and it is widely used in geoelectrical inversion problems. The main advantage of 1D survey is the rapid data acquisition in a large area, but in regions with two-dimensional structures or that need more details, is essential to use two-dimensional interpretation methodologies. For an efficient field acquisition we used in an innovative form the fixed-loop array, with a square transmitter loop (200m x 200m) and 25m spacing between the sounding points. The TEM surveys were conducted only inside the transmitter loop, in order to not deal with negative apparent resistivity values. Although it is possible to model the negative values, it makes the inversion convergence more difficult. Therefore the methodology described above has been developed in order to achieve maximum optimization of data acquisition. Since it is necessary only one transmitter loop disposition in the surface for each series of soundings inside the loop. The algorithms were tested with synthetic data and the results were essential to the interpretation of the results with real data and will be useful in future situations. With the inversion of the real data acquired over the Paraná Sedimentary Basin (PSB) was successful realized a 2D TEM inversion. The results indicate a robust geoelectrical characterization for the sedimentary and crystalline aquifers in the PSB. Therefore, using a new and relevant approach for 2D TEM inversion, this research effectively contributed to map the most

Ga2O3 and GaN nanocrystalline film: reverse micelle assisted solvothermal synthesis and characterization.

PubMed

Sinha, Godhuli; Ganguli, Dibyendu; Chaudhuri, Subhadra

2008-03-01

Gallium oxide (beta-Ga2O3) nanoparticles were successfully deposited on quartz glass substrates using sodium bis(2-ethylhexyl) sulfosuccinate (AOT)/n-hexane/ethylene glycol monomethyl ether (EGME) reverse micelle-mediated solvothermal process with different omega values. The mean diameter of Ga2O3 particles was approximately 2-3 nm and found to be approximately independent of omega values of the reverse micelles. However, when the Ga2O3 nanocrystalline films were nitrided at 900 degrees C under flowing NH3 atmosphere for 1 h, the mean diameter of the resulted gallium nitride (wurtzite-GaN) nanoparticles varied from 3-9 nm. Both nanocrystalline films of Ga2O3 and GaN were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, UV-vis spectroscopy and photoluminescence in order to study their chemical and physical properties explicitly.

Synthetic, XRD, non-covalent interactions and solvent dependent nonlinear optical studies of Sulfadiazine-Ortho-Vanillin Schiff base: (E)-4-((2-hydroxy-3-methoxy- benzylidene) amino)-N-(pyrimidin-2-yl)benzene-sulfonamide

NASA Astrophysics Data System (ADS)

Shahid, Muhammad; Salim, Muhammad; Khalid, Muhammad; Tahir, Muhammad Nawaz; Khan, Muhammad Usman; Braga, Ataualpa Albert Carmo

2018-06-01

In this study, Sulfadiazine-Ortho-Vanillin Schiff base namely (E)-4-((2-hydroxy-3-methoxybenzylidene)amino)sbnd N-(pyrimidin-2-yl)benzene-sulfonamide (BS) was synthesized. Chemical characterization and computational studies using different techniques like XRD, FT-IR, UV-Vis, NBO, FMO, and MEP have been employed. Density functional theory (DFT) calculations have been performed at M06-2X/6-311 + G(d,p) level of theory to obtain optimized geometry and vibrational wave numbers for (E)-4-((2-hydroxy-3-methoxybenzylidene)amino)sbnd N-(pyrimidin-2-yl)benzene-sulfonamide (BS). The DFT optimized geometry supports the experimental XRD parameters. Frontier molecular orbital (FMO) energies and molecular electrostatic potential (MEP) surfaces have been executed at M06-2X/6-311 + G(d,p) level of theory. NBO analysis has been carried out at M06-2X/6-311 + G(d,p) level which not only discovered the hyper conjugative interactions and stability in title molecule but also reconfirmed the existence of Nsbnd H⋯N hydrogen bonds between the dimer. The findings of small EHOMO-ELUMO gap shows less hardness and larger softness values which suggested the bioactiveness of the title molecule. Finally, the effect of solvent on nonlinear optical (NLO) properties has been executed using M06-2X level of theory and 6-311 + G (d,p) basis set. The solvent polarity enhanced the NLO response from 3.62 × 10-30 esu to 4.66 × 10-30 esu indicating the considerable NLO character hence in general may have potential applications in the development of non-linear optical materials.

Improvement of crystalline quality of N-polar AlN layers on c-plane sapphire by low-pressure flow-modulated MOCVD

NASA Astrophysics Data System (ADS)

Takeuchi, M.; Shimizu, H.; Kajitani, R.; Kawasaki, K.; Kumagai, Y.; Koukitu, A.; Aoyagi, Y.

2007-01-01

The growth of N-polar AlN layers on c-plane sapphire is reported. Low-temperature AlN (LT-AlN) layers were used as seeding buffer layers with pre-nitridation for sapphire. To avoid strong vapor-phase reaction between trimethylaluminum (TMA) and ammonia (NH 3) and to improve the crystalline quality, low-pressure flow-modulated (FM) metal-organic chemical vapor deposition (MOCVD) technique was introduced with careful optimization of the FM sequence. The surface morphologies and the crystalline quality defined by the X-ray diffraction (XRD) (0 0 2) and (1 0 0) rocking curve measurements strongly depended on the LT-AlN thickness and on the TMA coverage per cycle of the FM growth. The sample showing the best XRD data with a good morphology was almost completely etched in aqueous KOH solution owing to N-polarity. From the plan-view transmission electron microscopy (TEM) observation, the dislocation density was counted to be about 3×10 10 cm -2.

M23C6 carbides and Cr2N nitrides in aged duplex stainless steel: A SEM, TEM and FIB tomography investigation.

PubMed

Maetz, J-Y; Douillard, T; Cazottes, S; Verdu, C; Kléber, X

2016-05-01

The precipitation evolution during ageing of a 2101 lean duplex stainless steel was investigated, revealing that the precipitate type and morphology depends on the nature of the grain boundary. Triangular M23C6 carbides precipitate only at γ/δ interfaces and rod-like Cr2N nitrides precipitate at both γ/δ and δ/δ interfaces. After 15min of ageing, the M23C6 size no longer evolves, whereas that of the Cr2N continues to evolve. For Cr2N, the morphology is maintained at γ/δ interfaces, whereas percolation occurs to form a continuous layer at δ/δ interfaces. By combining 2D and 3D characterisation at the nanoscale using transmission electron microscopy (TEM) and focused ion beam (FIB) tomography, a complete description of the precipitation evolution was obtained, including the composition, crystallographic structure, orientation relationship with the matrix phases, location, morphology, size and volume fraction. Copyright © 2016 Elsevier Ltd. All rights reserved.

ERDA, RBS, TEM and SEM characterization of microstructural evolution in helium-implanted Hastelloy N alloy

NASA Astrophysics Data System (ADS)

Gao, Jie; Bao, Liangman; Huang, Hefei; Li, Yan; Lei, Qiantao; Deng, Qi; Liu, Zhe; Yang, Guo; Shi, Liqun

2017-05-01

Hastelloy N alloy was implanted with 30 keV, 5 × 1016 ions/cm2 helium ions at room temperature, and subsequent annealed at 600 °C for 1 h and further annealed at 850 °C for 5 h in vacuum. Using elastic recoil detection analysis (ERDA) and transmission electron microscopy (TEM), the depth profiles of helium concentration and helium bubbles in helium-implanted Hastelloy N alloy were investigated, respectively. The diffusion of helium and molybdenum elements to surface occurred during the vacuum annealing at 850 °C (5 h). It was also observed that bubbles in molybdenum-enriched region were much larger in size than those in deeper region. In addition, it is worth noting that plenty of nano-holes can be observed on the surface of helium-implanted sample after high temperature annealing by scanning electron microscope (SEM). This observation provides the evidence for the occurrence of helium release, which can be also inferred from the results of ERDA and TEM analysis.

Facile preparation and formation mechanism of Sr2Si5N8:Eu2+ red-emitting phosphors

NASA Astrophysics Data System (ADS)

Wang, Yang; Wang, Yunli; Wang, Ming; Shao, Yiran; Zhu, Yingchun

2018-05-01

The red-emitting Sr2Si5N8:Eu2+ phosphors have been synthesized in a new facile process using (oxy)nitride precursors by inductive calcination under N2 atmosphere at ordinary pressure. Different from the prevailing methods, lower cost raw materials, simpler pretreatment, without harsh conditions and a shorter reaction time are achieved. It was found that red-emitting Sr2Si5N8:Eu2+ phosphors were synthesized with high crystallinity and purity after 1 h inductive calcination. The formation mechanism was characterized by XRD, SEM, TEM and Fluorescence microscopy. It was demonstrated that a hexagonal mesophase of Sr-doped α-Si3N4 was primarily formed in the reaction process, which transformed into the final product of the orthorhombic Sr2Si5N8:Eu2+ phosphors. During the reaction process, the color of the samples transforms from greenish-yellow to orange and eventually to red. The as-prepared phosphors have a wide excitation in the range of 250 ∼ 570 nm which matches blue light chips and give a red-light emission peaking at 610 nm. The results indicate a promising prospect for a simple, efficient and inexpensive way to prepare Sr2Si5N8:Eu2+ phosphors for blue/UV-based warm-white LEDs and other fluorescent applications.

Construction of 1D SnO2-coated ZnO nanowire heterojunction for their improved n-butylamine sensing performances

NASA Astrophysics Data System (ADS)

Wang, Liwei; Li, Jintao; Wang, Yinghui; Yu, Kefu; Tang, Xingying; Zhang, Yuanyuan; Wang, Shaopeng; Wei, Chaoshuai

2016-10-01

One-dimensional (1D) SnO2-coated ZnO nanowire (SnO2/ZnO NW) N-N heterojunctions were successfully constructed by an effective solvothermal treatment followed with calcination at 400 °C. The obtained samples were characterized by means of XRD, SEM, TEM, Scanning TEM coupled with EDS and XPS analysis, which confirmed that the outer layers of N-type SnO2 nanoparticles (avg. 4 nm) were uniformly distributed onto our pre-synthesized n-type ZnO nanowire supports (diameter 80~100 nm, length 12~16 μm). Comparisons of the gas sensing performances among pure SnO2, pure ZnO NW and the as-fabricated SnO2/ZnO NW heterojunctions revealed that after modification, SnO2/ZnO NW based sensor exhibited remarkably improved response, fast response and recovery speeds, good selectivity and excellent reproducibility to n-butylamine gas, indicating it can be used as promising candidates for high-performance organic amine sensors. The enhanced gas-sensing behavior should be attributed to the unique 1D wire-like morphology of ZnO support, the small size effect of SnO2 nanoparticles, and the semiconductor depletion layer model induced by the strong interfacial interaction between SnO2 and ZnO of the heterojunctions. The as-prepared SnO2/ZnO NW heterojunctions may also supply other novel applications in the fields like photocatalysis, lithium-ion batteries, waste water purification, and so on.

[Study of the phase transformation of TiO2 with in-situ XRD in different gas].

PubMed

Ma, Li-Jing; Guo, Lie-Jin

2011-04-01

TiO2 sample was prepared by sol-gel method from chloride titanium. The phase transformation of the prepared TiO2 sample was studied by in-situ XRD and normal XRD in different gas. The experimental results showed that the phase transformation temperatures of TiO2 were different under in-situ or normal XRD in different kinds of gas. The transformation of amorphous TiO2 to anatase was controlled by kinetics before 500 degrees C. In-situ XRD showed that the growth of anatase was inhibited, but the transformation of anatase to rutile was accelerated under inactive nitrogen in contrast to air. Also better crystal was obtained under hydrogen than in argon. These all showed that external oxygen might accelerate the growth of TiO2, but reduced gas might partly counteract the negative influence of lack of external oxygen. The mechanism of phase transformation of TiO2 was studied by in-situ XRD in order to control the structure in situ.

Formation of hydroxyl radicals and kinetic study of 2-chlorophenol photocatalytic oxidation using C-doped TiO2, N-doped TiO2, and C,N Co-doped TiO2 under visible light.

PubMed

Ananpattarachai, Jirapat; Seraphin, Supapan; Kajitvichyanukul, Puangrat

2016-02-01

This work reports on synthesis, characterization, adsorption ability, formation rate of hydroxyl radicals (OH(•)), photocatalytic oxidation kinetics, and mineralization ability of C-doped titanium dioxide (TiO2), N-doped TiO2, and C,N co-doped TiO2 prepared by the sol-gel method. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and UV-visible spectroscopy were used to analyze the titania. The rate of formation of OH(•) for each type of titania was determined, and the OH-index was calculated. The kinetics of as-synthesized TiO2 catalysts in photocatalytic oxidation of 2-chlorophenol (2-CP) under visible light irradiation were evaluated. Results revealed that nitrogen was incorporated into the lattice of titania with the structure of O-Ti-N linkages in N-doped TiO2 and C,N co-doped TiO2. Carbon was joined to the Ti-O-C bond in the C-doped TiO2 and C,N co-doped TiO2. The 2-CP adsorption ability of C,N co-doped TiO2 and C-doped TiO2 originated from a layer composed of a complex carbonaceous mixture at the surface of TiO2. C,N co-doped TiO2 had highest formation rate of OH(•) and photocatalytic activity due to a synergistic effect of carbon and nitrogen co-doping. The order of photocatalytic activity per unit surface area was the same as that of the formation rate of OH(•) unit surface area in the following order: C,N co-doped TiO2 > C-doped TiO2 > N-doped TiO2 > undoped TiO2.

Catalyst-Free Growth of Large Scale Ga2O3 Nanowires

DTIC Science & Technology

2001-11-01

XRD and TEM analyses indicate that the Ga 20 3 nanowires exhibit a monoclinic structure. PL characteristic of the Ga2O3 nanowires shows a UV emission...using Ga metal and N2 / H 20 reactants. The Ga2O3 nanowires, which have diameters ranging from 60 to 150 nm and lengths of several micrometers, are 133

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

NASA Astrophysics Data System (ADS)

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

1999-03-01

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

Nanostructured multielement (TiHfZrNbVTa)N coatings before and after implantation of N+ ions (1018 cm-2): Their structure and mechanical properties

NASA Astrophysics Data System (ADS)

Pogrebnjak, A. D.; Bondar, O. V.; Borba, S. O.; Abadias, G.; Konarski, P.; Plotnikov, S. V.; Beresnev, V. M.; Kassenova, L. G.; Drodziel, P.

2016-10-01

Multielement high entropy alloy (HEA) nitride (TiHfZrNbVTa)N coatings were deposited by vacuum arc and their structural and mechanical stability after implantation of high doses of N+ ions, 1018 cm-2, were investigated. The crystal structure and phase composition were characterized by X-ray diffraction (XRD) and Transmission Electron Microscopy, while depth-resolved nanoindentation tests were used to determine the evolution of hardness and elastic modulus along the implantation depth. XRD patterns show that coatings exhibit a main phase with fcc structure, which preferred orientation varies from (1 1 1) to (2 0 0), depending on the deposition conditions. First-principles calculations reveal that the presence of Nb atoms could favor the formation of solid solution with fcc structure in multielement HEA nitride. TEM results showed that amorphous and nanostructured phases were formed in the implanted coating sub-surface layer (∼100 nm depth). Concentration of nitrogen reached 90 at% in the near-surface layer after implantation, and decreased at higher depth. Nanohardness of the as-deposited coatings varied from 27 to 38 GPa depending on the deposition conditions. Ion implantation led to a significant decrease of the nanohardness to 12 GPa in the implanted region, while it reaches 24 GPa at larger depths. However, the H/E ratio is ⩾0.1 in the sub-surface layer due to N+ implantation, which is expected to have beneficial effect on the wear properties.

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

NASA Technical Reports Server (NTRS)

Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

2012-01-01

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Synthesis and characterization of novel Sm2O3/S-doped g-C3N4 nanocomposites with enhanced photocatalytic activities under visible light irradiation

NASA Astrophysics Data System (ADS)

Jourshabani, Milad; Shariatinia, Zahra; Badiei, Alireza

2018-01-01

Novel Sm2O3/S-doped g-C3N4 (CNS) composites were synthesized with in situ method by simultaneous combining S doping in carbon nitride structure to produce CNS as well as hybridization of CNS with the Sm2O3 semiconductor. The obtained composite photocatalysts with different Sm2O3 contents were characterized by XRD, FT-IR, XPS, TEM, BET, DRS and PL techniques and their photocatalytic activities were investigated for the degradation of methylene blue (MB) as a model pollutant in aqueous solution under visible-light irradiation. The XRD structure phase and TEM morphology results showed that stacking degree of π-conjugated system in the CNS structure was disrupted in the precense of Sm2O3 particles. The optimal Sm2O3 loading value was determined to be 8.9 wt% and its corresponding MB photodegradation rate was about 93% after 150 min light irradiation, which was indeed greater compared with those of the individual CNS and Sm2O3 samples. This enhanced photocatalytic performance was originated from characteristics of the hybrid formed between the Sm2O3 and CNS so that it improved the effective charge transfer through interfacial interactions between both components. In addition, the CNS synthesized by S doping exhibited a significant enhancement in the photocatalytic activity relative to that of the pure g-C3N4; this was mostly caused by the increase in its visible light harvesting ability and charge mobility. The possible mechanism for the photocatalytic degradation of MB was suggested and discussed in detail based on the findings acquired from radical/hole trapping experiments.

Strain and grain size of TiO2 nanoparticles from TEM, Raman spectroscopy and XRD: The revisiting of the Williamson-Hall plot method

NASA Astrophysics Data System (ADS)

Kibasomba, Pierre M.; Dhlamini, Simon; Maaza, Malik; Liu, Chuan-Pu; Rashad, Mohamed M.; Rayan, Diaa A.; Mwakikunga, Bonex W.

2018-06-01

The Williamson-Hall (W-H) equation, which has been used to obtain relative crystallite sizes and strains between samples since 1962, is revisited. A modified W-H equation is derived which takes into account the Scherrer equation, first published in 1918, (which traditionally gives more absolute crystallite size prediction) and strain prediction from Raman spectra. It is found that W-H crystallite sizes are on average 2.11 ± 0.01 times smaller than the sizes from Scherrer equation. Furthermore the strain from the W-H plots when compared to strain obtained from Raman spectral red-shifts yield factors whose values depend on the phases in the materials - whether anatase, rutile or brookite. Two main phases are identified in the annealing temperatures (350 °C-700 °C) chosen herein - anatase and brookite. A transition temperature of 550 °C has been found for nano-TiO2 to irreversibly transform from brookite to anatase by plotting the Raman peak shifts against the annealing temperatures. The W-H underestimation on the strain in the brookite phase gives W-H/Raman factor of 3.10 ± 0.05 whereas for the anatase phase, one gets 2.46 ± 0.03. The new βtot2cos2θ-sinθ plot and when fitted with a polynomial yield less strain but much better matching with experimental TEM crystallite sizes and the agglomerates than both the traditional Williamson-Hall and the Scherrer methods. There is greater improvement in the model when linearized - that is the βtotcos2θ-sinθ plot rather than the βtot2cos2θ-sinθ plot.

Modified g-C3N4/TiO2 nanosheets/ZnO ternary facet coupled heterojunction for photocatalytic degradation of p-toluenesulfonic acid (p-TSA) under visible light

NASA Astrophysics Data System (ADS)

Jiang, Dong; Yu, Han; Yu, Hongbing

2017-01-01

Novel ternary nanocomposites with facet coupled structure were synthesized by using modified g-C3N4, TiO2 nanosheets and nano-ZnO. Nanosheet/nanosheet heterojunction structure was investigated by TEM, XPS and XRD. FT-IR and Nitrogen adsorption were illustrated for chemical/physical structure analyses. Solution of p-Toluenesulfonic acid (p-TSA) was chosen as target pollutant for visible light photodegradation and the excellent removal efficiency was achieved by this structurally modified g-C3N4/TiO2/ZnO hybrid. The visible light absorption improvement and quantum efficiency enhancement, which were testified by UV-vis DRS, PL and p-TSA photodegradation measurements, due to the facet coupled structure and appropriate quantity of modified g-C3N4 in the nanocomposites.

Selective Oxidation of n-Hexane by Cu (II) Nanoclusters Supported on Nanocrystalline Zirconia Catalyst.

PubMed

Acharyya, Shankha Shubhra; Ghosh, Shilpi; Adak, Shubhadeep; Singh, Raghuvir; Saran, Sandeep; Bal, Rajaram

2015-08-01

Cu (II) nanoclusters supported on nanocrystalline zirconia catalyst (with size ~15 nm), was prepared by using cationic surfactant cetyltrimethylammonium in a hydrothermal synthesis method. The catalyst was characterized by XRD, XPS, TGA, SEM, TEM, FTIR and ICP-AES. The catalyst was found to be efficient in selective oxidation of n-hexane to 2-hexanol. An n-hexane conversion of 55%, with a 2-hexanol selectivity of 70% was achieved over this catalyst in liquid phase, without the use of any solvent. The catalyst can be reused several times without any significant activity loss.

Preparation of N-doped ZnO-loaded halloysite nanotubes catalysts with high solar-light photocatalytic activity.

PubMed

Cheng, Zhi-Lin; Sun, Wei

2015-01-01

N-doped ZnO nanoparticles were successfully assembled into hollow halloysite nanotubes (HNTs) by using the impregnation method. The catalysts based on N-doped ZnO-loaded HNTs nanocomposites (N-doped ZnO/HNTs) were characterized by X-ray diffraction (XRD), transmission electron microscopy-energy dispersive X-ray (TEM-EDX), scanning electron microscopy-energy dispersive X-ray (SEM-EDX), UV-vis and Fourier transform infrared spectroscopy (FT-IR) techniques. The XRD pattern showed ZnO nanoparticles with hexagonal structure loaded on HNTs. The TEM-EDX analysis indicated ZnO particles with the crystal size of ca.10 nm scattered in hollow structure of HNTs, and furthermore the concentration of N atom in nanocomposites was up to 2.31%. The SEM-EDX verified most of N-ZnO nanoparticles existing in hollow nanotubes of HNTs. Besides containing an obvious ultraviolet absorbance band, the UV-vis spectra of the N-doped ZnO/HNTs catalysts showed an available visible absorbance band by comparing to HNTs and non-doped ZnO/HNTs. The photocatalytic activity of the N-doped ZnO/HNTs catalysts was evaluated by the degradation of methyl orange (MO) solution with the concentration of 20 mg/L under the simulated solar-light irradiation. The result showed that the N-doped ZnO/HNTs catalyst exhibited a desirable solar-light photocatalytic activity.

Design of a highly sensitive ethanol sensor using a nano-coaxial p-Co3O4/n-TiO2 heterojunction synthesized at low temperature.

PubMed

Liang, Y Q; Cui, Z D; Zhu, S L; Li, Z Y; Yang, X J; Chen, Y J; Ma, J M

2013-11-21

In this paper, we describe the design, fabrication and gas-sensing tests of nano-coaxial p-Co3O4/n-TiO2 heterojunction. Specifically, uniform TiO2 nanotubular arrays have been assembled by anodization and used as templates for generation of the Co3O4 one-dimensional nanorods. The structure morphology and composition of as-prepared products have been characterized by SEM, XRD, TEM, and XPS. A possible growth mechanism governing the formation of such nano-coaxial heterojunctions is proposed. The TiO2 nanotube sensor shows a normal n-type response to reducing ethanol gas, whereas TiO2-Co3O4 exhibits p-type response with excellent sensing performances. This conversion of sensing behavior can be explained by the formation of p-n heterojunction structures. A possible sensing mechanism is also illustrated, which can provide theoretical guidance for the further development of advanced gas-sensitive materials with p-n heterojunction.

Crystal structure, chemical composition, and extended defects of the high-Tc (Bi,Pb)2Sr2Ca(n)-1CunO4 + 2n + delta compounds.

PubMed

Eibl, O

1995-02-15

This paper summarizes results obtained by high-resolution transmission electron microscopy on the crystal structure and microstructure of the (Bi,Pb)2Sr2Ca(n)-1CunO4 + 2n + delta high-Tc superconducting oxides. The experimental basis for the work presented here are high-resolution structure images obtained at ultra-thin (3 nm) areas of carefully prepared transmission electron microscope (TEM) samples. The analysis was carried out on a 400 kV TEM equipped with a pole piece yielding 0.17 nm point-to-point resolution. From the images obtained the projected crystal potential of the cations can be extracted directly, as confirmed by detailed image simulation. Structural analysis of the oxygen sublattice remains an unsolved problem by high-resolution TEM (HRTEM), mainly because of the small scattering factors, and thus the contribution of the oxygen sublattice to the image contrast is small. The (BiPb)2Sr2Ca(n)-1CunO4 + 2n + delta phases are modulated structures that can be understood as an average structure plus a superimposed displacement field. The crystal structure consists of BiO double layers and perovskite-type cuboids (containing Sr, Ca, Cu, and O), which are sandwiched between the BiO double layers. The displacement field can be directly analyzed by HRTEM, and the largest displacement amplitudes of 70 pm were determined for the Bi atoms in the n = 1 compound. The chemical composition of the n = 2 and n = 3 compounds was determined by EDX in the TEM for the cation sublattice. A significant (Ca + Sr) deficiency (approximately 10%) with respect to Cu was found. The (Sr + Ca)/Cu mole fraction ratio was 1.31 for the Bi-2212 phase and 1.14 for the Bi(Pb)-2223 phase. The oxygen content cannot be determined by EDX in the TEM with the accuracy necessary for a correlation with electrical and superconducting properties. The defect structure present in these materials, that is, intergrown lamellae with different crystal structures and equal or different chemical

Growth of GaN@InGaN Core-Shell and Au-GaN Hybrid Nanostructures for Energy Applications

DOE PAGES

Kuykendall, Tevye; Aloni, Shaul; Jen-La Plante, Ilan; ...

2009-01-01

We demonstrated a method to control the bandgap energy of GaN nanowires by forming GaN@InGaN core-shell hybrid structures using metal organic chemical vapor deposition (MOCVD). Furthermore, we show the growth of Au nanoparticles on the surface of GaN nanowires in solution at room temperature. The work shown here is a first step toward engineering properties that are crucial for the rational design and synthesis of a new class of photocatalytic materials. The hybrid structures were characterized by various techniques, including photoluminescence (PL), energy dispersive x-ray spectroscopy (EDS), transmission and scanning electron microscopy (TEM and SEM), and x-ray diffraction (XRD).

Improvement in crystal quality and optical properties of n-type GaN employing nano-scale SiO2 patterned n-type GaN substrate.

PubMed

Jo, Min Sung; Sadasivam, Karthikeyan Giri; Tawfik, Wael Z; Yang, Seung Bea; Lee, Jung Ju; Ha, Jun Seok; Moon, Young Boo; Ryu, Sang Wan; Lee, June Key

2013-01-01

n-type GaN epitaxial layers were regrown on the patterned n-type GaN substrate (PNS) with different size of silicon dioxide (SiO2) nano dots to improve the crystal quality and optical properties. PNS with SiO2 nano dots promotes epitaxial lateral overgrowth (ELOG) for defect reduction and also acts as a light scattering point. Transmission electron microscopy (TEM) analysis suggested that PNS with SiO2 nano dots have superior crystalline properties. Hall measurements indicated that incrementing values in electron mobility were clear indication of reduction in threading dislocation and it was confirmed by TEM analysis. Photoluminescence (PL) intensity was enhanced by 2.0 times and 3.1 times for 1-step and 2-step PNS, respectively.

One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel Aqua(2,9-dimethyl-1,10-phenanthroline)NiCl2 Complex

PubMed Central

Barakat, Assem; Al-Noaimi, Mousa; Suleiman, Mohammed; Aldwayyan, Abdullah S.; Hammouti, Belkheir; Ben Hadda, Taibi; Haddad, Salim F.; Boshaala, Ahmed; Warad, Ismail

2013-01-01

[NiCl2(C14H12N2)(H2O)] complex has been synthesized from nickel chloride hexahydrate (NiCl2·6H2O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as N,N-bidentate ligand. The synthesized complex was characterized by elemental analysis, infrared (IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy and differential thermal/thermogravimetric analysis (TG/DTA). The complex was further confirmed by single crystal X-ray diffraction (XRD) as triclinic with space group P-1. The desired complex, subjected to thermal decomposition at low temperature of 400 ºC in an open atmosphere, revealed a novel and facile synthesis of pure NiO nanoparticles with uniform spherical particle; the structure of the NiO nanoparticles product was elucidated on the basis of Fourier transform infrared (FT-IR), UV-vis spectroscopy, TG/DTA, XRD, scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDXS) and transmission electron microscopy (TEM). PMID:24351867

High temperature XRD of Cu2.1Zn0.9SnSe4

NASA Astrophysics Data System (ADS)

Chetty, Raju; Mallik, Ramesh Chandra

2014-04-01

Quaternary compound with chemical composition Cu2.1Zn0.9SnSe4 is prepared by solid state synthesis. High temperature XRD (X-Ray Diffraction) of this compound is used in studying the effect of temperature on lattice parameters and thermal expansion coefficients. Thermal expansion coefficient is one of the important quantities in evaluating the Grüneisen parameter which further useful in determining the lattice thermal conductivity of the material. The high temperature XRD of the material revealed that the lattice parameters as well as thermal expansion coefficients of the material increased with increase in temperature which confirms the presence of anharmonicty.

Evolution of TEM-type enzymes: biochemical and genetic characterization of two new complex mutant TEM enzymes, TEM-151 and TEM-152, from a single patient.

PubMed

Robin, Frédéric; Delmas, Julien; Schweitzer, Cédric; Tournilhac, Olivier; Lesens, Olivier; Chanal, Catherine; Bonnet, Richard

2007-04-01

Two clinical isolates of Escherichia coli, CF1179 and CF1295, were isolated from a patient hospitalized in the hematology unit of the University Hospital of Clermont-Ferrand, Clermont-Ferrand, France. They were resistant to penicillin-clavulanate combinations and to ceftazidime. The double-disk synergy test was positive only for isolate CF1179. Molecular comparison of the isolates showed that they were clonally related. E. coli recombinant strains exhibiting the resistance phenotype of the clinical strains were obtained by cloning. The clones corresponding to strains CF1179 and CF1295 produced TEM-type beta-lactamases with pI values of 5.7 and 5.3, respectively. Sequencing analysis revealed two novel blaTEM genes encoding closely related complex mutant TEM enzymes, designated TEM-151 (pI 5.3) and TEM-152 (pI 5.7). These two genes also harbored a new promoter region which presented a 9-bp deletion. The two novel beta-lactamases differed from the parental enzyme, TEM-1, by the substitution Arg164His, previously observed in extended-spectrum beta-lactamases (ESBLs), and by the substitutions Met69Val and Asn276Asp, previously observed in the inhibitor-resistant penicillinase TEM-36/IRT-7. They differed by two amino acid substitutions: TEM-152 harbored a Glu240Lys ESBL-type substitution and TEM-151 had an Ala284Gly substitution. Functional analysis of TEM-151 and TEM-152 showed that both enzymes had hydrolytic activity against ceftazidime (kcat, 5 and 16 s-1, respectively). TEM-152 was more resistant than TEM-151 to the inhibitor clavulanic acid (50% inhibitory concentrations, 1 versus 0.17 microM). These results confirm the evolution of TEM-type enzymes toward complex enzymes harboring the two kinds of substitutions which confer an extended spectrum of action against beta-lactam antibiotics and resistance to inhibitors.

Synthesis, dynamic NMR characterization and XRD studies of novel N,N'-substituted piperazines for bioorthogonal labeling.

PubMed

Mamat, Constantin; Pretze, Marc; Gott, Matthew; Köckerling, Martin

2016-01-01

Novel, functionalized piperazine derivatives were successfully synthesized and fully characterized by 1 H/ 13 C/ 19 F NMR, MS, elemental analysis and lipophilicity. All piperazine compounds occur as conformers resulting from the partial amide double bond. Furthermore, a second conformational shape was observed for all nitro derivatives due to the limited change of the piperazine chair conformation. Therefore, two coalescence points were determined and their resulting activation energy barriers were calculated using 1 H NMR. To support this result, single crystals of 1-(4-nitrobenzoyl)piperazine ( 3a , monoclinic, space group C 2/ c , a = 24.587(2), b = 7.0726(6), c = 14.171(1) Å, β = 119.257(8)°, V = 2149.9(4) Å 3 , Z = 4, D obs = 1.454 g/cm 3 ) and the alkyne derivative 4-(but-3-yn-1-yl)-1-(4-fluorobenzoyl)piperazine ( 4b , monoclinic, space group P 2 1 / n , a = 10.5982(2), b = 8.4705(1), c = 14.8929(3) Å, β = 97.430(1)°, V = 1325.74(4) Å 3 , Z = 4, D obs = 1.304 g/cm 3 ) were obtained from a saturated ethyl acetate solution. The rotational conformation of these compounds was also verified by XRD. As proof of concept for future labeling purposes, both nitropiperazines were reacted with [ 18 F]F - . To test the applicability of these compounds as possible 18 F-building blocks, two biomolecules were modified and chosen for conjugation either using the Huisgen-click reaction or the traceless Staudinger ligation.

Photochemical degradation of an anionic surfactant by TiO2 nanoparticle doped with C, N in aqueous solution

NASA Astrophysics Data System (ADS)

Zamiri, M.; Giahi, M.

2016-12-01

Novel C,N-doped TiO2 nanoparticles were prepared by a solid phase reaction. The catalyst was characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDX). The results showed that crystallite size of synthesized C,N-doped TiO2 particles were in nanoscale. UV light photocatalytic studies were carried out using sodium naphthalenesulfonate formaldehyde condensate (SNF) as a model pollutant. The effects of initial concentration of surfactant, catalyst amount, pH, addition of oxidant on the reaction rate were ascertained and optimum conditions for maximum degradation was determined. The results indicated that for a solution of 20 mg/L of SNF, almost 98.7% of the substance were removed at pH 4.0 and 0.44 g/L photocatalyst load, with addition of 1 mM K2S2O8 and irradiation time of 90 min. The kinetics of the process was studied, and the photodegradation rate of SNF was found to obey pseudo-first-order kinetics equation represented by the Langmuir-Hinshelwood model.

Effect of SiO2/Al2O3 Ratio on Micro-Mesopore Formation for Pt/Beta-MCM-41 via NaOH Treatment and the Catalytic Performance in N-heptane Hydro isomerization

NASA Astrophysics Data System (ADS)

Gao, Li; Shi, Zhiyuan; Liu, Yingming; Zhao, Yuanshou; Liu, Qinghua; Xu, Chengguo; Bai, Peng; Yan, Zifeng

2018-01-01

Micro-mesoporous composite material Beta-MCM-41(BM) were hydrothermally synthesized by treating parent beta with molar SiO2/Al2O3 ratios of 12.5, 20 and 30 as precursors. The influence of SiO2/Al2O3 ratio of zeolite beta on effective micro-mesoporous composite formation was studied by investigating the crystallinity, morphology, chemical composition, acidity and textural property of Beta-MCM-41 through XRD, nitrogen adsorption, SEM, TEM, NH3-TPD, FTIR and Pyridine-FTIR. The catalytic performance was evaluated in terms of n-heptane hydro isomerization. The results demonstrated that Beta-MCM-41 supported Pt catalysts showed higher selectivity to isoheptanes than Pt/Beta. It was attributed to the superiorities of the pore structure and mesoporous accelerated the diffusion of larger molecules of isoheptanes.

XRD and 29Si MAS-NMR spectroscopy across the β-Lu 2Si 2O 7- β-Y 2Si 2O 7 solid solution

NASA Astrophysics Data System (ADS)

Becerro, Ana I.; Escudero, Alberto

2005-01-01

Samples in the system Lu 2-xY xSi 2O 7 (0⩽ x⩽2) have been synthesized following the sol-gel method and calcined to 1300 °C, a temperature at which the β-polymorph is known to be the stable phase for the end-members Lu 2Si 2O 7 and Y 2Si 2O 7. The XRD patterns of all the compositions studied are compatible with the structure of the β-polymorph. Unit cell parameters are calculated as a function of composition from XRD patterns. They show a linear change with increasing Y content, which indicates a solid solubility of β-Y 2Si 2O 7 in β-Lu 2Si 2O 7 at 1300 °C. 29Si MAS NMR spectra of the different members of the system agree with the XRD results, showing a linear decrease of the 29Si chemical shift with increasing Y content. Finally, a correlation reported in the literature to predict 29Si chemical shifts in silicates is applied here to obtain the theoretical variation in 29Si chemical shift values in the system Lu 2Si 2O 7-Y 2Si 2O 7 and the results compare favorably with the values obtained experimentally.

XRD measurement of mean crystallite thickness of illite and illite/smectite: Reappraisal of the Kubler index and the Scherrer equation

USGS Publications Warehouse

Drits, Victor A.; Środoń, Jan; Eberl, D.D.

1997-01-01

The standard form of the Scherrer equation, which has been used to calculate the mean thickness of the coherent scattering domain (CSD) of illite crystals from X-ray diffraction (XRD) full width data at half maximum (FWHM) intensity, employs a constant, Ksh, of 0.89. Use of this constant is unjustified, even if swelling has no effect on peak broadening, because this constant is valid only if all CSDs have a single thickness. For different thickness distributions, the Scherrer “constant” has very different values.Analysis of fundamental particle thickness data (transmission electron microscopy, TEM) for samples of authigenic illite and illite/smectite from diagenetically altered pyroclastics and filamentous illites from sandstones reveals a unique family of lognormal thickness distributions for these clays. Experimental relations between the distributions' lognormal parameters and mean thicknesses are established. These relations then are used to calculate the mean thickness of CSDs for illitic samples from XRD FWHM, or from integral XRD peak widths (integrated intensity/maximum intensity).For mixed-layer illite/smectite, the measured thickness of the CSD corresponds to the mean thickness of the mixed-layer crystal. Using this measurement, the mean thickness of the fundamental particles that compose the mixed-layer crystals can be calculated after XRD determination of percent smectitic interlayers. The effect of mixed layering (swelling) on XRD peak width for these samples is eliminated by using the 003 reflection for glycolated samples, and the 001, 002 or 003 reflection for dehydrated, K-saturated samples. If this technique is applied to the 001 reflection of air-dried samples (Kubler index measurement), mean CSD thicknesses are underestimated due to the mixed-layering effect.The technique was calibrated using NEW MOD©-simulated XRD profiles of illite, and then tested on well-characterized illite and illite/smectite samples. The XRD measurements are in good

AlGaN/GaN high electron mobility transistor grown on GaN template substrate by molecule beam epitaxy system

NASA Astrophysics Data System (ADS)

Tsai, Jenn-Kai; Chen, Y. L.; Gau, M. H.; Pang, W. Y.; Hsu, Y. C.; Lo, Ikai; Hsieh, C. H.

2008-03-01

In this study, AlGaN/GaN high electron mobility transistor (HEMT) structure was grow on GaN template substrate radio frequency plasma assisted molecular beam epitaxy (MBE) equipped with an EPI UNI-Bulb nitrogen plasma source. The undoped GaN template substrate was grown on c-sapphire substrate by metal organic vapor phase epitaxy system (MOPVD). After growth of MOVPE and MBE, the samples are characterized by double crystal X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (SEM), atomic force microscopy (AFM), and Hall effect measurements. We found that the RMS roughness of template substrate play the major role in got the high value of mobility on AlGaN/GaN HEMT. When the roughness was lower than 0.77 nm in a 25 μm x 25 μm area, the mobility of HEMT at the temperature of 77 K was over 10000 cm^2/Vs.

Structure, Elastic Constants and XRD Spectra of Extended Solids under High Pressure

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

Batyrev, I. G.; Coleman, S. P.; Ciezak-Jenkins, J. A.

We present results of evolutionary simulations based on density functional calculations of a potentially new type of energetic materials called extended solids: P-N and N-H. High-density structures with covalent bonds generated using variable and fixed concentration methods were analysed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction (XRD) spectra. X-ray diffraction spectra were calculated using a virtual diffraction algorithm that computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculated XRD patterns were used to search for the structure of extended solids present at experimental pressures by optimizing data accordingmore » to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Elastic constants has been calculated for thermodynamically stable structures of P-N system.« less

Influence of Fluoride Ion Concentrations on the Corrosion Behavior of Ta2N Nanocrystalline Coating for Dental Implant Applications

NASA Astrophysics Data System (ADS)

Xu, Jiang; Ma, Jin Jin; Munroe, Paul; Xie, Zong-Han

The development of new corrosion-resistant coatings is often challenging, but strongly driven by the potential benefits such coatings hold. A nanostructured Ta2N coating was deposited on a Ti-6Al-4V substrate in an Ar-N atmosphere using a double cathode glow discharge plasma method with the aim being to improve its corrosion resistance in oral environments. The microstructure of the coating was investigated by a range of methods including XRD, SEM-EDS and TEM. The as-deposited coating exhibited densely packed fibrous structure and the individual fibers were composed of equiaxed grains with an average grain size ˜13nm, arranged along the longitudinal axis of the individual fibers. The electrochemical behavior of the Ta2N nanocrystalline coating was characterized in artificial saliva containing different NaF concentrations by a range of electrochemical techniques, including potentiodynamic measurement, EIS, capacitance and PZFC measurements. It was shown that the coating possessed superior corrosion resistance compared to uncoated Ti-6Al-4V, because its passive film exhibited higher stability against the fluoride ion attack.

2.5D Modeling of TEM Data Applied to Hidrogeological Studies in PARANÁ Basin, Brazil

NASA Astrophysics Data System (ADS)

Bortolozo, C. A.; Porsani, J. L.; Santos, F. M.

2013-12-01

The transient electromagnetic method (TEM) is used all over the world and has shown great potential in hydrological, hazardous waste site characterization, mineral exploration, general geological mapping, and geophysical reconnaissance. However, the behavior of TEM fields are very complex and is not yet fully understood. Forward modeling is one of the most common and effective methods to understand the physical behavior and significance of the electromagnetics responses of a TEM sounding. Until now, there are a limited number of solutions for the 2D forward problem for TEM. More rare are the descriptions of a three-component response of a 3D source over 2D earth, which is the so-called 2.5D. The 2.5D approach is more realistic than the conventional 2D source previous used, once normally the source cannot be realistic represented for a 2D approximation (normally source are square loops). At present the 2.5D model represents the only way of interpreting TEM data in terms of a complex earth, due to the prohibitive amount of computer time and storage required for a full 3D model. In this work we developed a TEM modeling program for understanding the different responses and how the magnetic and electric fields, produced by loop sources at air-earth interface, behave in different geoelectrical distributions. The models used in the examples are proposed focusing hydrogeological studies, once the main objective of this work is for detecting different kinds of aquifers in Paraná sedimentary basin, in São Paulo State - Brazil. The program was developed in MATLAB, a widespread language very common in the scientific community.

One-step electrospinning synthesis of TiO2/g-C3N4 nanofibers with enhanced photocatalytic properties

NASA Astrophysics Data System (ADS)

Tang, Qian; Meng, Xianfeng; Wang, Zhiying; Zhou, Jianwei; Tang, Hua

2018-02-01

TiO2/g-C3N4 composite nanofibers have been successfully synthesized by one-step electrospinning method, using titanium (IV) n-butoxide (TNBT) and urea as raw materials. The structure and compositions of TiO2/g-C3N4 samples are characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Diffuse reflectance spectroscopy (DRS), Scanning electron microscopy (SEM), Transmission electron microscope (TEM), X-ray photoelectron spectrometer (XPS) and Brunauer-Emmett-Teller (BET), respectively. The results show that the porous uniform TiO2/g-C3N4 composite nanofibers, with diameter of 100-150 nm, can be successfully prepared through electrospinning method combining 550 °C calcination process. The photocatalytic activity is evaluated by the degradation of rhodamine B (RhB) under simulated solar light. The enhanced catalytic activity is attributed predominantly to the heterojunction between TiO2 and g-C3N4, which promotes the transferring of carriers and prohibits their recombination. With the optimal doping amount of 0.6 g urea (corresponding to 3 g TNBT), the TiO2/g-C3N4 composite nanofibers exhibit the highest rate towards the photocatalytic degradation of RhB. A diagram is presented to explicate the mechanism of the whole catalytic experiment. This study might provide a promising future of applying green catalysts to solving water pollution problems.

Synthesis, structural, optical and anti-rheumatic activity of metal complexes derived from (E)-2-amino-N-(1-(2-aminophenyl)ethylidene)benzohydrazide (2-AAB) with Ru(III), Pd(II) and Zr(IV)

NASA Astrophysics Data System (ADS)

Hosny, Nasser Mohammed; Sherif, Yousery E.

2015-02-01

Three new metal complexes derived from Pd(II), Ru(III) and Zr(IV) with (E)-2-amino-N-(1-(2-aminophenyl)ethylidene)benzohydrazide (2-AAB) have been synthesized. The isolated complexes were characterized by elemental analyses, FT-IR, UV-Vis, ES-MS, 1H NMR, XRD, thermal analyses (TGA and DTA) and conductance. The morphology and the particle size were determined by transmittance electron microscope (TEM). The results showed that, the ligand coordinates to Pd(II) in the enol form, while it coordinates to Ru(III) and Zr(IV) in the keto form. A square planar geometry is suggested for Pd(II) complex and octahedral geometries are suggested for Ru(III) and Zr(IV) complexes. The optical band gaps of the isolated complexes were measured and indicated the semi-conductivity nature of the complexes. The anti-inflammatory and analgesic activities of the ligand and its complexes showed that, Ru(III) complex has higher effect than the well known drug "meloxicam".

Biological and catalytic applications of green synthesized fluorescent N-doped carbon dots using Hylocereus undatus.

PubMed

Arul, Velusamy; Edison, Thomas Nesakumar Jebakumar Immanuel; Lee, Yong Rok; Sethuraman, Mathur Gopalakrishnan

2017-03-01

In this work, a simple hydrothermal route for the synthesis of fluorescent nitrogen doped carbon dots (N-CDs) is reported. The Hylocereus undatus (H. undatus) extract and aqueous ammonia are used as carbon and nitrogen source, respectively. The optical properties of synthesized N-CDs are analyzed using UV-Visible (UV-Vis) and fluorescence spectroscopy. The surface morphology, elemental composition, crystallinity and functional groups present in the N-CDs are examined using high resolution transmission electron microscopy (HR-TEM) with energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy, respectively. The synthesized N-CDs emit strong blue fluorescence at 400nm under the excitation of 320nm. Further, the excitation dependent emission properties are also observed from the fluorescence of synthesized N-CDs. The HR-TEM results reveal that synthesized N-CDs are in spherical shape with average diameter of 2.5nm. The XRD pattern exhibits, the graphitic nature of synthesized N-CDs. The doping of nitrogen is confirmed from the EDS and FT-IR studies. The cytotoxicity and biocompatibility of N-CDs are evaluated through MTT assay on L-929 (Lymphoblastoid-929) and MCF-7 (Michigan Cancer Foundation-7) cells. The results indicate that the fluorescent N-CDs show less cytotoxicity and good biocompatibility on both L-929 and MCF-7 cells. Moreover, the N-CDs show excellent catalytic activity towards the reduction of methylene blue by sodium borohydride. Copyright © 2017 Elsevier B.V. All rights reserved.

Facile synthesis of the Li-rich layered oxide Li1.23Ni0.09Co0.12Mn0.56O2 with superior lithium storage performance and new insights into structural transformation of the layered oxide material during charge-discharge cycle: in situ XRD characterization.

PubMed

Shen, Chong-Heng; Wang, Qin; Fu, Fang; Huang, Ling; Lin, Zhou; Shen, Shou-Yu; Su, Hang; Zheng, Xiao-Mei; Xu, Bin-Bin; Li, Jun-Tao; Sun, Shi-Gang

2014-04-23

In this work, the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 was synthesized through a facile route called aqueous solution-evaporation route that is simple and without waste water. The as-prepared Li1.23Ni0.09Co0.12Mn0.56O2 oxide was confirmed to be a layered LiMO2-Li2MnO3 solid solution through ex situ X-ray diffraction (ex situ XRD) and transmission electron microscopy (TEM). Electrochemical results showed that the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material can deliver a discharge capacity of 250.8 mAhg(-1) in the 1st cycle at 0.1 C and capacity retention of 86.0% in 81 cycles. In situ X-ray diffraction technique (in situ XRD) and ex situ TEM were applied to study structural changes of the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material during charge-discharge cycles. The study allowed observing experimentally, for the first time, the existence of β-MnO2 phase that is appeared near 4.54 V in the first charge process, and a phase transformation of the β-MnO2 to layered Li0.9MnO2 is occurred in the initial discharge process by evidence of in situ XRD pattrens and selected area electron diffraction (SAED) patterns at different states of the initial charge and discharge process. The results illustrated also that the variation of the in situ X-ray reflections during charge-discharge cycling are clearly related to the changes of lattice parameters of the as-prepared Li-rich oxide during the charge-discharge cycles.

High temperature XRD of Cu2GeSe3

NASA Astrophysics Data System (ADS)

Premkumar D., S.; Chetty, Raju; Malar, P.; Mallik, Ramesh Chandra

2015-06-01

The Cu2GeSe3 is prepared by solid state synthesis method. The high temperature XRD has been done at different temperature from 30 °C to 450 °C. The reitveld refinement confirms Cu2GeSe3 phase and orthorhombic crystal structure. The lattice constants are increasing with increase in the temperature and their rate of increase with respect to temperature are used for finding the thermal expansion coefficient. The calculation of the linear and volume coefficient of thermal expansion is done from 30 °C to 400 °C. Decrease in the values of linear expansion coefficients with temperature are observed along a and c axis. Since thermal expansion coefficient is the consequence of the distortion of atoms in the lattice; this can be further used to find the minimum lattice thermal conductivity at given temperature.

Synthesis, characterization and electrochemical performance of graphene decorated with 1D NiMoO4.nH2O nanorods

NASA Astrophysics Data System (ADS)

Ghosh, Debasis; Giri, Soumen; Das, Chapal Kumar

2013-10-01

One-dimensional NiMoO4.nH2O nanorods and their graphene based hybrid composite with good electrochemical properties have been synthesized by a cost effective hydrothermal procedure. The formation of the mixed metal oxide and the composite was confirmed by XRD, XPS and Raman analyses. The morphological characterizations were carried out using FESEM and TEM analyses. The materials were subjected to electrochemical characterization through cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) studies with 6 M KOH as the supporting electrolyte. For NiMoO4.nH2O, a maximum specific capacitance of 161 F g-1 was obtained at 5 A g-1 current density, accompanied with an energy density of 4.53 W h kg-1 at a steady power delivery rate of 1125 W kg-1. The high utility of the pseudocapacitive NiMoO4.nH2O was achieved in its graphene based composite, which exhibited a high specific capacitance of 367 F g-1 at 5 A g-1 current density and a high energy density of 10.32 W h kg-1 at a power density of 1125 W kg-1 accompanied with long term cyclic stability.One-dimensional NiMoO4.nH2O nanorods and their graphene based hybrid composite with good electrochemical properties have been synthesized by a cost effective hydrothermal procedure. The formation of the mixed metal oxide and the composite was confirmed by XRD, XPS and Raman analyses. The morphological characterizations were carried out using FESEM and TEM analyses. The materials were subjected to electrochemical characterization through cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) studies with 6 M KOH as the supporting electrolyte. For NiMoO4.nH2O, a maximum specific capacitance of 161 F g-1 was obtained at 5 A g-1 current density, accompanied with an energy density of 4.53 W h kg-1 at a steady power delivery rate of 1125 W kg-1. The high utility of the pseudocapacitive NiMoO4.nH2O was achieved in its graphene

One-pot green synthesis of zinc oxide nano rice and its application as sonocatalyst for degradation of organic dye and synthesis of 2-benzimidazole derivatives

NASA Astrophysics Data System (ADS)

Paul, Bappi; Vadivel, Sethumathavan; Dhar, Siddhartha Sankar; Debbarma, Shyama; Kumaravel, M.

2017-05-01

In this paper, we report novel and green approach for one-pot biosynthesis of zinc oxide (ZnO) nanoparticles (NPs). Highly stable and hexagonal phase ZnO nanoparticles were synthesized using seeds extract from the tender pods of Parkia roxburghii and characterized by XRD, FT-IR, EDX, TEM, and N2 adsorption-desorption (BET) studies. The present method of synthesis of ZnO NPs is very efficient and cost effective. The powder XRD pattern furnished evidence for the formation of hexagonal close packing structure of ZnO NPs having average crystallite size 25.6 nm. The TEM image reveals rice shapes ZnO NPs are with an average diameter of 40-60 nm. The as-synthesized ZnO NPs has proved to be an excellent sonocatalysts for degradation of organic dye and synthesis of 2-benzimidazole derivatives.

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

PubMed Central

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

2017-01-01

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

XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite.

PubMed

Reyes-Gasga, José; Martínez-Piñeiro, Esmeralda L; Rodríguez-Álvarez, Galois; Tiznado-Orozco, Gaby E; García-García, Ramiro; Brès, Etienne F

2013-12-01

The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI)XRD index is related to the crystal structure of the samples and the (CI)FTIR index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI)XRD value indicated that enamel is more crystalline than synthetic HAP, while (CI)FTIR indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. © 2013.

Crystallization and characterization of Y2O3-SiO2 glasses

NASA Technical Reports Server (NTRS)

Drummond, C. H., III; Lee, W. E.; Sanders, W. A.; Kiser, J. D.

1988-01-01

Glasses in the yttria-silica system with 20-40 mol pct Y2O3 have been subjected to recrystallization studies after melting at 1900-2100 C in W crucibles in 1 and 50 atm N2. The TEM and XRD results obtained indicate the presence of the delta, gamma, gamma-prime, and beta-Y2Si2O7 crystalline phases, depending on melting and quenching conditions. Heat-treatment in air at 1100-1600 C increased the amount of crystallization, and led to the formation of Y2SiO5, cristobalite, and polymorphs of Y2Si2O7. Also investigated were the effects of 5 and 10 wt pct zirconia additions.

Crystallization and characterization of Y2O3-SiO2 glasses

NASA Technical Reports Server (NTRS)

Drummond, Charles H., III; Lee, William E.; Sanders, W. A.; Kiser, J. D.

1991-01-01

Glasses in the yttria-silica system with 20 to 40 mol pct Y2O3 were subjected to recrystallization studies after melting at 1900 to 2100 C in W crucibles in 1 and 50 atm N2. The TEM and XRD results obtained indicate the presence of the delta, gamma, gamma prime, and beta-Y2Si2O7 crystalline phases, depending on melting and quenching conditions. Heat treatment in air at 1100 to 1600 C increased the amount of crystallization, and led to the formation of Y2SiO5, cristabalite, and polymorphs of Y2Si2O7. Also investigated were the effects of 5 and 10 wt pct zirconia additions.

Degradation mechanisms of 2 MeV proton irradiated AlGaN/GaN HEMTs

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

Greenlee, Jordan D., E-mail: jordan.greenlee.ctr@nrl.navy.mil; Anderson, Travis J.; Koehler, Andrew D.

2015-08-24

Proton-induced damage in AlGaN/GaN HEMTs was investigated using energy-dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM), and simulated using a Monte Carlo technique. The results were correlated to electrical degradation using Hall measurements. It was determined by EDS that the interface between GaN and AlGaN in the irradiated HEMT was broadened by 2.2 nm, as estimated by the width of the Al EDS signal compared to the as-grown interface. The simulation results show a similar Al broadening effect. The extent of interfacial roughening was examined using high resolution TEM. At a 2 MeV proton fluence of 6 × 10{sup 14} H{supmore » +}/cm{sup 2}, the electrical effects associated with the Al broadening and surface roughening include a degradation of the ON-resistance and a decrease in the electron mobility and 2DEG sheet carrier density by 28.9% and 12.1%, respectively.« less

RBS, TEM and SEM Characterization of Gold Nanoclusters in TiO2(110)

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

Shutthanandan, V; Zhang, Yanwen; Wang, Chong M.

2004-05-01

Nucleation of gold nanoclusters in TiO2(110) single crystal using ion implantation and subsequent annealing were studied by Rutherford backscattering spectrometry /channeling (RBS/C), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Approximately 1000 Au2+/nm2 was implanted at room temperature in TiO2(110) substrates. TEM and SEM measurements revel that rounded nanoclusters were formed during the implantation. In contrast subsequent annealing in air for 10 hours at 1275 K promoted the formation of faceted (rectangular shaped) Au nano structures in TiO2. RBS channeling measurements further reveled that Au atoms randomly occupied in the host TiO2 lattice during the implantation. However, some ofmore » the gold atoms were moved into the Ti lattice position after annealing.« less

Electronic properties and morphology of copper oxide/n-type silicon heterostructures

NASA Astrophysics Data System (ADS)

Lindberg, P. F.; Gorantla, S. M.; Gunnæs, A. E.; Svensson, B. G.; Monakhov, E. V.

2017-08-01

Silicon-based tandem heterojunction solar cells utilizing cuprous oxide (Cu2O) as the top absorber layer show promise for high-efficiency conversion and low production cost. In the present study, single phase Cu2O films have been realized on n-type Si substrates by reactive magnetron sputtering at 400 °C. The obtained Cu2O/Si heterostructures have subsequently been heat treated at temperatures in the 400-700 °C range in Ar flow and extensively characterized by x-ray diffraction (XRD) measurements, transmission electron microscopy (TEM) imaging and electrical techniques. The Cu2O/Si heterojunction exhibits a current rectification of ~5 orders of magnitude between forward and reverse bias voltages. High resolution cross-sectional TEM-images show the presence of a ~2 nm thick interfacial SiO2 layer between Cu2O and the Si substrate. Heat treatments below 550 °C result in gradual improvement of crystallinity, indicated by XRD. At and above 550 °C, partial phase transition to cupric oxide (CuO) occurs followed by a complete transition at 700 °C. No increase or decrease of the SiO2 layer is observed after the heat treatment at 550 °C. Finally, a thin Cu-silicide layer (Cu3Si) emerges below the SiO2 layer upon annealing at 550 °C. This silicide layer influences the lateral current and voltage distributions, as evidenced by an increasing effective area of the heterojunction diodes.

Structural, molecular orbital and optical characterizations of solvatochromic mixed ligand copper(II) complex of 5,5-Dimethyl cyclohexanate 1,3-dione and N,N,N',N'N″-pentamethyldiethylenetriamine.

PubMed

Taha, A; Farag, A A M; Ammar, A H; Ahmed, H M

2014-03-25

In this work, a new solvatochromic mononuclear mixed ligand complex with the formula, Cu(DMCHD)(Me5dien)NO3 (where, DMCHD=5,5-Dimethyl cyclohexanate 1,3-dione and (Me5dien)=N,N,N',N'N″-pentamethyldiethylenetriamine was synthesized and characterized by analytical, spectral, magnetic, molar conductance, thermal gravimetric analysis (TGA), X-ray diffraction (XRD) and transmission electron microscope (TEM) measurements. The formation constant-value for copper (II)-DMCHD was found to be much lower than the expected for similar β-diketones, revealing monobasic unidentate nature of this ligand. The d-d absorption bands of the prepared complex exhibit a color changes in various solvent (solvatochromic). Specific and non-specific interactions of solvent molecules with the complex were investigated using Multi Parametric Linear Regression Analysis (MLRA). Structural parameters of the free ligands and their Cu (II) - complex were calculated on the basis of semi-empirical PM3 level and compared with the experimental data. The crystallite size and morphology of Cu(DMCHD)(Me5dien)NO3 were examined using XRD analysis and TEM, revealing that the complex is well crystalline and correspond to the monoclinic crystal structure. The lattice strain and mean crystallite size were estimated by Williamson-Hall (W-H) plot using X-ray diffraction data. The main important absorption parameters such as extinction molar coefficient, oscillator strength and electric dipole strength of the principal optical transitions in the UV-Vis region were calculated. The analysis of absorption coefficient near the fundamental absorption edge reveals that the optical band gaps are direct allowed transitions with values of 2.78 eV and 3.59 eV. The present copper (II) complex was screened for its antimicrobial activity against Staphylococcus Aureus and Bacillus Subtilis as Gram-positive bacteria, Escherichia Coli and Salmonella Typhimurium as Gram-negative bacteria and Candida Albicans as fungus strain

Efficient water disinfection with Ag2WO4-doped mesoporous g-C3N4 under visible light.

PubMed

Li, Yi; Li, Yanan; Ma, Shuanglong; Wang, Pengfei; Hou, Qianlei; Han, Jingjing; Zhan, Sihui

2017-09-15

Ag 2 WO 4 /g-C 3 N 4 composite photocatalyst was synthesized by polymerization of thiourea and ammonia chloride combined with the deposition-precipitation method, which was applied as an efficient visible-light driven photocatalyst for inactivating Escherichia coli (E. coli). The physicochemical properties of these photocatalysts were systematically characterized by various techniques such as SEM, TEM, XRD, FT-IR, BET, UV-vis DRS and PL. The synthesized photocatalysts exhibited outstandingly enhanced photocatalytic disinfection efficiency compared with that of pure g-C 3 N 4 and Ag 2 WO 4 under visible light. Furthermore, the optimal mass ratio of the Ag 2 WO 4 to g-C 3 N 4 was 5wt%, and a number of live bacteria could be completely inactivated with Ag 2 WO 4 (5%)/g-C 3 N 4 (100μg/mL) after 90min under visible light irradiation. The high disinfection efficiency is due to the synergetic effect between g-C 3 N 4 and Ag 2 WO 4 , including a good distribution of Ag 2 WO 4 particles on the surface of g-C 3 N 4 and an improved separation rate of photogenerated electron-hole pairs. The enhanced disinfection mechanism was also investigated using photogenerated current densities and electrochemical impedance spectroscopy (EIS). Considering the bulk availability and excellent disinfection activity of Ag 2 WO 4 /g-C 3 N 4 composite, it is a promising solar-driven photocatalyst for cleaning the microbial contaminated water. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of characteristics of montmorillonite supported nano zero valent iron (M-nZVI) and nano zero valent iron (nZVI)

NASA Astrophysics Data System (ADS)

How, Ho Kuok; Wan Zuhairi W., Y.

2015-09-01

In this study, synthesized montmorillonite supported nano zero valent iron (M-nZVI) and nano zero valent iron (nZVI) are compared physically and chemically. The samples were prepared using chemical reduction method that includes sodium borohydride and ethanol. Due to the tendency of nZVI to aggregate, montmorillonite is used as a supporting material. TEM and FESEM images show that the M-nZVI has decreased the aggregation by dispersing the particles on the surface of montmorillonite whereas images of nZVI show chain-like particle due to aggregation. Both images also show particles synthesized are nanoparticles. With less aggregation, the surface area of the M-nZVI is greater than nZVI which is 45.46 m2/g and 10.49 m2/g respectively. XRD patterns have shown Fe0 are synthesized and small amount of iron oxides are produced. M-nZVI has the capability in reducing aggregation which might lead to the increase in reactivity of the particles thus enhancing the performance of nZVI.

Photocatalytic selective hydroxylation of phenol to dihydroxybenzene by BiOI/TiO2 p-n heterojunction photocatalysts for enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Li, Bin; Chen, Xingwei; Zhang, Tianyong; Jiang, Shuang; Zhang, Guanghui; Wu, Wubin; Ma, Xiaoyuan

2018-05-01

The BiOI/TiO2 heterostructures with different Bi/Ti molar ratios were synthesized by biomimetic synthesis and simple hydrothermal method. XRD, SEM, TEM, N2 adsorption-desorption isotherms, XPS, UV-vis diffuse reflection spectra and photoluminescence spectra (PL) were employed to characterize the as-prepared photocatalysts and confirm the presence of p-n heterojunction. The photocatalytic activities of these photocatalysts were measured by photocatalytic selective hydroxylation of phenol with high concentration under simulated solar light irradiation. The results showed that BiOI/TiO2 heterostructure exhibited more excellent photocatalytic performance than the pure TiO2 and BiOI. Moreover, 20% BiOI/TiO2 heterostructure exhibited the highest photocatalytic performance, which can be ascribed to the exposed reactive facets, narrow band gap and effective separation of the photogenerated electrons and holes because of p-n heterojunction between BiOI and TiO2. The results of reusability tests indicated that the as-prepared photocatalysts have excellent photochemical stability. Furthermore, active-species trapping experiments were conducted to confirm the formation of radOH, which played a chief role in the process of photocatalytic selective hydroxylation of phenol. The charge transfer process of BiOI/TiO2 heterostructure and a possible mechanism for photocatalytic selective hydroxylation of phenol were proposed.

Laser pyrolysis fabrication of ferromagnetic gamma'-Fe4N and FeC nanoparticles

NASA Technical Reports Server (NTRS)

Grimes, C. A.; Qian, D.; Dickey, E. C.; Allen, J. L.; Eklund, P. C.

2000-01-01

Using the laser pyrolysis method, single phase gamma'-Fe4N nanoparticles were prepared by a two step method involving preparation of nanoscale iron oxide and a subsequent gas-solid nitridation reaction. Single phase Fe3C and Fe7C3 could be prepared by laser pyrolysis from Fe(CO)5 and 3C2H4 directly. Characterization techniques such as XRD, TEM and vibrating sample magnetometer were used to measure phase structure, particle size and magnetic properties of these nanoscale nitride and carbide particles. c2000 American Journal of Physics.

Preparation of C60(O)n-ZnO nanocomposite under electric furnace and photocatalytic degradation of organic dyes.

PubMed

Cho, Bum Hwi; Oh, Youn Jun; Mun, Sang Mi; Ko, Weon Bae

2012-07-01

Zinc oxide (ZnO) nanoparticles were synthesized sonochemically by applying ultrasonic irradiation to a mixed aqueous-alcoholic solution of zinc nitrate with sodium hydroxide at room temperature. The morphology and optical properties of the ZnO nanoparticles were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV-vis spectroscopy. The C60(O)n nanoparticles were synthesized by heating a mixture of C60 and 3-chloroperoxybenzoic acid in a benzene solvent under the reflux system. The heated C60(O)n-ZnO nanocomposite was synthesized in an electric furnace at 700 degrees C for two hours. The heated C60(O)n-ZnO nanocomposite was characterized by XRD, SEM, and TEM, and examined as a catalyst in the photocatalytic degradation of organic dyes by UV-vis spectroscopy. The photocatalytic effect of the heated C60(O)n-ZnO nanocomposite was evaluated by a comparison with that of unheated C60(O)n nanoparticles, heated C60(O)n nanoparticles, and unheated C60(O)n-ZnO in organic dyes, such as methylene blue (MB), methyl orange (MO), and rhodamine B (RhB) under ultraviolet light at 365 nm.

Enhanced visible light activity on direct contact Z-scheme g-C3N4-TiO2 photocatalyst

NASA Astrophysics Data System (ADS)

Li, Juan; Zhang, Min; Li, Qiuye; Yang, Jianjun

2017-01-01

Direct contact Z-scheme g-C3N4-TiO2 nanocomposites without an electron mediator are prepared via simple annealing the mixture of bulk g-C3N4 and nanotube titanic acid (NTA) in air at 600 °C for 2 h. In the process of annealing, the bulk g-C3N4 transformed to ultra-thin g-C3N4 nanosheets, and NTA converted to a novel anatase TiO2, then the two components formed a close interaction. The XPS result reveals that some amount of nitrogen is doped into this novel-TiO2, and g-C3N4 nanosheets exist in the composites. The results of XRD, TEM and TG indicate that the thickness of g-C3N4 nanosheets is very thin. The ESR spectrum shows the existence of Ti3+ and single-electron-trapped oxygen vacancy in the 30%g-C3N4-TiO2 composites. In photocatalytic activity test, the 30%g-C3N4-TiO2 nanocomposites showed an excellent photo-oxidation activity of propylene under visible light irradiation (λ≥ 420 nm), and the removal efficiency of propylene reached as high as 56.6%, and the activity kept nearly 82% after four consecutive recycles. Photoluminescence (PL) result using terephthalic acid (TA) as a probe molecule indicated that the g-C3N4-TiO2 nanocomposites displayed a Z-sheme photocatalytic reaction system and this should be the main reason for the high photocatalytic activity. A possible photocatalytic mechanism was proposed on the basis of PL result and transient photocurrent-time curves.

Spectral studies of 2-pyrazoline derivatives: structural elucidation through single crystal XRD and DFT calculations.

PubMed

Chinnaraja, D; Rajalakshmi, R; Srinivasan, T; Velmurugan, D; Jayabharathi, J

2014-04-24

A series of biologically active N-thiocarbamoyl pyrazoline derivatives have been synthesized using anhydrous potassium carbonate as the catalyst. All the synthesized compounds were characterized by FT-IR, (1)H NMR, (13)C NMR spectral studies, LCMS, CHN Analysis and X-ray diffraction analysis (compound 7). In order to supplement the XRD parameters, molecular modelling was carried out by Gaussian 03W. From the optimized structure, the energy, dipolemoment and HOMO-LUMO energies of all the systems were calculated. Copyright © 2014 Elsevier B.V. All rights reserved.

Recognition and Resistance in TEM [superscript beta]-Lactamase

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

Wang, Xiaojun; Minasov, George; Blazquez, Jesus

Developing antimicrobials that are less likely to engender resistance has become an important design criterion as more and more drugs fall victim to resistance mutations. One hypothesis is that the more closely an inhibitor resembles a substrate, the more difficult it will be to develop resistant mutations that can at once disfavor the inhibitor and still recognize the substrate. To investigate this hypothesis, 10 transition-state analogues, of greater or lesser similarity to substrates, were tested for inhibition of TEM-1 beta-lactamase, the most widespread resistance enzyme to penicillin antibiotics. The inhibitors were also tested against four characteristic mutant enzymes: TEM-30, TEM-32,more » TEM-52, and TEM-64. The inhibitor most similar to the substrate, compound 10, was the most potent inhibitor of the WT enzyme, with a K(i) value of 64 nM. Conversely, compound 10 was the most susceptible to the TEM-30 (R244S) mutant, for which inhibition dropped by over 100-fold. The other inhibitors were relatively impervious to the TEM-30 mutant enzyme. To understand recognition and resistance to these transition-state analogues, the structures of four of these inhibitors in complex with TEM-1 were determined by X-ray crystallography. These structures suggest a structural basis for distinguishing inhibitors that mimic the acylation transition state and those that mimic the deacylation transition state; they also suggest how TEM-30 reduces the affinity of compound 10. In cell culture, this inhibitor reversed the resistance of bacteria to ampicillin, reducing minimum inhibitory concentrations of this penicillin by between 4- and 64-fold, depending on the strain of bacteria. Notwithstanding this activity, the resistance of TEM-30, which is already extant in the clinic, suggests that there can be resistance liabilities with substrate-based design.« less

Photocatalytic degradation of pentachlorophenol in aqueous solution by visible light sensitive N-F-codoped TiO{sub 2} photocatalyst

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

Govindan, Kadarkarai, E-mail: govindanmu@gmail.com; Water Chemistry Lab, Water Institute, Karunya University, Coimbatore 641 114; Murugesan, Sepperumal

Graphical abstract: Schematic representation for the visible light photocatalytic process of N and F codoped TiO{sub 2}. Highlights: ► Visible light sensitive N-F-codoped TiO{sub 2}. ► Photocatalytic degradation of pentachlorophenol. ► Effect of oxidants on photocatalytic degradation of pentachlorophenol. ► PMS is a more efficient oxidant for the photodegradation of PCP. - Abstract: In this present study, N-F-codoped titanium dioxide nanocatalyst (NFTO) has been synthesized by simple sol–gel assisted solvothermal method for the effective utilization of visible light in photocatalytic reactions. Structural characterization of the photocatalyst is analyzed by XRD, UV–vis diffuse reflectance spectra (DRS), SEM and TEM. Moreover themore » chemical statuses of NFTO are gathered by X-ray photoelectron spectroscopy (XPS). The results show that a high surface area with photoactive anatase phase crystalline is obtained. In addition, nitrogen and fluorine atoms are doped into TiO{sub 2} crystal lattice to extend the visible light absorption and higher photocatalytic activity. The photocatalytic degradation of pentachlorophenol in aqueous solution is examined under visible light irradiation, the addition of oxidants such as PMS, PDS and H{sub 2}O{sub 2} is analyzed in detail. The rate of photocatalytic degradation of pentachlorophenol is obtained in the following order: PMS > PDS > H{sub 2}O{sub 2}.« less

Quantitative energy-filtered TEM imaging of interfaces

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

Bentley, J.; Kenik, E.A.; Siangchaew, K.

Quantitative elemental mapping by inner shell core-loss energy-filtered transmission electron microscopy (TEM) with a Gatan Imaging Filter (GIF) interfaced to a Philips CM30 TEM operated with a LaB{sub 6} filament at 300 kV has been applied to interfaces in a range of materials. In sensitized type 304L stainless steel aged 15 h at 600{degrees}C, grain-boundary Cr depletion occurs between Cr-rich intergranular M{sub 23}C{sub 6} particles. Images of net Cr L{sub 23} intensity show segregation profiles that agree quantitatively with focused-probe spectrum-line measurements recorded with a Gatan PEELS on a Philips EM400T/FEG (0.8 nA in 2-nm-diam probe) of the same regions.more » Rare-earth oxide additives that are used for the liquid-phase sintering of Si{sub 3}N{sub 4} generate second phases of complex composition at grain boundaries and edges. These grain boundary phases often control corrosion, crack growth and creep damage behavior. High resolution imaging has been widely and with focused probes can be compromised by beam damage, but elemental mapping by EFTEM appears not to cause appreciable beam damage.« less

Size-controlled synthesis of NiFe2O4 nanospheres via a PEG assisted hydrothermal route and their catalytic properties in oxidation of alcohols by periodic acid

NASA Astrophysics Data System (ADS)

Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar

2016-05-01

A novel and facile approach for synthesis of spinel nickel ferrites (NiFe2O4) nanoparticles (NPs) employing homogeneous chemical precipitation followed by hydrothermal heating is reported. The synthesis involves use of tributylamine (TBA) as a hydroxylating agent in synthesis of nickel ferrites. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized NiFe2O4 NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption-desorption isotherm (BET) and vibrating sample magnetometry (VSM). The XRD pattern revealed formation of cubic face-centered NiFe2O4 and TEM image showed spherical particles of sizes 2-10 nm. These NiFe2O4 NPs were used as magnetically recoverable catalyst in oxidation of cyclic alcohols to their corresponding aldehydes by periodic acid. This eco-friendly procedure affords products in very high yield and selectivity. The reusability of the catalyst is proved to be noteworthy as the material exhibits no significant changes in its catalytic activity even after five cycles of reuse.

Potassium ions intercalated into g-C3N4-modified TiO2 nanobelts for the enhancement of photocatalytic hydrogen evolution activity under visible-light irradiation

NASA Astrophysics Data System (ADS)

Ma, Jian; Zhou, Wei; Tan, Xin; Yu, Tao

2018-05-01

Solar-to-chemical energy conversion is a challenging photochemical reaction for renewable energy storage. In recent decades, photocatalytic H2 evolution has been studied extensively. TiO2 is a well-established semiconductor in the field of photocatalytic H2 production; however, its low efficiency for solar energy utilization, and high photocarrier recombination rate, restrict its photocatalytic efficiency. Here, a series of K-intercalated g-C3N4-modified TiO2 nanobelts (TCN–Kx) with different dosages of K atoms were fabricated using a hydrothermal method followed by a calcination process. XRD, TEM and XPS tests indicate that a tight interfacial connection is formed between K–g-C3N4 and the TiO2 nanobelts. DFT calculations indicated that K dopants prefer to be at the interlayer sites of g-C3N4, suggesting increased charge transfer efficiency. The H2 production efficiency of the TCN–Kx composite materials from water splitting under visible-light irradiation was clearly improved. Steady fluorescence spectroscopy and photocurrent measurements confirmed that the improvement in photocatalytic H2 production activity was due to the superior charge separation and electron transfer efficiency of TCN–Kx composite materials.

Potassium ions intercalated into g-C3N4-modified TiO2 nanobelts for the enhancement of photocatalytic hydrogen evolution activity under visible-light irradiation.

PubMed

Ma, Jian; Zhou, Wei; Tan, Xin; Yu, Tao

2018-05-25

Solar-to-chemical energy conversion is a challenging photochemical reaction for renewable energy storage. In recent decades, photocatalytic H 2 evolution has been studied extensively. TiO 2 is a well-established semiconductor in the field of photocatalytic H 2 production; however, its low efficiency for solar energy utilization, and high photocarrier recombination rate, restrict its photocatalytic efficiency. Here, a series of K-intercalated g-C 3 N 4 -modified TiO 2 nanobelts (TCN-Kx) with different dosages of K atoms were fabricated using a hydrothermal method followed by a calcination process. XRD, TEM and XPS tests indicate that a tight interfacial connection is formed between K-g-C 3 N 4 and the TiO 2 nanobelts. DFT calculations indicated that K dopants prefer to be at the interlayer sites of g-C 3 N 4 , suggesting increased charge transfer efficiency. The H 2 production efficiency of the TCN-Kx composite materials from water splitting under visible-light irradiation was clearly improved. Steady fluorescence spectroscopy and photocurrent measurements confirmed that the improvement in photocatalytic H 2 production activity was due to the superior charge separation and electron transfer efficiency of TCN-Kx composite materials.

Structural, magnetic and electronic structural properties of Mn doped CeO2 nanoparticles

NASA Astrophysics Data System (ADS)

Kumari, Kavita; Vij, Ankush; Hashim, Mohd.; Chae, K. H.; Kumar, Shalendra

2018-05-01

Nanoparticles of Ce1-xMnxO2, (x=0.0, 0.01, and 0.05) have been synthesized by using co-precipitation method, and then characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), near edge x-ray absorption fine structure (NEXAFS) spectroscopy and dc magnetization measurements. XRD results clearly showed that the all the samples have single phase nature and exclude the presence of any secondary phase. The average particle size calculated using XRD TEM measurements found to decrease with increase in Mn doping in the range of 4.0 - 9.0 nm. The structural parameters such as strain, interplaner distance and lattice parameter is observed to decrease with increase in doping. The morphology of Ce1-xMnxO2 nanoparticles measured using TEM micrographs indicate that nanoparticle have spherical shape morphology. Magnetic hysteresis curve for Ce1-xMnxO2, (x = 0.0, 0.01, and 0.05) confirms the ferromagnetic ordering room temperature. The value of saturation magnetization is observed to decrease with increase in temperature from 10 K to 300 K. The NEXAFS spectra measured at Ce M4,5 edge reveals that Ce-ions are in +4 valance state.

High temperature XRD of Cu{sub 2.1}Zn{sub 0.9}SnSe{sub 4}

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

Chetty, Raju, E-mail: rcmallik@physics.iisc.ernet.in; Mallik, Ramesh Chandra, E-mail: rcmallik@physics.iisc.ernet.in

2014-04-24

Quaternary compound with chemical composition Cu{sub 2.1}Zn{sub 0.9}SnSe{sub 4} is prepared by solid state synthesis. High temperature XRD (X-Ray Diffraction) of this compound is used in studying the effect of temperature on lattice parameters and thermal expansion coefficients. Thermal expansion coefficient is one of the important quantities in evaluating the Grüneisen parameter which further useful in determining the lattice thermal conductivity of the material. The high temperature XRD of the material revealed that the lattice parameters as well as thermal expansion coefficients of the material increased with increase in temperature which confirms the presence of anharmonicty.

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.

TiO{sub 2}/N-graphene nanocomposite via a facile in-situ hydrothermal sol–gel strategy for visible light photodegradation of eosin Y

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

Liu, Yingliang; Pei, Fuyun, E-mail: xusg@zzu.edu.cn; Lu, Ruijuan

2014-12-15

Highlights: • TiO{sub 2}/N-graphene is synthesized via in-situ hydrothermal sol–gel strategy. • TiO{sub 2} nanoparticles are chemically anchored on N-graphene nanosheets. • The band gap of TiO{sub 2}/N-graphene is red-shifted from neat TiO{sub 2} nanoparticles. • 5-NGT nanocomposite has the best visible light photodegradation performance. - Abstract: TiO{sub 2}/N-graphene nanocomposites are synthesized via a facile in-situ hydrothermal sol–gel strategy in order to improve the photocatalytic efficiency for pollutant photodegradation under visible light irradiation. The as-prepared nanocomposites are respectively characterized by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and UV–vis diffuse reflectance spectroscopy. Results indicated that neatmore » TiO{sub 2} nanoparticles have an average diameter about 6.70 nm while TiO{sub 2} nanoparticles in TiO{sub 2}/N-graphene nanocomposites synthesized through in-situ hydrothermal sol–gel strategy bear an average diameter of ∼1 nm and are anchored on N-graphene nanosheets via chemical bonding. Both neat TiO{sub 2} nanoparticles and chemically anchored TiO{sub 2} nanoparticles in TiO{sub 2}/N-graphene nanocomposites take on the crystal type of anatase. The band gap of TiO{sub 2}/N-graphene nanocomposites is red-shifted compared with neat TiO{sub 2} nanoparticles. The evaluation of photodegradation performance under visible light irradiation suggested that the nanocomposite with 5 wt% N-graphene content has the best visible light photodegradation performance.« less

FTIR, XRD and DSC studies of nanochitosan, cellulose acetate and polyethylene glycol blend ultrafiltration membranes.

PubMed

Vinodhini, P Angelin; K, Sangeetha; Thandapani, Gomathi; P N, Sudha; Jayachandran, Venkatesan; Sukumaran, Anil

2017-11-01

In the present work, a series of novel nanochitosan/cellulose acetate/polyethylene glycol (NCS/CA/PEG) blend flat sheet membranes were fabricated in different ratios (1:1:1, 1:1:2, 2:1:1, 2:1:2, 1:2:1, 2:2:1) in a polar solvent of N,N'-dimethylformamide (DMF) using the most popular phase inversion method. Nanochitosan was prepared by the ionotropic gelation method and its average particle size has been analyzed using Dynamic Light Scattering (DLS) method. The effect of blending of the three polymers was investigated using FTIR and XRD studies. FTIR results confirmed the formation of well-blended membranes and the XRD analysis revealed enhanced amorphous nature of the membrane ratio 2:1:2. DSC study was conducted to find out the thermal behavior of the blend membranes and the results clearly indicated good thermal stability and single glass transition temperature (T g ) of all the prepared membranes. Asymmetric nature and rough surface morphology was confirmed using SEM analysis. From the results it was evident that the blending of the polymers with higher concentration of nanochitosan can alter the nature of the resulting membranes to a greater extent and thus amorphous membranes were obtained with good miscibility and compatibility. Copyright © 2017 Elsevier B.V. All rights reserved.

Structural and magnetic characterizations of Co2FeGa/SiO2 nanoparticles prepared via chemical route

NASA Astrophysics Data System (ADS)

Priyanka, Dhaka, Rajendra S.

2018-04-01

We report the synthesis of Co2FeGa/SiO2 nanoparticles by sol-gel method and characterization usingx-ray diffraction (XRD), transmission electron microscopy (TEM) and magnetic measurements. The Rietveld refinementsof XRD data with space group Fm-3m clearly show the formation of A2 disordersingle phase and the lattice constant isfound to be 5.738 Å. The energy-dispersive x-ray spectroscopy (EDX) confirm the elemental composition close the desired values. The value of coercivity is found to be around 283 Oe and 126 Oe, measured at 10 K and 300 K, respectively. We observed the saturation magnetization significantly lower than expected from Slater-Pauling rule. This decrease in the magnetic moment might be due to the presence of amorphous SiO2 during the synthesis process. A large content of small size SiO2 particles along with Co2FeGa nanoparticles are also found in TEM study.

Influence of tumor microenvironment on prognosis in colorectal cancer: Tissue architecture-dependent signature of endosialin (TEM-1) and associated proteins

PubMed Central

O'Shannessy, Daniel J.; Somers, Elizabeth B.; Chandrasekaran, Lakshmi K.; Nicolaides, Nicholas C.; Bordeaux, Jennifer; Gustavson, Mark D.

2014-01-01

Tumor survival is influenced by interactions between tumor cells and the stromal microenvironment. One example is Endosialin (Tumor Endothelial Marker-1 (TEM-1) or CD248), which is expressed primarily by cells of mesenchymal origin and some tumor cells. The expression, as a function of architectural masking, of TEM-1 and its pathway-associated proteins was quantified and examined for association with five-year disease-specific survival on a colorectal cancer (CRC) cohort divided into training (n=330) and validation (n=164) sets. Although stromal expression of TEM-1 had prognostic value, a more significant prognostic signature was obtained through linear combination of five compartment-specific expression scores (TEM-1 Stroma, TEM-1 Tumor Vessel, HIF2α Stromal Vessel, Collagen IV Tumor, and Fibronectin Stroma). This resulted in a single continuous risk score (TAPPS: TEM-1 Associated Pathway Prognostic Signature) which was significantly associated with decreased survival on both the training set [HR=1.76 (95%CI: 1.44-2.15); p<0.001] and validation set [HR=1.38 (95%CI: 1.02-1.88); p=0.04]. Importantly, since prognosis is a critical clinical question in Stage II patients, the TAPPS score also significantly predicted survival in the Stage II patient (n=126) cohort [HR=1.75 (95%CI: 1.22-2.52); p=0.002] suggesting the potential of using the TAPPS score to assess overall risk in CRC patients, and specifically in Stage II patients. PMID:24980818

TEM prospection on quaternary faults: the case of San Ramón Fault (SRF), Central Chile

NASA Astrophysics Data System (ADS)

Estay, N. P.; Yanez, G. A.; Maringue, J. I.

2016-12-01

Quaternary faults are relevant study objects in geosciences to better estimation of seismic risk. Nowadays main efforts are focused on the improvement of paleoseismology and geophysics techniques. At this regard, we present here a TEM prospection of the San Ramón quaternary fault in the southern Andes. This fault has no record of historic activation, however, given its proximity to the Chilean capital, hazardous estimate is mandatory. Evidences of the SRF are restricted to geomorphologic features, and associated secondary faults on the hanging wall block, but any outcrop of the main fault have been identified. To observe the main fault in the basement rock, cover by a 30-100 m sedimentary basin, we carried out a TEM experiment. The best advantage of the TEM methodology compared to other near-surface electrical methods is it capacity to reach greater penetration depth compared to its spatial sampling rate. Taking this advantage, we define a 25x25 m transmitter loop (Tx) and 5x5 m receiver loop (Rx), allowing the suitable resolution to observe the fault core. To reach a deeper penetration depth but keeping high resolution of the shallow parts, we made two complementary measurements, the first with one-turn transmitter loop, and the second with 4-turn transmitter loops, to resolve the early and late times properly. As result we define vertical profiles of 100-150m depth, and including 48 measures (24 of one-turn transmitter loop, and 24 of four-turn transmitter loop), the resulting pseudo 2D image is a 500m profile with depth extent of 150m. In this section we can observe different resistivity domain, with a horizontal continuity in many measures. The experiment allows to cross the sedimentary cover, and observe the top of the basement rock. In the rock domain, it can be observed a high resistivity body, interpreted as a pristine rock, and some extremely low resistivity bodies, that are interpreted as a fractured rock saturated with water, and eventually mapping a

MoS2 quantum dots decorated g-C3N4/Ag heterostructures for enhanced visible light photocatalytic activity

NASA Astrophysics Data System (ADS)

Fu, Yanhui; Liang, Wei; Guo, Jinqiu; Tang, Hua; Liu, Shuaishuai

2018-02-01

A novel MoS2 quantum dots (QDs) decorated g-C3N4/Ag heterostructured photocatalyst has been synthesized via a two-step method including in situ microemulsion-assisted reduction and wetness impregnation method. The obtained heterostructure photocatalyst was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (DRS) and photoluminescence spectrosxopy (PL). The photocatalytic activity was evaluated by the degradation of methyl orange (MO) under visible-light irradiation. The MoS2 QDs decorated hybrid photocatalysts exhibited significantly enhanced photocatalytic performance. The concentration of Ag and MoS2 QDs showing the optimal photocatalytic performance was determined to be 10% and 0.3% respectively, which exceeded the photocatalytic performance of pure g-C3N4 by more than 4.7 times. Recycling experiments confirmed that the hybrid catalysts had superior cycle performance and stability. The enhanced photocatalytic activity of MoS2 QDs decorated g-C3N4/Ag hybrid photocatalysts can be mainly ascribed to enhanced visible-light absorption, the efficient separation of photogenerated charge carriers and the stronger oxidation and reduction ability through a Z-scheme system composed of g-C3N4, Ag and MoS2 QDs, in which Ag nanoparticles act as the charge separation center. The evidence of the Z-scheme photocatalytic mechanism of the composite photocatalysts was obtained from the active species trapping experiments.

Fabricaion of improved novel p–n junction BiOI/Bi{sub 2}Sn{sub 2}O{sub 7} nanocomposite for visible light driven photocatalysis

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

Xu, Weicheng; Fang, Jianzhang, E-mail: fangjzh@scnu.edu.cn; Guangdong Technology Research Center for Ecological Management and Remediation of Urban Water System, Guangzhou 510006

2015-12-15

Graphical abstract: - Highlights: • A p–n heterojunction photocatalyst BiOI/Bi{sub 2}Sn{sub 2}O{sub 7} was prepared by hydrothermal method. • 4% BiOI/Bi{sub 2}Sn{sub 2}O{sub 7} with maximal photocatalytic degradation efficiency (RhB) of 99.9%. • A specific degradation routes of RhB was illustrated. • The photocatalytic mechanism is discussed according to p–n junction principles. • • O{sub 2}{sup −} and h+ are the main reactive species for the degradation of RhB. - Abstract: A series of novel p−n junction photocatalysts BiOI/Bi{sub 2}Sn{sub 2}O{sub 7} (BiOI/BSO) were successfully fabricated via a facile hydrothermal method. The phase structures, morphologies and optical properties of themore » as-prepared samples were studied by XRD, TEM, HRTEM, BET, XPS, UV–vis DRS and photoluminescence (PL) spectroscopy. The results showed that BiOI/BSO heteronanostructures displayed much higher photocatalytic activity than pure BSO and BiOI for the degradation of rhodamine B (RhB). The best photocatalytic activity of BiOI/BSO with almost 99.9% RhB degradation situated at molar percentage ratio of 4% after 6 h irradiation. The enhanced photocatalytic performance of BiOI/BSO could be mainly attributed to the formation of the heterojunction between p-BiOI and n-BSO, which effectively restrains the recombination of photoinduced electron–hole pairs. Moreover, the study of radical scavengers affirmed that h{sup +} and • O{sub 2}{sup −} were the primary reactive species for the degradation of RhB.« less

Compressive Classification for TEM-EELS

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

Hao, Weituo; Stevens, Andrew; Yang, Hao

Electron energy loss spectroscopy (EELS) is typically conducted in STEM mode with a spectrometer, or in TEM mode with energy selction. These methods produce a 3D data set (x, y, energy). Some compressive sensing [1,2] and inpainting [3,4,5] approaches have been proposed for recovering a full set of spectra from compressed measurements. In many cases the final form of the spectral data is an elemental map (an image with channels corresponding to elements). This means that most of the collected data is unused or summarized. We propose a method to directly recover the elemental map with reduced dose and acquisitionmore » time. We have designed a new computational TEM sensor for compressive classification [6,7] of energy loss spectra called TEM-EELS.« less

Sequestration of Ag(I) from aqueous solution as Ag(0) nanostructures by nanoscale zero valent iron (nZVI)

NASA Astrophysics Data System (ADS)

Zhang, Yalei; Yan, Jing; Dai, Chaomeng; Li, Yuting; Zhu, Yan; Zhou, Xuefei

2015-11-01

This study investigates the application of nanoparticle zero valent iron (nZVI) to sequester Ag(I) as Ag(0) nanostructures from aqueous solution. Batch experiments were performed with nZVI exposed to aqueous Ag(I) to investigate the effects of environmental parameters, including nZVI dose, temperature and pH. High temperature facilitates Ag(I) sequestration, and the rate constants are determined to be 0.02, 0.12, and 0.31 mg L/m2 at 30, 50, and 60 °C, respectively. Ag(I) sequestration was adversely affected by adding nitric acid to the solution due to significant acid washing, decreasing the available nZVI active sites. Characterization techniques including TEM, XRD, and HR-XPS revealed that nZVI is oxidized to lepidocrocite and magnetite/maghemite and confirmed the formation of nanocrystalline silver. HR-XPS analysis indicated that Ag2O forms rapidly as an intermediate due to Ag(I) adsorption onto the FeOOH layer. The Ag(0) nanostructures that are formed are fractal, spherical, and dendritic or rod-like, respectively, in morphology by FE-TEM images at different Ag/Fe mass ratios. A general reaction model for the interaction Ag(I) with nZVI is proposed. Our results suggest that nZVI is effective for Ag(I) removal.

Radiation-Induced Changes in Quartz, A Mineral Analog of Nuclear Power Plant Concrete Aggregates.

PubMed

Silva, Chinthaka M; Rosseel, Thomas M; Kirkegaard, Marie C

2018-03-19

Quartz single-crystal samples consisting of α-quartz crystal structure were neutron irradiated to fluences of 5 × 10 18 , 4 × 10 19 , and 2 × 10 20 n/cm 2 (E > 0.1 MeV) at two temperatures (52 and 95 °C). The changes in the α-quartz phase as a function of these two conditions (temperature and fluence) were studied using X-ray powder diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM), and the results acquired using these complementary techniques are presented in a single place for the first time. XRD studies showed that the lattice parameters of α-quartz increased with increasing neutron flux. The lattice growth was larger for the samples that were neutron irradiated at 52 °C than at 95 °C. Moreover, an amorphous content was determined in the quartz samples neutron irradiated at 4 × 10 19 n/cm 2 , with the greater amount being in the 52 °C irradiated sample. Complete amorphization of quartz was observed at a fluence of 2 × 10 20 n/cm 2 (E > 0.1 MeV) using XRD and confirmed by TEM characterization and Raman spectroscopic studies. The cause for α-quartz lattice expansion and sample amorphization was also explored using XRD and Raman spectroscopic studies.

Influence of N2 partial pressure on structural and microhardness properties of TiN/ZrN multilayers deposited by Ar/N2 vacuum arc discharge

NASA Astrophysics Data System (ADS)

Naddaf, M.; Abdallah, B.; Ahmad, M.; A-Kharroub, M.

2016-08-01

The influence of N2 partial pressure on structural, mechanical and wetting properties of multilayered TiN/ZrN thin films deposited on silicon substrates by vacuum arc discharge of (N2 + Ar) gas mixtures is investigated. X-ray diffraction (XRD) results show that the average texturing coefficient of (1 1 1) orientation and the grain size of both TiN and ZrN individual layers increase with increasing the N2 partial pressure. The Rutherford back scattering (RBS) measurements and analysis reveal that incorporation of the nitrogen in the film increases with increasing the N2 partial pressure and both TiN and ZrN individual layers have a nitrogen over-stoichiometry for N2 partial pressure ⩾50%. The change in the film micro-hardness is correlated to the changes in crystallographic texture, grain size, stoichiometry and the residual stress in the film as a function of the N2 partial pressure. In particular, stoichiometry of ZrN and TiN individual is found to play the vital role in determining the multilayer hardness. The multilayer film deposited at N2 partial pressure of 25% has the best stoichiometric ratio of both TiN and ZrN layers and the highest micro-hardness of about 32 GPa. In addition, water contact angle (WCA) measurements and analysis show a decrease in the work of adhesion on increasing the N2 partial pressure.

Research of obtaining TiO2 by sol-gel method using titanium isopropoxide TIP and tetra-n-butyl orthotitanate TNB

NASA Astrophysics Data System (ADS)

Gómez de Salazar, J. M.; Nutescu Duduman, C.; Juárez Gonzalez, M.; Palamarciuc, I.; Barrena Pérez, M. I.; Carcea, I.

2016-08-01

Titanium dioxide crystallises in three polymorphs: anatase, rutile and brookite. Rutile is most stable form of the TiO2 polymorphs. In this paper we concentrate on obtaining rutile and anatase, both used in various applications. The chosen method is sol-gel, which is a reliable method used for obtaining titanium oxides. We prepared titanium dioxide with using titanium isopropoxide (TIP) with chemical construction (C12H28O4Ti) and tetra-n-butyl orthotitanate (TNB) with chemical construction (C16H36O4Ti). The experiments were carried out in order to compare the results of the samples with similar reaction conditions, but with different precursors, thus concluding which precursor gives best results. Using different analysis techniques as X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Thermogravimetric Analysis (TGA) we characterised the samples morphologically and structurally.

Preparation and characterization of NiW-nHA composite catalyst for hydrocracking

NASA Astrophysics Data System (ADS)

Zhou, Gang; Hou, Yongzhao; Liu, Lei; Liu, Hongru; Liu, Can; Liu, Jing; Qiao, Huiting; Liu, Wenyong; Fan, Yubo; Shen, Shituan; Rong, Long

2012-11-01

The synthesis, characterization and catalytic capability of the NiW-nano-hydroxyapatite (NiW-nHA) composite were investigated in this paper. The NiW-nHA catalyst was prepared by a co-precipitation method. Then Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive spectroscopy (EDX) were used to analyze this material. In addition, the catalytic capacity of the NiW-nHA composite was also examined by FT-IR and gas chromatography (GC). The results of FT-IR analysis indicated that Ni, W and nHA combined closely. TEM observation revealed that this catalyst was needle shaped and the crystal retained a nanometer size. XRD data also suggested that a new phase of CaWO4 appeared and the lattice parameters of nHA changed in this system. nHA was the carrier of metals. The rates of Ni/W-loading were 73.24% and 65.99% according to the EDX data, respectively. Furthermore, the conversion of 91.88% Jatropha oil was achieved at 360 °C and 3 MPa h-1 over NiW-nHA catalyst. The straight chain alkanes ranging from C15 to C18 were the main components in the production. The yield of C15-C18 alkanes was up to 83.56 wt%. The reaction pathway involved hydrocracking of the C&z.dbd;C bonds of these triglycerides from Jatropha oil. This paper developed a novel non-sulfided catalyst to obtain a ``green biofuel'' from vegetable oil.

Fabrication of multilayered Ge nanocrystals embedded in SiO xGeN y films

NASA Astrophysics Data System (ADS)

Gao, Fei; Green, Martin A.; Conibeer, Gavin; Cho, Eun-Chel; Huang, Yidan; Perez-Wurfl, Ivan; Flynn, Chris

2008-09-01

Multilayered Ge nanocrystals embedded in SiO xGeN y films have been fabricated on Si substrate by a (Ge + SiO 2)/SiO xGeN y superlattice approach, using a rf magnetron sputtering technique with a Ge + SiO 2 composite target and subsequent thermal annealing in N 2 ambient at 750 °C for 30 min. X-ray diffraction (XRD) measurement indicated the formation of Ge nanocrystals with an average size estimated to be 5.4 nm. Raman scattering spectra showed a peak of the Ge-Ge vibrational mode downward shifted to 299.4 cm -1, which was caused by quantum confinement of phonons in the Ge nanocrystals. Transmission electron microscopy (TEM) revealed that Ge nanocrystals were confined in (Ge + SiO 2) layers. This superlattice approach significantly improved both the size uniformity of Ge nanocrystals and their uniformity of spacing on the 'Z' growth direction.

Chemical and morphological characterization of TSP and PM2.5 by SEM-EDS, XPS and XRD collected in the metropolitan area of Monterrey, Mexico

NASA Astrophysics Data System (ADS)

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

2016-10-01

Total suspended particles (TSP) and particles smaller than 2.5 μm (PM2.5) were collected at four sites in the metropolitan area of Monterrey (MAM) in Mexico. The samples were characterized by X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), and Scanning Electron Microscopy (SEM). In order to determine the possible sources of emissions of atmospheric particulate matter, a principal component analysis (PCA) was performed. The XRD results showed that the major crystalline compounds found in the TPS were CaCO3 and SiO2; while in the PM2.5 CaSO4 was found. The XPS analysis showed that the main elements found on the surface of the particles were C, O, Si, Ca, S, and N. The deconvolution carried out on the high-resolution spectra for C1s, S2p and N1s, showed that the aromatics, sulfates and pyrrolic-amides were the main groups contributing to the signal of these elements, respectively. The C-rich particles presented a spherical morphology, while the Ca- and Si-based particles mostly showed a prismatic shape. The PCA analysis together with the results obtained from the characterization techniques, suggested that the main contributors to the CaCO3 particles collected in the PM were most probably produced and emitted into the atmosphere by local construction industries and exploitation of rich-deposits of calcite. Meanwhile, the SiO2 found in the MAM originated from the suspension of geological material abundant in the region, and the carbon particles were mainly produced by the combustion of fossil fuels.

Novel microwave-assisted synthesis of porous g-C3N4/SnO2 nanocomposite for solar water-splitting

NASA Astrophysics Data System (ADS)

Seza, A.; Soleimani, F.; Naseri, N.; Soltaninejad, M.; Montazeri, S. M.; Sadrnezhaad, S. K.; Mohammadi, M. R.; Moghadam, H. Asgari; Forouzandeh, M.; Amin, M. H.

2018-05-01

Highly porous nanocomposites of graphitic-carbon nitride and tin oxide (g-C3N4/SnO2) were prepared through simple pyrolysis of urea molecules under microwave irradiation. The initial amount of tin was varied in order to investigate the effect of SnO2 content on preparation and properties of the composites. The synthesized nanocomposites were well-characterized by XRD, FE-SEM, HR-TEM, BET, FTIR, XPS, DRS, and PL. A homogeneous distribution of SnO2 nanoparticles with the size of less than 10 nm on the porous C3N4 sheets could be obtained, suggesting that in-situ synthesis of SnO2 nanoparticles was responsible for the formation of g-C3N4. The process likely occurred by the aid of the large amounts of OH groups formed on the surfaces of SnO2 nanoparticles during the polycondensation reactions of tin derivatives which could facilitate the pyrolysis of urea to carbon nitride. The porous nanocomposite prepared with initial tin amount of 0.175 g had high specific surface area of 195 m2 g-1 which showed high efficiency photoelectrochemical water-splitting ability. A maximum photocurrent density of 33 μA cm-2 was achieved at an applied potential of 0.5 V when testing this nanocomposite as photo-anode in water-splitting reactions under simulated visible light irradiation, introducing it as a promising visible light photoactive material.

Multiscale structural characterizations of mixed U(iv)-An(iii) oxalates (An(iii) = Pu or Am) combining XAS and XRD measurements.

PubMed

Arab-Chapelet, B; Martin, P M; Costenoble, S; Delahaye, T; Scheinost, A C; Grandjean, S; Abraham, F

2016-04-28

Mixed actinide(III,IV) oxalates of the general formula M2.2UAn(C2O4)5·nH2O (An = Pu or Am and M = H3O(+) and N2H5(+)) have been quantitatively precipitated by oxalic precipitation in nitric acid medium (yield >99%). Thorough multiscale structural characterization using XRD and XAS measurements confirmed the existence of mixed actinide oxalate solid solutions. The XANES analysis confirmed that the oxidation states of the metallic cations, tetravalent for uranium and trivalent for plutonium and americium, are maintained during the precipitation step. EXAFS measurements show that the local environments around U(+IV), Pu(+III) and Am(+III) are comparable, and the actinides are surrounded by ten oxygen atoms from five bidentate oxalate anions. The mean metal-oxygen distances obtained by XAS measurements are in agreement with those calculated from XRD lattice parameters.

Synthesis, spectroscopic (UV-Vis, FT-IR and NMR), single crystal XRD of 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate: A comprehensive experimental and computational study

NASA Astrophysics Data System (ADS)

Arockia doss, M.; Rajarajan, G.; Thanikachalam, V.; Selvanayagam, S.; Sridhar, B.

2017-01-01

A piperidin-4-one containing picrate 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate [3,5-DPPP] was synthesized. The molecular structure of 3,5-DPPP was confirmed by FT-IR, NMR, Uv-Vis, single crystal XRD analysis and DFT and HF methods with 6-31G(d,p) basis set. The XRD data confirm the transfer of protons from picric acid (O2) to piperidin-4-one ring (N1). The 3,5-DPPP compound is stabilized by the presence of intermolecular and intramolecular hydrogen bonds (N-H⋯O, C-H⋯S and C-H⋯O). Density functional theory and HF calculations have been used widely for calculating a wide variety of molecular properties such as optimized structure, FT-IR and Uv-Vis spectra, and provided reliable results which are in agreement with experimental data. The charge density data have been used to understand the properties of molecular systems. Furthermore, several quantum chemical insights have been obtained in the form of the total and partial density of states, the HOMO-LUMO energy gap and electrostatic potential map etc. In addition, the polarizability and first hyperpolarizability were calculated to show the potential applications of 3,5-DPPP in nonlinear optics.

High temperature XRD of Cu{sub 2}GeSe{sub 3}

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

Premkumar, D. S.; Malar, P.; Chetty, Raju

2015-06-24

The Cu{sub 2}GeSe{sub 3} is prepared by solid state synthesis method. The high temperature XRD has been done at different temperature from 30 °C to 450 °C. The reitveld refinement confirms Cu{sub 2}GeSe{sub 3} phase and orthorhombic crystal structure. The lattice constants are increasing with increase in the temperature and their rate of increase with respect to temperature are used for finding the thermal expansion coefficient. The calculation of the linear and volume coefficient of thermal expansion is done from 30 °C to 400 °C. Decrease in the values of linear expansion coefficients with temperature are observed along a andmore » c axis. Since thermal expansion coefficient is the consequence of the distortion of atoms in the lattice; this can be further used to find the minimum lattice thermal conductivity at given temperature.« less

Effects of calcining temperature on formation of hierarchical TiO2/g-C3N4 hybrids as an effective Z-scheme heterojunction photocatalyst

NASA Astrophysics Data System (ADS)

Lu, Lianying; Wang, Guohong; Zou, Min; Wang, Juan; Li, Jun

2018-05-01

Hierarchical TiO2/g-C3N4 heterojunction photocatalysts with well-defined multiscale porous TiO2 framework are synthesized by simply calcinating tetrabutyl titanate and melamine precursors. The samples have been characterized by XRD, XPS, SEM, TEM, FTIR, nitrogen absorption-desorption equipment and TGA. The photocatalytic activity of these samples has been investigated in photo-degradation of Rhodamine B (RhB). The results show that calcining temperature critically affects the microstructure, surface area, interface structure and catalytic properties of the prepared samples. At the optimal calcining temperature of 550 °C, the apparent reaction rate constant of the catalyst is 55.0 × 10-3 min-1, which is 16.2 fold of pure TiO2 (3.4 × 10-3 min-1) and 3.4 fold of pure g-C3N4 (16.4 × 10-3 min-1), respectively. The strengthened visible-light-driven photocatalytic activity is attributed to the formation of a unique Z-scheme TiO2/g-C3N4 heterojunction due to C- or N-doping at the surface of the porous TiO2 framework. This mechanism explains the observation in a series of radical trapping experiments that superoxide ions and photo-generated holes play major roles in the photo-decolorizing process while hydroxyl radicals are also involved with a minor role.

A 4-(o-chlorophenyl)-2-aminothiazole: Microwave assisted synthesis, spectral, thermal, XRD and biological studies

NASA Astrophysics Data System (ADS)

Rajmane, S. V.; Ubale, V. P.; Lawand, A. S.; Nalawade, A. M.; Karale, N. N.; More, P. G.

2013-11-01

A 4-(o-chlorophenyl)-2-aminothiazole (CPAT) has been synthesized by reacting o-chloroacetophenone, iodine and thiourea under microwave irradiation as a green chemistry approach. The reactions proceed selectively and within a couple of minutes giving high yields of the products. The compound was characterized by elemental, spectral (UV-visible, IR, NMR and GC-MS), XRD and thermal analyses. The TG curve of the compound was analyzed to calculate various kinetic parameters (n, E, Z, ΔS and ΔG) by using Coats-Redfern (C.R.), MacCallum-Tanner (M.T.) and Horowitz-Metzger (H.M.) method. The compound was tested for the evaluation of antibacterial activity against B. subtilis and E. coli and antifungal activity against A. niger and C. albicans. The compound was evaluated for their in vitro nematicidal activity on plant parasitic nematode Meloidogyne javanica and molluscicidal activity on fresh water helminthiasis vector snail Lymnea auricularia. The compound is biologically active in very low concentration. X-ray diffraction study suggests a triclinic crystal system for the compound.

In-situ preparation of N-TiO2/graphene nanocomposite and its enhanced photocatalytic hydrogen production by H2S splitting under solar light.

PubMed

Bhirud, Ashwini P; Sathaye, Shivaram D; Waichal, Rupali P; Ambekar, Jalindar D; Park, Chan-J; Kale, Bharat B

2015-03-21

Highly monodispersed nitrogen doped TiO2 nanoparticles were successfully deposited on graphene (N-TiO2/Gr) by a facile in-situ wet chemical method for the first time. N-TiO2/Gr has been further used for photocatalytic hydrogen production using a naturally occurring abundant source of energy i.e. solar light. The N-TiO2/Gr nanocomposite composition was optimized by varying the concentrations of dopant nitrogen and graphene (using various concentrations of graphene) for utmost hydrogen production. The structural, optical and morphological aspects of nanocomposites were studied using XRD, UV-DRS, Raman, XPS, FESEM, and TEM. The structural study of the nanocomposite shows existence of anatase N-TiO2. Further, the details of the components present in the composition were confirmed with Raman and XPS. The morphological study shows that very tiny, 7-10 nm sized, N-TiO2 nanoparticles are deposited on the graphene sheet. The optical study reveals a drastic change in absorption edge and consequent total absorption due to nitrogen doping and presence of graphene. Considering the extended absorption edge to the visible region, these nanocomposites were further used as a photocatalyst to transform hazardous H2S waste into eco-friendly hydrogen using solar light. The N-TiO2/Gr nanocomposite with 2% graphene exhibits enhanced photocatalytic stable hydrogen production i.e. ∼5941 μmol h(-1) under solar light irradiation using just 0.2 gm nanocomposite, which is much higher as compared to P25, undoped TiO2 and TiO2/Gr nanocomposite. The enhancement in the photocatalytic activity is attributed to 'N' doping as well as high specific surface area and charge carrier ability of graphene. The recycling of the photocatalyst shows a good stability of the nanocomposites. This work may provide new insights to design other semiconductor deposited graphene novel nanocomposites as a visible light active photocatalyst.

Automated SEM and TEM sample preparation applied to copper/low k materials

NASA Astrophysics Data System (ADS)

Reyes, R.; Shaapur, F.; Griffiths, D.; Diebold, A. C.; Foran, B.; Raz, E.

2001-01-01

We describe the use of automated microcleaving for preparation of both SEM and TEM samples as done by SELA's new MC500 and TEMstation tools. The MC500 is an automated microcleaving tool that is capable of producing cleaves with 0.25 μm accuracy resulting in SEM-ready samples. The TEMstation is capable of taking a sample output from the MC500 (or from SELA's earlier MC200 tool) and producing a FIB ready slice of 25±5 μm, mounted on a TEM-washer and ready for FIB thinning to electron transparency for TEM analysis. The materials selected for the tool set evaluation mainly included the Cu/TaN/HOSP low-k system. The paper is divided into three sections, experimental approach, SEM preparation and analysis of HOSP low-k, and TEM preparation and analysis of Cu/TaN/HOSP low-k samples. For the samples discussed, data is presented to show the quality of preparation provided by these new automated tools.

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.

Degradation product analysis from the photocatalytic oxidation/reduction of 2,4-dichlorophenol in the presence of mesoporous silica encapsulated TiO2 particles and TiO2 dispersions (presentation)

EPA Science Inventory

Thin films of Degussa P-25 TiO2 encapsulated in an SBA-15 mesoporous silica matrix were prepared. The TiO2/SBA-15 thin film structure was verified using transmission electron microscopy (TEM) and small angle X-ray diffraction (XRD). During irradiation with 350 nm light, the TiO...

Crystallization behaviour of nanostructured hybrid SiO2-TiO2 gel glasses to nanocomposites.

PubMed

Tsvetelina, Gerganova; Yordanka, Ivanova; Yuliya, Vueva; Miranda, Salvado Isabel M; Helena, Fernandes Maria

2010-04-01

The crystallization behaviour of hybrid SiO2-TiO2 nanocomposites derived from titanosiloxanes by sol-gel method has been investigated depending on the type of siloxane precursor and the pirolysis temperature. The resulting hybrid titanosiloxanes, crosslinked with trimethylsilil isocyanate (nitrogen-modified) or methyltrietoxisilane (carbon-modified), were pirolyzed in an inert atmosphere in the temperature range between 600 to 1100 degrees C in order to form C-(N)-Si-O-TiO2 nanocomposites. By means of XRD, FTIR, 29Si NMR, SEM, TEM and AFM investigations have been established that the transformation of the nanostructured SiO2-TiO2 hybrid materials into nanocomposites as well as the crystalline size depend on the titanium content and the type of cross-linking agents used in the synthesizes.

New application of Z-scheme Ag3PO4/g-C3N4 composite in converting CO2 to fuel.

PubMed

He, Yiming; Zhang, Lihong; Teng, Botao; Fan, Maohong

2015-01-06

This research was designed for the first time to investigate the activities of photocatalytic composite, Ag3PO4/g-C3N4, in converting CO2 to fuels under simulated sunlight irradiation. The composite was synthesized using a simple in situ deposition method and characterized by various techniques including Brunauer-Emmett-Teller method (BET), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (DRS), photoluminescence spectroscopy (PL), and an electrochemical method. Thorough investigation indicated that the composite consisted of Ag3PO4, Ag, and g-C3N4. The introduction of Ag3PO4 on g-C3N4 promoted its light absorption performance. However, more significant was the formation of heterojunction structure between Ag3PO4 and g-C3N4, which efficiently promoted the separation of electron-hole pairs by a Z-scheme mechanism and ultimately enhanced the photocatalytic CO2 reduction performance of the Ag3PO4/g-C3N4. The optimal Ag3PO4/g-C3N4 photocatalyst showed a CO2 conversion rate of 57.5 μmol · h(-1) · gcat(-1), which was 6.1 and 10.4 times higher than those of g-C3N4 and P25, respectively, under simulated sunlight irradiation. The work found a new application of the photocatalyst, Ag3PO4/g-C3N4, in simultaneous environmental protection and energy production.

Boosted surface acidity in TiO2 and Al2O3-TiO2 nanotubes as catalytic supports

NASA Astrophysics Data System (ADS)

Camposeco, R.; Castillo, S.; Mejía-Centeno, Isidro; Navarrete, J.; Nava, N.

2015-11-01

In this study, titanate nanotubes (NT) and titanate nanotubes with alumina (NT-Al) were studied as solid acid catalytic supports to show the relationship between the kind of acidity and catalytic activity. The supports were characterized by XRD, TEM, FTIR, XPS, and tested in the SCR-NO with NH3. It was found that the amount of Brönsted acid sites was maintained and the Lewis acid sites were significantly affected by the addition of alumina (1, 3, 5 and 10 wt.%); such acidity was higher than that of the titanate nanotubes (NT) by two-fold. To confirm the formation of titanate nanotubes and titanate nanotubes with alumina, transmission electron microscopy (TEM) was used. X-ray diffraction (XRD) revealed the formation of the H2Ti4O9·H2O phase. All NT and NT-Al supports presented catalytic activity to remove NO with NH3 under lean conditions, confirming the presence of an important amount of Brönsted and Lewis acid sites in both NT and NT-Al supports.

A weak-light-responsive TiO2/g-C3N4 composite film: photocatalytic activity under low-intensity light irradiation.

PubMed

Wang, Peifang; Guo, Xiang; Rao, Lei; Wang, Chao; Guo, Yong; Zhang, Lixin

2018-05-10

A TiO 2 /g-C 3 N 4 composite photocatalytic film was prepared by in situ synthesis method and its photocatalytic capability under weak-visible-light condition was studied. The co-precursor with different ratio of melamine and TiO 2 sol-gel precursor were treated using ultrasonic mixing, physical deposition, and co-sintering method to form the smooth, white-yellow, and compact TiO 2 /g-C 3 N 4 composite films. The prepared TiO 2 /g-C 3 N 4 materials were characterized by SEM, TEM, EDS, XRD, BET, VBXPS, and UV-vis diffuse reflectance spectra. The results of composite showed that TiO 2 and g-C 3 N 4 have close interfacial connections which are favorable to charge transfer between these two semiconductors with suitable band structure, g-C 3 N 4 retard the anatase-to-rutile phase transition of TiO 2 significantly, the specific surface area were increased with g-C 3 N 4 ratio raised. Under weak-light irradiation, composite films photocatalytic experiments exhibited RhB removal efficiency approaching 90% after three recycles. Powders suspension degradation experiments revealed the removal efficiency of TiO 2 /g-C 3 N 4 (90.8%) was higher than pure TiO 2 (52.1%) and slightly lower than pure g-C 3 N 4 (96.6%). By control experiment, the enhanced photocatalysis is ascribed to the combination of TiO 2 and g-C 3 N 4 , which not only produced thin films with greater stability but also formed heterojunctions that can be favorable to charge transfer between these two semiconductors with suitable band structure. This study presents the potential application of photocatalytic film in the wastewater treatment under weak-light situation.

Sulfur Nanoparticles Synthesis and Characterization from H2S Gas, Using Novel Biodegradable Iron Chelates in W/O Microemulsion

NASA Astrophysics Data System (ADS)

Deshpande, Aniruddha S.; Khomane, Ramdas B.; Vaidya, Bhalchandra K.; Joshi, Renuka M.; Harle, Arti S.; Kulkarni, Bhaskar D.

2008-06-01

Sulfur nanoparticles were synthesized from hazardous H2S gas using novel biodegradable iron chelates in w/o microemulsion system. Fe3+ malic acid chelate (0.05 M aqueous solution) was studied in w/o microemulsion containing cyclohexane, Triton X-100 and n-hexanol as oil phase, surfactant, co-surfactant, respectively, for catalytic oxidation of H2S gas at ambient conditions of temperature, pressure, and neutral pH. The structural features of sulfur nanoparticles have been characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), energy dispersive spectroscopy (EDS), diffused reflectance infra-red Fourier transform technique, and BET surface area measurements. XRD analysis indicates the presence of α-sulfur. TEM analysis shows that the morphology of sulfur nanoparticles synthesized in w/o microemulsion system is nearly uniform in size (average particle size 10 nm) and narrow particle size distribution (in range of 5 15 nm) as compared to that in aqueous surfactant systems. The EDS analysis indicated high purity of sulfur (>99%). Moreover, sulfur nanoparticles synthesized in w/o microemulsion system exhibit higher antimicrobial activity (against bacteria, yeast, and fungi) than that of colloidal sulfur.

In situ TEM of radiation effects in complex ceramics.

PubMed

Lian, Jie; Wang, L M; Sun, Kai; Ewing, Rodney C

2009-03-01

In situ transmission electron microscopy (TEM) has been extensively applied to study radiation effects in a wide variety of materials, such as metals, ceramics and semiconductors and is an indispensable tool in obtaining a fundamental understanding of energetic beam-matter interactions, damage events, and materials' behavior under intense radiation environments. In this article, in situ TEM observations of radiation effects in complex ceramics (e.g., oxides, silicates, and phosphates) subjected to energetic ion and electron irradiations have been summarized with a focus on irradiation-induced microstructural evolution, changes in microchemistry, and the formation of nanostructures. New results for in situ TEM observation of radiation effects in pyrochlore, A(2)B(2)O(7), and zircon, ZrSiO(4), subjected to multiple beam irradiations are presented, and the effects of simultaneous irradiations of alpha-decay and beta-decay on the microstructural evolution of potential nuclear waste forms are discussed. Furthermore, in situ TEM results of radiation effects in a sodium borosilicate glass subjected to electron-beam exposure are introduced to highlight the important applications of advanced analytical TEM techniques, including Z-contrast imaging, energy filtered TEM (EFTEM), and electron energy loss spectroscopy (EELS), in studying radiation effects in materials microstructural evolution and microchemical changes. By combining ex situ TEM and advanced analytical TEM techniques with in situ TEM observations under energetic beam irradiations, one can obtain invaluable information on the phase stability and response behaviors of materials under a wide range of irradiation conditions. (c) 2009 Wiley-Liss, Inc.

Facile synthesis of novel CaFe2O4/g-C3N4 nanocomposites for degradation of methylene blue under visible-light irradiation.

PubMed

Vadivel, S; Maruthamani, D; Habibi-Yangjeh, A; Paul, Bappi; Dhar, Siddhartha Sankar; Selvam, Kaliyamoorthy

2016-10-15

Hybrid organic/inorganic nanocomposites comprised of calcium ferrite (CaFe2O4) and graphitic carbon nitride (g-C3N4) were prepared via a simple two-step process. The hybridized CaFe2O4/g-C3N4 heterostructure was characterized by a variety of techniques, including X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FT-IR), UV-vis diffuse reflectance spectroscopy (UV-vis DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive analysis of X-rays (EDS), X-ray photoelectron spectroscopy (XPS), photoluminescence spectroscopy, electrochemical impedance spectroscopy (EIS), and photoelectrochemical studies. Photocatalytic activity of the prepared samples was evaluated against degradation of methylene blue (MB) under visible-light irradiation. The photocatalytic activity of CaFe2O4 30%/g-C3N4 nanocomposite, as optimum photocatalyst, for degradation of MB was superior to the pure CaFe2O4 and g-C3N4 samples. It was demonstrated that the photogenerated holes and superoxide ion radicals were the two main reactive species towards the photocatalytic degradation of MB over the nanocomposite. Based on the experimental results, a possible photocatalytic mechanism for the MB degradation over the nanocomposite was proposed. This work may provide some inspiration for the fabrication of spinel ferrites with efficient photocatalytic performance. Copyright © 2016 Elsevier Inc. All rights reserved.

Nano ZSM-5 type ferrisilicates as novel catalysts for ethylbenzene dehydrogenation in the presence of N 2O

NASA Astrophysics Data System (ADS)

Khatamian, M.; Khandar, A. A.; Haghighi, M.; Ghadiri, M.

2011-11-01

Nanosized ZSM-5 type ferrisilicates were successfully prepared using hydrothermal process. Several parameters including gel initiative compositions (Na+ or K+ alkali system), SiO2/Fe2O3 molar ratios and hydrothermal temperature were systematically investigated. The samples were characterized by XRD, TEM, SEM-EDS, BET surface area and ICP techniques. It was found that surface areas and the total pore volume increase with increasing in the SiO2/Fe2O3 molar ratio at Na-FZ ferrisilicates. The catalytic performance of the synthesized catalysts was evaluated in ethylbenzene dehydrogenation to styrene in the presence of N2O or steam at temperatures ranging from 400 °C to 660 °C under atmospheric pressure. The effects of gel initiative compositions, SiO2/Fe2O3 molar ratio as well as the hydrothermal synthesis temperature on the catalytic performance of these catalysts have been addressed. It was shown that styrene yield significantly influenced by altering in the SiO2/Fe2O3 ratio but was not greatly influenced by changes in hydrothermal synthesis temperatures. The comparison between performance of potassium and sodium containing catalysts was shown that the one with potassium has higher yield and selectivity toward styrene production at an optimum temperature of 610 °C.

Recombination-related properties of a-screw dislocations in GaN: A combined CL, EBIC, TEM study

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

Medvedev, O. S., E-mail: o.s.medvedev@spbu.ru; Mikhailovskii, V. Yu.; IRC for Nanotechnology, Research Park, St.-Petersburg State University

2016-06-17

Cathodoluminescence (CL), electron beam current (EBIC) and transmission electron microscopy (TEM) techniques have been applied to investigate recombination properties and structure of freshly introduced dislocations in low-ohmic GaN crystals. It was confirmed that the only a-screw dislocations exhibited an intense characteristic dislocation-related luminescence (DRL) which persisted up to room temperature and was red-shifted by about 0.3 eV with respect to the band gap energy not only in HVPE but also in MOCVD grown samples. EBIC contrast of the dislocations was found to be temperature independent indicating that the dislocation-related recombination level is situated below 200 meV with respect of conductionmore » band minimum. With the increasing of the magnification of the dislocation TEM cross-sectional images they were found to disappear, probably, due to the recombination enhanced dislocation glide (REDG) under electron beam exposure which was immediately observed in CL investigations on a large scale. The stacking fault ribbon in the core of dissociated a-screw dislocation which form a quantum well for electrons was proposed to play an important role both in DRL spectrum formation and in REDG.« less

Leonardo da Vinci's drapery studies: characterization of lead white pigments by µ-XRD and 2D scanning XRF

NASA Astrophysics Data System (ADS)

Gonzalez, Victor; Calligaro, Thomas; Pichon, Laurent; Wallez, Gilles; Mottin, Bruno

2015-11-01

This work focuses on the composition and microstructure of the lead white pigment employed in a set of paintworks, using a combination of µ-XRD and 2D scanning XRF, directly applied on five drapery studies attributed to Leonardo da Vinci (1452-1519) and conserved in the Département des Arts Graphiques, Musée du Louvre and in the Musée des Beaux- Arts de Rennes. Trace elements present in the composition as well as in the lead white highlights were imaged by 2D scanning XRF. Mineral phases were determined in a fully noninvasive way using a special µ-XRD diffractometer. Phase proportions were estimated by Rietveld refinement. The analytical results obtained will contribute to differentiate lead white qualities and to highlight the artist's technique.

Radiation-Induced Changes in Quartz, A Mineral Analog of Nuclear Power Plant Concrete Aggregates

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

Silva, Chinthaka M.; Rosseel, Thomas M.; Kirkegaard, Marie C.

Quartz single-crystal samples consisting of α-quartz crystal structure were neutron irradiated to fluences of 5 × 10 18, 4 × 10 19, and 2 × 10 20 n/cm 2 (E > 0.1 MeV) at two temperatures (52 and 95 °C). The changes in the α-quartz phase as a function of these two conditions (temperature and fluence) were studied using X-ray powder diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM), and the results acquired using these complementary techniques are presented in a single place for the first time. XRD studies showed that the lattice parameters of α-quartz increased with increasingmore » neutron flux. The lattice growth was larger for the samples that were neutron irradiated at 52 °C than at 95 °C. Moreover, an amorphous content was determined in the quartz samples neutron irradiated at 4 × 10 19 n/cm 2, with the greater amount being in the 52 °C irradiated sample. Complete amorphization of quartz was observed at a fluence of 2 × 10 20 n/cm 2 (E > 0.1 MeV) using XRD and confirmed by TEM characterization and Raman spectroscopic studies. In conclusion, the cause for α-quartz lattice expansion and sample amorphization was also explored using XRD and Raman spectroscopic studies.« less

Radiation-Induced Changes in Quartz, A Mineral Analog of Nuclear Power Plant Concrete Aggregates

DOE PAGES

Silva, Chinthaka M.; Rosseel, Thomas M.; Kirkegaard, Marie C.

2018-03-07

Quartz single-crystal samples consisting of α-quartz crystal structure were neutron irradiated to fluences of 5 × 10 18, 4 × 10 19, and 2 × 10 20 n/cm 2 (E > 0.1 MeV) at two temperatures (52 and 95 °C). The changes in the α-quartz phase as a function of these two conditions (temperature and fluence) were studied using X-ray powder diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM), and the results acquired using these complementary techniques are presented in a single place for the first time. XRD studies showed that the lattice parameters of α-quartz increased with increasingmore » neutron flux. The lattice growth was larger for the samples that were neutron irradiated at 52 °C than at 95 °C. Moreover, an amorphous content was determined in the quartz samples neutron irradiated at 4 × 10 19 n/cm 2, with the greater amount being in the 52 °C irradiated sample. Complete amorphization of quartz was observed at a fluence of 2 × 10 20 n/cm 2 (E > 0.1 MeV) using XRD and confirmed by TEM characterization and Raman spectroscopic studies. In conclusion, the cause for α-quartz lattice expansion and sample amorphization was also explored using XRD and Raman spectroscopic studies.« less

Prevalence of bla TEM-220 gene in Penicillinase-producing Neisseria gonorrhoeae strains carrying Toronto/Rio plasmid in Argentina, 2002 - 2011.

PubMed

Gianecini, Ricardo; Oviedo, Claudia; Guantay, Cristina; Piccoli, Laura; Stafforini, Graciela; Galarza, Patricia

2015-12-16

Penicillinase-producing Neisseria gonorroheae (PPNG) was first isolated in 1976. PPNG strains carrying bla TEM-1 and bla TEM-135 gene have been described in different countries. Recently, a novel bla TEM-220 allele was detected in PPNG isolates carrying Toronto/Rio plasmid. The prevalence and characteristics of TEM-220 strains worldwide are unknown, and therefore, it needs to be studied. The purpose of this study was to detect bla TEM-220 gene in PPNG strains possessing Toronto/Rio plasmid over a period of ten years in Argentina, and to evaluate the proportion of isolates producing non-TEM-220 containing the T539C substitution in the bla TEM allele. One hundred and fifty one PPNG isolates carrying Toronto/Rio plasmid were studied between 2002 and 2011. A mismatch amplification mutation assay (MAMA) PCR was used to identify the T539C substitution in the bla TEM allele and a MAMA-PCR protocol was developed to detect the G547A substitution in the bla TEM-220. The reference agar dilution method of the Clinical and Laboratory Standard Institute (CLSI) was used for susceptibility testing to five β-lactams antibiotics, ciprofloxacin, tetracycline and azithromycin. In all TEM-220-producing isolates, the whole bla TEM gene was sequenced and the isolates were typed using N. gonorroheae multiantigen sequence typing (NG-MAST). MAMA PCR successfully identified the G547A substitution in the bla TEM-220 allele. The proportion of isolates that possessed the bla TEM-220 allele was 2.6 %, and 93.2 % MAMA TEM-220 PCR-negative isolates showed the T539C substitution in the bla TEM gene. No differences in the susceptibility to five beta-lactam antibiotics tested were observed in PPNG isolates TEM-220-producing and PPNG isolates carrying the T539C substitution in the bla TEM gene. All TEM-220 isolates were indistinguishable by NG-MAST. This is the first study which shows the prevalence of bla TEM-220 in N. gonorrhoeae isolates carrying Toronto/Rio plasmid in Argentina. Although the bla

Photocatalytic behaviour of WO3/TiO2-N for diclofenac degradation using simulated solar radiation as an activation source.

PubMed

Cordero-García, A; Turnes Palomino, G; Hinojosa-Reyes, L; Guzmán-Mar, J L; Maya-Teviño, L; Hernández-Ramírez, A

2017-02-01

In this study, the photocatalytic removal of an emerging contaminant, diclofenac (DCF) sodium, was performed using the nitrogen-doped WO 3 /TiO 2 -coupled oxide catalyst (WO 3 /TiO 2 -N). The catalyst synthesis was accomplished by a sol-gel method using tetrabutyl orthotitanate (C 16 H 36 O 4 Ti), ammonium p-tungstate [(NH 4 ) 10 H 2 W 12 O 42 ·4H 2 O] and ammonium nitrate (NH 4 NO 3 ) as the nitrogen source. For comparison, TiO 2 and WO 3 /TiO 2 were also prepared under similar conditions. Analysis by X-ray diffraction (XRD), N 2 adsorption-desorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance UV-Vis spectroscopy (DRS) and X-ray photoelectron spectroscopy (XPS) were conducted to characterize the synthesized materials. The photocatalytic efficiency of the semiconductors was determined in a batch reactor irradiated with simulated solar light. Residual and mineralized DCF were quantified by high-performance liquid chromatography, total organic carbon analysis and ion exchange chromatography. The results indicated that the tungsten atoms were dispersed on the surface of TiO 2 as WO 3 . The partial substitution of oxygen by nitrogen atoms into the lattice of TiO 2 was an important factor to improve the photocatalytic efficiency of WO 3 /TiO 2 . Therefore, the best photocatalytic activity was obtained with the WO 3 /TiO 2 -N 0.18 catalyst, reaching 100% DCF transformation at 250 kJ m -2 and complete mineralization at 400 kJ m -2 of solar-accumulated energy.

Effects of GaN/AlGaN/Sputtered AlN nucleation layers on performance of GaN-based ultraviolet light-emitting diodes

PubMed Central

Hu, Hongpo; Zhou, Shengjun; Liu, Xingtong; Gao, Yilin; Gui, Chengqun; Liu, Sheng

2017-01-01

We report on the demonstration of GaN-based ultraviolet light-emitting diodes (UV LEDs) emitting at 375 nm grown on patterned sapphire substrate (PSS) with in-situ low temperature GaN/AlGaN nucleation layers (NLs) and ex-situ sputtered AlN NL. The threading dislocation (TD) densities in GaN-based UV LEDs with GaN/AlGaN/sputtered AlN NLs were determined by high-resolution X-ray diffraction (XRD) and cross-sectional transmission electron microscopy (TEM), which revealed that the TD density in UV LED with AlGaN NL was the highest, whereas that in UV LED with sputtered AlN NL was the lowest. The light output power (LOP) of UV LED with AlGaN NL was 18.2% higher than that of UV LED with GaN NL owing to a decrease in the absorption of 375 nm UV light in the AlGaN NL with a larger bandgap. Using a sputtered AlN NL instead of the AlGaN NL, the LOP of UV LED was further enhanced by 11.3%, which is attributed to reduced TD density in InGaN/AlInGaN active region. In the sputtered AlN thickness range of 10–25 nm, the LOP of UV LED with 15-nm-thick sputtered AlN NL was the highest, revealing that optimum thickness of the sputtered AlN NL is around 15 nm. PMID:28294166

Synthesis and characterization of Pd-poly(N-vinyl-2-pyrrolidone)/KIT-5 nanocomposite as a polymer-inorganic hybrid catalyst for the Suzuki-Miyaura cross-coupling reaction

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

Kalbasi, Roozbeh Javad, E-mail: rkalbasi@iaush.ac.ir; Mosaddegh, Neda

2011-11-15

Composite poly(N-vinyl-2-pyrrolidone)/KIT-5 (PVP/KIT-5) was prepared by in situ polymerization method and used as a support for palladium nanoparticles obtained through the reduction of Pd(OAc){sub 2} by hydrazine hydrate. The physical and chemical properties of the catalyst were investigated by XRD, FT-IR, UV-vis, TG, BET, SEM, and TEM techniques. The catalytic performance of this novel heterogeneous catalyst was determined for the Suzuki-Miyaura cross-coupling reaction between aryl halides and phenylboronic acid in the presence of water at room temperature. The stability of the nanocomposite catalyst was excellent and could be reused 8 times without much loss of activity in the Suzuki-Miyaura cross-couplingmore » reaction. - Graphical Abstract: Pd-poly(N-vinyl-2-pyrrolidone)/KIT-5 was prepared as an organic-inorganic hybrid catalyst for the Suzuki-Miyaura reaction. The stability of the catalyst was excellent and could be reused 8 times in the Suzuki-Miyaura reaction. Highlights: > Pd-poly(N-vinyl-2-pyrrolidone)/KIT-5 was prepared as a novel nanocomposite. > Nanocomposite was prepared based on a cage-type mesoporous system. > Catalyst showed excellent activity for Suzuki-Miyaura reaction in water. > Stability of the catalyst was excellent and could be reused 8 times.« less

Identification of a deleterious phase in photocatalyst based on Cd1 - xZnxS/Zn(OH)2 by simulated XRD patterns.

PubMed

Cherepanova, Svetlana; Markovskaya, Dina; Kozlova, Ekaterina

2017-06-01

The X-ray diffraction (XRD) pattern of a deleterious phase in the photocatalyst based on Cd 1 - x Zn x S/Zn(OH) 2 contains two relatively intense asymmetric peaks with d-spacings of 2.72 and 1.56 Å. Very small diffraction peaks with interplanar distances of (d) ≃ 8.01, 5.40, 4.09, 3.15, 2.49 and 1.35 Å are characteristic of this phase but not always observed. To identify this phase, the XRD patterns for sheet-like hydroxide β-Zn(OH) 2 and sheet-like hydrozincite Zn 5 (CO 3 ) 2 (OH) 6 as well as for turbostratic hydrozincite were simulated. It is shown that the XRD pattern calculated on the basis of the last model gives the best correspondence with experimental data. Distances between layers in the turbostratically disordered hydrozincite fluctuate around d ≃ 8.01 Å. This average layer-to-layer distance is significantly higher than the interlayer distance 6.77 Å in the ordered Zn 5 (CO 3 ) 2 (OH) 6 probably due to a deficiency of CO 3 2- anions, excess OH - and the presence of water molecules in the interlayers. It is shown by variable-temperature XRD and thermogravimetric analysis (TGA) that the nanocrystalline turbostratic nonstoichiometric hydrozincite-like phase is quite thermostable. It decomposes into ZnO in air above 473 K.

Thermal decomposition of dolomite under CO2: insights from TGA and in situ XRD analysis.

PubMed

Valverde, Jose Manuel; Perejon, Antonio; Medina, Santiago; Perez-Maqueda, Luis A

2015-11-28

Thermal decomposition of dolomite in the presence of CO2 in a calcination environment is investigated by means of in situ X-ray diffraction (XRD) and thermogravimetric analysis (TGA). The in situ XRD results suggest that dolomite decomposes directly at a temperature around 700 °C into MgO and CaO. Immediate carbonation of nascent CaO crystals leads to the formation of calcite as an intermediate product of decomposition. Subsequently, decarbonation of this poorly crystalline calcite occurs when the reaction is thermodynamically favorable and sufficiently fast at a temperature depending on the CO2 partial pressure in the calcination atmosphere. Decarbonation of this dolomitic calcite occurs at a lower temperature than limestone decarbonation due to the relatively low crystallinity of the former. Full decomposition of dolomite leads also to a relatively low crystalline CaO, which exhibits a high reactivity as compared to limestone derived CaO. Under CO2 capture conditions in the Calcium-Looping (CaL) process, MgO grains remain inert yet favor the carbonation reactivity of dolomitic CaO especially in the solid-state diffusion controlled phase. The fundamental mechanism that drives the crystallographic transformation of dolomite in the presence of CO2 is thus responsible for its fast calcination kinetics and the high carbonation reactivity of dolomitic CaO, which makes natural dolomite a potentially advantageous alternative to limestone for CO2 capture in the CaL technology as well as SO2in situ removal in oxy-combustion fluidized bed reactors.

Fabrication of Bi modified Bi2S3 pillared g-C3N4 photocatalyst and its efficient photocatalytic reduction and oxidation performances

NASA Astrophysics Data System (ADS)

Chen, Dongdong; Fang, Jianzhang; Lu, Shaoyou; Zhou, GuangYing; Feng, Weihua; Yang, Fan; Chen, Yi; Fang, ZhanQiang

2017-12-01

A novel efficient Bi modified Bi2S3 pillared g-C3N4 (BBC) plasmonic semiconductor photocatalyst has been successfully developed in a mixed solvothermal environment. The photocatalytic abilities of the as-prepared samples are examined by the photocatalytic reduction of Cr(VI) and oxidation of tetracycline (TC). And the chemical composition, structure, morphology and photo-absorption properties of the photocatalysts have been investigated by XRD, FT-IR, XPS, TEM, HRTEM and DRS methods, respectively. It is found that the addition of triethanolamine (TEA) results in the formation of the pillared-g-C3N4 (PG) nanostructure. The agglomeration of g-C3N4 nanosheets moiety and Bi2S3 nanorods moiety can be both hindered effectively by the special PG structure. And the photocatalytic results indicate that BBC exhibits the best photoreduction and photooxidation performances among all the samples, and meanwhile possesses superior photo-stability during the recycling runs. The enhanced photocatalytic activity of BBC could be ascribed to the furtherance of charge separation, localized surface plasma resonance (SPR) effect of metallic Bi and the excellent reaction interface. Finally, a tentative mechanism of BBC for photocatalytic reduction of Cr(VI) and oxidation of TC is discussed in detail.

Synthesis and photocatalytic studies of ZnS nanoparticles from heteroleptic complex of Zn(II) 1-cyano-1-carboethoxy-2,-2-ethylenedithiolato diisopropylthiourea and its adducts with N-donor ligands

NASA Astrophysics Data System (ADS)

Osuntokun, Jejenija; Ajibade, Peter A.; Onwudiwe, Damian C.

2016-12-01

Zinc complexes of the type [Zn(diptu)2(ced)] (1), [Zn(diptu)2(ced)py] (2), [Zn(diptu)2(ced)bpy] (3), and [Zn(diptu)2(ced)phen] (4), (where (diptu)2(ced) = 1-cyano-1-carboethoxyethylene-2,2-dithiolato-κS,S‧-bis(N,N-diisopropyllthiourea), py = pyridine, bpy = 2, 2‧ bipyridine and phen = 1, 10 phenanthroline have been synthesized and characterized by elemental analyses, Fourier transform infra-red (FTIR) and Nuclear magnetic resonance (NMR) spectroscopies. The parent complex (1) was formulated as four coordinate species, which gave rise to 5 coordinate complex in (2) and six coordinate compounds in (3) and (4), with the dithiolate acting as bidentate chelating ligand. The complexes were used as single-source precursors for the synthesis of HDA-capped ZnS nanoparticles. The nanoparticles gave different morphologies with sizes in the range of 1.92-4.72 nm as observed from the TEM analysis and supported by XRD. The UV-vis spectroscopy showed that all the ZnS nanoparticles are blue shifted, with respect to the bulk, which confirmed quantum confinement. The photoluminescence spectra showed narrow and broad emission peaks around 290 and 360 nm which are ascribed to spontaneous emission peaks from band to band transition and surface states respectively. Photocatalytic activities of all the nanoparticles were investigated with methylene blue (MB) acting as the organic dye, and the UV-vis spectral revealed a gradual decrease in absorption peak that confirmed the degradation of the MB.

TEMs but not DKK1 could serve as complementary biomarkers for AFP in diagnosing AFP-negative hepatocellular carcinoma.

PubMed

Mao, Liping; Wang, Yueguo; Wang, Delin; Han, Gang; Fu, Shouzhong; Wang, Jianxin

2017-01-01

Hepatitis B virus (HBV)-related hepatocellular carcinoma (HCC) is prevalent worldwide. Despite its limitations, serum alpha-fetoprotein (AFP) remains the most widely-used biomarker for the diagnosis of HCC. This study aimed to assess whether measurement of peripheral plasma Dickkopf-1 (DKK1) and Tie2-expressing monocytes (TEMs) could overcome the limitations of AFP and improve the diagnostic accuracy of HCC. Plasma DKK1 level and the percentage of TEMs in peripheral CD14+CD16+ monocytes from HCC patients (n = 82), HBV-related liver cirrhosis (LC) patients (n = 29), chronic hepatitis B (CHB) infected patients (n = 28) and healthy volunteers (n = 31) were analyzed by ELISA and flow cytometry. Receiver operating characteristic (ROC) curves were used to analyze a single biomarker, or a combination of two or three biomarkers. Univariate and multivariate analyses were performed to assess the significance of each marker in prediction of HCC and AFP-negative HCC from LC patients. The percentage of TEMs in peripheral CD14+CD16+ monocytes and plasma level of DKK1 in HCC group were significantly higher than those in LC, CHB and healthy control groups (all P-values <0.05). The percentage of TEMs alone was also significantly higher in AFP-negative HCC group than that in LC, CHB and healthy control groups (all P-values <0.05). Plasma DKK1 level alone could not distinguish between AFP-negative HCC and LC patients. ROC curves showed that the optimal diagnostic cutoff value was 550.93 ng/L for DKK1 and 4.95% for TEMs. There was no significant difference in AUC of DKK1, TEMs and AFP in HCC diagnosis between the four groups (all P>0.05). A combination of DKK1, TEMs and AFP measurements increased the AUC for HCC diagnosis as compared with either marker alone (0.833; 95%CI 0.768-0.886). The AUC for TEMs was 0.692 (95% CI 0.564-0.819) in differentiating AFP-negative HCC from LC, with a sensitivity of 80.0% and a specificity of 65.52%. Only TEMs prevailed as a significant predictor for

Nano-TiO2, ultrasound and sequential nano-TiO2/ultrasonic degradation of N-acetyl-para-aminophenol from aqueous solution.

PubMed

Ayanda, Olushola S; Nelana, Simphiwe M; Petrik, Leslie F; Naidoo, Eliazer B

2017-10-01

The application of nano-TiO 2 as adsorbent combined with ultrasound for the degradation of N-acetyl-para-aminophenol (AAP) from aqueous solution was investigated. The nano-TiO 2 was characterized by means of powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), and attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR). Experimental results revealed that the adsorption of AAP by nano-TiO 2 fitted the pseudo-second-order kinetic model, the equilibrium could be explained by the Freundlich isotherm and the treatment process is exothermic. The optimum removal efficiency of AAP (128.89 mg/g (77.33%)) was achieved at pH 4 when 0.03 g of nano-TiO 2 was mixed with 50 mL of 100 mg/L AAP aqueous solution at ambient temperature, 60 min contact time, and a stirring speed of 120 rpm. Ultrasound at 20 kHz and pH 3 was favorable and it resulted in 52.61% and 57.43% removal efficiency with and without the addition of nano-TiO 2 , respectively. The degradation of AAP by ultrasound followed by nano-TiO 2 treatment resulted in approximately 99.50% removal efficiency. This study showed that a sequential ultrasound and nano-TiO 2 treatment process could be employed for the removal of AAP or other emerging water and wastewater contaminants.

Fabrication of a transparent ultraviolet detector by using n-type Ga2O3 and p-type Ga-doped SnO2 core-shell nanowires.

PubMed

Hsu, Cheng-Liang; Lu, Ying-Ching

2012-09-21

This study investigates the feasibility of synthesizing high-density transparent Ga(2)O(3)/SnO(2):Ga core-shell nanowires on a sapphire substrate at 1000 °C by VLS. The doping Ga concentrations are 0.46, 1.07, 2.30 and 17.53 atomic%. The XRD spectrum and HR-TEM reveal Ga(2)O(3) and SnO(2) as having monoclinic and tetragonal rutile structures, respectively. Experimental results indicate that the XRD peak shift of SnO(2) to a larger angle increases with the increasing amount of Ga doping. According to the CL spectrum, SnO(2) and Ga(2)O(3) peak at approximately 528-568 nm and 422-424 nm, respectively. The maximum quantum efficiency of Ga(2)O(3)/SnO(2):Ga core-shell nanowires is around 0.362%. The UV light on-off current contrast ratio of Ga(2)O(3)/SnO(2):Ga core-shell nanowires is around 1066.7 at a bias of 5 V. Moreover, the dynamic response of Ga(2)O(3)/SnO(2):Ga core-shell nanowires has an on-off current contrast ratio of around 16. Furthermore, the Ga(2)O(3) region functions similar to a capacitor and continues to accumulate SnO(2):Ga excited electrons under UV light exposure.

Experimental investigation of nearly monodispersed ternary Mn_{0.5}Zn_{0.5}Fe_{2}O_{4} magnetic fluid

NASA Astrophysics Data System (ADS)

Parekh, K.; Upadhyay, R. V.; Mehta, R. V.; Aswal, V. K.

2008-03-01

The experimental investigations of a nearly monodispersed magnetic fluid, containing a ternary Mn_{0.5}Zn_{0.5}Fe_{2}O_{4} (MZ5) magnetic fluid, are carried out using XRD, TEM, Small Angle Neutron Scattering (SANS) and a SQUID magnetometer. The XRD and TEM measurements give the particle size to be 7.5 and 8.4 nm respectively, and confirms the single phase cubic spinel structure. The size distribution retrieved from TEM is found to be very narrow (<10{%}). Room temperature magnetic measurement fits with the Langevin's function modified for the particle size distribution as well as for the particle-particle interaction parameter. M(H)-measurements as a function of field for different temperatures show that the system is superparamagnetic at room temperature and develops coercivity at 5 K. Figs 4, Refs 12.

Phase Evaluation in Al2O3 Fiber-Reinforced Ti2AlC During Sintering in the 1300 degrees C-1500 degrees C Temperature Range

DTIC Science & Technology

2011-01-01

composition: 97% Al2O3 and 3% SiO2] fibers. In both cases, the fibers were chopped with a razor blade into 5 cm lengths. Mixing of the powder and...the presence of XRD amorphous Ti- aluminides (see below) or other phases cannot be ruled out at this juncture. When the XRD spectrum of the as-received...not shown). No peaks belonging to any Ti- aluminide were found suggesting them to be amorphous or at most nano-crystalline. A typical TEM micrograph of

Effect of Temperature, Precursor Type and Dripping Time on the Crystallite Size of Nano ZnO Obtained by One-Pot Synthesis: 2 k Full Factorial Design Analysis.

PubMed

Machado, Morgana de Medeiros; Savi, Bruna Martinello; Perucchi, Mariana Borges; Benedetti, Alessandro; Oliveira, Luis Felipe Silva; Bernardin, Adriano Michael

2018-06-01

The aim of this work was to determine the effect of temperature, precursor and dripping time on the crystallite size of ZnO nanoparticles synthesized by controlled precipitation according a 2k full factorial design. ZnCl2, Zn(NO3)2 and NaOH were used as precursors. After synthesis, the nano crystalline powder was characterized by XRD (Cu Kα), UV-Vis, and HR-TEM. The nano ZnO particles presented a crystallite size between 210 and 260 Å (HR-TEM and XRD). The results show that the crystallite size depends on the type of precursor and temperature of synthesis, but not on the dripping time.

The new insight into the structure-activity relation of Pd/CeO2-ZrO2-Nd2O3 catalysts by Raman, in situ DRIFTS and XRD Rietveld analysis.

PubMed

Yang, X; Yang, L; Lin, J; Zhou, R

2016-01-28

Pd/CeO2-ZrO2-Nd2O3 (CZN) catalysts with different CeO2/ZrO2 molar ratios were synthesized and have been characterized by multiple techniques, e.g. XRD in combination with Rietveld refinement, UV-Raman, XPS and in situ DRIFTS. The XRD pattern of CZN with CeO2/ZrO2 molar ratios ≥1/2 can be indexed satisfactorily to the fluorite structure with a space group Fm3̄m, while the XRD patterns of CZ12 only display diffraction peaks of the tetragonal phase (S.G. P42/nmc). Nd addition can effectively stabilize the cubic structure of the CZN support and increase the enrichment of defect sites on the surface, which may be related to the better catalytic activity of Pd/CZN12 catalysts compared with Pd/CZ12. The presence of moderate ZrO2 can increase the concentration of O* active species, leading to accelerate the formation of nitrate species and thus enhance the catalytic activity of NOx and HC elimination. The Pd-dispersion decreases with the increasing Zr content, leading to the decreased CO catalytic activity, especially for the aged catalysts. The change regularity of the OSC value is almost the same with the in situ dynamic operational window, demonstrating that the in situ dynamic operational window is basically affected by the OSC value.

Combustion synthesized TiO{sub 2} for enhanced photocatalytic activity under the direct sunlight-optimization of titanylnitrate synthesis

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

Daya Mani, A.; Laporte, V.; Ghosal, P.

2012-09-15

Graphical abstract: Effect of oxidant on the combustion synthesis of TiO{sub 2} has been studied by preparing titanylnitrate in four different ways from Ti(IV) iso-propoxide. It is observed that oxidant preparation method has a significant effect on physico-chemical as well as photocatalytic properties of TiO{sub 2}. All the catalysts showed excellent photocatalytic activity than Degussa P-25 under direct sunlight for the degradation of a textile dye (methylene blue), without the need of external light sources, oxygen supply and reactor systems. Highlights: ► Optimized synthesis of titanylnitrate. ► Influence of titanylnitrate synthesis on the physico-chemical properties of TiO{sub 2} prepared bymore » combustion synthesis. ► Development of highly efficient TiO{sub 2} photocatalysts those are active under the direct sunlight in open atmosphere. ► Degradation of the textile dye (methylene blue) under direct sunlight. -- Abstract: Optimized synthesis of Ti-precursor ‘titanylnitrate’ for one step combustion synthesis of N- and C-doped TiO{sub 2} catalysts were reported and characterized by using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), diffused reflectance UV–vis spectroscopy, N{sub 2} adsorption and X-ray photoelectron spectroscopy (XPS). XRD confirmed the formation of TiO{sub 2} anatase and nano-crystallite size which was further confirmed by TEM. UV-DRS confirmed the decrease in the band gap to less than 3.0 eV, which was assigned due to the presence of C and N in the framework of TiO{sub 2} as confirmed by X-ray photoelectron spectroscopy. Degradation of methylene blue in aqueous solution under the direct sunlight was carried out and typical results indicated the better performance of the synthesized catalysts than Degussa P-25.« less

In search of the elusive IrB{sub 2}: Can mechanochemistry help?

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

Xie, Zhilin; Blair, Richard G.; Department of Physics, University of Central Florida, Orlando, FL 32816

The previously unknown hexagonal ReB{sub 2}-type IrB{sub 2} diboride and orthorhombic IrB monoboride phases were produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. In addition to XRD, scanning electron microscopy and transmission electron microscopy were employed to further characterize the microstructure of the phases produced. - Graphical abstract: ReB{sub 2}-type IrB{submore » 2} and a new IrB have been successfully synthesized for the first time using mechanochemical method. Crystal structures of IrB{sub 2} and IrB were studied by synchrotron X-ray diffraction. Microstructures of the new phases were characterized by SEM and TEM. - Highlights: • ReB{sub 2}-type IrB{sub 2} and a new IrB have been synthesized by mechanochemical method. • Crystal structures of IrB{sub 2} and IrB were studied by synchrotron XRD. • Microstructures of the new phases were characterized by SEM and TEM.« less

Preparation and characterization of bismuth oxichloride (BiOCl) nanoparticles and nano zerovalent iron (nZVI)

NASA Astrophysics Data System (ADS)

Sarwan, Bhawna; Pare, Brijesh; Deep Acharya, Aman

2017-05-01

In this work, we have synthesized nano scale zerovalent iron (nZVI) particles by borohydride reduction method and bismuth oxichloride (BiOCl) by a hydrolysis method. X-ray powder diffraction (XRD) was used for the structural and chemical characterization, while scanning/transmission electron microscopy (SEM/TEM) were employed to determine the physical properties of the nanoparticles. The reactivity of synthesized nanoparticles was compared by decolorization of nile blue (NB) dye under visible irradiation.

In-situ TEM observation of nano-void formation in UO2 under irradiation

NASA Astrophysics Data System (ADS)

Sabathier, C.; Martin, G.; Michel, A.; Carlot, G.; Maillard, S.; Bachelet, C.; Fortuna, F.; Kaitasov, O.; Oliviero, E.; Garcia, P.

2014-05-01

Transmission electron microscopy (TEM) observations of UO2 polycrystals irradiated in situ with 4 MeV Au ions were performed at room temperature (RT) to better understand the mechanisms of cavity and ultimately fission products nucleation in UO2. Experiments were carried out at the JANNuS Orsay facility that enables in situ ion irradiations inside the microscope to be carried out. The majority of 4 MeV gold ions were transmitted through the thin foil, and the induced radiation defects were investigated by TEM. Observations showed that nano-void formation occurs at ambient temperature in UO2 thin foils irradiated with energetic heavy ions under an essentially nuclear energy loss regime. The diameter and density of nano-objects were measured as a function of the gold irradiation dose at RT. A previous paper has also revealed a similar nano-object population after a Xe implantation performed at 390 keV at 870 K. The nano-object density was modelled using simple concepts derived from Classical Molecular Dynamics simulations. The results are in good agreement, which suggests a mechanism of heterogeneous nucleation induced by energetic cascade overlaps. This indicates that nano-void formation mechanism is controlled by radiation damage. Such nanovoids are likely to act as sinks for mobile fission products during reactor operation.

β-lactamases produced by amoxicillin-clavulanate-resistant enterobacteria isolated in Buenos Aires, Argentina: a new blaTEM gene.

PubMed

Di Conza, José A; Badaracco, Alejandra; Ayala, Juan; Rodríguez, Cynthia; Famiglietti, Angela; Gutkind, Gabriel O

2014-01-01

Resistance to β-lactam/β-lactamase inhibitors in enterobacteria is a growing problem that has not been intensively studied in Argentina. In the present work, 54/843 enterobacteria collected in a teaching hospital of Buenos Aires city were ampicillin-sulbactam-resistant isolates remaining susceptible to second- and third-generation cephalosporins. The enzymatic mechanisms present in the isolates, which were also amoxicillin-clavulanic acid (AMC)-resistant (18/54) were herein analyzed. Sequencing revealed two different variants of blaTEM-1, being blaTEM-1b the most frequently detected allelle (10 Escherichia coli, 3 Klebsiella pneumoniae, 2 Proteus mirabilis and 1 Raoultella terrigena) followed by blaTEM-1a (1 K. pneumoniae). Amoxicillin-clavulanate resistance seems to be mainly associated with TEM-1 overproduction (mostly in E. coli) or co-expressed with OXA-2-like and/or SHV β-lactamases (K. pneumoniae and P. mirabilis). A new blaTEM variant (TEM-163) was described in an E. coli strain having an AMC MIC value of 16/8μg/ml. TEM-163 contains Arg275Gln and His289Leu amino acid substitutions. On the basis of the high specific activity and low IC50 for clavulanic acid observed, the resistance pattern seems to be due to overproduction of the new variant of broad spectrum β-lactamase rather than to an inhibitor-resistant TEM (IRT)-like behavior. Copyright © 2014 Asociación Argentina de Microbiología. Publicado por Elsevier España. All rights reserved.

Visible-light-driven N-TiO2@SiO2@Fe3O4 magnetic nanophotocatalysts: Synthesis, characterization, and photocatalytic degradation of PPCPs.

PubMed

Kumar, Ashutosh; Khan, Musharib; Fang, Liping; Lo, Irene M C

2017-07-24

TiO 2 -based photocatalysis offers certain advantages like rapid degradation and mineralization of organic compounds. However, the practical applicability of photocatalysts in degradation of pharmaceuticals and personal care products (PPCPs) is still restricted by challenges including their limited photocatalytic activity under visible light and difficulty in their separation from suspension. To overcome these challenges, a visible-light-driven magnetic N-TiO 2 @SiO 2 @Fe 3 O 4 nanophotocatalyst was developed through fine-tuning the pertinent factors (calcination temperature, Fe 3 O 4 loading, and nitrogen doping) involved during synthesis process, on the basis of degradation of ibuprofen (a typical PPCP). The TEM-EDX, XRD and XPS analyses confirmed the successful synthesis of nanophotocatalyst. By comparing nanophotocatalyst's performance on ibuprofen under two visible light sources, i.e., compact fluorescent lamps (CFLs) and light emitting diodes (LEDs) of similar irradiance, CFLs of irradiance 320μWcm -2 and peak emissive wavelength 543nm served as a better source, resulting in 94% degradation. Furthermore, 93% of benzophenone-3 within 5h and 71% of carbamazepine within 9h was degraded under visible light emitted by CFLs. The superparamagnetic behavior of the nanophotocatalyst enabled its successful magnetic separation (95% efficiency) from the suspension within 20-25min under an electromagnetic field of ∼200mT. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultrathin nanosheets of graphitic carbon nitride heterojunction with flower like Bi2O3 for photodegradation of organic pollutants

NASA Astrophysics Data System (ADS)

Bano, Zahira; Muhmood, Tahir; Xia, Mingzhu; Lei, Wu; Wang, Fengyun

2018-05-01

The flower like microrods (MR) of α-Bi2O3 defined as (MR-Bi2O3) and ultrathin g-C3N4(UT-C3N4) p-n junction was successfully prepared by loading different concentrations of UT-C3N4 over MR-Bi2O3. Their morphology and structure were thoroughly studied by XRD, SEM, XPS, TEM, UV–vis diffuse reflectance spectra, FT-IR and PL spectra. The results showed that the UT-C3N4 has been wrapped in the flower like MR-Bi2O3. The designing of the p-n junction of UT- C3N4 and MR-Bi2O3 can enhance the separation efficiency of the electron-hole pairs. The photocatalytic degradation of RhB was drastically increased by designing of the p-n junction that is due to the photogenerated electron–hole pair’s separation efficiency.

Magnetically separable nanocomposites with photocatalytic activity under visible light for the selective transformation of biomass-derived platform molecules

EPA Science Inventory

Novel magnetically separable TiO2-guanidine-(Ni,Co)Fe2O4 nanomaterials were prepared and characterised by a series of techniques including XRD, SEM, TEM, N2 physisorption as well as XPS and subsequently tested for their photocatalytic activities in the selective transformation of...

Real-Time XRD Studies of Li-O2 Electrochemical Reaction in Nonaqueous Lithium-Oxygen Battery.

PubMed

Lim, Hyunseob; Yilmaz, Eda; Byon, Hye Ryung

2012-11-01

Understanding of electrochemical process in rechargeable Li-O2 battery has suffered from lack of proper analytical tool, especially related to the identification of chemical species and number of electrons involved in the discharge/recharge process. Here we present a simple and straightforward analytical method for simultaneously attaining chemical and quantified information of Li2O2 (discharge product) and byproducts using in situ XRD measurement. By real-time monitoring of solid-state Li2O2 peak area, the accurate efficiency of Li2O2 formation and the number of electrons can be evaluated during full discharge. Furthermore, by observation of sequential area change of Li2O2 peak during recharge, we found nonlinearity of Li2O2 decomposition rate for the first time in ether-based electrolyte.

Concise N-doped Carbon Nanosheets/Vanadium Nitride Nanoparticles Materials via Intercalative Polymerization for Supercapacitors.

PubMed

Tan, Yongtao; Liu, Ying; Tang, Zhenghua; Wang, Zhe; Kong, Lingbin; Kang, Long; Liu, Zhen; Ran, Fen

2018-02-13

N-doped carbon nanosheets/vanadium nitride nanoparticles (N-CNS/VNNPs) are synthesized via a novel method combining surface-initiated in-situ intercalative polymerization and thermal-treatment process in NH 3 /N 2 atmosphere. The pH value of the synthesis system plays a critical role in constructing the structure and enhancing electrochemical performance for N-CNS/VNNPs, which are characterized by SEM, TEM, XRD, and XPS, and measured by electrochemical station, respectively. The results show that N-CNS/VNNPs materials consist of 2D N-doped carbon nanosheets and 0D VN nanoparticles. With the pH value decreasing from 2 to 0, the sizes of both carbon nanosheets and VN nanoparticles decreased to smaller in nanoscale. The maximum specific capacitance of 280 F g -1 at the current density of 1 A g -1 for N-CNS/VNNPs is achieved in three-electrode configuration. The asymmetric energy device of Ni(OH) 2 ||N-CNS/VNNPs offers a specific capacitance of 89.6 F g -1 and retention of 60% at 2.7 A g -1 after 5000 cycles. The maximum energy density of Ni(OH) 2 ||N-CNS/VNNPs asymmetric energy device is as high as 29.5 Wh kg -1 .

Improving the photocatalytic hydrogen production of Ag/g-C3N4 nanocomposites by dye-sensitization under visible light irradiation

NASA Astrophysics Data System (ADS)

Qin, Jiayi; Huo, Jingpei; Zhang, Piyong; Zeng, Jian; Wang, Tingting; Zeng, Heping

2016-01-01

Ag nanoparticles were deposited on the surface of g-C3N4 by a chemical reduction method to increase visible-light absorption via the localized surface plasmon resonance effect, resulting in the reduced recombination of photo-generated electron-holes and enhanced photocatalytic activity. The Ag/g-C3N4 composite with a Ag loading of 3 wt% has the optimum photoactivity that is almost 3.6 and 3.4 times higher than pure g-C3N4 and the same photocatalysis system which has been reported, respectively. Fluorescein was introduced as a photosensitizer and H2 evolution soared to 2014.20 μmol g-1 h-1 and the rate is even about 4.8 times higher than that of the 3 wt% Ag/g-C3N4 composite. The chemical structure, composites, morphologies and optical properties of the obtained products are well-characterized by XRD, FTIR, TEM, EDS, XPS and UV-Vis DRS. Meanwhile, the photocatalyst exhibits high stability and reusability.Ag nanoparticles were deposited on the surface of g-C3N4 by a chemical reduction method to increase visible-light absorption via the localized surface plasmon resonance effect, resulting in the reduced recombination of photo-generated electron-holes and enhanced photocatalytic activity. The Ag/g-C3N4 composite with a Ag loading of 3 wt% has the optimum photoactivity that is almost 3.6 and 3.4 times higher than pure g-C3N4 and the same photocatalysis system which has been reported, respectively. Fluorescein was introduced as a photosensitizer and H2 evolution soared to 2014.20 μmol g-1 h-1 and the rate is even about 4.8 times higher than that of the 3 wt% Ag/g-C3N4 composite. The chemical structure, composites, morphologies and optical properties of the obtained products are well-characterized by XRD, FTIR, TEM, EDS, XPS and UV-Vis DRS. Meanwhile, the photocatalyst exhibits high stability and reusability. Electronic supplementary information (ESI) available: TEM images, TGA curves, PXRD and FTIR spectra, the recycling experiment of 3% Ag/g-C3N4, the specific

Synthesis and detection the oxidization of Co cores of Co@SiO2 core-shell nanoparticles by in situ XRD and EXAFS.

PubMed

Zhang, Kunhao; Zhao, Ziyan; Wu, Zhonghua; Zhou, Ying

2015-01-01

In this paper, the Co@SiO2 core-shell nanoparticles were prepared by the sol-gel method. The oxidization of Co core nanoparticles was studied by the synchrotron radiation-based techniques including in situ X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS) up to 800°C in air and N2 protection conditions, respectively. It was found that the oxidization of Co cores is undergoing three steps regardless of being in air or in N2 protection condition. In the first step ranging from room temperature to 200°C, the Co cores were dominated by Co(0) state as well as small amount of Co(2+) ions. When temperature was above 300°C, the interface between Co cores and SiO2 shells was gradually oxidized into Co(2+), and the CoO layer was observed. As the temperature increasing to 800°C, the Co cores were oxidized to Co3O4 or Co3O4/CoO. Nevertheless, the oxidization kinetics of Co cores is different for the Co@SiO2 in air and N2 gas conditions. Generally, the O2 in the air could get through the SiO2 shells easily onto the Co core surface and induce the oxidization of the Co cores due to the mesoporous nature of the SiO2 shells. However, in N2 gas condition, the O atoms can only be from the SiO2 shells, so the diffusion effect of O atoms in the interface between Co core and SiO2 shell plays a key role.

Photocatalytic reductive dechlorination of 2-chlorodibenzo-p-dioxin by Pd modified g-C3N4 photocatalysts under UV-vis irradiation: Efficacy, kinetics and mechanism.

PubMed

Ding, Jiafeng; Long, Gaoyuan; Luo, Yang; Sun, Runze; Chen, Mengxia; Li, Yajun; Zhou, Yanfang; Xu, Xinhua; Zhao, Weirong

2018-05-09

Polychlorinated dibenzo-p-dioxins (PCDDs), as a group of notorious anthropogenic environmental toxicants, are arguably ubiquitous in nature. In this study, we investigated the photocatalytic reductive dechlorination of 2-chlorodibenzo-p-dioxin (2-CDD) over Pd/g-C 3 N 4 catalysts under UV-vis irradiation. The g-C 3 N 4 and a series of Pd/g-C 3 N 4 catalysts were prepared by thermal polymerization and mechanical mixing-illumination method and characterized by XRD, TEM, BET, SEM and UV-vis DRS analyses. Among all the samples, the Pd/g-C 3 N 4 (5 wt%) yielded the optimal dechlorination activity with a total 2-CDD conversion of 54% within 4 h, and 76% of those converted 2-CDD were evolved to dibenzo-p-dioxin (DD). The kinetics of dechlorination could be described as pseudo-first-order decay model (R 2  > 0.84). Corresponding rate constants (k) increased from 0.052 to 0.17 h -1 with Pd contents up to 5 wt% and decreased to 0.13 h -1 with a 10 wt% of Pd. The enhanced activities originated from the surface plasmonic resonance (SPR) effect of Pd nanoparticles and the formation of Schottky barrier between Pd and g-C 3 N 4 , which extend the spectrum responsive range and suppress the charge recombination of g-C 3 N 4 . This is the first report on the photocatalytic reductive removal of PCDDs and may provide a new approach for PCDDs pollution control. Copyright © 2018 Elsevier B.V. All rights reserved.

Microstructure & properties of SiC-AlN multiphase ceramics

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

Pan, Y.B.; Tan, S.H.; Jiang, D.L.

It is that AlN and SiC mixture could form solid solution at the temperature from 1800{degrees}C to 2100{degrees}C, its result will be conducive to important benefits for the improving to study and develop on the silicon carbide ceramics. The effect of AlN as a mainly additive phase on silicon carbide ceramic were investigated in this paper. For the optimum hot press(HP) process, SiC and AlN mixture formed solid solution at the 1950{degrees}C--2050{degrees}C in Ar environment. The properties of SiC-AlN composition were that bending strength more than 600 MPa and fracture toughness more than 7 MPa.m{sup 1/2} at the room temperature(R.T)more » could be received, at the same time the strength hold ascertain value from R.T. to 1400{degrees}C in air. The dense samples were examined by metallograph, X-ray diffraction (XRD), scanning electron microscope (SEM) & transmission electron microscope (TEM) to determine the fracture structure, interface phase, crack spread etc.« less

A comparative study of CeO2-Al2O3 support prepared with different methods and its application on MoO3/CeO2-Al2O3 catalyst for sulfur-resistant methanation

NASA Astrophysics Data System (ADS)

Jiang, Minhong; Wang, Baowei; Yao, Yuqin; Li, Zhenhua; Ma, Xinbin; Qin, Shaodong; Sun, Qi

2013-11-01

The CeO2-Al2O3 supports prepared with impregnation (IM), deposition precipitation (DP), and solution combustion (SC) methods for MoO3/CeO2-Al2O3 catalyst were investigated in the sulfur-resistant methanation. The supports and catalysts were characterized by N2-physisorption, transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy (RS), and temperature-programmed reduction (TPR). The N2-physisorption results indicated that the DP method was favorable for obtaining better textural properties. The TEM and RS results suggested that there is a CeO2 layer on the surface of the support prepared with DP method. This CeO2 layer not only prevented the interaction between MoO3 and γ-Al2O3 to form Al2(MoO4)3 species, but also improved the dispersion of MoO3 in the catalyst. Accordingly, the catalysts whose supports were prepared with DP method exhibited the best catalytic activity. The catalysts whose supports were prepared with SC method had the worst catalytic activity. This was caused by the formation of Al2(MoO4)3 and crystalline MoO3. Additionally, the CeO2 layer resulted in the instability of catalysts in reaction process. The increasing of calcination temperature of supports reduced the catalytic activity of all catalysts. The decrease extent of the catalysts whose supports were prepared with DP method was the lowest as the CeO2 layer prevented the interaction between MoO3 and γ-Al2O3.

Results of Neoadjuvant Short-Course Radiation Therapy Followed by Transanal Endoscopic Microsurgery for T1-T2 N0 Extraperitoneal Rectal Cancer

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

Arezzo, Alberto, E-mail: alberto.arezzo@unito.it; Arolfo, Simone; Allaix, Marco Ettore

Purpose: This study was undertaken to assess the short-term outcomes of neoadjuvant short-course radiation therapy (SCRT) followed by transanal endoscopic microsurgery (TEM) for T1-T2 N0 extraperitoneal rectal cancer. Recent studies suggest that neoadjuvant radiation therapy followed by TEM is safe and has results similar to those with abdominal rectal resection for the treatment of extraperitoneal early rectal cancer. Methods and Materials: We planned a prospective pilot study including 25 consecutive patients with extraperitoneal T1-T2 N0 M0 rectal adenocarcinoma undergoing SCRT followed by TEM 4 to 10 weeks later (SCRT-TEM). Safety, efficacy, and acceptability of this treatment modality were compared with historicalmore » groups of patients with similar rectal cancer stage and treated with long-course radiation therapy (LCRT) followed by TEM (LCRT-TEM), TEM alone, or laparoscopic rectal resection with total mesorectal excision (TME) at our institution. Results: The study was interrupted after 14 patients underwent SCRT of 25 Gy in 5 fractions followed by TEM. Median time between SCRT and TEM was 7 weeks (range: 4-10 weeks). Although no preoperative complications occurred, rectal suture dehiscence was observed in 7 patients (50%) at 4 weeks follow-up, associated with an enterocutaneous fistula in the sacral area in 2 cases. One patient required a colostomy. Quality of life at 1-month follow-up, according to European Organization for Research and Treatment of Cancer QLQ-C30 survey score, was significantly worse in SCRT-TEM patients than in LCRT-TEM patients (P=.0277) or TEM patients (P=.0004), whereas no differences were observed with TME patients (P=.604). At a median follow-up of 10 months (range: 6-26 months), we observed 1 (7%) local recurrence at 6 months that was treated with abdominoperineal resection. Conclusions: SCRT followed by TEM for T1-T2 N0 rectal cancer is burdened by a high rate of painful dehiscence of the suture line and

Structural, magnetic and dielectric properties of polyaniline/MnCoFe2O4 nanocomposites

NASA Astrophysics Data System (ADS)

Chitra, Palanisamy; Muthusamy, Athianna; Jayaprakash, Rajan

2015-12-01

Ferromagnetic PANI containing MnCoFe2O4 nanocomposites were synthesized by in-situ chemical polymerization of aniline incorporated MnCoFe2O4 nanoparticles (20%, 10% w/w of fine powders) with and without ultrasonic treatment. The MnCoFe2O4 nanoparticles were synthesized by auto combustion method. The PANI/MnCoFe2O4 nanocomposites were characterized with Fourier transform infrared (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The average particle size of the resulting PANI/MnCoFe2O4 nanocomposites was confirmed from the TEM and XRD analysis. The structure and morphology of the composites were confirmed by FT-IR spectroscopy, XRD and SEM. In addition, the electrical and magnetic properties of the nanocomposites were investigated. The PANI/MnCoFe2O4 nanocomposites under applied magnetic field exhibited the hysteresis loops of ferromagnetic nature at room temperature. The variation of Dielectric constant, Dielectric loss, and AC conductivity of PANI/MnCoFe2O4 nanocomposites at room temperature as a function of frequency in the range 50 Hz-5 MHz has been studied. Effect of ultrasonication on the PANI/MnCoFe2O4 nanocomposites was also investigated.

Stable tetragonal phase and magnetic properties of Fe-doped HfO2 nanoparticles

NASA Astrophysics Data System (ADS)

Sales, T. S. N.; Cavalcante, F. H. M.; Bosch-Santos, B.; Pereira, L. F. D.; Cabrera-Pasca, G. A.; Freitas, R. S.; Saxena, R. N.; Carbonari, A. W.

2017-05-01

In this paper, the effect in structural and magnetic properties of iron doping with concentration of 20% in hafnium dioxide (HfO2) nanoparticles is investigated. HfO2 is a wide band gap oxide with great potential to be used as high-permittivity gate dielectrics, which can be improved by doping. Nanoparticle samples were prepared by sol-gel chemical method and had their structure, morphology, and magnetic properties, respectively, investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) with electron back scattering diffraction (EBSD), and magnetization measurements. TEM and SEM results show size distribution of particles in the range from 30 nm to 40 nm with small dispersion. Magnetization measurements show the blocking temperature at around 90 K with a strong paramagnetic contribution. XRD results show a major tetragonal phase (94%).

Evaluation of electrical properties of Cr/CrN nano-multilayers for electronic applications.

PubMed

Marulanda, D M; Olaya, J J; Patiño, E J

2011-06-01

The electrical properties of Cr/CrN nano-multilayers produced by Unbalanced Magnetron Sputtering have been studied as a function of bilayer period and total thickness. Two groups of multilayers were produced: in the first group the bilayer period varied between 20 nm, 100 nm and 200 nm with total thickness of 1 microm, and in the second group the bilayer period varied between 25 nm, 50 nm and 100 nm and a total thickness of 100 nm. X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) were used in order to investigate the microstructure characteristics of the multilayers, and the Four Point Probe (FPP) method was used to evaluate in-plane and transverse electrical resistivity. XRD results show (111) and (200) orientations for all the CrN coatings and the presence of a multilayer structure was confirmed through SEM studies. Transverse electrical resistivity results show that this property is strongly dependent on the bilayer period.

Effect of porphyrin on photocatalytic activity of TiO2 nanoparticles toward Rhodamine B photodegradation.

PubMed

Ahmed, M A; Abou-Gamra, Z M; Medien, H A A; Hamza, M A

2017-11-01

As known, porphyrins have central role in photosynthesis, biological oxidation and reduction and oxygen transport beside to their intensive color which qualify them to be good photosensitizers. Herein, tetra (4-carboxyphenyl) porphyrin (TCPP) was prepared by a simple one-pot synthesis to use as a visible antenna for TiO 2 nanoparticles that were prepared via a simple template-free sol-gel method. Various loading percentages of TCPP (0.05-1%) were incorporated on the surface of TiO 2 as photosensitizer for photocatalytic degradation of Rhodamine B (Rh B) dye as a primary cationic pollutant model. Among them, 0.1% TCPP-TiO 2 was the most reactive sample. It was found that the photoactivity of 0.1% TCPP-TiO 2 sample (0.5g/L) was approximately 1.5 times greater than that of pure TiO 2 (0.5g/L) toward the degradation of Rh B (1×10 -5 M) under UV-A irradiation. Transient fluorescence decay measurements showed that the life time of TiO 2 excited state has doubled after anchoring TCPP, thus the probability of electron-hole recombination has decreased. The samples were characterized by XRD, HR-TEM, DRS and N 2 adsorption-desorption isotherms. The XRD patterns confirmed the successful preparation of TiO 2 nanoparticles with average crystalline size of 25.7nm. Also, XRD patterns suggested the presence of mixed phase TiO 2 nanoparticles of 77% anatase and 23% rutile. DRS showed that the characteristic peaks of TCPP covered the whole visible range 400-700nm. HR-TEM images showed the spheroids shape of TiO 2 nanoparticles and confirmed the presence of anatase and rutile phases as suggested from XRD data. The different parameters affecting the photodegradation of Rh B dye such as catalyst dose, dye concentration and pH were studied to obtain the optimum conditions. Almost complete degradation of Rh B was obtained which confirmed by HPLC and TOC measurements. The effect of scavengers was studied to indicate the most active species. TCPP-TiO 2 gave a good response toward the

Synthesis of Fe3O4@SiO2@OSi(CH2)3NHRN(CH2PPh2)2PdCl2 type nanocomposite complexes: Highly efficient and magnetically-recoverable catalysts in vitamin K3 synthesis.

PubMed

Uruş, Serhan

2016-12-15

The synthesis of aminomethylphosphine-metal complexes have opened a new perspective to the catalytic applications of organic compounds. Magnetic Fe3O4 nano-core was synthesized using the closed quartz tube with Teflon cover and microwaved 200°C for 1h with power controlled instrument set to max. 600W. Novel nano-composite supported; Fe3O4@SiO2(CH2)3NHArN(CH2PPh2)2 and Fe3O4@SiO2(CH2)3N(CH2PPh2)2 type bis(diphenylphosphinomethyl)amino ligands and their Pd(II) complexes have been synthesized and characterized with FT-IR, SEM, EDX, TEM, UV-Visible, XRD and TG/DTA techniques. All the complexes were used as heterogeneous catalysts in the oxidation of 2-methyl naphthalene (2MN) to 2-methyl-1, 4-naphthoquinone (vitamin K3, menadione, 2MNQ) in the presence of hydrogen peroxide and acetic acid. Selectivity reached about 55-60% with a conversion of 90-96% using the nano-magnetite supported aminomethylphosphine-Pd(II) complexes. The complexes were very active in three times in the catalytic recycling experiments in five catalytic cycles. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis of ultrasmooth nanostructured diamond films by microwave plasma chemical vapor deposition using a He/H(2)/CH(4)/N(2) gas mixture.

PubMed

Chowdhury, S; Hillman, Damon A; Catledge, Shane A; Konovalov, Valery V; Vohra, Yogesh K

2006-10-01

Ultrasmooth nanostructured diamond (USND) films were synthesized on Ti-6Al-4V medical grade substrates by adding helium in H(2)/CH(4)/N(2) plasma and changing the N(2)/CH(4) gas flow from 0 to 0.6. We were able to deposit diamond films as smooth as 6 nm (root-mean-square), as measured by an atomic force microscopy (AFM) scan area of 2 μm(2). Grain size was 4-5 nm at 71% He in (H(2) + He) and N(2)/CH(4) gas flow ratio of 0.4 without deteriorating the hardness (~50-60 GPa). The characterization of the films was performed with AFM, scanning electron microscopy, x-ray diffraction (XRD), Raman spectroscopy, and nanoindentation techniques. XRD and Raman results showed the nanocrystalline nature of the diamond films. The plasma species during deposition were monitored by optical emission spectroscopy. With increasing N(2)/CH(4) feedgas ratio (CH(4) was fixed) in He/H(2)/CH(4)/N(2) plasma, a substantial increase of CN radical (normalized by Balmer H(α) line) was observed along with a drop in surface roughness up to a critical N(2)/CH(4) ratio of 0.4. The CN radical concentration in the plasma was thus correlated to the formation of ultrasmooth nanostructured diamond films.

Flower-like morphology of blue and greenish-gray ZnCoxAl2-xO4 nanopigments

NASA Astrophysics Data System (ADS)

Wahba, Adel Maher; Imam, N. G.; Mohamed, Mohamed Bakr

2016-02-01

In the present work, ZnCoxAl2 - xO4 (x = 0.00-1.50) nanosized pigments were synthesized for the first time by citrate-precursor autocombustion method and heat treatment at 900 °C. In this new nanopigment system the vacancies participate in the spinel structure since the divalent cobalt ions substitute the trivalent Al ions. Structural, microstructural and optical properties were investigated using XRD, FTIR, TEM, HRSEM, XRF, and PL techniques. XRD and FTIR spectra proved the formation of a pure cubic spinel phase. Size of the synthesized nano-crystals ranges from 15 to 60 nm, which is further confirmed with TEM micrographs. HRSEM confirms the microporous nature with flower-like morphology of the prepared nanopigments. Cation distribution has been suggested for the whole samples that matches quite well with XRD and IR experimental data. PL results show that the ZnCoxAl2 - xO4 pigments have good potential for use as a yellow-orange phosphor for displays and/or white light-emitting diodes.

Phase Transformation of VO2 Nanoparticles Assisted by Microwave Heating

PubMed Central

Sikong, Lek.

2014-01-01

The microwave assisted synthesis nowadays attracts a great deal of attention. Monoclinic phase VO2 (M) was prepared from NH4VO3 and H2C2O4 · 2H2O by a rapid microwave assisted technique. The synthesis parameters, microwave irradiation time, microwave power, and calcinations temperature were systematically varied and their influences on the structure and morphology were evaluated. The microwave power level has been carried out in range 180–600 W. TEM analysis demonstrated nanosized samples. The structural and morphological properties were measured using XRD, TEM, and thermal analyses. The variations of vanadium phase led to thermochromic properties. PMID:24688438

Synthesis and photocatalytic properties of TiO{sub 2} nanostructures

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

Xia, X.H.; Liang, Y.; Wang, Z.

2008-08-04

TiO{sub 2} particles, rods, flowers and sheets were prepared by hydrothermal method via adjusting the temperature, the pressure and the concentration of TiCl{sub 4}. The as-prepared TiO{sub 2} powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra and N{sub 2} adsorption-desorption measurements. It was found that pressure is the most important factor influencing the morphology of TiO{sub 2}. The photocatalytic activity of the products was evaluated by the photodegradation of aqueous brilliant red X-3B solution under UV light. Among the as-prepared nanostructures, the flower-like TiO{sub 2}more » exhibited the highest photocatalytic activity.« less

Preparation and photoelectrocatalytic performance of N-doped TiO2/NaY zeolite membrane composite electrode material.

PubMed

Cheng, Zhi-Lin; Han, Shuai

2016-01-01

A novel composite electrode material based on a N-doped TiO2-loaded NaY zeolite membrane (N-doped TiO2/NaY zeolite membrane) for photoelectrocatalysis was presented. X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-visible (UV-vis) and X-ray photoelectron spectroscopy (XPS) characterization techniques were used to analyze the structure of the N-doped TiO2/NaY zeolite membrane. The XRD and SEM results verified that the N-doped TiO2 nanoparticles with the size of ca. 20 nm have been successfully loaded on the porous stainless steel-supported NaY zeolite membrane. The UV-vis result showed that the N-doped TiO2/NaY zeolite membrane exhibited a more obvious red-shift than that of N-TiO2 nanoparticles. The XPS characterization revealed that the doping of N element into TiO2 was successfully achieved. The photoelectrocatalysis performance of the N-doped TiO2/NaY zeolite membrane composite electrode material was evaluated by phenol removal and also the effects of reaction conditions on the catalytic performance were investigated. Owing to exhibiting an excellent catalytic activity and good recycling stability, the N-doped TiO2/NaY zeolite membrane composite electrode material was of promising application for photoelectrocatalysis in wastewater treatment.

In situ TEM observation of heterogeneous phase transition of a constrained single-crystalline Ag2Te nanowire.

PubMed

In, Juneho; Yoo, Youngdong; Kim, Jin-Gyu; Seo, Kwanyong; Kim, Hyunju; Ihee, Hyotchel; Oh, Sang Ho; Kim, Bongsoo

2010-11-10

Laterally epitaxial single crystalline Ag2Te nanowires (NWs) are synthesized on sapphire substrates by the vapor transport method. We observed the phase transitions of these Ag2Te NWs via in situ transmission electron microscopy (TEM) after covering them with Pt layers. The constrained NW shows phase transition from monoclinic to a body-centered cubic (bcc) structure near the interfaces, which is ascribed to the thermal stress caused by differences in the thermal expansion coefficients. Furthermore, we observed the nucleation and growth of bcc phase penetrating into the face-centered cubic matrix at 200 °C by high-resolution TEM in real time. Our results would provide valuable insight into how compressive stresses imposed by overlayers affect behaviors of nanodevices.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

ZrO2-modified mesoporous nanocrystalline TiO2-xNx as efficient visible light photocatalysts.

PubMed

Wang, Xinchen; Yu, Jimmy C; Chen, Yilin; Wu, Ling; Fu, Xianzhi

2006-04-01

Mesoporous nanocrystalline TiO2-xNx and TiO2-xNx/ZrO2 visible-light photocatalysts have been prepared by a sol-gel method. The photocatalysts were characterized by XRD, N2 adsorption-desorption, TEM, XPS, UV/Vis, and IR spectroscopy. The photocatalytic activity of the samples was evaluated by the decomposition of ethylene in air under visible light (lambda > 450 nm) illumination. Results revealed that nitrogen was doped into the lattice of TiO2 by the thermal treatment of NH3-adsorbed TiO2 hydrous gels, converting the TiO2 into a visible-light responsive catalyst. The introduction of ZrO2 into TiO2-xNx considerably inhibits the undesirable crystal growth during calcination. Consequently, the ZrO2-modified TiO2-xNx displays higher porosity, higher specific surface area, and an improved thermal stability over the corresponding unmodified TiO2-xNx samples.

Realizing p-Type MoS2 with Enhanced Thermoelectric Performance by Embedding VMo2S4 Nanoinclusions.

PubMed

Kong, Shuang; Wu, Tianmin; Zhuang, Wei; Jiang, Peng; Bao, Xinhe

2018-01-18

Two-dimensional transition-metal dichalcogenide semiconductors (TMDCs) such as MoS 2 are attracting increasing interest as thermoelectric materials owing to their abundance, nontoxicity, and promising performance. Recently, we have successfully developed n-type MoS 2 thermoelectric material via oxygen doping. Nevertheless, an efficient thermoelectric module requires both n-type and p-type materials with similar compatibility factors. Here, we present a facile approach to obtain a p-type MoS 2 thermoelectric material with a maximum figure of merit of 0.18 through the introduction of VMo 2 S 4 as a second phase by vanadium doping. VMo 2 S 4 nanoinclusions, confirmed by X-ray powder diffraction (XRD) and transmission electron microscopy (TEM) measurements, not only improve the electrical conductivity by simultaneously increasing the carrier concentration and the mobility but also result in the reduction of lattice thermal conductivity by enhancing the interface phonon scattering. Our studies not only shed new light toward improving thermoelectric performance of TMDCs by a facile elemental doping strategy but also pave the way toward thermoelectric devices based on TMDCs.

Study the oxidation kinetics of uranium using XRD and Rietveld method

NASA Astrophysics Data System (ADS)

Zhang, Yanzhi; Guan, Weijun; Wang, Qinguo; Wang, Xiaolin; Lai, Xinchun; Shuai, Maobing

2010-03-01

The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50~300°C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO2 was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO2 can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

PubMed

Saravanan, Thulasingam; Raj, Srinivasan Gokul; Chandar, Nagamuthu Raja Krishna; Jayavel, Ramasamy

2015-06-01

Y2O3 nanoparticles were synthesized by co-precipitation route using yttrium nitrate hexahydrate and ammonium hydroxide as precursors. The prepared sample was calcined at 500 degrees C and subjected to various characterization studies like thermal analysis (TG/DTA), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-visible (UV-Vis) and photoluminescence (PL) spectroscopy. The XRD pattern showed the cubic fluorite structure of Y2O3 without any impurity peaks, revealing high purity of the prepared sample. TEM images revealed that the calcined Y2O3 nanoparticles consist of spherical-like morphology with an average particle size of 12 nm. The absorption spectrum of calcined samples shows blue-shift compared to the as-prepared sample, which was further confirmed by PL studies. The possible formation mechanism of Y2O3 nanoparticles has been discussed based on the experimental results. Electrochemical behavior of Y2O3 nanoparticles was studied by cyclic voltammetry to assess their suitability for supercapacitor applications.

Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

n-Hexane hydro-isomerization over promoted Pd/HZSM-5 catalysts

NASA Astrophysics Data System (ADS)

Thoa Dao, Thi Kim; Loc Luu, Cam

2015-09-01

A series of Pd/HZSM-5 catalysts modified by various metallic species, including Co, Ni, Fe, Re, and Cu, was prepared by sequential impregnation. Contents of Pd and second metals in modified catalysts were 0.8 and 1.0 wt%, respectively. Physico-chemical characteristics of catalysts were investigated by nitrogen physi-sorption (BET), x-ray diffraction (XRD), transmission electron microscopy (TEM), ammonia temperature programmed desorption (NH3-TPD), temperature programmed reduction (TPR) and hydrogen pulse chemisorption (HPC). Coke formation was studied by the method of thermogravimetric analysis (TGA). The activities of catalysts in n-hexane isomerization were studied in a micro-flow reactor under atmospheric pressure at 250 °C, and molar ratio of H2: n-hexane of 5.92. It was found that Co, Ni, Fe, and Re additives exhibited geometric and electronic effects toward Pd/HZSM-5 catalyst, leading to an enhancement of its activity and stability. On the contrary, Cu additive caused Pd/HZSM-5 to become poorer in activity and stability.

Epitaxial integration of CoFe2O4 thin films on Si (001) surfaces using TiN buffer layers

NASA Astrophysics Data System (ADS)

Prieto, Pilar; Marco, José F.; Prieto, José E.; Ruiz-Gomez, Sandra; Perez, Lucas; del Real, Rafael P.; Vázquez, Manuel; de la Figuera, Juan

2018-04-01

Epitaxial cobalt ferrite thin films with strong in-plane magnetic anisotropy have been grown on Si (001) substrates using a TiN buffer layer. The epitaxial films have been grown by ion beam sputtering using either metallic, CoFe2, or ceramic, CoFe2O4, targets. X-ray diffraction (XRD) and Rutherford spectrometry (RBS) in random and channeling configuration have been used to determine the epitaxial relationship CoFe2O4 [100]/TiN [100]/Si [100]. Mössbauer spectroscopy, in combination with XRD and RBS, has been used to determine the composition and structure of the cobalt ferrite thin films. The TiN buffer layer induces a compressive strain in the cobalt ferrite thin films giving rise to an in-plane magnetic anisotropy. The degree of in-plane anisotropy depends on the lattice mismatch between CoFe2O4 and TiN, which is larger for CoFe2O4 thin films grown on the reactive sputtering process with ceramic targets.

Technical Evaluation Motor No. 7 (TEM-7)

NASA Technical Reports Server (NTRS)

Hughes, Phil

1991-01-01

The Technical Evaluation Motor No. 7 (TEM-7) test was a full-scale, full duration static test firing of a high performance motor-configuration solid rocket motor with nozzle vectoring. The final test report documents the procedures, performance, and results of the static test firing of TEM-7. All observations, discussions, conclusions, and recommendations included in the report are complete and final except for the TEM-7 fixed housing unbond investigation. A presentation and discussion of TEM-7 performance, anomalies, and test result concurrence with the objectives outlined in CTP-0107, Rev A, Space Shuttle Technical Evaluation Motor No. 7 (TEM-7) Static Fire Test Plan are included.

In-situ heating TEM observation of microscopic structural changes of size-controlled metallic copper/gelatin composite.

PubMed

Narushima, Takashi; Hyono, Atsushi; Nishida, Naoki; Yonezawa, Tetsu

2012-10-01

Copper/gelatin composite particles with controlled sizes were prepared at room temperature from cupric sulfate pentahydrate in the presence of gelatin as a protective reagent by using hydrazine monohydrate as a reducing agent. The formed particles with the size between 190-940 nm were secondary aggregated particles which were composed of smaller nanosized particles ("particle-in-particle"), the presence of which was established by XRD patterns and a cross-sectional TEM image. The sintering behavior of these copper/gelatin composite particles was demonstrated by in-situ heating TEM under a high vacuum (approximately 10(-5) Pa) and separately with the oxygen partial pressure controlled at the 10(-4) Pa level. It was established that the particles began to sinter at about 330 degrees C with the oxygen and that they sublimate above 450 degrees C both in the vacuum and oxygen conditions. This result shows that the introduction of an adequate amount of oxygen was effective to remove the gelatin surrounding the particles. It can also be concluded that the sintering of the copper/gelatin composite particles occurred even in the absence of a reducing agent such as hydrogen gas.

Formation of Al15Mn3Si2 Phase During Solidification of a Novel Al-12%Si-4%Cu-1.2%Mn Heat-Resistant Alloy and Its Thermal Stability

NASA Astrophysics Data System (ADS)

Suo, Xiaojing; Liao, Hengcheng; Hu, Yiyun; Dixit, Uday S.; Petrov, Pavel

2018-02-01

The formation of Al15Mn3Si2 phase in Al-12Si-4Cu-1.2Mn (wt.%) alloy during solidification was investigated by adopting CALPHAD method and microstructural observation by optical microscopy, SEM-EDS, TEM-EDS/SAD and XRD analysis; SEM fixed-point observation method was applied to evaluate its thermal stability. As-cast microstructural observation consistently demonstrates the solidification sequence of the studied alloy predicted by phase diagram calculation. Based on the phase diagram calculation, SEM-EDS, TEM-EDS/SAD and XRD analysis, as well as evidences on Al-Si-Mn-Fe compounds from the literature, the primary and eutectic Mn-rich phases with different morphologies in the studied alloy are identified to be Al15Mn3Si2 that has a body-centered cubic (BCC) structure with a lattice constant of a = 1.352 nm. SEM fixed-point observation and XRD analysis indicate that Al15Mn3Si2 phase has more excellent thermal stability at high temperature than that of CuAl2 phase and can serve as the major strengthening phase in heat-resistant aluminum alloy that has to face a high-temperature working environment. Results of tension test show that addition of Mn can improve the strength of Al-Si-Cu alloy, especially at elevated temperature.

In-situ XRD vs ex-situ vacuum annealing of tantalum oxynitride thin films: Assessments on the structural evolution

NASA Astrophysics Data System (ADS)

Cunha, L.; Apreutesei, M.; Moura, C.; Alves, E.; Barradas, N. P.; Cristea, D.

2018-04-01

The purpose of this work is to discuss the main structural characteristics of a group of tantalum oxynitride (TaNxOy) thin films, with different compositions, prepared by magnetron sputtering, and to interpret and compare the structural changes, by X-ray diffraction (XRD), when the samples are vacuum annealed under two different conditions: i) annealing, followed by ex-situ XRD: one sample of each deposition run was annealed at a different temperature, until a maximum of 800 °C, and the XRD patterns were obtained, at room temperature, after each annealing process; ii) annealing with in-situ XRD: the diffraction patterns are obtained, at certain temperatures, during the annealing process, using always the same sample. In-situ XRD annealing could be an interesting process to perform annealing, and analysing the evolution of the structure with the temperature, when compared to the classical process. A higher structural stability was observed in some of the samples, particularly on those with highest oxygen content, but also on the sample with non-metal (O + N) to metal (Ta) ratio around 0.5.

Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

NASA Technical Reports Server (NTRS)

Blake, D. F.; Bish, D.; Vaniman, D.; Chipera, S.; Sarrazin, P.; Collins, S. A.; Elliott, S. T.

2001-01-01

X-Ray Diffraction (XRD) is the most direct and accurate method for determining mineralogy. The CHEMIN XRD/XRF instrument has shown promising results on a variety of mineral and rock samples. Additional information is contained in the original extended abstract.

Comparing Time Domain Electromagnetics (TEM) and Early-Time TEM for Mapping Highly Conductive Groundwater in Mars Analog Environments

NASA Astrophysics Data System (ADS)

Jernsletten, J. A.

2005-05-01

Introduction: The purpose of this study is to evaluate the use of (diffusive) Time Domain Electromagnetics (TEM) for sounding of subsurface water in conductive Mars analog environments. To provide a baseline for such studies, I show data from two field studies: 1) Diffusive sounding data (TEM) from Pima County, Arizona; and 2) Shallower sounding data using the Fast-Turnoff TEM method from Peña de Hierro in the Rio Tinto region of Spain. The latter is data from work conducted under the auspices of the Mars Analog Research and Technology Experiment (MARTE). Pima County TEM Survey: A TEM survey was carried out in Pima County, Arizona, in January 2003. Data was collected using 100 m Tx loops and a ferrite-cored magnetic coil Rx antenna, and processed using commercial software. The survey used a 16 Hz sounding frequency, which is sensitive to slightly salty groundwater. Prominent features in the data from Arizona are the ~500 m depth of investigation and the ~120 m depth to the water table, confirmed by data from four USGS test wells surrounding the field area. Note also the conductive (~20-40 ω m) clay-rich soil above the water table. Rio Tinto Fast-Turnoff TEM Survey: During May and June of 2003, a Fast-Turnoff (early time) TEM survey was carried out at the Peña de Hierro field area of the MARTE project, near the town of Nerva, Spain. Data was collected using 20 m and 40 m Tx loop antennae and 10 m loop Rx antennae, with a 32 Hz sounding frequency. Data from Line 4 (of 16) from this survey, collected using 40 m Tx loops, show ~200 m depth of investigation and a conductive high at ~90 m depth below Station 20 (second station of 10 along this line). This is the water table, matching the 431 m MSL elevation of the nearby pit lake. The center of the "pileup" below Station 60 is spatially coincident with the vertical fault plane located here. Data from Line 15 and Line 14 of the Rio Tinto survey, collected using 20 m Tx loops, achieve ~50 m depth of investigation and

The Differential Roles of Budding Yeast Tem1p, Cdc15p, and Bub2p Protein Dynamics in Mitotic ExitD⃞V⃞

PubMed Central

Molk, Jeffrey N.; Schuyler, Scott C.; Liu, Jenny Y.; Evans, James G.; Salmon, E. D.; Pellman, David; Bloom, Kerry

2004-01-01

In the budding yeast Saccharomyces cerevisiae the mitotic spindle must be positioned along the mother-bud axis to activate the mitotic exit network (MEN) in anaphase. To examine MEN proteins during mitotic exit, we imaged the MEN activators Tem1p and Cdc15p and the MEN regulator Bub2p in vivo. Quantitative live cell fluorescence microscopy demonstrated the spindle pole body that segregated into the daughter cell (dSPB) signaled mitotic exit upon penetration into the bud. Activation of mitotic exit was associated with an increased abundance of Tem1p-GFP and the localization of Cdc15p-GFP on the dSPB. In contrast, Bub2p-GFP fluorescence intensity decreased in mid-to-late anaphase on the dSPB. Therefore, MEN protein localization fluctuates to switch from Bub2p inhibition of mitotic exit to Cdc15p activation of mitotic exit. The mechanism that elevates Tem1p-GFP abundance in anaphase is specific to dSPB penetration into the bud and Dhc1p and Lte1p promote Tem1p-GFP localization. Finally, fluorescence recovery after photobleaching (FRAP) measurements revealed Tem1p-GFP is dynamic at the dSPB in late anaphase. These data suggest spindle pole penetration into the bud activates mitotic exit, resulting in Tem1p and Cdc15p persistence at the dSPB to initiate the MEN signal cascade. PMID:14718561

Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods

NASA Astrophysics Data System (ADS)

Sivakami, R.; Dhanuskodi, S.; Karvembu, R.

2016-01-01

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55 eV. BET measurements show a high specific surface area (SSA) of 118-133 m2/g and pore diameter (10-25 nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM.

Investigation of Y/SBA Composite Molecular Sieves Morphology Control and Catalytic Performance for n-Pentane Aromatization

PubMed Central

Shi, Chun-Wei; Wu, Wen-Yuan; Li, Shuai; Bian, Xue; Zhao, Shan-lin; Pei, Ming-Yuan

2016-01-01

Using Y molecular sieve as the core, Y/SBA-15 composite molecular sieves were prepared by different crystallization methods in the paper. The growth process and morphologies of the composite molecular sieves were controlled by adjusting the synthesis factors. The structures and acidity of two kinds of composite molecular sieves were characterized by X-ray diffraction (XRD), N2 adsorption/desorption, transmission electron microscopy (TEM), and NH3-TPD. The catalysis performances of the composite molecular sieves were investigated in the aromatization reaction of n-pentane. The results indicated that the desired core-shell composite molecular sieves were obtained when the crystallization conditions were 36 hours, 100 °C and secondary crystallization. The aromatization results showed that core-shell composite molecular sieves had better selectivity for producing high application value xylenes compared to mixed-crystal composite molecular sieves. PMID:27029526

A facile method to synthesize nitrogen and fluorine co-doped TiO2 nanoparticles by pyrolysis of (NH4)2TiF6

NASA Astrophysics Data System (ADS)

Chen, Daimei; Jiang, Zhongyi; Geng, Jiaqing; Zhu, Juhong; Yang, Dong

2009-02-01

The nitrogen and fluorine co-doped TiO2 (N-F-TiO2) nanoparticles of anatase crystalline structure were prepared by a facile method of (NH4)2TiF6 pyrolysis, and characterized by thermogravimetry-differential thermal analysis (TG-DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and ultraviolet visible (UV-Vis) spectroscopy etc. With the increase of calcination temperature, (NH4)2TiF6 decomposed into TiOF2 and NH4TiOF3 at first, and then formed anatase-type TiO2 with thin sheet morphology. H3BO3 as oxygen source can promote the formation of anatase TiO2, but decrease the F content in the N-F-TiO2 materials due to the formation of volatile BF3 during the precursor decomposition. The photocatalytic activity of the obtained N-F-TiO2 samples was evaluated by the methylene blue degradation under visible light, and all the samples exhibited much higher photocatalytic activity than P25. Moreover, the merits and disadvantages of this proposed method to prepare doped TiO2 are discussed.

XMCD and TEM studies of as-cast and rapidly quenched Fe50Nd50 alloys

NASA Astrophysics Data System (ADS)

Menushenkov, V. P.; Menushenkov, A. P.; Shchetinin, I. V.; Wilhelm, F.; Ivanov, A. A.; Rudnev, I. A.; Ivanov, V. G.; Rogalev, A.; Savchenko, A. G.; Zhukov, D. G.; Rafalskiy, A. V.; Ketov, S. V.

2017-12-01

We present the XMCD analysis of as-cast and melt spun Fe50Nd50 samples performed at L2,3 -Nd and K-Fe absorption edges at 5 and 50 K in comparison with macroscopic data of XRD, TEM and magnetic properties measurements. In addition, we have measured the magnetic field dependence of XMCD signal for both types of the samples in magnetic fields up/down to 17 T. The obtained results pointed to the strong difference between structure and magnetic properties of the as-cast and melt spun Fe50Nd50 alloys for both macroscopic and local measurements. The element selective XMCD loops for melt spun alloy show almost identical value of the coercive force Hci for L 2-Nd and K-Fe edges and practically do not depend on temperature. XMCD loop at K-Fe edge is a sum of contributions of the Fe-based phases. The main Fe-rich phase has high Hci ≈ 2,4 T as a highly anisotropic phase. The absence of the K-Fe XMCD loop saturation in the field up to 17 T points to presence of the second Nd-rich Nd-Fe phase which is ferromagnetic at temperature lower than 50 K. In accordance to the TEM results these both phases may coexist as the mixture of nanocrystals which was formed as a result of decomposition of the amorphous-like matrix phase. The XMCD loop at L2 -Nd edge with Hci ≈ 1,9 T is the sum of contributions from two Nd-based phases: hard Fe-rich phase (Hci ≈ 2,4 T) and Nd-Fe matrix phase of medium hardness with Hci ≈ 1,3 T. The macroscopic loop showed the higher Hci compared to XMCD loops. Such discrepancy may be caused by the fact that XMCD signal is collected from a 5-10 mcm thick surface layer, which contains many defects that reduce anisotropy and coercivity.

Growth of high quality AlN films on CVD diamond by RF reactive magnetron sputtering

NASA Astrophysics Data System (ADS)

Chen, Liang-xian; Liu, Hao; Liu, Sheng; Li, Cheng-ming; Wang, Yi-chao; An, Kang; Hua, Chen-yi; Liu, Jin-long; Wei, Jun-jun; Hei, Li-fu; Lv, Fan-xiu

2018-02-01

A highly oriented AlN layer has been successfully grown along the c-axis on a polycrystalline chemical vapor deposited (CVD) diamond by RF reactive magnetron sputtering. Structural, morphological and mechanical properties of the heterostructure were investigated by Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), Transmission Electron Microscopy (TEM), X-ray diffraction (XRD), Nano-indentation and Four-probe meter. A compact AlN film was demonstrated on the diamond layer, showing columnar grains and a low surface roughness of 1.4 nm. TEM results revealed a sharp AlN/diamond interface, which was characterized by the presence of a distinct 10 nm thick buffer layer resulting from the initial AlN growth stage. The FWHM of AlN (002) diffraction peak and its rocking curve are as low as 0.41° and 3.35° respectively, indicating a highly preferred orientation along the c-axis. AlN sputtered films deposited on glass substrates show a higher bulk resistivity (up to 3 × 1012 Ω cm), compared to AlN films deposited on diamond (∼1010 Ω cm). Finally, the film hardness and Young's modulus of AlN films on diamond are 25.8 GPa and 489.5 GPa, respectively.

Effect of stabilization temperature during pyrolysis process of P84 co-polyimide-based tubular carbon membrane for H2/N2 and He/N2 separations

NASA Astrophysics Data System (ADS)

Sazali, N.; Salleh, W. N. W.; Ismail, A. F.; Ismail, N. H.; Aziz, F.; Yusof, N.; Hasbullah, H.

2018-04-01

In this study, the effect of stabilization temperature on the performance of tubular carbon membrane was being investigated. P84 co-polyimide-based tubular carbon membrane will be fabricated through the dip-coating technique. The tubular carbon membrane performance can be controlled by manipulating the pyrolysis conditions which was conducted at different stabilization temperatures of 250, 300, 350, 400, and 450°C under N2 environment (200 ml/min). The prepared membranes were characterized by using scanning electron microscopy (SEM), x-ray diffraction (XRD), and pure gas permeation system. The pure gas of H2, He, and N2 were used to determine the permeation properties of the carbon membrane. The P84 co-polyimide-based tubular carbon membrane stabilized at 300°C demonstrated an excellent permeation property with H2, He, and N2 gas permeance of 1134.51±2.87, 1287.22±2.86 and 2.98±1.28GPU, respectively. The highest H2/N2 and He/N2 selectivity of 380.71±2.34 and 431.95±2.61 was obtained when the stabilization temperature of 450°C was applied. It is concluded that the stabilization temperatures have protrusive effect on the carbon membrane properties specifically their pore structure, and eventually their gas separation properties.

RECENT DEVELOPMENT IN TEM CHARACTERIZATION OF IRRADIATED RERTR FUELS

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

J. Gan; B.D. Miller; D.D. Keiser Jr.

2011-10-01

The recent development on TEM work of irradiated RERTR fuels includes microstructural characterization of the irradiated U-10Mo/alloy-6061 monolithic fuel plate, the RERTR-7 U-7Mo/Al-2Si and U-7Mo/Al-5Si dispersion fuel plates. It is the first time that a TEM sample of an irradiated nuclear fuel was prepared using the focused-ion-beam (FIB) lift-out technical at the Idaho National Laboratory. Multiple FIB TEM samples were prepared from the areas of interest in a SEM sample. The characterization was carried out using a 200kV TEM with a LaB6 filament. The three dimensional orderings of nanometer-sized fission gas bubbles are observed in the crystalline region of themore » U-Mo fuel. The co-existence of bubble superlattice and dislocations is evident. Detailed microstructural information along with composition analysis is obtained. The results and their implication on the performance of these fuels are discussed.« less

Ultrasonic-assisted synthesis of nano lead(II) coordination polymer as precursors for preparation of lead(II) oxide nano-structures: Thermal, optical properties and XRD studies.

PubMed

Ghavidelaghdam, Elham; Shahverdizadeh, Gholam Hossein; Motameni Tabatabai, Javad; Mirtamizdoust, Babak

2018-04-01

Nano structure of a lead (II) coordination polymer [Pb 2 (C 2 Cl 3 O 2 ) 2 (NO 3 ) 2 (C l2 H 8 N 2 ) 2 ] n (1), has been synthesized by a sonochemical method in different concentrations. The nano particles were characterized by scanning electron microscopy (SEM) X-ray powder diffraction (XRD), FT-IR spectroscopy and elemental analyses. The thermal stability of nano structure is closely investigated via thermal gravimetric (TGA), and compared with crystalline structure. The compounds are then heated to 600 °C to produce PbO nano particles. The resulting PbO is characterized through XRD and SEM analyses. Concentration of initial reagents effects on size and morphology of nano-structured compound 1 have been studied and show that low concentrations of initial reagents decreased particles size and leaded to uniform nano particles morphology. The photoluminescence properties of the prepared compound, as crystalline and as nanoparticles, have been investigated. The result showed a good correlation between the size and emission wavelength. Copyright © 2017. Published by Elsevier B.V.

Synthesis, molecular structure, FT-IR and XRD investigations of 2-(4-chlorophenyl)-2-oxoethyl 2-chlorobenzoate: a comparative DFT study.

PubMed

Chidan Kumar, C S; Fun, Hoong Kun; Tursun, Mahir; Ooi, Chin Wei; Chandraju, Siddegowda; Quah, Ching Kheng; Parlak, Cemal

2014-04-24

2-(4-Chlorophenyl)-2-oxoethyl 2-chlorobenzoate has been synthesized, its structural and vibrational properties have been reported using FT-IR and single-crystal X-ray diffraction (XRD) studies. The conformational analysis, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of the synthesized compound (C15H10Cl2O3) have been examined by means of Becke-3-Lee-Yang-Parr (B3LYP) density functional theory (DFT) method together with 6-31++G(d,p) basis set. Furthermore, reliable conformational investigation and vibrational assignments have been made by the potential energy surface (PES) and potential energy distribution (PED) analyses, respectively. Calculations are performed with two possible conformations. The title compound crystallizes in orthorhombic space group Pbca with the unit cell dimensions a=12.312(5) Å, b=8.103(3) Å, c=27.565(11) Å, V=2750.0(19) Å(3). B3LYP method provides satisfactory evidence for the prediction of vibrational wavenumbers and structural parameters. Copyright © 2014 Elsevier B.V. All rights reserved.

Tetramethylene glycol mediated hydrothermal synthesis of defect-rich SnO2 nanoparticles for fast adsorption and degradation of MB dye

NASA Astrophysics Data System (ADS)

Rani, Barkha; Jadhao, Charushila Vasant; Sahu, Niroj Kumar

2018-04-01

Defect-rich pristine tin oxide nanoparticles (SnO2 NPs) with high colloidal stability have been synthesized by tetramethylene glycol (TMG) mediated hydrothermal process and characterized by XRD, TEM, Zeta Potential, PL spectroscopy and porosity measurement techniques. XRD result suggests the formation of rutile phase of SnO2 with average crystallite size of 2.65 nm. TMG act as a structure directing agent assist in the formation of network like structure of SnO2 NPs as confirmed from TEM. Significant blue shifts in the UV absorption spectrum as that of the bulk and defect bands in the PL spectrum are observed. The nanomaterial possesses very high surface area of 263.102 m2/g and large pore volume. The above properties strongly influence the photocatalytic degradation of methylene blue dye. Very fast adsorption and 96% degradation (under UV irradiation) has been achieved when 10 ppm methylene blue solutions is catalysed by 20 mg SnO2 NPs which pave the way for potential environmental application.

Technical Evaluation Motor No. 10 (TEM-10)

NASA Technical Reports Server (NTRS)

1993-01-01

Technical Evaluation Motor No. 10 (TEM-10) was static fired on 27 Apr. 1993 at the Thiokol Corporation full-scale motor static test bay, T-24. This final test report documents the procedures, performance, and results of the static test firing of TEM-10. All observations, discussions, conclusions, and recommendations contained are final. Included is a presentation and discussion of TEM-10 performance, anomalies, and test results in concurrence with the objectives outlined in CTP-0110, Revision D, Space Shuttle Technical Evaluation Motor No. 10 (TEM-10) Static Fire Test Plan.

Catalytic activity of Ru-Sn/Al2O3 in reduction reaction of pollutant 4-Nitrophenol

NASA Astrophysics Data System (ADS)

Rini, A. S.; Radiman, S.; Yarmo, M. A.

2018-03-01

Ru-Sn/Al2O3 bimetallic nanocatalysts have been synthesized by using conventional and microwave impregnation methods. Structure and morphology of the samples were characterized using XRD, XPS, and TEM. XRD and XPS measurement have confirmed the presence of Ru and Sn in the samples. According to TEM results, the morphology of the catalyst strongly depends on the preparation route and stabilizing agent (i.e. PVP). The sample with PVP (polyvinylpyrrolidone) has better nanoparticles distribution over the support. A sample prepared by conventional method has an agglomeration of nanoparticles on the support. Catalytic activities of both samples were examined in the reduction reaction of pollutant, i.e. 4-nitrophenol. Catalytic examination showed that reaction rate of 4-nitrophenol reduction by using microwave-assisted sample has improved 3.5 times faster than conventional impregnation sample.

Bio-mediated synthesis of TiO2 nanoparticles and its photocatalytic effect on aquatic biofilm.

PubMed

Dhandapani, Perumal; Maruthamuthu, Sundram; Rajagopal, Gopalakrishnan

2012-05-02

The nano-TiO(2) was synthesized biologically employing Bacillus subtilis (FJ460362). These nanoparticles were characterized by FTIR, TGA-DTA, UV-Visible spectroscopy, XRD and TEM. FTIR and TGA results confirm that the organic impurities were completely removed while calcinating the resultant products. Band gap value was estimated from the UV-Visible spectrum and anatase crystal phase was confirmed by XRD. TEM images reveal that these particles were agglomerated; mostly spherical in shape with an average particle size of 10-30nm. The synthesized nano-TiO(2) particles were coated on glass slides, biofilm were grown and subjected to irradiation of polychromatic light to understand photocatalytic activity in controlling the aquatic biofilm. The bacterial killing process was established by Epi-fluorescence microscopy. The results reveal that biogenic TiO(2) nanomaterial acts as good photocatalyst by the generation of H(2)O(2) in the vicinity of the TiO(2)-biofilm interfaces to suppress the growth of the aquatic biofilm. Copyright © 2012 Elsevier B.V. All rights reserved.

Study of GaN nanorods converted from β-Ga2O3

NASA Astrophysics Data System (ADS)

Li, Yuewen; Xiong, Zening; Zhang, Dongdong; Xiu, Xiangqian; Liu, Duo; Wang, Shuang; Hua, Xuemei; Xie, Zili; Tao, Tao; Liu, Bin; Chen, Peng; Zhang, Rong; Zheng, Youdou

2018-05-01

We report here high-quality β-Ga2O3 nanorods (NRs) grown on sapphire substrates by hydrothermal method. Ammoniating the β-Ga2O3 NRs results in strain-free wurtzite gallium nitride (GaN) NRs. It was shown by XRD and Raman spectroscopy that β-Ga2O3 was partially converted to GaN/β-Ga2O3 at 1000 °C and then completely converted to GaN NRs at 1050 °C, as confirmed by high-resolution transmission electron microscopy (HRTEM). There is no band-edge emission of β-Ga2O3 in the cathodoluminescence spectrum, and only a deep-level broad emission observed at 3.68-3.73 eV. The band edge emission (3.39 eV) of GaN NRs converted from β-Ga2O3 can also be observed.

Fabrication of novel ternary Au/CeO2@g-C3N4 nanocomposite: kinetics and mechanism investigation of 4-nitrophenol reduction, and benzyl alcohol oxidation

NASA Astrophysics Data System (ADS)

Kohantorabi, Mona; Gholami, Mohammad Reza

2018-06-01

Au nanoparticles supported on cerium oxide/graphitic carbon nitride (CeO2@g-C3N4) was synthesized and used as heterogeneous catalyst in redox reaction. The catalyst was characterized by different techniques such as FT-IR, XRD, FE-SEM, EDS, TEM, BET, TGA, and ICP. The as-prepared ternary nanocomposite was used as an effective catalyst for the reduction of toxic 4-nitrophenol to useful 4-aminophenol by NaBH4. The rate constant value of reduction reaction reached up to 0.106 s-1 by Au/CeO2@g-C3N4, which was 3.8, and 8.8 times higher than that of Au@CeO2 (0.028 s-1), and Au@g-C3N4 (0.012 s-1) nanocomposites, respectively. The superior catalytic performance of as-prepared catalyst in 4-NP reduction can be attributed to synergistic effect between Au nanoparticles and CeO2@g-C3N4 support, and efficient electron transfer. The reduction reaction was carried out at different temperatures, and the energy of activation ({Ea}), and thermodynamic parameters including, activation of entropy (Δ S^ ≠), enthalpy (Δ H^ ≠), and Gibbs free energy (Δ G^ ≠) were determined. Additionally, the mechanism of reaction was studied in details, and equilibrium constants of 4-NP ( K 4-NP), and {BH}4^{ - } ({K_{{BH}4^{{ - }} }}) were calculated using Langmuir-Hinshelwood model. Furthermore, this nanocomposite exhibited excellent catalytic activity in oxidation of benzyl alcohol by molecular oxygen as a green oxidant. This study revealed that the ternary Au/CeO2@g-C3N4 nanocomposite is an attractive candidate for catalytic applications.

Realization of improved metallization-Ti/Al/Ti/W/Au ohmic contacts to n-GaN for high temperature application

NASA Astrophysics Data System (ADS)

Motayed, A.; Davydov, A. V.; Boettinger, W. J.; Josell, D.; Shapiro, A. J.; Levin, I.; Zheleva, T.; Harris, G. L.

2005-05-01

Tungsten metal layer was used for the first time as an effective diffusion barrier for the standard Ti/Al/Ti/Au ohmic metallization scheme to obtain thermally stable ohmic contact suitable for high temperature applications. Comparative studies were performed on three distinct metallization schemes: 1) standard GaN/Ti/Al/Ti/Au, 2) GaN/Ti/Al/W/Au, and 3) GaN/Ti/Al/Ti/W/Au. For the GaN with doping level of 5 × 1017 cm-3, the lowest specific contact resistance for the Ti/Al/Ti/W/Au metallization scheme annealed in argon at 750 °C for 30 sec was 5 × 10-6 .cm2, which is comparable to the standard Ti/Al/Ti/Au scheme. X-ray diffractions (XRD), auger electron spectroscopy (AES) depth profiling, field-emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), and cross-sectional transmission electron microscopy (TEM) revealed that the Ti/Al/Ti/W/Au metallization has superior morphology and microstructural properties compared to standard Ti/Al/Ti/Au metallizations. Remarkably, this metallization was able to withstand thermal aging at 500 °C for 50 hrs with only marginal morphological and electrical deterioration. These studies revealed that the utilization of a compound diffusion barrier stack, as in the Ti/Al/Ti/W/Au metallization, yields electrically, structurally, and morphologically superior metallizations with exceptional thermal stability.

Non-Metal Doped Titania Photocatalysts for the Degradation of Neonicotinoid Insecticides Under Visible Light Irradiation.

PubMed

Joseph, Amala Infant Joice; Thiripuranthagan, Sivakumar

2018-05-01

Recombination of e-/h+ pair, the major issue of any titania based photocatalytic material, is addressed here by doping non-metals such as C, N, B, F into the lattice of nano TiO2. The as-synthesised catalysts were characterized by using various instrumental techniques such as X-ray diffraction (XRD), UV-Diffuse reflectance spectroscopy (UV-DRS), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Nanosize of titania was confirmed by both XRD and TEM studies. Visible light inactivity of TiO2 is overcome by C, N, B, F doped titania catalysts in the degradation of neonicotinoid type insecticides namely imidacloprid (IMI) and thiamethoxam (TMX). The degradation efficiencies of the catalysts under different irradiations namely UV, visible and solar were compared. Among the catalysts, CNBF/TiO2 degraded IMI completely at 150, 240 and 330 min whereas TMX has been degraded completely at 210, 270 and 420 min under UV, solar and visible irradiations respectively. The recyclability test of CNBF/TiO2 confirmed its stability towards photocatalytic reaction.

Thiol-modified MoS2 nanosheets as a functional layer for electrical bistable devices

NASA Astrophysics Data System (ADS)

Li, Guan; Tan, Fenxue; Lv, Bokun; Wu, Mengying; Wang, Ruiqi; Lu, Yue; Li, Xu; Li, Zhiqiang; Teng, Feng

2018-01-01

Molybdenum disulfide nanosheets have been synthesized by one-pot method using 1-ODT as sulfur source and surfactant. The structure, morphology and optical properties of samples were investigated by XRD, FTIR, Abs spectrum and TEM patterns. The XRD pattern indicated that the as-obtained MoS2 belong to hexagonal system. The as-obtained MoS2 nanosheets blending with PVK could be used to fabricate an electrically bistable devices through a simple spin-coating method and the device exhibited an obvious electrical bistability properties. The charge transport mechanism of the device was discussed based on the filamentary switching models.

Surfactant-free bio-synthesised Tio2 nanorods from Turbinaria conoides-a study on photocatalytic and anti-bacterial activity

NASA Astrophysics Data System (ADS)

Subhapriya, S.; Gomathipriya, P.

2018-06-01

In this study, Titania nanorods were synthesised from aqueous extract of Turbinaria conoides (brown seaweeds) (TiO2NRs-TC) under surfactant free medium. The photocatalytic activity of the synthesised nanorods was tested towards the photocatalytic decolourization using simulated dye wastewater containing Navy Blue HER (NBHER). The synthesised Titania nanorods were characterized by using x-ray diffraction (XRD), UV–visible spectroscopy (UV–vis), Scanning Electron Microscopy (SEM), Energy Dispersive Spectrophotometer (EDS) and Transmission Electron Microscopy (TEM). XRD pattern confirms the anatase phase formation and HR-SEM micrograph shows the presence of rod like structure with the size of about 50 nm. TEM analysis proves the rod like structure with a size of 45–50 nm which was in agreement with the XRD analysis and HR-SEM images. EDS and XDS confirmed the formation of Titania nanoparticles. The formation of TiO2NRs-TC has a beneficial influence on the dye Navy blue HER photodegradation. TiO2-TC nano rods also show superior photocatalytic ability in hydrogen generation (2.1 mmol/h‑1g‑1). The antibacterial activity of the synthesised nanoparticles was examined using disc diffusion method which showed diverse susceptibility of microorganisms to the Titania nanoparticles.

Effects of Nd-, Pr-, Tb- and Y-doping on the structural, textural, electrical and N2O decomposition activity of mesoporous NiO nanoparticles

NASA Astrophysics Data System (ADS)

Abu-Zied, Bahaa M.; Bawaked, Salem M.; Kosa, Samia A.; Ali, Tarek T.; Schwieger, Wilhelm; Aqlan, Faisal M.

2017-10-01

Recently, nickel oxide, NiO, promoted with various dopants showed an interesting activity behavior in N2O direct decomposition. In this paper, the activity of a series of rare earth (Nd, Pr, Tb and Y) doped NiO catalysts was investigated for this reaction. These catalysts have been prepared by the calcination of their corresponding oxalate mixtures, which have been synthesized via the microwave-assisted precipitation route using oxalic acid as precipitant. Characterization of the obtained catalysts was carried out by using various physico-chemical techniques including TGA, FT-IR, XRD, FE-SEM, TEM, TPR, XPS and electrical conductivity. The results obtained revealed the nanocrystalline nature of the prepared catalysts. Moreover, the presence of the various dopants has led to a noticeable decrease of the NiO crystallites size, mesoporosity development and an increase of its surface area and pore volume. There is a substantial activity increase upon doping NiO with the various rare earth oxides. Such activity increase is associated with the structural modifications as well as the electrical conductivity increase of these catalysts.

Modeling and measurements of XRD spectra of extended solids under high pressure

NASA Astrophysics Data System (ADS)

Batyrev, I. G.; Coleman, S. P.; Stavrou, E.; Zaug, J. M.; Ciezak-Jenkins, J. A.

2017-06-01

We present results of evolutionary simulations based on density functional calculations of various extended solids: N-Si and N-H using variable and fixed concentration methods of USPEX. Predicted from the evolutionary simulations structures were analyzed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction spectra. Stability of the predicted system was estimated from convex-hull plots. X-ray diffraction spectra were calculated using a virtual diffraction algorithm which computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculations of thousands of XRD spectra were used to search for a structure of extended solids at certain pressures with best fits to experimental data according to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Comparison of Raman and IR spectra calculated for best fitted structures with available experimental data shows reasonable agreement for certain vibration modes. Part of this work was performed by LLNL, Contract DE-AC52-07NA27344. We thank the Joint DoD / DOE Munitions Technology Development Program, the HE C-II research program at LLNL and Advanced Light Source, supported by BES DOE, Contract No. DE-AC02-05CH112.

Robotics Collaborative Technology Alliance (RCTA): Technical Exchange Meeting (TEM) 2015

DTIC Science & Technology

2017-05-01

ARL-CR-0814 ● MAY 2017 US Army Research Laboratory Robotics Collaborative Technology Alliance (RCTA): Technical Exchange Meeting...0814 ● MAY 2017 US Army Research Laboratory Robotics Collaborative Technology Alliance (RCTA): Technical Exchange Meeting (TEM) 2015 by...SUBTITLE Robotics Collaborative Technology Alliance (RCTA): Technical Exchange Meeting (TEM) 2015 5a. CONTRACT NUMBER W911NF-10-2-0016 5b. GRANT

[Identification of Dens Draconis and Os Draconis by XRD method].

PubMed

Chen, Guang-Yun; Wu, Qi-Nan; Shen, Bei; Chen, Rong

2012-04-01

To establish an XRD method for evaluating the quality of Os Draconis and Dens Draconis and applying in judgement of the counterfeit. Dens Draconis, Os Draconis and the counterfeit of Os Draconis were analyzed by XRD. Their diffraction patterns were clustered analysis and evaluated their similarity degree. Established the analytical method of Dens Draconis and Os Draconis basing the features fingerprint information of the 10 common peaks by XRD pattern. Obtained the XRD pattern of the counterfeit of Os Draconis. The similarity degree of separate sources of Dens Draconis was high,while the similarity degree of separate sources of Os Draconis was significant different from each other. This method can be used for identification and evaluation of Os Draconis and Dens Draconis. It also can be used for identification the counterfeit of Os Draconis effectively.

Nanomechanical study of amorphous and polycrystalline ALD HfO2 thin films

Treesearch

K. Tapily; J.E. Jakes; D. Gu; H. Baumgart; A.A. Elmustafa

2011-01-01

Thin films of hafnium oxide (HfO2) were deposited by atomic layer deposition (ALD). The structural properties of the deposited films were characterised by transmission electron microscopy (TEM) and X-ray diffraction (XRD). We investigated the effect of phase transformations induced by thermal treatments on the mechanical properties of ALD HfO

The Crystal Structure of Micro- and Nanopowders of ZnS Studied by EPR of Mn2+ and XRD.

PubMed

Nosenko, Valentyna; Vorona, Igor; Grachev, Valentyn; Ishchenko, Stanislav; Baran, Nikolai; Becherikov, Yurii; Zhuk, Anton; Polishchuk, Yuliya; Kladko, Vasyl; Selishchev, Alexander

2016-12-01

The crystal structure of micro- and nanopowders of ZnS doped with different impurities was analyzed by the electron paramagnetic resonance (EPR) of Mn 2+ and XRD methods. The powders of ZnS:Cu, ZnS:Mn, ZnS:Co, and ZnS:Eu with the particle sizes of 5-7 μm, 50-200 nm, 7-10 μm, and 5-7 nm, respectively, were studied. Manganese was incorporated in the crystal lattice of all the samples as uncontrolled impurity or by doping. The Mn 2+ ions were used as EPR structural probes. It is found that the ZnS:Cu has the cubic structure, the ZnS:Mn has the hexagonal structure with a rhombic distortion, the ZnS:Co is the mixture of the cubic and hexagonal phases in the ratio of 1:10, and the ZnS:Eu has the cubic structure and a distorted cubic structure with stacking defects in the ratio 3:1. The EPR technique is shown to be a powerful tool in the determination of the crystal structure for mixed-polytype ZnS powders and powders with small nanoparticles. It allows observation of the stacking defects, which is revealed in the XRD spectra.

Porous VO(x)N(y) nanoribbons supported on CNTs as efficient and stable non-noble electrocatalysts for the oxygen reduction reaction.

PubMed

Huang, K; Bi, K; Lu, Y K; Zhang, R; Liu, J; Wang, W J; Tang, H L; Wang, Y G; Lei, M

2015-11-30

Novel nanocomposites of carbon nanotubes supported porous VO(x)N(y) nonoribbons (VO(x)N(y)-CNTs) have been synthesized by the annealing of the sol-gel mixture of CNTs and V2O5 under NH3 atmosphere as well as the ageing process in air. Besides the morphological and structural characterizations revealed by TEM, SEAD, EDS, XRD and XPS measurements, typical electrochemical tests including cyclic voltammetry (CV), rotating disk electrode (RDE) and chronoamperometry have been employed to determine the oxygen reduction reaction (ORR) performance of VO(x)N(y)-CNTs. Inspiringly, the results indicate that VO(x)N(y)-CNTs catalyst exhibits a 0.4 mA/cm(2) larger diffusion-limited current density, a 0.10  V smaller onset potential value, a 10.73% less of ORR current decay and an excellent methanol-tolerance compared with commercial Pt/C catalyst. Therefore, we have reasonable grounds to believe that this new VO(x)N(y)-CNTs nanocomposites can be regarded as a promising non-precious methanol-tolerant ORR catalyst candidate for alkaline fuel cells.

Ni@Fe2O3 heterodimers: controlled synthesis and magnetically recyclable catalytic application for dehalogenation reactions

NASA Astrophysics Data System (ADS)

Nakhjavan, Bahar; Tahir, Muhammad Nawaz; Natalio, Filipe; Panthöfer, Martin; Gao, Haitao; Dietzsch, Michael; Andre, Rute; Gasi, Teuta; Ksenofontov, Vadim; Branscheid, Robert; Kolb, Ute; Tremel, Wolfgang

2012-07-01

Ni@Fe2O3 heterodimer nanoparticles (NPs) were synthesized by thermal decomposition of organometallic reactants. After functionalization, these Ni@Fe2O3 heterodimers became water soluble. The pristine heterodimeric NPs were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Mössbauer spectroscopy and magnetic susceptibility measurements. A special advantage of the heterodimers lies in the fact that nanodomains of different composition can be used as catalysts for the removal of environmentally hazardous halogenated pollutants.Ni@Fe2O3 heterodimer nanoparticles (NPs) were synthesized by thermal decomposition of organometallic reactants. After functionalization, these Ni@Fe2O3 heterodimers became water soluble. The pristine heterodimeric NPs were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Mössbauer spectroscopy and magnetic susceptibility measurements. A special advantage of the heterodimers lies in the fact that nanodomains of different composition can be used as catalysts for the removal of environmentally hazardous halogenated pollutants. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr12121b

In-Situ-Reduced Synthesis of Ti 3+ Self-Doped TiO 2 /g-C 3 N 4 Heterojunctions with High Photocatalytic Performance under LED Light Irradiation

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

Li, Kai; Gao, Shanmin; Wang, Qingyao

2015-04-27

A simple one-step calcination route was used to prepare Ti3+ self-doped TiO2/g-C3N4 heterojunctions by mixture of H2Ti3O7 and melamine. X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), electron spin resonance (ESR) spectroscopy, and UV-Vis diffuse reflectance spectroscopy (UV-vis DRS) technologies were used to characterize the structure, crystallinity, morphology, and chemical state of the as-prepared samples. The absorption of the prepared Ti3+ self-doped TiO2/g-C3N4 heterojunctions shifted to a longer wavelength region in comparison with pristine TiO2 and g-C3N4. The photocatalytic activities of the heterojunctions were studied by degrading methylene blue under a 30more » W visible-light-emitting diode irradiation source. The visible-light photocatalytic activities enhanced by the prepared Ti3+ self-doped TiO2/g-C3N4 heterojunctions were observed and proved to be better than that of pure TiO2 and g-C3N4. The photocatalysis mechanism was investigated and discussed. The intensive separation efficiency of photogenerated electron-hole in the prepared heterojunction was confirmed by photoluminescence (PL) spectra. The removal rate constant reached 0.038 min(-1) for the 22.3 wt % Ti3+ self-doped TiO2/g-C3N4 heterojunction, which was 26.76 and 7.6 times higher than that of pure TiO2 and g-C3N4, respectively. The established heterojunction between the interfaces of TiO2 nanoparticles and g-C3N4 nanosheets as well as introduced Ti3+ led to the rapid electron transfer rate and improved photoinduced electron-hole pair's separation efficiency, resulting in the improved photocatalytic performance of the Ti3+ self-doped TiO2/g-C3N4 heterojunctions.« less

Influence of N2 annealing on TiO2 tubes structure and its photocatalytic activity

NASA Astrophysics Data System (ADS)

Chen, Xiaoxiang; Pan, Zhanchang; Yu, Ke; Xiao, Jun; Wu, Shoukun; Li, Jinghong; Chen, Chun; Lin, Yingsheng; Hu, Guanghui; Xu, Yanbin

2018-02-01

In this work, the TiO2 tubes (TBs) were prepared by solvothermal method. The morphology and phase structure of TiO2 TBs is significantly affected by N2 annealing temperature. XRD was used to characterize the phase structure of the as-prepared samples. The morphology and surface areas were characterized by SEM and N2 adsorption-desorption, which show that the tubes were assembled with about 100-nm nanosheets and small ball particles under 400 and 600 °C N2 annealing; when temperature reached 800 °C, the surface of tubes appeared a lot of collapse and many large holes. In addition, the surface areas of 400 °C TiO2, 600 °C TiO2, and 800 °C TiO2 TBs were significantly affected by N2 annealing. Most importantly, the UV-vis and electrochemical tests demonstrate 600 °C TiO2 TBs exhibit higher absorption intensity and photocurrent; thus, it possess on better photocatalytic activity. Therefore, the photocatalytic performance for TiO2 TBs is significantly co-affected by surface area and mix-phase. [Figure not available: see fulltext.

Microstructural, optical and electrical transport properties of Cd-doped SnO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ahmad, Naseem; Khan, Shakeel; Mohsin Nizam Ansari, Mohd

2018-03-01

We have successfully investigated the structural, optical and dielectric properties of Cd assimilated SnO2 nanoparticles synthesized via very convenient precipitation route. The structural properties were studied by x-ray diffraction method (XRD) and Fourier Transform Infrared (FTIR) Spectroscopy. As-synthesized samples in the form of powder were examined for its morphology and average particle size by Transmission electron microscopy (TEM). The optical properties were studied by diffuse reflectance spectroscopy. Dielectric properties such that complex dielectric constant and ac conductivity were investigated by LCR meter. Average crystallite size calculated by XRD and average particle size obtained from TEM were found to be consistent and below 50 nm for all samples. The optical band gap of as-synthesized powder samples from absorption study was found in the range of 3.76 to 3.97 eV. The grain boundary parameters such that Rgb, Cgb and τ were evaluated using impedance spectroscopy.

Chemical vapor deposited carbon nanotubes for aqueous H2-Cl2 fuel cells.

PubMed

Suryavanshi, U B; Bhosale, C H

2010-06-01

Carbon nanotubes having large surface area is an interesting material to develop H2-Cl2 fuel cell electrodes. The attempts were made to deposit carbon nanotubes on porous substrates by chemical vapour deposition. Turpentine oil (C10H16) was used as a precursor, decomposed at 1100 degrees C reactor temperature. Nickel, platinum, tin, Ni-Pt, Ni-Sn, Pt-Sn, Ni-Pt-Sn catalysts were used to grow carbon nanotubes. Nickel was deposited with electrodeposition, platinum with sputter coater and tin with vacuum deposition technique. The developed electrodes were characterized by XRD, SEM, TEM, FTIR, and resistivity by van-der Pauw method. Carbon nanotubes have been formed for 0.25 N nickel deposited for 45 and 60 min; 0.5 N, 0.75 N and 1 N nickel deposited for 15 to 60 min, at the interval of 15. Ni-Pt, Ni-Sn, Pt-Sn and Ni-Pt-Sn activated carbon also shows the well grown CNTs. Aqueous H2-Cl2 fuel cell performance was tested with these grown carbon nanotubes. 40% KCl with 1067 mohm(-1) cm(-1) conductivity was used as electrolyte. Linear sweep voltametry shows reduction potential for hydrogen gas. Chronoamperometry results show better half cell performance for nickel, deposited with 1 N, 45 min deposition time period; and combination of Ni-Pt-Sn with 140, and 110-100 mA/cm2 stable current density respectively.

The effect of Fe-Rh alloying on CO hydrogenation to C 2+ oxygenates

DOE PAGES

Palomino, Robert; Magee, Joseph W.; Llorca, Jordi; ...

2015-05-20

A combination of reactivity and structural studies using X-ray diffraction (XRD), pair distribution function (PDF), and transmission electron microscopy (TEM) was used to identify the active phases of Fe-modified Rh/TiO 2 catalysts for the synthesis of ethanol and other C 2+ oxygenates from CO hydrogenation. XRD and TEM confirm the existence of Fe–Rh alloys for catalyst with 1–7 wt% Fe and ~2 wt% Rh. Rietveld refinements show that FeRh alloy content increases with Fe loading up to ~4 wt%, beyond which segregation to metallic Fe becomes favored over alloy formation. Catalysts that contain Fe metal after reduction exhibit some carburizationmore » as evidenced by the formation of small amounts of Fe 3C during CO hydrogenation. Analysis of the total Fe content of the catalysts also suggests the presence of FeO x also increased under reaction conditions. Reactivity studies show that enhancement of ethanol selectivity with Fe loading is accompanied by a significant drop in CO conversion. Comparison of the XRD phase analyses with selectivity suggests that higher ethanol selectivity is correlated with the presence of Fe–Rh alloy phases. As a result, the interface between Fe and Rh serves to enhance the selectivity of ethanol, but suppresses the activity of the catalyst which is attributed to the blocking or modifying of Rh active sites.« less

Discontinuous precipitation in a nickel-free high nitrogen austenitic stainless steel on solution nitriding

NASA Astrophysics Data System (ADS)

Mohammadzadeh, Roghayeh; Akbari, Alireza; Grumsen, Flemming B.; Somers, Marcel A. J.

2017-10-01

Chromium-rich nitride precipitates in production of nickel-free austenitic stainless steel plates via pressurised solution nitriding of Fe-22.7Cr-2.4Mo ferritic stainless steel at 1473 K (1200 °C) under a nitrogen gas atmosphere was investigated. The microstructure, chemical and phase composition, morphology and crystallographic orientation between the resulted austenite and precipitates were investigated using optical microscopy, X-ray Diffraction (XRD), Scanning and Transmission Electron Microscopy (TEM) and Electron Back Scatter Diffraction (EBSD). On prolonged nitriding, Chromium-rich nitride precipitates were formed firstly close to the surface and later throughout the sample with austenitic structure. Chromium-rich nitride precipitates with a rod or strip-like morphology was developed by a discontinuous cellular precipitation mechanism. STEM-EDS analysis demonstrated partitioning of metallic elements between austenite and nitrides, with chromium contents of about 80 wt.% in the precipitates. XRD analysis indicated that the Chromium-rich nitride precipitates are hexagonal (Cr, Mo)2N. Based on the TEM studies, (Cr, Mo)2N precipitates presented a (1 1 1)γ//(0 0 2)(Cr, Mo)2N, ?γ//?(Cr, Mo)2N orientation relationship with respect to the austenite matrix. EBSD studies revealed that the austenite in the regions that have transformed into austenite and (Cr, Mo)2N have no orientation relation to the untransformed austenite.

XRD analysis of undoped and Fe doped TiO{sub 2} nanoparticles by Williamson Hall method

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

Bharti, Bandna; Barman, P. B.; Kumar, Rajesh, E-mail: rajesh.kumar@juit.ac.in

2015-08-28

Undoped and Fe doped titanium dioxide (TiO{sub 2}) nanoparticles were synthesized by sol-gel method at room temperature. The synthesized samples were annealed at 500°C. For structural analysis, the prepared samples were characterized by X-ray diffraction (XRD). The crystallite size of TiO{sub 2} and Fe doped TiO{sub 2} nanoparticles were calculated by Scherer’s formula, and was found to be 15 nm and 11 nm, respectively. Reduction in crystallite size of TiO{sub 2} with Fe doping was observed. The anatase phase of Fe-doped TiO{sub 2} nanoparticles was also confirmed by X-ray diffraction. By using Williamson-Hall method, lattice strain and crystallite size weremore » also calculated. Williamson–Hall plot indicates the presence of compressive strain for TiO{sub 2} and tensile strain for Fe-TiO{sub 2} nanoparticles annealed at 500°C.« less

TEM00 mode Nd:YAG solar laser by side-pumping a grooved rod

NASA Astrophysics Data System (ADS)

Vistas, Cláudia R.; Liang, Dawei; Almeida, Joana; Guillot, Emmanuel

2016-05-01

A simple TEM00 mode solar laser system with a grooved Nd:YAG rod pumped through a heliostat-parabolic mirror system is reported here. The radiation coupling capacity of a fused silica tube lens was combined with the multipass pumping ability of a 2 V-shaped cavity to provide efficient side-pumping along a 4.0 mm diameter grooved Nd:YAG single-crystal rod. TEM00 mode solar laser power of 3.4 W was measured by adopting an asymmetric large-mode laser resonant cavity. Record TEM00 mode solar laser collection efficiency of 3.4 W/m2and slope efficiency of 1.9% was achieved, which corresponds to 1.8 and 2.4 times more than the previous TEM00 mode Nd:YAG solar laser using the PROMES-CNRS heliostat-parabolic mirror system, respectively.

XRD and XAS structural study of CuAlO2 under high pressure.

PubMed

Pellicer-Porres, J; Segura, A; Ferrer-Roca, Ch; Polian, A; Munsch, P; Kim, D

2013-03-20

We present the results of x-ray diffraction and x-ray absorption spectroscopy experiments in CuAlO(2) under high pressure. We discuss the polarization dependence of the x-ray absorption near-edge structure at the Cu K-edge. XRD under high pressure evidences anisotropic compression, the a-axis being more compressible than the c-axis. EXAFS yields the copper-oxygen bond length, from which the only internal parameter of the delafossite structure is deduced. The combination of anisotropic compression and the internal parameter decrease results in a regularization of the AlO(6) octahedra. The anisotropic compression is related to the chemical trends observed in the lattice parameters when Al is substituted by other trivalent cations. Both experiments evidence the existence of an irreversible phase transition that clearly manifests at 35 ± 2 GPa. The structure of the high-pressure polymorph could not be determined, but it implies a change of the Cu environment, which remains anisotropic. Precursor effects are observed from the lowest pressures, which are possibly related to crystal breaking at a submicroscopic scale with partial reorientation of the crystallites.

XRD and XAS structural study of CuAlO2 under high pressure

NASA Astrophysics Data System (ADS)

Pellicer-Porres, J.; Segura, A.; Ferrer-Roca, Ch; Polian, A.; Munsch, P.; Kim, D.

2013-03-01

We present the results of x-ray diffraction and x-ray absorption spectroscopy experiments in CuAlO2 under high pressure. We discuss the polarization dependence of the x-ray absorption near-edge structure at the Cu K-edge. XRD under high pressure evidences anisotropic compression, the a-axis being more compressible than the c-axis. EXAFS yields the copper-oxygen bond length, from which the only internal parameter of the delafossite structure is deduced. The combination of anisotropic compression and the internal parameter decrease results in a regularization of the AlO6 octahedra. The anisotropic compression is related to the chemical trends observed in the lattice parameters when Al is substituted by other trivalent cations. Both experiments evidence the existence of an irreversible phase transition that clearly manifests at 35 ± 2 GPa. The structure of the high-pressure polymorph could not be determined, but it implies a change of the Cu environment, which remains anisotropic. Precursor effects are observed from the lowest pressures, which are possibly related to crystal breaking at a submicroscopic scale with partial reorientation of the crystallites.

The bipyridine adducts of N-phenyldithiocarbamato complexes of Zn(II) and Cd(II); synthesis, spectral, thermal decomposition studies and use as precursors for ZnS and CdS nanoparticles

NASA Astrophysics Data System (ADS)

Onwudiwe, Damian C.; Strydom, Christien A.

2015-01-01

Bipyridine adducts of N-phenyldithiocarbamato complexes, [ML12L2] (M = Cd(II), Zn(II); L1 = N-phenyldithiocarbamate, L2 = 2,2‧ bipyridine), have been synthesized and characterised. The decomposition of these complexes to metal sulphides has been investigated by thermogravimetric analysis (TGA). The complexes were used as single-source precursors to synthesize MS (M = Zn, Cd) nanoparticles (NPs) passivated by hexadecyl amine (HDA). The growth of the nanoparticles was carried out at two different temperatures: 180 and 220 °C, and the optical and structural properties of the nanoparticles were studied using UV-Vis spectroscopy, photoluminescence spectroscopy (PL), transmission emission microscopy (TEM) and powdered X-ray diffraction (p-XRD). Nanoparticles, whose average diameters are 2.90 and 3.54 nm for ZnS, and 8.96 and 9.76 nm for CdS grown at 180 and 220 °C respectively, were obtained.

Structural phase analysis and photoluminescence properties of Mg-doped TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ali, T.; Ashraf, M. Anas; Ali, S. Asad; Ahmed, Ateeq; Tripathi, P.

2018-05-01

In this paper, we report the synthesis, characterization and photoluminescence properties of Mg-doped TiO2 nanoparticles (NPs). The samples were synthesized by sol-gel method and characterized using the standard analytical techniques such as X-ray diffraction (XRD), Transmission electron microscope (TEM), Energy dispersive X-ray spectroscopy (EDX), UV-visible and photoluminescence spectroscopy. The powder XRD spectra revealed that the synthesized samples are pure and crystalline in nature and showing tetragonal anatase phase of TiO2 NPs. UV-visible spectrum illustrates that an absorption edge shifts toward the visible region. This study may provide a new insight for making the nanomaterials which can be used in photocatalytic applications.

Synthesis and characterization of Cu2O/TiO2 photocatalysts for H2 evolution from aqueous solution with different scavengers

NASA Astrophysics Data System (ADS)

Li, Yanping; Wang, Baowei; Liu, Sihan; Duan, Xiaofei; Hu, Zongyuan

2015-01-01

A series of Cu2O/TiO2 photocatalysts with different molar fraction of Cu2O were prepared by a facile modified ethanol-induced approach followed by a calcination process. The chemical state of copper compound was proved to be cuprous oxide by the characterization of X-ray photoelectron spectra (XPS). Furthermore, these composite oxides were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption desorption and UV-vis techniques to study the morphologies, structures, and optical properties of the as-prepared samples. The results indicated that the photocatalytic activity of n-type TiO2 was significantly enhanced by combined with p-type Cu2O, due to the efficient p-n heterojunction. The p-n heterojunction between Cu2O and TiO2 can enhance visible-light adsorption, efficiently suppress charge recombination, improve interfacial charge transfer, and especially provide plentiful reaction active sites on the surface of photocatalyst. As a consequence, the prepared 2.5-Cu2O/TiO2 photocatalyst exhibited the highest photocatalytic activity for H2 evolution rate and reached 2048.25 μmol/(g h), which is 14.48 times larger than that of pure P25. The apparent quantum yield (AQY) of the 2.5-Cu2O/TiO2 sample at 365 nm was estimated to be 4.32%. In addition, the influence of different scavengers, namely methanol, anhydrous ethanol, ethylene glycol and glycerol, on the photocatalytic activity for H2 evolution rate was discussed.

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloy

NASA Astrophysics Data System (ADS)

Mori, A.; Mamiya, H.; Ohnuma, M.; Ilavsky, J.; Ohishi, K.; Woźniak, Jarosław; Olszyna, A.; Watanabe, N.; Suzuki, J.; Kitazawa, H.; Lewandowska, M.

2018-04-01

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and alloy contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small-angle X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 °C. Sintering at 1000 °C for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128 nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.

Technical Evaluation Motor no. 5 (TEM-5)

NASA Technical Reports Server (NTRS)

Cook, M.

1990-01-01

Technical Evaluation Motor No. 5 (TEM-5) was static test fired at the Thiokol Corporation Static Test Bay T-97. TEM-5 was a full scale, full duration static test fire of a high performance motor (HPM) configuration solid rocket motor (SRM). The primary purpose of TEM static tests is to recover SRM case and nozzle hardware for use in the redesigned solid rocket motor (RSRM) flight program. Inspection and instrumentation data indicate that the TEM-5 static test firing was successful. The ambient temperature during the test was 41 F and the propellant mean bulk temperature (PMBT) was 72 F. Ballistics performance values were within the specified requirements. The overall performance of the TEM-5 components and test equipment was nominal. Dissembly inspection revealed that joint putty was in contact with the inner groove of the inner primary seal of the ignitor adapter-to-forward dome (inner) joint gasket; this condition had not occurred on any previous static test motor or flight RSRM. While no qualification issues were addressed on TEM-5, two significant component changes were evaluated. Those changes were a new vented assembly process for the case-to-nozzle joint and the installation of two redesigned field joint protection systems. Performance of the vented case-to-nozzle joint assembly was successful, and the assembly/performance differences between the two field joint protection system (FJPS) configurations were compared.

UV-light-assisted ethanol sensing characteristics of g-C3N4/ZnO composites at room temperature

NASA Astrophysics Data System (ADS)

Zhai, Jiali; Wang, Tao; Wang, Chuang; Liu, Dechen

2018-05-01

A highly efficient UV-light-assisted room temperature sensor based on g-C3N4/ZnO composites were prepared by an in situ precipitation method. The thermostability, composition, structure, and morphology properties of the as-prepared g-C3N4/ZnO composites were characterized by TGA, XRD, FT-IR, TEM, and XPS, respectively. And then, we studied the ethanol (C2H5OH) sensing performance of the g-C3N4/ZnO composites at the room temperature. Compared with pure ZnO and g-C3N4, the gas sensing activity of g-C3N4/ZnO composites was greatly improved at room temperature, for example, the g-C3N4/ZnO-8% composites showed an obvious response of 121-40 ppm C2H5OH at room temperature, which was 60 times higher than the pure ZnO based on the sensors under the same condition. The great enhancement of the C2H5OH sensing properties of composites can be understood by the efficient separation of photogenerated charge carriers of g-C3N4/ZnO heterogeneous and the UV-light catalytic effect. Finally, a possible mechanism for the gas sensing activity was proposed.

Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods.

PubMed

Sivakami, R; Dhanuskodi, S; Karvembu, R

2016-01-05

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55eV. BET measurements show a high specific surface area (SSA) of 118-133m(2)/g and pore diameter (10-25nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM. Copyright © 2015 Elsevier B.V. All rights reserved.

Photo-catalytic decolourisation of toxic dye with N-doped titania: a case study with Acid Blue 25.

PubMed

Chakrabortty, Dhruba; Gupta, Susmita Sen

2013-05-01

Dyes are one of the hazardous water pollutants. Toxic Acid Blue 25, an anthraquinonic dye, has been decolourised by photo-catalysing it with nitrogen doped titania in aqueous medium. The photo catalyst was prepared from 15% TiCl3 and 25% aqueous NH3 solution as precursor. XRD and TEM revealed the formation of well crystalline anatase phase having particle size in the nano-range. BET surface area of the sample was higher than that of pure anatase TiO2. DRS showed higher absorption of radiation in visible range compared to pure anatase TiO2. XPS revealed the presence of nitrogen in N-Ti-O environment. The experimental parameters, namely, photocatalyst dose, initial dye concentration as well as solution pH influence the decolourisation process. At pH 3.0, the N-TiO2 could decolourise almost 100% Acid Blue 25 within one hour. The influence of N-TiO2 dose, initial concentration of Acid Blue 25 and solution pH on adsorption-desorption equilibrium is also studied. The adsorption process follows Lagergren first order kinetics while the modified Langmuir-Hinselwood model is suitably fitted for photocatalytic decolourisation of Acid Blue 25.

Preparation of SiO2-Protecting Metallic Fe Nanoparticle/SiO2 Composite Spheres for Biomedical Application

PubMed Central

Hsieh, Pin-Wei; Tseng, Ching-Li; Kuo, Dong-Hau

2015-01-01

Functionalized Fe nanoparticles (NPs) have played an important role in biomedical applications. In this study, metallic Fe NPs were deposited on SiO2 spheres to form a Fe/SiO2 composite. To protect the Fe from oxidation, a thin SiO2 layer was coated on the Fe/SiO2 spheres thereafter. The size and morphology of the SiO2@Fe/SiO2 composite spheres were examined by transmission electron microscopy (TEM). The iron form and its content and magnetic properties were examined by X-ray diffraction (XRD), inductively-coupled plasma mass spectrometry (ICP-MS) and a superconducting quantum interference device (SQUID). The biocompatibility of the SiO2@Fe/SiO2 composite spheres was examined by Cell Counting Kit-8 (CCK-8) and lactate dehydrogenase (LDH) tests. The intracellular distribution of the SiO2@Fe/SiO2 composite spheres was observed using TEM. XRD analysis revealed the formation of metallic iron on the surface of the SiO2 spheres. According to the ICP-MS and SQUID results, using 0.375 M FeCl3·6H2O for Fe NPs synthesis resulted in the highest iron content and magnetization of the SiO2@Fe/SiO2 spheres. Using a dye loading experiment, a slow release of a fluorescence dye from SiO2@Fe/SiO2 composite spheres was confirmed. The SiO2@Fe/SiO2 composite spheres co-cultured with L929 cells exhibit biocompatibility at concentrations <16.25 µg/mL. The TEM images show that the SiO2@Fe/SiO2 composite spheres were uptaken into the cytoplasm and retained in the endosome. The above results demonstrate that the SiO2@Fe/SiO2 composite spheres could be used as a multi-functional agent, such as a magnetic resonance imaging (MRI) contrast agent or drug carriers in biomedical applications.

Synthesis and evaluation of optical and antimicrobial properties of Ag-SnO2 nanocomposites

NASA Astrophysics Data System (ADS)

Kumar Nair, Kishore; Kumar, Promod; Kumar, Vinod; Harris, R. A.; Kroon, R. E.; Viljoen, Bennie; Shumbula, P. M.; Mlambo, M.; Swart, H. C.

2018-04-01

We report on the sol-gel based room temperature synthesis of undoped SnO2 and Ag-SnO2 nanostructures. The synthesized nanostructures were characterized by Fourier transform infrared spectroscopy, X-ray diffraction (XRD), Raman spectroscopy, High-resolution transmission electron microscopy (HR-TEM) and UV-visible spectroscopy. The XRD pattern confirmed that the obtained nanostructures have a tetragonally rutile structure. No extra phase changes were observed after Ag doping. UV-visible spectroscopy measurements indicated that the band gap of 3.59 eV for pure SnO2 nanostructures, decreased to 3.39 eV after doping. TEM analysis showed that no regular shape morphology existed and some rod-shaped particles were also detected in the nanostructures. The antibacterial activity of the nanostructures against E. coli was evaluated and a continuous decrease of microbial count was observed. The microbial population decreased from 6 × 105 cfu/ml to 7 × 104 cfu/ml and 5 × 104 cfu/ml on SnO2 and Ag-SnO2 treatments, respectively. Thus, the nanostructures can be used for the biorational management of E. coli for waste water treatment before discharge.

High-quality III-nitride films on conductive, transparent (2̅01)-oriented β-Ga2O3 using a GaN buffer layer.

PubMed

Muhammed, M M; Roldan, M A; Yamashita, Y; Sahonta, S-L; Ajia, I A; Iizuka, K; Kuramata, A; Humphreys, C J; Roqan, I S

2016-07-14

We demonstrate the high structural and optical properties of InxGa1-xN epilayers (0 ≤ x ≤ 23) grown on conductive and transparent (01)-oriented β-Ga2O3 substrates using a low-temperature GaN buffer layer rather than AlN buffer layer, which enhances the quality and stability of the crystals compared to those grown on (100)-oriented β-Ga2O3. Raman maps show that the 2″ wafer is relaxed and uniform. Transmission electron microscopy (TEM) reveals that the dislocation density reduces considerably (~4.8 × 10(7) cm(-2)) at the grain centers. High-resolution TEM analysis demonstrates that most dislocations emerge at an angle with respect to the c-axis, whereas dislocations of the opposite phase form a loop and annihilate each other. The dislocation behavior is due to irregular (01) β-Ga2O3 surface at the interface and distorted buffer layer, followed by relaxed GaN epilayer. Photoluminescence results confirm high optical quality and time-resolved spectroscopy shows that the recombination is governed by bound excitons. We find that a low root-mean-square average (≤1.5 nm) of InxGa1-xN epilayers can be achieved with high optical quality of InxGa1-xN epilayers. We reveal that (01)-oriented β-Ga2O3 substrate has a strong potential for use in large-scale high-quality vertical light emitting device design.

Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

NASA Technical Reports Server (NTRS)

Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

2004-01-01

Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

Resistive switching mechanism in the one diode-one resistor memory based on p+-Si/n-ZnO heterostructure revealed by in-situ TEM

NASA Astrophysics Data System (ADS)

Zhang, Lei; Zhu, Liang; Li, Xiaomei; Xu, Zhi; Wang, Wenlong; Bai, Xuedong

2017-03-01

One diode-one resistor (1D1R) memory is an effective architecture to suppress the crosstalk interference, realizing the crossbar network integration of resistive random access memory (RRAM). Herein, we designed a p+-Si/n-ZnO heterostructure with 1D1R function. Compared with the conventional multilayer 1D1R devices, the structure and fabrication technique can be largely simplified. The real-time imaging of formation/rupture process of conductive filament (CF) process demonstrated the RS mechanism by in-situ transmission electron microscopy (TEM). Meanwhile, we observed that the formed CF is only confined to the outside of depletion region of Si/ZnO pn junction, and the formation of CF does not degrade the diode performance, which allows the coexistence of RS and rectifying behaviors, revealing the 1D1R switching model. Furthermore, it has been confirmed that the CF is consisting of the oxygen vacancy by in-situ TEM characterization.

Complete Tem-Tomography: 3D Structure of Gems Cluster

NASA Technical Reports Server (NTRS)

Matsuno, J.; Miyake, A.; Tsuchiyama, A.; Messenger, S.; Nakamura-Messenger, K.

2015-01-01

GEMS (glass with embedded metal and sulfide) grains in interplanetary dust particles (IDPs) are considered to be one of the ubiquitous and fundamental building blocks of solids in the Solar System. They have been considered to be interstellar silicate dust that survived various metamorphism or alteration processes in the protoplanetary disk but the elemental and isotopic composition measurements suggest that most of them have been formed in the protoplanetary disk as condensates from high temperature gas. This formation model is also supported by the formation of GEMS-like grains with respect to the size, mineral assemblage, texture and infrared spectrum by condensation experiments from mean GEMS composition materials. Previous GEMS studies were performed only with 2D observation by transmission electron microscopy (TEM) or scanning TEM (STEM). However, the 3D shape and structure of GEMS grains and the spatial distribution of Fe/FeS's has critical information about their formation and origin. Recently, the 3D structure of GEMS grains in ultrathin sections of cluster IDPs was revealed by electron tomography using a TEM/STEM (JEM-2100F, JEOL). However, CT images of thin sections mounted on Cu grids acquired by conventional TEM-tomography are limited to low tilt angles (e. g., less than absolute value of 75 deg. In fact, previous 3D TEM observations of GEMS were affected by some artifacts related to the limited tilt range in the TEM used. Complete tomographic images should be acquired by rotating the sample tilt angle over a range of more than absolute value of 80 deg otherwise the CT images lose their correct structures. In order to constrain the origin and formation process of GEMS grains more clearly, we performed complete electron tomography for GEMS grains. Here we report the sample preparation method we have developed for this study, and the preliminary results.

Degradation of bromamine acid by nanoscale zero-valent iron (nZVI) supported on sepiolite.

PubMed

Fei, Xuening; Cao, Lingyun; Zhou, Lifeng; Gu, Yingchun; Wang, Xiaoyang

2012-01-01

Sepiolite, a natural nano-material, was chosen as a carrier to prepare supported nanoscale zero-valent iron (nZVI). The effects of preparation conditions, including mass ratio of nZVI and activated sepiolite and preparation pH value, on properties of the supported nZVI were investigated. The results showed that the optimal mass ratio of nZVI and sepiolite was 1.12:1 and the optimal pH value was 7. The supported nZVI was characterized by X-ray diffraction (XRD), transmission electron microscope (TEM) and energy dispersive spectrometer (EDS), and furthermore an analogy model of the supported nZVI was set up. Compared with the nZVI itself, the supported nZVI was more stable in air and possessed better water dispersibility, which were beneficial for the degradation of bromamine acid aqueous solution. The degradation characteristics, such as effects of supported nZVI dosage, initial concentration and initial pH value of the solution on the decolorization efficiency were also investigated. The results showed that in an acidic environment the supported nZVI with a dosage of 2 g/L showed high activity in the degradation of bromamine acid with an initial concentration of 1,000 mg/L, and the degree of decolorization could reach up to 98%.

TEM PSHA2015 Reliability Assessment

NASA Astrophysics Data System (ADS)

Lee, Y.; Wang, Y. J.; Chan, C. H.; Ma, K. F.

2016-12-01

The Taiwan Earthquake Model (TEM) developed a new probabilistic seismic hazard analysis (PSHA) for determining the probability of exceedance (PoE) of ground motion over a specified period in Taiwan. To investigate the adequacy of the seismic source parameters adopted in the 2015 PSHA of the TEM (TEM PSHA2015), we conducted several tests of the seismic source models. The observed maximal peak ground acceleration (PGA) of the ML > 4.0 mainshocks in the 23-year data period of 1993-2015 were used to test the predicted PGA of PSHA from the areal and subduction zone sources with the time-independent Poisson assumption. This comparison excluded the observations from 1999 Chi-Chi earthquake, as this was the only earthquake associated with the identified active fault in this past 23 years. We used tornado diagrams to analyze the sensitivities of these source parameters to the ground motion values of the PSHA. This study showed that the predicted PGA for a 63% PoE in the 23-year period corresponded to the empirical PGA and the predicted numbers of PGA exceedances to a threshold value 0.1g close to the observed numbers, confirming the parameter applicability for the areal and subduction zone sources. We adopted the disaggregation analysis from a hazard map to determine the contribution of the individual seismic sources to hazard for six metropolitan cities in Taiwan. The sensitivity tests of the seismogenic structure parameters indicated that the slip rate and maximum magnitude are dominant factors for the TEM PSHA2015. For densely populated faults in SW Taiwan, maximum magnitude is more sensitive than the slip rate, giving the concern on the possible multiple fault segments rupture with larger magnitude in this area, which was not yet considered in TEM PSHA2015. The source category disaggregation also suggested that special attention is necessary for subduction zone earthquakes for long-period shaking seismic hazards in Northern Taiwan.

Influence of temperature on oxidation mechanisms of fiber-textured AlTiTaN coatings.

PubMed

Khetan, Vishal; Valle, Nathalie; Duday, David; Michotte, Claude; Delplancke-Ogletree, Marie-Paule; Choquet, Patrick

2014-03-26

The oxidation kinetics of AlTiTaN hard coatings deposited at 265 °C by DC magnetron sputtering were investigated between 700 and 950 °C for various durations. By combining dynamic secondary ion mass spectrometry (D-SIMS), X-ray diffraction (XRD), and transmission electron microscopy (TEM) investigations of the different oxidized coatings, we were able to highlight the oxidation mechanisms involved. The TEM cross-section observations combined with XRD analysis show that a single amorphous oxide layer comprising Ti, Al, and Ta formed at 700 °C. Above 750 °C, the oxide scale transforms into a bilayer oxide comprising an Al-rich upper oxide layer and a Ti/Ta-rich oxide layer at the interface with the coated nitride layer. From the D-SIMS analysis, it could be proposed that the oxidation mechanism was governed primarily by inward diffusion of O for temperatures of ≤700 °C, while at ≥750 °C, it is controlled by outward diffusion of Al and inward diffusion of O. Via a combination of structural and chemical analysis, it is possible to propose that crystallization of rutile lattice favors the outward diffusion of Al within the AlTiTa mixed oxide layer with an increase in the temperature of oxidation. The difference in the mechanisms of oxidation at 700 and 900 °C also influences the oxidation kinetics with respect to oxidation time. Formation of a protective alumina layer decreases the rate of oxidation at 900 °C for long durations of oxidation compared to 700 °C. Along with the oxidation behavior, the enhanced thermal stability of AlTiTaN compared to that of the TiAlN coating is illustrated.

Clay pigment structure characterisation as a guide for provenance determination--a comparison between laboratory powder micro-XRD and synchrotron radiation XRD.

PubMed

Švarcová, Silvie; Bezdička, Petr; Hradil, David; Hradilová, Janka; Žižak, Ivo

2011-01-01

Application of X-ray diffraction (XRD)-based techniques in the analysis of painted artworks is not only beneficial for indisputable identification of crystal constituents in colour layers, but it can also bring insight in material crystal structure, which can be affected by their geological formation, manufacturing procedure or secondary changes. This knowledge might be helpful for art historic evaluation of an artwork as well as for its conservation. By way of example of kaolinite, we show that classification of its crystal structure order based on XRD data is useful for estimation of its provenance. We found kaolinite in the preparation layer of a Gothic wall painting in a Czech church situated near Karlovy Vary, where there are important kaolin deposits. Comparing reference kaolin materials from eight various Czech deposits, we found that these can be differentiated just according to the kaolinite crystallinity. Within this study, we compared laboratory powder X-ray micro-diffraction (micro-XRD) with synchrotron radiation X-ray diffraction analysing the same real sample. We found that both techniques led to the same results.

XRD and FTIR structural investigation of gadolinium-zinc-borate glass ceramics

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

Borodi, G.; Pascuta, P.; Dan, V.

2013-11-13

X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy measurements have been employed to investigate the (Gd{sub 2}O{sub 3}){sub x}⋅(B{sub 2}O{sub 3}){sub (60−x)}⋅(ZnO){sub 40} glass ceramics system, with 0 ≤ x ≤ 15 mol%. After heat treatment applied at 860 °C for 2 h, some structural changes were observed and new crystalline phases appeared in the structure of the samples. In these glass ceramics four crystalline phases were identified using powder diffraction files (PDF 2), namely ZnB{sub 4}O{sub 7}, Zn{sub 4}O(B{sub 6}O{sub 12}), Zn{sub 3}(BO{sub 3}){sub 2} and GdBO{sub 3}. From the XRD data, the average unit-cell parameter and themore » quantitative ratio of the crystallographic phases in the studied samples were evaluated. FTIR data revealed that the BO{sub 3}, BO{sub 4} and ZnO{sub 4} are the main structural units of these glass ceramics network. The compositional dependence of the different structural units which appear in the studied samples was followed.« less

Response Time Measurements of the NIF DANTE XRD-31 X-Ray Diodes (Pre-print)

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

Don Pellinen and Michael Griffin

2009-01-23

The XRD-31 is a fast, windowless X-ray vacuum photodiode developed by EG&G. It is currently the primary fast X-ray detector used to diagnose the X-rays on NIF and OMEGA on the multichannel DANTE spectrometer. The XRD-31 has a dynamic range of less than 1e-12 amps to more than 10 amps. A technique is described to measure the impulse response of the diodes to a 150 fs pulse of 200 nm laser light and a method to calculate the “risetime” for a square pulse and compare it with the computed electron transit time from the photocathode to the anode. Measured responsemore » time for 5 XRD-31s assembled in early 2004 was 149.7 ps +-2.75 ps.« less

The bipyridine adducts of N-phenyldithiocarbamato complexes of Zn(II) and Cd(II); synthesis, spectral, thermal decomposition studies and use as precursors for ZnS and CdS nanoparticles.

PubMed

Onwudiwe, Damian C; Strydom, Christien A

2015-01-25

Bipyridine adducts of N-phenyldithiocarbamato complexes, [ML(1)2L(2)] (M=Cd(II), Zn(II); L(1)=N-phenyldithiocarbamate, L(2)=2,2' bipyridine), have been synthesized and characterised. The decomposition of these complexes to metal sulphides has been investigated by thermogravimetric analysis (TGA). The complexes were used as single-source precursors to synthesize MS (M=Zn, Cd) nanoparticles (NPs) passivated by hexadecyl amine (HDA). The growth of the nanoparticles was carried out at two different temperatures: 180 and 220 °C, and the optical and structural properties of the nanoparticles were studied using UV-Vis spectroscopy, photoluminescence spectroscopy (PL), transmission emission microscopy (TEM) and powdered X-ray diffraction (p-XRD). Nanoparticles, whose average diameters are 2.90 and 3.54 nm for ZnS, and 8.96 and 9.76 nm for CdS grown at 180 and 220 °C respectively, were obtained. Copyright © 2014 Elsevier B.V. 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.

[Hydrothermal synthesis and luminescence of one-dimensional Mn(2+)-doped CdS nanocrystals].

PubMed

Yuan, Qiu-Li; Zhao, Jin-Tao; Nie, Qiu-Lin

2007-06-01

One-dimensional Mn(2+)-doped CdS nanocrystals were synthesized by the hydrothermal route. The products were characterized by SEM, EDS, XRD, TEM, HRTEM and PL, respectively. The results revealed that dopant Mn2+ completely substitutes Cd2+ in CdS nanocrystals, and the product was of good crystallite. Further more, a complete suppression of the emission from surface states at room temperature when doping with ions Mn2+ has been observed.

Preparation and enhanced daylight-induced photocatalytic activity of C,N,S-tridoped titanium dioxide powders.

PubMed

Zhou, Minghua; Yu, Jiaguo

2008-04-15

A simple method for preparing highly daylight-induced photoactive nanocrystalline C,N,S-tridoped TiO2 powders was developed by a solid-phase reaction. The as-prepared TiO2 powders were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra, N2 adsorption-desorption measurements and transmission electron microscopy (TEM). The photocatalytic activity was evaluated by the photocatalytic oxidation of formaldehyde under daylight irradiation in air. The results show that daylight-induced photocatalytic activities of the as-prepared TiO2 powders were improved by C,N,S-tridoping. The C,N,S-tridoped TiO2 powders exhibited stronger absorption in the near UV and visible-light region with red shift in the band-gap transition. When the molar ratio of CS(NH2)2 to xerogel TiO2 powders (prepared by hydrolysis of Ti(OC4H9)4 in distilled water) (R) was kept in 3, the daylight-induced photocatalytic activities of the as-prepared C,N,S-tridoped TiO2 powders were about more than six times greater than that of Degussa P25 and un-doped TiO2 powders. The high activities of the C,N,S-tridoped TiO2 can be attributed to the results of the synergetic effects of strong absorption in the near UV and visible-light region, red shift in adsorption edge and two phase structures of un-doped TiO2 and C,N,S-tridoped TiO2.

Bi2O3 nanoparticles encapsulated in surface mounted metal-organic framework thin films

NASA Astrophysics Data System (ADS)

Guo, Wei; Chen, Zhi; Yang, Chengwu; Neumann, Tobias; Kübel, Christian; Wenzel, Wolfgang; Welle, Alexander; Pfleging, Wilhelm; Shekhah, Osama; Wöll, Christof; Redel, Engelbert

2016-03-01

We describe a novel procedure to fabricate a recyclable hybrid-photocatalyst based on Bi2O3@HKUST-1 MOF porous thin films. Bi2O3 nanoparticles (NPs) were synthesized within HKUST-1 (or Cu3(BTC)2) surface-mounted metal-organic frame-works (SURMOFs) and characterized using X-ray diffraction (XRD), a quartz crystal microbalance (QCM) and transmission electron microscopy (TEM). The Bi2O3 semiconductor NPs (diameter 1-3 nm)/SURMOF heterostructures exhibit superior photo-efficiencies compared to NPs synthesized using conventional routes, as demonstrated via the photodegradation of the nuclear fast red (NFR) dye.We describe a novel procedure to fabricate a recyclable hybrid-photocatalyst based on Bi2O3@HKUST-1 MOF porous thin films. Bi2O3 nanoparticles (NPs) were synthesized within HKUST-1 (or Cu3(BTC)2) surface-mounted metal-organic frame-works (SURMOFs) and characterized using X-ray diffraction (XRD), a quartz crystal microbalance (QCM) and transmission electron microscopy (TEM). The Bi2O3 semiconductor NPs (diameter 1-3 nm)/SURMOF heterostructures exhibit superior photo-efficiencies compared to NPs synthesized using conventional routes, as demonstrated via the photodegradation of the nuclear fast red (NFR) dye. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr00532b

Synthesis and characterization of ZnO incorporated magnetically recoverable KIT-6 as a novel and efficient catalyst in the preparation of symmetrical N, N‧-alkylidene bisamides

NASA Astrophysics Data System (ADS)

Saadati-Moshtaghin, Hamid Reza; Zonoz, Farrokhzad Mohammadi; Amini, Mostafa M.

2018-04-01

A novel magnetically recoverable nanocomposite consisting of the NiFe2O4 core and KIT-6 mesoporous silica shell incorporated with ZnO nanoparticles was constructed. This nanocomposite was characterized by Fourier transform infrared (FT-IR), powder X-ray diffraction (XRD), Brunauer Emmett Teller (BET), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). This new nanocomposite demonstrated a catalytic performance in the synthesis of symmetrical N,N‧-alkylidene bisamides at the condensation reaction under solvent-free conditions. The nanocatalyst could simply be recovered from the reaction environment by using an exterior magnet and reused five times without a remarkable losing in the catalytic property.

Ion-pairing in aqueous CaCl 2 and RbBr solutions. Simultaneous structural refinement of XAFS and XRD data

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

Pham, Thai V.; Fulton, John L.

2013-01-22

We present a new methodology involving the simultaneous refinement of both x-ray absorption and x-ray diffraction spectra (X-ray Absorption/Diffraction Structural Refinement,XADSR), to study hydration and ion pair structure of CaCl 2 and RbBr salts in concentrated aqueous solutions. The XADSR analysis includes the XAFS spectra analysis of both the cation and anion as a probe of their short-range structure with an XRD spectral analysis as a probe of the global structural. Together they deliver a comprehensive picture of the cation and anion hydration, the contact ion pair (CIP) structure and the solvent-separated ion pair (SSIP) structure. XADSR analysis of 6.0more » m aqueous CaCl 2 reveals that there are an insignificant number of Ca 2+-Cl- CIP’s, but there are approximately 3.4 SSIP’s separated by about 4.99 Å. In contrast XADSR analysis of aqueous RbBr yields about 0.7 pair CIP at a bond length 3.51 Å. The present work demonstrates a new approach for a direct co-refinement of XRD and XAFS spectra in a simple and reliable fashion, opening new opportunities for analysis in various disordered and crystalline systems. This work was supported by the U.S. Department of Energy (DOE), Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences and Biosciences. Pacific Northwest National Laboratory (PNNL) is operated for the U.S. Department of Energy by Battelle.« less

Microstructural, electrical and frequency-dependent properties of Au/p-Cu2ZnSnS4/n-GaN heterojunction.

PubMed

Rajagopal Reddy, V; Janardhanam, V; Won, Jonghan; Choi, Chel-Jong

2017-08-01

An Au/Cu 2 ZnSnS 4 (CZTS)/n-GaN heterojunction (HJ) is fabricated with a CZTS interlayer and probed its chemical states, structural, electrical and frequency-dependent characteristics by XPS, TEM, I-V and C-V measurements. XPS and TEM results confirmed that the CZTS films are formed on the n-GaN surface. The band gap of deposited CZTS film is found to be 1.55eV. The electrical properties of HJ correlated with the Au/n-GaN Schottky junction (SJ). The Au/CZTS/n-GaN HJ reveals a good rectification nature with high barrier height (0.82eV) compared to the Au/n-GaN SJ (0.69eV), which suggests the barrier height is influenced by the CZTS interlayer. The barrier height values assessed by I-V, Cheung's and Norde functions are closely matched with one other, thus the methods used here are reliable and valid. The extracted interface state density (N SS ) of Au/CZTS/n-GaN HJ is lower compared to the Au/n-GaN SJ that suggests the CZTS interlayer plays an important role in the reduction of N SS . Moreover, the capacitance-frequency (C-f) and conductance-frequency (G-f) characteristics of SJ and HJ are measured in the range of 1kHz-1MHz, and found that the capacitance and conductance strappingly dependent on frequency. It is found that the N SS estimated from C-f and G-f characteristics is lower compared to those estimated from I-V characteristics. Analysis confirmed that Poole-Frenkel emission dominates the reverse leakage current in both SJ and HJ, probably related to the structural defects and trap levels in the CZTS interlayer. Copyright © 2017 Elsevier Inc. All rights reserved.

TEM-nanoindentation studies of semiconducting structures.

PubMed

Le Bourhis, E; Patriarche, G

2007-01-01

This paper reviews the application of nanoindentation coupled with transmission electron microscopy (TEM) to investigations of the plastic behaviour of semiconducting structures and its implication for device design. Instrumented nanoindentation has been developed to extract the mechanical behaviour of small volumes scaled to those encountered in semiconductor heterostructures. We illustrate that TEM is a powerful complementary tool for the study of local plasticity induced by nanoindentation. TEM-nanoindentation allows for detailed understanding of the plastic deformation in semiconducting structures and opens practical routes for improvement of devices. Performances of heterostructures are deteriously affected by dislocations that relax the lattice mismatched layers. Different ways to obtain compliant substructures are being developed in order to concentrate the plastic relaxation underneath the heterostructure. Such approaches allow for mechanical design of micro- and opto-electronic devices to be considered throughout the fabrication process.

High-quality III-nitride films on conductive, transparent (2̅01)-oriented β-Ga2O3 using a GaN buffer layer

PubMed Central

Muhammed, M. M.; Roldan, M. A.; Yamashita, Y.; Sahonta, S.-L.; Ajia, I. A.; Iizuka, K.; Kuramata, A.; Humphreys, C. J.; Roqan, I. S.

2016-01-01

We demonstrate the high structural and optical properties of InxGa1−xN epilayers (0 ≤ x ≤ 23) grown on conductive and transparent (01)-oriented β-Ga2O3 substrates using a low-temperature GaN buffer layer rather than AlN buffer layer, which enhances the quality and stability of the crystals compared to those grown on (100)-oriented β-Ga2O3. Raman maps show that the 2″ wafer is relaxed and uniform. Transmission electron microscopy (TEM) reveals that the dislocation density reduces considerably (~4.8 × 107 cm−2) at the grain centers. High-resolution TEM analysis demonstrates that most dislocations emerge at an angle with respect to the c-axis, whereas dislocations of the opposite phase form a loop and annihilate each other. The dislocation behavior is due to irregular (01) β-Ga2O3 surface at the interface and distorted buffer layer, followed by relaxed GaN epilayer. Photoluminescence results confirm high optical quality and time-resolved spectroscopy shows that the recombination is governed by bound excitons. We find that a low root-mean-square average (≤1.5 nm) of InxGa1−xN epilayers can be achieved with high optical quality of InxGa1−xN epilayers. We reveal that (01)-oriented β-Ga2O3 substrate has a strong potential for use in large-scale high-quality vertical light emitting device design. PMID:27412372

Synthesis and characterization of AlTiSiN/CrSiN multilayer coatings by cathodic arc ion-plating

NASA Astrophysics Data System (ADS)

Yang, B.; Tian, C. X.; Wan, Q.; Yan, S. J.; Liu, H. D.; Wang, R. Y.; Li, Z. G.; Chen, Y. M.; Fu, D. J.

2014-09-01

AlTiSiN/CrSiN multilayer coatings were deposited on Si (1 0 0) and cemented carbide substrates using Cr, AlTi cathodes and SiH4 gases by cathodic arc ion plating system. The influences of SiH4 gases flowrate on the structural and mechanical properties of the coatings were investigated, systematically. AlTiSiN/CrSiN coatings exhibit a B1 NaCl-type nano-multilayered structure in which the CrSiN nano-layers alternate with AlTiSiN nano-layers with multiple orientations of crystal planes indicated by XRD patterns and TEM. Si contents of the coatings increase with increasing SiH4 flowrate. The hardness of the coatings increases to the maximum value of 3500 Hv0.05 with increasing SiH4 flowrate from 20 to 40 sccm and then decreases with further addition of SiH4 gases. A higher adhesive force of 73 N is obtained at the flowrate of 48 sccm. The coatings exhibit different tribological performance when the mating materials were varied from Si3N4 to cemented carbide balls and the variation of friction coefficients of the coatings against Si3N4 influenced by SiH4 flowrate are not obvious as against cemented carbide balls.

Epitaxial growth of mixed conducting layered Ruddlesden–Popper La{sub n+1}Ni{sub n}O{sub 3n+1} (n = 1, 2 and 3) phases by pulsed laser deposition

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

Wu, Kuan-Ting; Soh, Yeong-Ah; Skinner, Stephen J., E-mail: s.skinner@imperial.ac.uk

2013-10-15

Graphical abstract: - Highlights: • High quality epitaxial thin films of layered Ruddlesden–Popper nickelates were prepared. • For the first time this has been achieved by the PLD process. • n = 1, 2 and 3 films were successfully deposited on SrTiO{sub 3} and NdGaO{sub 3} substrates. • c-Axis oriented films were confirmed by XRD analysis. • In-plane and out-of-plane strain effects on lattice are discussed. - Abstract: Layered Ruddlesden–Popper phases of composition La{sub n+1}Ni{sub n}O{sub 3n+1} (n = 1, 2 and 3) have been epitaxially grown on SrTiO{sub 3} (0 0 1) or NdGaO{sub 3} (1 1 0) singlemore » crystal substrates using the pulsed laser deposition technique. X-ray diffraction analyses (θ/2θ, rocking curves, and φ-scans) and atomic force microscopy confirms the high-quality growth of the series of films with low surface roughness values (less than 1 nm). In particular, epitaxial growth of the higher order phases (n = 2 and 3) of lanthanum nickelate have been demonstrated for the first time.« less

The K 2S 2O 8-KOH photoetching system for GaN

NASA Astrophysics Data System (ADS)

Weyher, J. L.; Tichelaar, F. D.; van Dorp, D. H.; Kelly, J. J.; Khachapuridze, A.

2010-09-01

A recently developed photoetching system for n-type GaN, a KOH solution containing the strong oxidizing agent potassium peroxydisulphate (K 2S 2O 8), was studied in detail. By careful selection of the etching parameters, such as the ratio of components and the hydrodynamics, two distinct modes were defined: defect-selective etching (denoted by KSO-D) and polishing (KSO-P). Both photoetching methods can be used under open-circuit (electroless) conditions. Well-defined dislocation-related etch whiskers are formed during KSO-D etching. All types of dislocations are revealed, and this was confirmed by cross-sectional TEM examination of the etched samples. Extended electrically active defects are also clearly revealed. The known relationship between etch rate and carrier concentration for photoetching of GaN in KOH solutions was confirmed for KSO-D etch using Raman measurements. It is shown that during KSO-P etching diffusion is the rate-limiting step, i.e. this etch is suitable for polishing of GaN. Some constraints of the KSO etching system for GaN are discussed and peculiar etch features, so far not understood, are described.

Microstructure, mechanical and tribological performance of hybrid A359/(SiC  +  Si3N4) composites for automotive applications

NASA Astrophysics Data System (ADS)

Shalaby, Essam A. M.; Churyumov, Alexander Yu

2017-11-01

In this study, microstructure analysis, yield strength at high temperatures and wear rate of hybrid A359/(SiC  +  Si3N4) composites were investigated. Different weight percent of (SiC  +  Si3N4) particles were introduced to synthesis the composites using stir/squeeze process. XRD, SEM, TEM and EDS were utilized to investigate the distribution of particles throughout the matrix, and the interfacial reaction at matrix/particle interface. It confirmed the existence of MgAl2O4 which enhances the wettability between the particles and the matrix, and the absence of particle agglomeration. The (SiC  +  Si3N4) addition not only enhances the hardness measurements but also leads to a reduction in the dendritic arm spacing (DAS). Moreover, it develops the wear performance and the yield strength at high temperatures. The developed composites provide a promising material suitable for automotive industries.

Synthesis and Enhanced Ethanol Gas Sensing Properties of the g-C3N4 Nanosheets-Decorated Tin Oxide Flower-Like Nanorods Composite

PubMed Central

Qin, Cong; Zhang, Bo; Sun, Guang; Zhang, Zhanying

2017-01-01

Flower-like SnO2/g-C3N4 nanocomposites were synthesized via a facile hydrothermal method by using SnCl4·5H2O and urea as the precursor. The structure and morphology of the as-synthesized samples were characterized by using the X-ray powder diffraction (XRD), electron microscopy (FESEM and TEM), and Fourier transform infrared spectrometer (FT-IR) techniques. SnO2 displays the unique 3D flower-like microstructure assembled with many uniform nanorods with the lengths and diameters of about 400–600 nm and 50–100 nm, respectively. For the SnO2/g-C3N4 composites, SnO2 flower-like nanorods were coupled by a lamellar structure 2D g-C3N4. Gas sensing performance test results indicated that the response of the sensor based on 7 wt. % 2D g-C3N4-decorated SnO2 composite to 500 ppm ethanol vapor was 150 at 340 °C, which was 3.5 times higher than that of the pure flower-like SnO2 nanorods-based sensor. The gas sensing mechanism of the g-C3N4nanosheets-decorated SnO2 flower-like nanorods was discussed in relation to the heterojunction structure between g-C3N4 and SnO2. PMID:28937649

Effect of H2O on the morphological changes of KNO3 formed on K2O/Al2O3 NOx storage materials: Fourier transform infra-red (FTIR) and time-resolved x-ray diffraction (TR-XRD) studies

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

Kim, Do Heui; Mudiyanselage, Kumudu K.; Szanyi, Janos

Based on combined FTIR and XRD studies, we report here that H2O induces a morphological change of KNO3 species formed on model K2O/Al2O3 NOx storage-reduction catalysts. Specifically as evidenced by FTIR, the contact of H2O with NO2 pre-adsorbed on K2O/Al2O3 promotes the transformation from bidentate (surface-like) KNO3 species to ionic (bulk-like) ones irrespective of K loadings. Once H2O is removed from the sample, a reversible transformation into bidentate KNO3 is observed, demonstrating a significant dependence of H2O on such morphological changes. TR-XRD results show the formation of two different types of bulk KNO3 phases (orthorhomobic and rhombohedral) in an as-impregnatedmore » sample. Once H2O begins to desorb above 400 K, the former is transformed into the latter, resulting in the existence of only the rhombohedral KNO3 phase. On the basis of consistent FTIR and TR-XRD results, we propose a model for the morphological changes of KNO3 species with respect to NO2 adsorption/desorption, H2O and/or heat treatments. Compared with the BaO/Al2O3 system, K2O/Al2O3 shows some similarities with respect to the formation of bulk nitrates upon H2O contact. However, there are significant differences that originate from the lower melting temperature of KNO3 relative to Ba(NO3)2.« less

Physicochemical characterizations of nano-palm oil fuel ash

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

Rajak, Mohd Azrul Abdul, E-mail: azrulrajak88@gmail.com; Preparatory Centre of Science and Technology, Universiti Malaysia Sabah, Jalan UMS, 88400, Kota Kinabalu, Sabah; Majid, Zaiton Abdul, E-mail: zaiton@kimia.fs.utm.my

2015-07-22

Palm Oil Fuel Ash (POFA) is known as a good supplementary cementing material due to its siliceous-rich content. The application of nanotechnology in the pozzolanic materials could invent new functions in the efficiency of physical and chemical properties of materials. Thus, the present study aims to generate nano-sized POFA and characterize the physicochemical properties of nano-palm oil fuel ash (nPOFA). The nPOFA was prepared by mechanically grinding micro POFA using a high intensity ball milling for 6 hours. The physicochemical properties of nPOFA were characterized via X-Ray Fluoresence (XRF), Scanning Emission microscopy- Energy Dispersive X-Ray (SEM-EDX), Transmission Electron Microscope (TEM)more » and X-Ray Diffraction (XRD). The particle size of nPOFA acquired from TEM analysis was in the range of 20 nm to 90 nm, while the average crystallite size calculated from XRD diffractogram was 61.5 nm. The resulting nPOFA has a BET surface area of 145.35 m{sup 2}/g, which is more than 85% increment in surface area compared to micro-sized POFA. The morphology and elemental studies showed the presence of spherical as well as irregularly shaped and fine nPOFA particles contains with high silicon content. The presence of α-quartz as the major phase of the nPOFA was identified through XRD analysis. The study concludes that nPOFA has the potential as a supplementary cementing material due to the high silica content, high surface area and the unique behaviors of nano-structured particles.« less

Physicochemical characterizations of nano-palm oil fuel ash

NASA Astrophysics Data System (ADS)

Rajak, Mohd Azrul Abdul; Majid, Zaiton Abdul; Ismail, Mohammad

2015-07-01

Palm Oil Fuel Ash (POFA) is known as a good supplementary cementing material due to its siliceous-rich content. The application of nanotechnology in the pozzolanic materials could invent new functions in the efficiency of physical and chemical properties of materials. Thus, the present study aims to generate nano-sized POFA and characterize the physicochemical properties of nano-palm oil fuel ash (nPOFA). The nPOFA was prepared by mechanically grinding micro POFA using a high intensity ball milling for 6 hours. The physicochemical properties of nPOFA were characterized via X-Ray Fluoresence (XRF), Scanning Emission microscopy- Energy Dispersive X-Ray (SEM-EDX), Transmission Electron Microscope (TEM) and X-Ray Diffraction (XRD). The particle size of nPOFA acquired from TEM analysis was in the range of 20 nm to 90 nm, while the average crystallite size calculated from XRD diffractogram was 61.5 nm. The resulting nPOFA has a BET surface area of 145.35 m2/g, which is more than 85% increment in surface area compared to micro-sized POFA. The morphology and elemental studies showed the presence of spherical as well as irregularly shaped and fine nPOFA particles contains with high silicon content. The presence of α-quartz as the major phase of the nPOFA was identified through XRD analysis. The study concludes that nPOFA has the potential as a supplementary cementing material due to the high silica content, high surface area and the unique behaviors of nano-structured particles.

The promotional role of Ni in FeVO4/TiO2 monolith catalyst for selective catalytic reduction of NOx with NH3

NASA Astrophysics Data System (ADS)

Wu, Ganxue; Feng, Xi; Zhang, Hailong; Zhang, Yanhua; Wang, Jianli; Chen, Yaoqiang; Dan, Yi

2018-01-01

The promotional effect of nickel additive on the catalytic performance of the representative FeVO4/TiO2 for NH3-SCR reaction is systematically studied for the first time in the present work. The experimental results showed that NOx conversion at low temperature and N2 selectivity could be significantly improved by Ni doping and 0.4Ni-FeV-Ti exhibited the highest NOx removal efficiency. Analysis by XRD, SEM/HR-TEM, Raman, TPD, DRIFTS, TPR and XPS showed that nickel doping effectively promoted the interaction of FeVO4 nanoparticles with TiO2, consequently resulting in an enhanced acidity property, improved redox activity and giving rise to the formation of the surface oxygen vacancies and defect sites.

Practical aspects of the use of the X(2) holder for HRTEM-quality TEM sample preparation by FIB.

PubMed

van Mierlo, Willem; Geiger, Dorin; Robins, Alan; Stumpf, Matthias; Ray, Mary Louise; Fischione, Paul; Kaiser, Ute

2014-12-01

The X(2) holder enables the effective production of thin, electron transparent samples for high-resolution transmission electron microscopy (HRTEM). Improvements to the X(2) holder for high-quality transmission electron microscopy (TEM) sample preparation are presented in this paper. We discuss the influence of backscattered electrons (BSE) from the sample holder in determining the lamella thickness in situ and demonstrate that a significant improvement in thickness determination can be achieved by comparatively simple means using the relative BSE intensity. We show (using Monte Carlo simulations) that by taking into account the finite collection angle of the electron backscatter detector, an approximately 20% underestimation of the lamella thickness in a silicon sample can be avoided. However, a correct thickness determination for light-element lamellas still remains a problem with the backscatter method; we introduce a more accurate method using the energy dispersive X-ray spectroscopy (EDX) signal for in situ thickness determination. Finally, we demonstrate how to produce a thin lamella with a nearly damage-free surface using the X(2) holder in combination with sub-kV polishing in the Fischione Instruments׳ NanoMill(®) TEM specimen preparation system. Copyright © 2014 Elsevier B.V. All rights reserved.

Reduction of Selenite to Red Elemental Selenium by Rhodopseudomonas palustris Strain N

PubMed Central

Li, Baozhen; Liu, Na; Li, Yongquan; Jing, Weixin; Fan, Jinhua; Li, Dan; Zhang, Longyan; Zhang, Xiaofeng; Zhang, Zhaoming; Wang, Lan

2014-01-01

The trace metal selenium is in demand for health supplements to human and animal nutrition. We studied the reduction of selenite (SeO3 −2) to red elemental selenium by Rhodopseudomonas palustris strain N. This strain was cultured in a medium containing SeO3 −2 and the particles obtained from cultures were analyzed using transmission electron microscopy (TEM), energy dispersive microanalysis (EDX) and X ray diffraction analysis (XRD). Our results showed the strain N could reduce SeO3 −2 to red elemental selenium. The diameters of particles were 80–200 nm. The bacteria exhibited significant tolerance to SeO3 −2 up to 8.0 m mol/L concentration with an EC50 value of 2.4 m mol/L. After 9 d of cultivation, the presence of SeO3 2− up to 1.0 m mol/L resulted in 99.9% reduction of selenite, whereas 82.0% (p<0.05), 31.7% (p<0.05) and 2.4% (p<0.05) reduction of SeO3 −2 was observed at 2.0, 4.0 and 8.0 m mol/L SeO3 2− concentrations, respectively. This study indicated that red elemental selenium was synthesized by green technology using Rhodopseudomonas palustris strain N. This strain also indicated a high tolerance to SeO3 −2. The finding of this work will contribute to the application of selenium to human health. PMID:24759917

Preparation of Cu2O modified TiO2 nanopowder and its application to the visible light photoelectrocatalytic reduction of CO2 to CH3OH

NASA Astrophysics Data System (ADS)

Li, Bin; Niu, Wenchao; Cheng, Yongwei; Gu, Junjie; Ning, Ping; Guan, Qingqing

2018-05-01

Cu2O/TiO2 nanopowders were prepared and used as thin film electrode raw materials for CO2 photoelectroreduction. Characterization results from XRD, TEM, UV-Vis and BET show that Cu2O/TiO2 composites have regular morphology, narrow band gap, excellent textural properties, and exhibits marked response of visible light. The photoelectrocatalytic results show that CO2 can be reduced to formaldehyde (i.e., intermediate) and finally methanol (i.e., end product). In addition, the CO2 photoelectroreduction pathway and the mechanism of photoelectrocatalysis are discussed. In summary, the work reports a potential method of CO2 reduction by visible-light photocatalysis without an external bias.

Effect of aluminum contents on sputter deposited CrAlN thin films

NASA Astrophysics Data System (ADS)

Vyas, A.; Zhou, Z. F.; Shen, Y. G.

2018-02-01

Pure CrN and CrAlN films with varied Al concentrations were prepared onto Si(100) substrates by an unbalanced reactive dc-magnetron sputtering system. The crystal structure, chemical states, and microstructure of the films were characterized by X-ray diffraction, X-ray photoelectron microscopy, transmission electron microscopy whereas mechanical properties were determined by nano-indentation measurements. XRD results showed a prominent (200) reflection in both CrN and CrAlN films. Results demonstrate that CrAlN films formed a solid solution and doping of Al atoms replace the Cr atoms affecting the lattice parameter and crystallization of the films. All Al doped films were of B1 NaCl-type structure, demonstrating that CrAlN films primarily crystallized in cubic structure. Microstructural investigation by TEM for a CrAlN film containing Al content of 24.1 at.%, revealed that there exists an amorphous/nanocrystalline domains (grains of about ∼ 11 nm) and hardness increases 22% when compared with pure CrN film.

Photocatalytic activity of SnO{sub 2} nanoparticles in methylene blue degradation

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

Kim, Sung Phil; Choi, Myong Yong, E-mail: mychoi@gnu.ac.kr; Choi, Hyun Chul, E-mail: chc12@chonnam.ac.kr

2016-02-15

Highlights: • Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method. • SnO{sub 2} nanoparticles displayed high photocatalytic activities for the MB degradation. • OH radicals are the main active species in photocatalysis on the SnO{sub 2} nanoparticles. - Abstract: Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method and were characterized by performing transmission electron microscopy (TEM), powder X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The powder XRD results revealed that the SnO{sub 2} nanoparticles have a typical tetragonal rutile (cassiterite) structure and the average crystallite size was found to be approximately 4.5 nm by usingmore » the Debye–Scherrer equation. The prepared SnO{sub 2} nanoparticles consist of agglomerated particles with a mean diameter of around 4–5 nm according to the analysis of TEM images. The XAS data confirmed that the prepared samples have cassiterite structures with tin oxidation state of +4. The prepared SnO{sub 2} nanoparticles were found to exhibit approximately 3.8 times higher activity than bulk SnO{sub 2} in the photodegradation of methylene blue. On the basis of a trapping experiment, we developed a possible mechanism for the photodegradation on SnO{sub 2} nanoparticles.« less

XRD investigation of the Effect of MgO Additives on ZTA-TiO2 Ceramic Composites

NASA Astrophysics Data System (ADS)

Azhar, Ahmad Zahirani Ahmad; Manshor, Hanisah; Ali, Afifah Mohd

2018-01-01

Alumina (Al2O3) based ceramics possess good mechanical properties and suitable for the application of cutting inserts. However, this monolithic ceramics suffer from lack of toughness. Hence, there are some modification were made such as the addition of yttria stabilized zirconia (YSZ) to the Al2O3 helps in increasing the toughness of the Al2O3 ceramics. Some additives such as MgO and TiO2 were used to further improve the mechanical properties of ZTA. In this study, high purity raw materials which consist of ZTA-TiO2 were mixed with different amount of MgO (0.0 - 1.0 wt %). The mixture of materials was going through wet mixing, compaction and pressureless sintering at 1600°C for one hour. The samples were characterized for phase analysis, microstructure, shrinkage rate, bulk density, Vickers hardness and fracture toughness. Based on the XRD analysis results, the secondary phase (MgAl2O4) was detected in the sample with 0.5 wt% of MgO onwards which leads to grains refinement, thus improve the density and hardness of ZTA-TiO2-MgO ceramics composites.

Graphene oxide coated with porous iron oxide ribbons for 2, 4-Dichlorophenoxyacetic acid (2,4-D) removal.

PubMed

Nethaji, S; Sivasamy, A

2017-04-01

Graphene oxide (GO) was prepared from commercially available graphite powder. Porous iron oxide ribbons were grown on the surface of GO by solvothermal process. The prepared GO-Fe 3 O 4 nanocomposites are characterized by FT-IR, XRD, VSM, SEM, TEM, Raman spectroscopy, surface functionality and zero point charge studies. The morphology of the iron oxide ribbons grown on GO is demonstrated with TEM at various magnifications. The presence of magnetite nanoparticles is evident from XRD peaks and the magnetization value is found to be 37.28emu/g. The ratio of intensity of D-peak to G-peak from Raman spectrum is 0.995. The synthesized Graphene oxide-Fe 3 O 4 nanocomposites (GO-Fe 3 O 4 ) were explored for its surface adsorptive properties by using a model organic compound, 2,4-Dichlorophenoxy acetic acid (2,4-D) from aqueous solution. Batch adsorption studies were performed and the equilibrium data are modelled with Langmuir, Freundlich and Temkin isotherms. The maximum monolayer capacity from Langmuir isotherm is 67.26mg/g. Kinetic studies were also carried out and the studied adsorption process followed pseudo second-order rate equation. Mechanism of the adsorption process is studied by fitting the data with intraparticle diffusion model and Boyd plot. The studied adsorption process is both by film diffusion and intraparticle diffusion. Copyright © 2017 Elsevier Inc. All rights reserved.

Microstructures of Ni-AlN composite coatings prepared by pulse electrodeposition technology

NASA Astrophysics Data System (ADS)

Xia, Fafeng; Xu, Huibin; Liu, Chao; Wang, Jinwu; Ding, Junjie; Ma, Chunhua

2013-04-01

Ni-AlN composite coating was fabricated onto the surface of steel substrates by using pulse electrodeposition (PED) technique in this work. The effect of pulse current on the nucleation and growth of grains was investigated using transmission electronic microscopy (TEM), X-ray diffraction (XRD), scanning electronic microscopy (SEM) and atomic force microscopy (AFM), respectively. The results show that the contents of AlN nanoparticles increase with density of pulse current and on-duty ratio of pulse current increasing. Whereas the size of nickel grains decreases with density of pulse current increasing and on-duty ratio of pulse current decreasing. Ni-AlN composite coating consists of crystalline nickel (˜68 nm) and AlN particles (˜38 nm). SEM and AFM observations show that the composite coatings obtained by PED showed more compact surfaces and less grain sizes, whereas those obtained by direct current electrodepositing have rougher surfaces and bigger grain sizes.

TEM-72, a New Extended-Spectrum β-Lactamase Detected in Proteus mirabilis and Morganella morganii in Italy

PubMed Central

Perilli, Mariagrazia; Segatore, Bernardetta; Rosaria De Massis, Maria; Riccio, Maria Letizia; Bianchi, Ciro; Zollo, Alessandro; Rossolini, Gian Maria; Amicosante, Gianfranco

2000-01-01

A new natural TEM-2 derivative, named TEM-72, was identified in a Proteus mirabilis strain and in a Morganella morganii strain isolated in Italy in 1999. Compared to TEM-1, TEM-72 contains the following amino acid substitutions: Q39K, M182T, G238S, and E240K. Kinetic analysis showed that TEM-72 exhibits an extended-spectrum activity, including activity against oxyimino-cephalosporins and aztreonam. Expression of blaTEM-72 in Escherichia coli was capable of decreasing the host susceptibility to the above drugs. PMID:10952610

Frequency dependent dielectric properties of combustion synthesized Dy2Ti2O7 pyrochlore oxide

NASA Astrophysics Data System (ADS)

Jeyasingh, T.; Saji, S. K.; Kavitha, V. T.; Wariar, P. R. S.

2018-05-01

Nanocrystalline pyrochlore material Dysprosium Titanate (Dy2Ti2O7) has been synthesized through a single step optimized combustion route. The phase purity and phase formation of the combustion product has been characterized using X-Ray diffraction analysis (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) analysis. X-Ray diffraction analysis (XRD) reveal that Dy2Ti2O7 is highly crystalline in nature with cubic structure in the Fd3m space group. The microstructures and average particle size of the prepared nanopowder were examined by High Resolution Transmission Electron Microscopy (HR-TEM). The optical band gap of the Dy2Ti2O7 nanoparticles is determined from the absorption spectrum, was attributed to direct allowed transitions through optical band gap of 3.98 eV. The frequency dependent dielectric measurements have been carried out on the sintered pellet in the frequency range 1 Hz-10 MHz. The measured value of dielectric constant (ℇ') was ˜ 43 and loss tangent (tan δ) was 4×10-3 at 1 MHz, at room temperature.

Comparison of antibacterial activities of Ag@TiO2 and Ag@SiO2 core-shell nanoparticles

NASA Astrophysics Data System (ADS)

Dhanalekshmi, K. I.; Meena, K. S.

2014-07-01

Core-shell type Ag@TiO2 nanoparticles were prepared by one pot simultaneous reduction of AgNO3 and hydrolysis of Ti (IV) isopropoxide and Ag@SiO2 core-shell nanoparticles were prepared by Stober's method. They were characterized by absorption, XRD, and HR-TEM techniques. XRD patterns show the presence of anatase form of TiO2 and amorphous form of SiO2 and the noble metal (Ag). High resolution transmission electron microscopy measurements revealed that their size is below 50 nm. The antibacterial properties of Ag@TiO2 and Ag@SiO2 core-shell nanoparticles against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) were examined by the agar diffusion method. As a result E. coli and S. aureus were shown to be substantially inhibited by Ag@TiO2 and Ag@SiO2 core-shell nanoparticles. These results demonstrated that TiO2 and SiO2 supported on the surface of Ag NPs without aggregation was proved to have enhanced antibacterial activity.

Comparison of antibacterial activities of Ag@TiO2 and Ag@SiO2 core-shell nanoparticles.

PubMed

Dhanalekshmi, K I; Meena, K S

2014-07-15

Core-shell type Ag@TiO2 nanoparticles were prepared by one pot simultaneous reduction of AgNO3 and hydrolysis of Ti (IV) isopropoxide and Ag@SiO2 core-shell nanoparticles were prepared by Stober's method. They were characterized by absorption, XRD, and HR-TEM techniques. XRD patterns show the presence of anatase form of TiO2 and amorphous form of SiO2 and the noble metal (Ag). High resolution transmission electron microscopy measurements revealed that their size is below 50 nm. The antibacterial properties of Ag@TiO2 and Ag@SiO2 core-shell nanoparticles against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) were examined by the agar diffusion method. As a result E. coli and S. aureus were shown to be substantially inhibited by Ag@TiO2 and Ag@SiO2 core-shell nanoparticles. These results demonstrated that TiO2 and SiO2 supported on the surface of Ag NPs without aggregation was proved to have enhanced antibacterial activity. Copyright © 2014 Elsevier B.V. All rights reserved.

Mineralogical composition of the meteorite El Pozo (Mexico): a Raman, infrared and XRD study.

PubMed

Ostrooumov, Mikhail; Hernández-Bernal, Maria del Sol

2011-12-01

The Raman (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of El Pozo meteorite (an ordinary chondrite L5 type; village Valle of Allende, founded in State of Chihuahua, Mexico: 26°56'N and 105°24'W, 1998). RMP measurements in the range of 100-3500 cm(-1) revealed principal characteristic bands of the major minerals: olivine, two polymorph modifications of pyroxene (OPx and CPx) and plagioclase. Some bands of the minor minerals (hematite and goethite) were also identified. All these minerals were clearly distinguished using IR and XRD techniques. XRD technique has shown the presence of some metallic phases such as kamacite and taenite as well as troilite and chromite. These minerals do not have characteristic Raman spectra because Fe-Ni metals have no active modes for Raman spectroscopy and troilite is a weak Raman scatterer. Raman mapping microspectroscopy was a key part in the investigation of El Pozo meteorite's spatial distribution of the main minerals because these samples are structurally and chemically complex and heterogeneous. The mineral mapping by Raman spectroscopy has provided information for a certain spatial region on which a spatial distribution coexists of the three typical mineral assemblages: olivine; olivine+orthopyroxene; and orthopyroxene. Copyright © 2011 Elsevier B.V. All rights reserved.

Thermally Oxidized C, N Co-Doped ANATASE-TiO2 Coatings on Stainless Steel for Tribological Properties

NASA Astrophysics Data System (ADS)

Wang, Hefeng; Shu, Xuefeng; Li, Xiuyan; Tang, Bin; Lin, Naiming

2013-07-01

Ti(C, N) coatings were prepared on stainless steel (SS) substrates by plasma surface alloying technique. Carbon-nitrogen co-doped titanium dioxide (C-N-TiO2) coatings were fabricated by oxidative of the Ti(C, N) coatings in air. The prepared C-N-TiO2 coatings were characterized by SEM, XPS and XRD. Results reveal that the SS substrates were entirely shielded by the C-N-TiO2 coatings. The C-N-TiO2 coatings are anatase in structure as characterized by X-ray diffraction. The tribological behavior of the coatings was tested with ball-on-disc sliding wear and compared with substrate. Such a C-N-TiO2 coatings showed good adhesion with the substrate and tribological properties of the SS in terms of much reduced friction coefficient and increased wear resistance.

Characterisation of 1,3-diammonium propylselenate monohydrate by XRD, FT-IR, FT-Raman, DSC and DFT studies

NASA Astrophysics Data System (ADS)

Thirunarayanan, S.; Arjunan, V.; Marchewka, M. K.; Mohan, S.; Atalay, Yusuf

2016-03-01

The crystals of 1,3-diammonium propylselenate monohydrate (DAPS) were prepared and characterised X-ray diffraction (XRD), FT-IR, FT-Raman spectroscopy, and DFT/B3LYP methods. It comprises protonated propyl ammonium moieties (diammonium propyl cations), selenate anions and water molecule which are held together by a number of hydrogen bonds and form infinite chains. The XRD data confirm the transfer of two protons from selenic acid to 1,3-diaminopropane molecule. The DAPS complex is stabilised by the presence of O-H···O and N-H···O hydrogen bonds and the electrostatic interactions as well. The N···O and O···O bond distances are 2.82-2.91 and 2.77 Å, respectively. The FT-IR and FT-Raman spectra of 1,3-diammonium propyl selenate monohydrate are recorded and the complete vibrational assignments have been discussed. The geometry is optimised by B3LYP method using 6-311G, 6-311+G and 6-311+G* basis sets and the energy, structural parameters, vibrational frequencies, IR and Raman intensities are determined. Differential scanning colorimetry (DSC) data were also presented to analyse the possibility of the phase transition. Complete natural bonding orbital (NBO) analysis is carried out to analyse the intramolecular electronic interactions and their stabilisation energies. The electrostatic potential of the complex lies in the range +1.902e × 10-2 to -1.902e × 10-2. The limits of total electron density of the complex is +8.43e × 10-2 to -8.43e × 10-2.

Effect of heat treatment on CO2 adsorption of KOH-activated graphite nanofibers.

PubMed

Meng, Long-Yue; Park, Soo-Jin

2010-12-15

In this work, graphite nanofibers (GNFs) were successfully expanded intercalating KOH followed by heat treatment in the temperature range of 700-1000 °C. The aim was to improve the CO(2) adsorption capacity of the GNFs by increasing the porosity of GNFs. The effects of heat treatment on the pore structures of GNFs were investigated by N(2) full isotherms, XRD, SEM, and TEM. The CO(2) adsorption capacity was measured by CO(2) isothermal adsorption at 25 °C and 1 atm. From the results, it was found that the activation temperature had a major influence on CO(2) adsorption capacity and textural properties of GNFs. The specific surface area, total pore volume, and mesopore volume of the GNFs increased after heat treatment. The CO(2) adsorption isotherms showed that G-900 exhibited the best CO(2) adsorption capacity with 59.2 mg/g. Copyright © 2010 Elsevier Inc. All rights reserved.

Transformation and composition evolution of nanoscale zero valent iron (nZVI) synthesized by borohydride reduction in static water.

PubMed

Liu, Airong; Liu, Jing; Zhang, Wei-Xian

2015-01-01

The reactivity of nanoscale zero valent iron (nZVI) toward targeted contaminants is affected by the initial nZVI composition and the iron oxides formed during the aging process in aquatic systems. In this paper, the aging effects of nZVI, prepared using a borohydride reduction method in static water over a period of 90 days (d), are investigated. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy are used to characterize the corrosion products of nZVI. Results show that both the structures and the compositions of the corrosion products change with the process of aging. The products of nZVI aged for 5 d in static water media are mainly magnetite (Fe3O4) and maghemite (γ-Fe2O3), accompanied by lepidocrocite (γ-FeOOH). For products aged 10 d, XRD data show the formation of ferrihydrite and lepidocrocite. When aged up to 90 d, the products are mainly γ-FeOOH mixed with small amounts of Fe3O4 and γ-Fe2O3. Transmission electronic microscopy (TEM) images show that the core-shell structure forms into a hollow spherical shape after 30 d of aging in aquatic media. The results indicate first that iron ions in the Fe(0) core diffuse outwardly toward the shell, and hollowed-out iron oxide shells emerge. Then, the iron oxide shell collapses and becomes a flaky, acicular-shaped structure. The type and the crystal phase of second iron oxide minerals are vastly different at various aging times. This study helps to explain the patterns of occurrence of specific iron oxides in different natural conditions. Copyright © 2014 Elsevier Ltd. All rights reserved.

Appendix B: Summary of TEM Particle Size Distribution Datasets

EPA Pesticide Factsheets

As discussed in the main text (see Section 5.3.2), calculation of the concentration of asbestos fibers in each of the bins of potential interest requires particle size distribution data derived using transmission electron microscopy (TEM).

Morphology and thermal studies of zinc sulfide and cadmium sulfide nanoparticles in polyvinyl alcohol matrix

NASA Astrophysics Data System (ADS)

Osuntokun, Jejenija; Ajibade, Peter A.

2016-09-01

Zn(II) and Cd(II) metal complexes of 1-cyano-1-carboethoxyethylene-2,2-dithiolato-κS,S'-bis(N,N-dimethylthiourea-κS) have been synthesized and characterized with analytical and spectroscopic techniques. The complexes were thermolysed in hexadecylamine at 200 °C to prepare ZnS and CdS nanoparticles. The nanoparticles were characterized with scanning electron microscope (SEM), transmission electron microscope (TEM), and powder X-ray diffraction (p-XRD). TEM images showed spherically shaped nanoparticles, whose sizes are in the range 4.33-7.21 nm for ZnS and 4.95-7.7 nm CdS respectively and XRD confirmed cubic crystalline phases for the nanoparticles. The optical band gap energy evaluated from the absorption spectra are 2.88 eV (430 nm) and 2.81 eV (440 nm) for the ZnS and CdS nanoparticles respectively. The as-prepared metal sulfide nanoparticles were further incorporated into polyvinyl alcohol (PVA) to give ZnS/PVA and CdS/PVA composites. The polymer nanocomposites were studied to investigate their morphology and thermal properties relative to the pure PVA. XRD diffractions indicated that the crystalline phases of the nanoparticles and the sizes in PVA matrices remained unaltered. Infra-red spectra studies revealed interactions between the PVA and the metal sulfide nanoparticles and TGA studies show that the ZnS/PVA and CdS/PVA nanocomposites exhibit better thermal stability than the pure PVA.

MultiLaue: A Technique to Extract d-spacings from Laue XRD

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

Gainsforth, Zack; Marcus, Matthew A.; Tamura, Nobumichi

We present that broad spectrum X-ray Diffraction (XRD) is named Laue after Max von Laue, and is the original XRD technique. Today, monochromatic XRD is more common because Bragg's equation allows determination of d-spacings where Laue does not. Laue still remains in use for single crystal systems because it can be used to make very accurate unit cell determinations as well as for strain and orientation mapping. Lastly, a Laue technique which could provide unambiguous determination of lattice spacings, a la Bragg's equation would be a huge leap forward, especially for multiphase samples such as meteorites, interplanetary dust particles andmore » some geological specimens.« less

MultiLaue: A Technique to Extract d-spacings from Laue XRD

DOE PAGES

Gainsforth, Zack; Marcus, Matthew A.; Tamura, Nobumichi; ...

2016-07-25

We present that broad spectrum X-ray Diffraction (XRD) is named Laue after Max von Laue, and is the original XRD technique. Today, monochromatic XRD is more common because Bragg's equation allows determination of d-spacings where Laue does not. Laue still remains in use for single crystal systems because it can be used to make very accurate unit cell determinations as well as for strain and orientation mapping. Lastly, a Laue technique which could provide unambiguous determination of lattice spacings, a la Bragg's equation would be a huge leap forward, especially for multiphase samples such as meteorites, interplanetary dust particles andmore » some geological specimens.« less

Objective function analysis for electric soundings (VES), transient electromagnetic soundings (TEM) and joint inversion VES/TEM

NASA Astrophysics Data System (ADS)

Bortolozo, Cassiano Antonio; Bokhonok, Oleg; Porsani, Jorge Luís; Monteiro dos Santos, Fernando Acácio; Diogo, Liliana Alcazar; Slob, Evert

2017-11-01

Ambiguities in geophysical inversion results are always present. How these ambiguities appear in most cases open to interpretation. It is interesting to investigate ambiguities with regard to the parameters of the models under study. Residual Function Dispersion Map (RFDM) can be used to differentiate between global ambiguities and local minima in the objective function. We apply RFDM to Vertical Electrical Sounding (VES) and TEM Sounding inversion results. Through topographic analysis of the objective function we evaluate the advantages and limitations of electrical sounding data compared with TEM sounding data, and the benefits of joint inversion in comparison with the individual methods. The RFDM analysis proved to be a very interesting tool for understanding the joint inversion method of VES/TEM. Also the advantage of the applicability of the RFDM analyses in real data is explored in this paper to demonstrate not only how the objective function of real data behaves but the applicability of the RFDM approach in real cases. With the analysis of the results, it is possible to understand how the joint inversion can reduce the ambiguity of the methods.

Synthesis of Cu/SiO2 Core-Shell Particles Using Hyperbranched Polyester as Template and Dispersant

NASA Astrophysics Data System (ADS)

Han, Wensong

2017-07-01

Third-generation hyperbranched polyester (HBPE3) was synthesized by stepwise polymerization with N, N-diethylol-3-amine methylpropionate as AB2 monomer and pentaerythritol as core molecule. Then, Cu particles were prepared by reduction of copper nitrate with ascorbic acid in aqueous solution using HBPE3 as template. Finally, Cu/SiO2 particles were prepared by coating silica on the surface of Cu particles. The structure and morphology of the samples were characterized by Fourier-transform infrared (FT-IR) spectrometry, x-ray diffraction (XRD) analysis, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The results confirmed the formation of the silica coating on the surface of Cu and that the Cu/SiO2 particles had spherical shape with particle size in the range of 0.8 μm to 2 μm. Compared with pure Cu, the synthesized Cu/SiO2 core-shell particles exhibited better oxidation resistance at high temperature. Moreover, the oxidation resistance of the Cu/SiO2 particles increased significantly with increasing tetraethyl orthosilicate (TEOS) concentration.

Application of Mythen detector: In-situ XRD study on the thermal expansion behavior of metal indium

NASA Astrophysics Data System (ADS)

Du, Rong; Chen, ZhongJun; Cai, Quan; Fu, JianLong; Gong, Yu; Wu, ZhongHua

2016-07-01

A Mythen detector has been equipped at the beamline 4B9A of Beijing Synchrotron Radiation Facility (BSRF), which is expected to enable BSRF to perform time-resolved measurement of X-ray diffraction (XRD) full-profiles. In this paper, the thermal expansion behavior of metal indium has been studied by using the in-situ XRD technique with the Mythen detector. The indium was heated from 303 to 433 K with a heating rate of 2 K/min. The in-situ XRD full-profiles were collected with a rate of one profile per 10 seconds. Rietveld refinement was used to extract the structural parameters. The results demonstrate that these collected quasi-real-time XRD profiles can be well used for structural analysis. The metal indium was found to have a nonlinear thermal expansion behavior from room temperature to the melting point (429.65 K). The a-axis of the tetragonal unit cell expands with a biquadratic dependency on temperature, while the c-axis contracts with a cubic dependency on temperature. By the time-resolved XRD measurements, it was observed that the [200] preferred orientation can maintain to about 403.15 K. While (110) is the last and detectable crystal plane just before melting of the polycrystalline indium foil. This study is not only beneficial to the application of metal indium, but also exhibits the capacity of in-situ time-resolved XRD measurements at the X-ray diffraction station of BSRF.

Template-free hydrothermal synthesis of MgO-TiO2 microcubes toward high potential removal of toxic water pollutants

NASA Astrophysics Data System (ADS)

Chowdhury, Ipsita Hazra; Kundu, Sukanya; Naskar, Milan Kanti

2018-01-01

MgO-TiO2 microcubes were synthesized by a facile template-free hydrothermal method followed by calcination. Different analytical tools such as XRD, DTA/TG, FTIR, N2 adsorption-desorption study, FESEM, TEM and UV-DRS were used to characterize the sample. The FESEM images exhibited cube shaped particles of size 2-4 μm. The MgO-TiO2 microcubes exhibit a high potential removal of toxic Pb (II) ions and photocatalytic degradation of organic dye methyl orange from water. The absorption capacity was determined by changing different experimental conditions. The spontaneity of the reaction was confirmed by thermodynamic study. The prepared MgO-TiO2 microcubes showed superior adsorption capacity up to 2900 mg g-1 for Pb (II) ions, and about 95% of photodegradation of methyl orange (MO), the water pollutants.

Technical Evaluation Motor No. 7 (TEM-07)

NASA Technical Reports Server (NTRS)

Hugh, Phil

1991-01-01

Technical Evaluation Motor Number 7 (TEM-7) was a full scale, full-duration static test firing of a high performance motor (HPM) configuration solid rocket motor (SRM) with nozzle vectoring. The static test fire occurred on 11 December 1990 at the Thiokol Corporation Static Test Bay T-97. Documented here are the procedures, performance, and results available through 22 January 1991. Critical post test hardware activities and assessment of the test data are not complete. A completed test report will be submitted 60 days after the test date. Included here is a presentation and discussion of the TEM-7 performance, anomalies, and test result concurrence with the objectives outlined in CTP-0107 Revision A, Space Shuttle Technical Evaluation Motor number 7 (TEM-07) Static Fire Test Plan.

Synthesis of PVP-stabilized ruthenium colloids with low boiling point alcohols.

PubMed

Zhang, Yuqing; Yu, Jiulong; Niu, Haijun; Liu, Hanfan

2007-09-15

A route to the preparation of poly(N-vinyl-2-pyrrolidone) (PVP)-stabilized ruthenium colloids by refluxing ruthenium(III) chloride in low boiling point alcohols was developed. Deep purple colloids with shuttle-like ruthenium particles were also synthesized. XPS measurement verified the nanoparticles were in the metallic state. The morphology of metal nanoparticles was characterized by UV-visible absorption spectrophotometry, TEM and XRD.

Optical and dielectric properties of isothermally crystallized nano-KNbO3 in Er3+-doped K2O-Nb2O5-SiO2 glasses.

PubMed

Chaliha, Reenamoni Saikia; Annapurna, K; Tarafder, Anal; Tiwari, V S; Gupta, P K; Karmakar, Basudeb

2010-01-01

Precursor glass of composition 25K(2)O-25Nb(2)O(5)-50SiO(2) (mol%) doped with Er(2)O(3) (0.5 wt% in excess) was isothermally crystallized at 800 degrees C for 0-100 h to obtain transparent KNbO(3) nanostructured glass-ceramics. XRD, FESEM, TEM, FTIRRS, dielectric constant, refractive index, absorption and fluorescence measurements were carried out to analyze the morphology, dielectric, structure and optical properties of the glass-ceramics. The crystallite size of KNbO(3) estimated from XRD and TEM is found to vary in the range 7-23 nm. A steep rise in the dielectric constant of glass-ceramics with heat-treatment time reveals the formation of ferroelectric nanocrystalline KNbO(3) phase. The measured visible photoluminescence spectra have exhibited green emission transitions of (2)H(11/2), (4)S(3/2)-->(4)I(15/2) upon excitation at 377 nm ((4)I(15/2)-->(4)G(11/2)) absorption band of Er(3+) ions. The near infrared (NIR) emission transition (4)I(13/2)-->(4)I(15/2) is detected around 1550 nm on excitation at 980 nm ((4)I(15/2)-->(4)I(11/2)) of absorption bands of Er(3+) ions. It is observed that photoluminescent intensity at 526 nm ((2)H(11/2)-->(4)I(15/2)), 550 nm ((4)S(3/2)-->(4)I(15/2)) and 1550 nm ((4)I(13/2)-->(4)I(15/2)) initially decrease and then gradually increase with increase in heat-treatment time. The measured lifetime (tau(f)) of the (4)I(13/2)-->(4)I(15/2) transition also possesses a similar trend. The measured absorption and fluorescence spectra reveal that the Er(3+) ions gradually enter into the KNbO(3) nanocrystals. Copyright 2009 Elsevier B.V. All rights reserved.

Role of Eu{sup 2+} on the blue‐green photoluminescence of In{sub 2}O{sub 3}:Eu{sup 2+} nanocrystals

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

Devi, Konsam Reenabati, E-mail: reena.kay14@manipuruniv.ac.in; Meetei, Sanoujam Dhiren, E-mail: sdmdhiren@gmail.com; Department of Physics, North Eastern Regional Institute of Science & Technology, Nirjuli, Itanagar 791109, Arunachal Pradesh

Blue‐green light emitting undoped and europium doped indium oxide nanocrystal were synthesized by simple precipitation method. X-ray diffraction (XRD) pattern confirmed the cubic phase of undoped and europium doped samples. Further, transmission electron microscopy (TEM), scanning electron microscopy (SEM) , energy dispersive analysis of X-rays (EDAX), Fourier transform infra-red (FT-IR), photoluminescence (PL), electron paramagnetic resonance (EPR) studies were performed to characterise the samples. PL analysis of the samples is the core of the present research. It includes excitation, emission and CIE (Commission Internationale de l’e´ clairage) studies of the samples. On doping europium to In{sub 2}O{sub 3} lattice, ln{sup 3+}more » site is substituted by Eu{sup 2+} thereby increasing the concentration of singly ionized oxygen vacancy and hence blue–green emission from the host is found to increase. Further, this increase in blue–green emission after doping may also be attributed to 4f → 5d transitions of Eu{sup 2+}. However, the blue–green PL emission is found to decrease after an optimum dopant concentration (Eu{sup 2+} = 4%) due to luminescence and size quenching. CIE co-ordinates of the samples are calculated to know colour of light emitted from the samples. It suggests that this blue–green light emitting In{sub 2}O{sub 3}: Eu{sup 2+} nanocrystals may find application in lighting such as in generation of white light. - Highlight: • XRD and TEM study confirms the synthesis of cubic doped and europium doped nanocrystals. • EPR study reveals the doped europium is in + 2 oxidation state. • Enhance PL emission intensity of host material due to increase in singly ionized oxygen vacancy and 4f–5d transitions of Eu{sup 2+} • CIE co-ordinates suggest the blue–green colour of the samples.« less

Third-order optical nonlinearity of N-doped graphene oxide nanocomposites at different GO ratios

NASA Astrophysics Data System (ADS)

Kimiagar, Salimeh; Abrinaei, Fahimeh

2018-05-01

In the present work, the influence of GO ratios on the structural, linear and nonlinear optical properties of nitrogen-doped graphene oxide nanocomposites (N-GO NCs) has been studied. N-GO NCs were synthesized by hydrothermal method. The XRD, FTIR, SEM, and TEM results confirmed the reduction of GO by nitrogen doping. The energy band gaps of N-GO NCs calculated from UV-Vis analyzed by using Tauc plot. To obtain further insight into potential optical changes in the N-GO NCs by increasing GO contents, Z-scan analysis was performed with nanosecond Nd-YAG laser at 532 nm. The nonlinear absorption coefficient, β, and nonlinear refractive index, n2, for N-GO NCs at the laser intensity of 113 MW/cm were measured and an increase was observed in both parameters after addition of nitrogen to GO. The third-order nonlinear optical susceptibilities of N-GO NCs were measured in the order of 10-9 esu. The results showed that N-GO NCs have negative nonlinearity which can be controlled by GO contents to obtain the highest values for nonlinear optical parameters. The nonlinear optical results not only imply that N-GO NCs can serve as an important material in the advancing of optoelectronics but also open new possibilities for the design of new graphene-based materials by variation of N and GO ratios as well as manufacturing conditions.

Enhancement of Electrochemical Performance of LiMn2O4 Spinel Cathode Material by Synergetic Substitution with Ni and S

PubMed Central

Bakierska, Monika; Świętosławski, Michał; Gajewska, Marta; Kowalczyk, Andrzej; Piwowarska, Zofia; Chmielarz, Lucjan; Dziembaj, Roman; Molenda, Marcin

2016-01-01

Nickel and sulfur doped lithium manganese spinels with a nominal composition of LiMn2−xNixO4–ySy (0.1 ≤ x ≤ 0.5 and y = 0.01) were synthesized by a xerogel-type sol-gel method followed by subsequent calcinations at 300 and 650 °C in air. The samples were investigated in terms of physicochemical properties using X-ray powder diffraction (XRD), transmission electron microscopy (EDS-TEM), N2 adsorption-desorption measurements (N2-BET), differential scanning calorimetry (DSC), and electrical conductivity studies (EC). Electrochemical characteristics of Li/Li+/LiMn2−xNixO4–ySy cells were examined by galvanostatic charge/discharge tests (CELL TEST), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV). The XRD showed that for samples calcined at 650 °C containing 0.1 and 0.2 mole of Ni single phase materials of Fd-3m group symmetry and nanoparticles size of around 50 nm were obtained. The energy dispersive X-ray spectroscopy (EDS) mapping confirmed homogenous distribution of nickel and sulfur in the obtained spinel materials. Moreover, it was revealed that the adverse phase transition at around room temperature typical for the stoichiometric spinel was successfully suppressed by Ni and S substitution. Electrochemical results indicated that slight substitution of nickel (x = 0.1) and sulfur (y = 0.01) in the LiMn2O4 enhances the electrochemical performance along with the rate capability and capacity retention. PMID:28773491

Chemical synthesis of hierarchical NiCo2S4 nanosheets like nanostructure on flexible foil for a high performance supercapacitor.

PubMed

Kim, D -Y; Ghodake, G S; Maile, N C; Kadam, A A; Sung Lee, Dae; Fulari, V J; Shinde, S K

2017-08-29

In this study, hierarchical interconnected nickel cobalt sulfide (NiCo 2 S 4 ) nanosheets were effectively deposited on a flexible stainless steel foil by the chemical bath deposition method (CBD) for high-performance supercapacitor applications. The resulting NiCo 2 S 4 sample was characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), and electrochemical measurements. XRD and X-ray photoelectron spectroscopy (XPS) results confirmed the formation of the ternary NiCo 2 S 4 sample with a pure cubic phase. FE-SEM and HR-TEM revealed that the entire foil surface was fully covered with the interconnected nanosheets like surface morphology. The NiCo 2 S 4 nanosheets demonstrated impressive electrochemical characteristics with a specific capacitance of 1155 F g -1 at 10 mV s -1 and superior cycling stability (95% capacity after 2000 cycles). These electrochemical characteristics could be attributed to the higher active area and higher conductivity of the sample. The results demonstrated that the interconnected NiCo 2 S 4 nanosheets are promising as electrodes for supercapacitor and energy storage applications.

The photocatalytic properties of hollow (GaN)1-x(ZnO)x composite nanofibers synthesized by electrospinning

NASA Astrophysics Data System (ADS)

Wang, Ding; Zhang, Minglu; Zhuang, Huaijuan; Chen, Xu; Wang, Xianying; Zheng, Xuejun; Yang, Junhe

2017-02-01

(GaN)1-x(ZnO)x composite nanofibers with hollow structure were prepared by initial electrospinning, and the subsequent calcination and nitridation. The structure and morphology characteristics of samples were investigated by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM). The characterization results showed the phase transition from ZnGa2O4 to (GaN)1-x(ZnO)x solid-solution under ammonia atmosphere. The preparation conditions were explored and the optimum nitridation temperature and holding time are 750 °C and 2 h, respectively. The photocatalytic properties of (GaN)1-x(ZnO)x with different Ga:Zn atomic ratios were investigated by degrading Rhodamine B under the visible light irradiation. The photocatalytic activity sequence is (GaN)1-x(ZnO)x (Ga:Zn = 1:2) > (GaN)1-x(ZnO)x (Ga:Zn = 1:3) > ZnO nanofibers > (GaN)1-x(ZnO)x (Ga:Zn = 1:4) > (GaN)1-x(ZnO)x (Ga:Zn = 1:1). The photocatalytic mechanism of the (GaN)1-x(ZnO)x hollow nanofibers was further studied by UV-vis diffuse reflectance spectra. The excellent photocatalytic performance of (GaN)1-x(ZnO)x hollow nanofibers was attributed to the narrow band gap and high surface area of porous nanofibers with hollow structure.

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloys

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

Kowalska-Mori, A.; Mamiya, H.; Ohnuma, M.

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 ºC. Sintering at 1000 ºC for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128more » nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.« less

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloys

DOE PAGES

Kowalska-Mori, A.; Mamiya, H.; Ohnuma, M.; ...

2018-01-17

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 ºC. Sintering at 1000 ºC for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128more » nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.« less

Structural and morphological characterization of Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} hydrotalcite produced by mechanochemistry method

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

Fahami, Abbas, E-mail: fahami@txstate.edu; Beall, Gary W., E-mail: gb11@txstate.edu; Physics Department, Faculty of Science, King Abdulaziz University, Jeddah 21589

2016-01-15

Chlorine intercalated Mg–Al layered double hydroxides (Mg–Al–Cl–LDH) with a chemical formula Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} were successfully produced by the one-step mechanochemistry method and subsequent water washing followed by drying in oven for 1 h at 80 °C. The samples were characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FT–IR), field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS), elemental mapping analysis, transmission electron microscopy (TEM), X-ray fluorescence (XRF), and the differential thermogravimetric analysis (DTGA). Results revealed that the structural characteristics of Mg–Al–Cl–LDH were affected strongly by milling time. At the beginning of milling (up to 1more » h), Hydrotalcite (HT) and Brucite were the dominant phases, while the progressive mechanical activation was completed as milling time increased, which resulted in the formation of nanostructured Mg–Al–Cl–LDH. Based on XRD and FTIR data, Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} with high purity was obtained at 5 h milling. The interlayer spacing of LDH is also strongly influenced by milling time so that it escalated from 7.737±0.001 to 8.005±0.002 (1–15 h) and then decreased to 7.937±0.001 for 20 h milled sample. Electron microscopic observation displayed that the final product had hexagonal platelet structure with lateral dimension of 20–100 nm. Therefore, the synthesis of Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} via mechanochemistry owing to simplicity and versatility can be a promising candidate for use in catalyst carriers, drug delivery, and gene delivery. - Graphical Abstract: TEM image of milled sample (Mg–Al–Cl–LDH). - Highlights: • Chlorine intercalated LDH was synthesized by a facile solid-state process. • Structural features of products were influenced strongly by the milling time. • XRD and FTIR spectra suggested predominant Mg�

In situ fabrication of ZnO@N-doped nanoporous carbon core-shell heterostructures with high photocatalytic and adsorption capacity by a calcination of ZnO@MOF strategy

NASA Astrophysics Data System (ADS)

Qi, Qi; Liu, Sujuan; Li, Xing; Kong, Chunlong; Guo, Zhiyong; Chen, Liang

2017-11-01

This report describes the controllable encapsulation of ZnO nanoparticles with N-doped nanoporous carbon (N-NpC) via a simple fabrication and calcination of ZnO@ZIF-8 (zeolitic imidazolate framework). In the fabrication of ZnO@ZIF-8, ZnO was used both as the support and Zn source for the formation of ZIF-8. After calcination under N2 atmosphere, the ZnO@N-NpC core-shell heterostructures were formed and characterized by IR, UV-vis, XRD, XPS, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). As expected, the well-defined ZnO@N-NpC core-shell nanospheres demonstrated distinct photocatalytic activity and adsorption capacity in response to the dye methylene blue (MB) in aqueous solution, and the degradation efficiency of MB is up to 99% under UV irradiation for 20 min after catalysts were reused for 5 cycles and stored for two months. Therefore, it is reasonable to believe that the ZnO@N-NpC core-shell heterostructures are new-type nanomaterials for photodegradation of the organic pollutants from wastewater.

Comparative study of GaN-based ultraviolet LEDs grown on different-sized patterned sapphire substrates with sputtered AlN nucleation layer

NASA Astrophysics Data System (ADS)

Zhou, Shengjun; Hu, Hongpo; Liu, Xingtong; Liu, Mengling; Ding, Xinghuo; Gui, Chengqun; Liu, Sheng; Guo, L. Jay

2017-11-01

GaN-based ultraviolet-light-emitting diodes (UV LEDs) with 375 nm emission were grown on different-sized patterned sapphire substrates (PSSs) with ex situ 15-nm-thick sputtered AlN nucleation layers by metal-organic chemical vapor deposition (MOCVD). It was observed through in situ optical reflectance monitoring that the transition time from a three-dimensional (3D) island to a two-dimensional (2D) coalescence was prolonged when GaN was grown on a larger PSS, owing to a much longer lateral growth time of GaN. The full widths at half-maximum (FWHMs) of symmetric GaN(002) and asymmetric GaN(102) X-ray diffraction (XRD) rocking curves decreased as the PSS size increased. By cross-sectional transmission electron microscopy (TEM) analysis, it was found that the threading dislocation (TD) density in UV LEDs decreased with increasing pattern size and fill factor of the PSS, thereby resulting in a marked improvement in internal quantum efficiency (IQE). Finite-difference time-domain (FDTD) simulations quantitatively demonstrated a progressive decrease in light extraction efficiency (LEE) as the PSS size increased. However, owing to the significantly reduced TD density in InGaN/AlInGaN multiple quantum wells (MQWs) and thus improved IQE, the light output power of the UV LED grown on a large PSS with a fill factor of 0.71 was 131.8% higher than that of the UV LED grown on a small PSS with a fill factor of 0.4, albeit the UV LED grown on a large PSS exhibited a much lower LEE.

Facile fabrication of BiOI decorated NaNbO3 cubes: A p-n junction photocatalyst with improved visible-light activity

NASA Astrophysics Data System (ADS)

Sun, Meng; Yan, Qing; Shao, Yu; Wang, Changqian; Yan, Tao; Ji, Pengge; Du, Bin

2017-09-01

To enhance the separation efficiency of photo-generated carriers, a p-n junction photocatalyst BiOI/NaNbO3 has been fabricated by a facile method. The obtained samples were characterized by XRD, SEM, TEM, HRTEM, PL, N2 sorption-desorption and DRS. DRS results showed that the light absorption edges of BiOI/NaNbO3 hybrids were red-shifted with the increase of BiOI content. The SEM and TEM images revealed that the BiOI was widely decorated over the surfaces of NaNbO3 cubes. The formation of p-n heterojunction at their interfaces was proved by the HRTEM image. The visible light-driven photocatalytic activity was evaluated by the degradation of methylene blue (MB) in aqueous solution. Compared with single NaNbO3 and BiOI, the BiOI/NaNbO3 hybrid photocatalysts have exhibited significantly enhanced activities. Meanwhile, the mass ratio of BiOI/NaNbO3 displayed important influence on the MB degradation. The hybrid photocatalyst with BiOI content of 40% performed the optimal activity. This activity enhancement should be attributed to the strong visible light absorption, the high migration and separation efficiency of photo-induced carriers. The photocurrent and PL measurements confirmed that the interfacial charge separation efficiency was greatly improved by coupling BiOI with NaNbO3. Controlled experiments proved that the degradation of pollutants was mainly attributed to the oxidizing ability of the generated holes (h+), ·O2-, and ·OH radicals.

Structural transformation of biochar black carbon by C60 superstructure: Environmental implications

USDA-ARS?s Scientific Manuscript database

Aqueous fullerene C60 nanoparticles (nC60) are frequently considered within the environmental engineering community as the aggregate of 60-carbon molecules. This study employed transmission electron microscopy (TEM) and x-ray diffraction (XRD) to demonstrate that nC60 formed via prolonged stirring ...

Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

NASA Technical Reports Server (NTRS)

Morris, R. V.; Rampe, E. B.; Graff, T. G.; Archer, P. D., Jr.; Le, L.; Ming, D. W.; Sutter, B.

2015-01-01

The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters <150 microns by a sieve. To date, diffraction patterns have been obtained for one basaltic soil (Rocknest (RN)) and four drill fines of coherent rock (John Klein (JK), Cumberland (CB), Windjana (WJ), and Confidence Hills (CH)). The CheMin instrument has detected and quantified the abundance of both primary igneous (e.g., feldspar, olivine, and pyroxene) and secondary (e.g., Ca-sulfates, hematite, akaganeite, and Fe-saponite) minerals. The diffraction patterns of all CheMin samples are also characterized by a broad diffraction band centered near 30deg 2theta and by increasing diffraction intensity (scattering continuum) from approx.15deg to approx.5deg, the 2theta minimum. Both the broad band and the scattering continuum are attributed to the presence of an XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous

Preparation of carbon-free TEM microgrids by metal sputtering.

PubMed

Janbroers, S; de Kruijff, T R; Xu, Q; Kooyman, P J; Zandbergen, H W

2009-08-01

A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775K under vacuum conditions.

ToTem: a tool for variant calling pipeline optimization.

PubMed

Tom, Nikola; Tom, Ondrej; Malcikova, Jitka; Pavlova, Sarka; Kubesova, Blanka; Rausch, Tobias; Kolarik, Miroslav; Benes, Vladimir; Bystry, Vojtech; Pospisilova, Sarka

2018-06-26

High-throughput bioinformatics analyses of next generation sequencing (NGS) data often require challenging pipeline optimization. The key problem is choosing appropriate tools and selecting the best parameters for optimal precision and recall. Here we introduce ToTem, a tool for automated pipeline optimization. ToTem is a stand-alone web application with a comprehensive graphical user interface (GUI). ToTem is written in Java and PHP with an underlying connection to a MySQL database. Its primary role is to automatically generate, execute and benchmark different variant calling pipeline settings. Our tool allows an analysis to be started from any level of the process and with the possibility of plugging almost any tool or code. To prevent an over-fitting of pipeline parameters, ToTem ensures the reproducibility of these by using cross validation techniques that penalize the final precision, recall and F-measure. The results are interpreted as interactive graphs and tables allowing an optimal pipeline to be selected, based on the user's priorities. Using ToTem, we were able to optimize somatic variant calling from ultra-deep targeted gene sequencing (TGS) data and germline variant detection in whole genome sequencing (WGS) data. ToTem is a tool for automated pipeline optimization which is freely available as a web application at  https://totem.software .

Optimisation of the Photonic Efficiency of TiO2 Decorated on MWCNTs for Methylene Blue Photodegradation.

PubMed

Abdullahi, Nura; Saion, Elias; Shaari, Abdul Halim; Al-Hada, Naif Mohammed; Keiteb, Aysar

2015-01-01

MWCNTs/TiO2 nanocomposite was prepared by oxidising MWCNT in H2SO4/HNO3 then decorating it with TiO2-p25 nanopowder. The composites were characterised using XRD, TEM, FT-IR PL and UV-vis spectroscopy. The TEM images have shown TiO2 nanoparticles immobilised onto the sidewalls of the MWCNTs. The UV-vis spectrum confirms that the nanocomposites can significantly absorb more light in the visible regions compared with the commercial TiO2 (P25). The catalytic activity of these nanocomposites was determined by photooxidation of MB aqueous solution in the presence of visible light. The MWCNTs/TiO2 (1:3) mass ratio showed maximum degradation efficiency. However, its activity was more favourable in alkaline and a neutral pH than an acidic medium.

Paper-based transparent flexible thin film supercapacitors

NASA Astrophysics Data System (ADS)

Gao, Kezheng; Shao, Ziqiang; Wu, Xue; Wang, Xi; Zhang, Yunhua; Wang, Wenjun; Wang, Feijun

2013-05-01

Paper-based transparent flexible thin film supercapacitors were fabricated using CNF-[RGO]n hybrid paper as an electrode material and charge collector. Owing to the self-anti-stacking of distorted RGO nanosheets and internal electrolyte nanoscale-reservoirs, the device exhibited good electrochemical performance (about 1.73 mF cm-2), and a transmittance of about 56% (at 550 nm).Paper-based transparent flexible thin film supercapacitors were fabricated using CNF-[RGO]n hybrid paper as an electrode material and charge collector. Owing to the self-anti-stacking of distorted RGO nanosheets and internal electrolyte nanoscale-reservoirs, the device exhibited good electrochemical performance (about 1.73 mF cm-2), and a transmittance of about 56% (at 550 nm). Electronic supplementary information (ESI) available: Experimental, TEM image, IR spectra, and XRD spectra of cellulose nanofibers, TEM image, and XRD spectra of RGO, graphite, GO nanosheets, CNF paper, and CNF-[RGO]20 hybrid paper, high-resolution C1s spectra of GO, Raman spectra of GO nanosheets, cross-sectional FESEM image of CNF-[RGO]20 hybrid paper and stress-strain curve of T-SC-20. See DOI: 10.1039/c3nr00674c

Retrofit implementation of Zernike phase plate imaging for cryo-TEM

PubMed Central

Marko, Michael; Leith, ArDean; Hsieh, Chyongere; Danev, Radostin

2011-01-01

In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. PMID:21272647

Design of a TEM cell EMP simulator

NASA Astrophysics Data System (ADS)

Sevat, Pete

1991-06-01

Electromagnetic pulse (EMP) simulators are designed to simulate the EMP generated by a nuclear weapon and are used to harden equipment against the effects of EMP. A transverse electromagnetic (TEM) cell is a square or rectangular coaxial transmission line tapered at each end to form a closed cell. The cell is fed at one end with a signal generator, a continuous wave or pulse generator, and terminated at the other end with a resistor equal to the characteristic impedance of the line. An advantage of the TEM cell is that the field is well characterized and reasonably uniform. A small, symmetric, TEM cell EMP simulator is described which is intended for applications such as susceptibility testing of small equipment, calibration of sensors, design and testing of countermeasures, measurement of transfer functions, and research and development. A detailed design is presented for a 50 ohm and 100 ohm TEM cell with an inner volume of 4 m(exp 3) and a test volume of 0.24 m(exp 3). The pulse generator and terminating network are integrated into the cell to form a completely shielded structure. In this way no interference from the inside of the cell to the outside, or vice versa, will occur.

From single-site tantalum complexes to nanoparticles of Ta x N y and TaO x N y supported on silica: elucidation of synthesis chemistry by dynamic nuclear polarization surface enhanced NMR spectroscopy and X-ray absorption spectroscopy.

PubMed

Mohandas, Janet C; Abou-Hamad, Edy; Callens, Emmanuel; Samantaray, Manoja K; Gajan, David; Gurinov, Andrei; Ma, Tao; Ould-Chikh, Samy; Hoffman, Adam S; Gates, Bruce C; Basset, Jean-Marie

2017-08-01

Air-stable catalysts consisting of tantalum nitride nanoparticles represented as a mixture of Ta x N y and TaO x N y with diameters in the range of 0.5 to 3 nm supported on highly dehydroxylated silica were synthesized from TaMe 5 (Me = methyl) and dimeric Ta 2 (OMe) 10 with guidance by the principles of surface organometallic chemistry (SOMC). Characterization of the supported precursors and the supported nanoparticles formed from them was carried out by IR, NMR, UV-Vis, extended X-ray absorption fine structure, and X-ray photoelectron spectroscopies complemented with XRD and high-resolution TEM, with dynamic nuclear polarization surface enhanced NMR spectroscopy being especially helpful by providing enhanced intensities of the signals of 1 H, 13 C, 29 Si, and 15 N at their natural abundances. The characterization data provide details of the synthesis chemistry, including evidence of (a) O 2 insertion into Ta-CH 3 species on the support and (b) a binuclear to mononuclear transformation of species formed from Ta 2 (OMe) 10 on the support. A catalytic test reaction, cyclooctene epoxidation, was used to probe the supported nanoparticles, with 30% H 2 O 2 serving as the oxidant. The catalysts gave selectivities up to 98% for the epoxide at conversions as high as 99% with a 3.4 wt% loading of Ta present as Ta x N y /TaO x N y .

A Facile One-Pot Synthesis of Au/Cu2O Nanocomposites for Nonenzymatic Detection of Hydrogen Peroxide

NASA Astrophysics Data System (ADS)

Chen, Ting; Tian, Liangliang; Chen, Yuan; Liu, Bitao; Zhang, Jin

2015-06-01

Au/Cu2O nanocomposites were successfully synthesized by a facile one-pot redox reaction without additional reducing agent under room temperature. The morphologies and structures of the as-prepared products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The electrocatalytic performance of Au/Cu2O nanocomposites towards hydrogen peroxide was evaluated by cyclic voltammetry (CV) and chronoamperometry (CA). The prepared Au/Cu2O nanocomposite electrode showed a wide linear range from 25 to 11.2 mM ( R = 0.9989) with a low detection limit of 1.05 μM ( S/ N = 3) and high sensitivity of 292.89 mA mM-1 cm-2. The enhanced performance for H2O2 detection can be attributed to the introduction of Au and the synergistic effect between Au and Cu2O. It is demonstrated that the Au/Cu2O nanocomposites material could be a promising candidate for H2O2 detection.

Synthesis of mesoporous cerium compound for CO2 capture

NASA Astrophysics Data System (ADS)

Liu, Guiqing; Tatsuda, Kou; Yoneyama, Yoshiharu; Tsubaki, Noritatsu

2017-11-01

A mesoporous adsorbent was simply synthesized by adding alkaline substances to cerium(III) nitric hydrate. The surface characteristics of the synthesized cerium compound were determined with BET, XRD and TEM analysis. It was found that although the specific surface areas of the synthesized cerium compounds were among about 120-200m2 per gram (BET area) which were smaller than the common used zeolite 13X (BET area 743 m2/g) and activated carbon (BET area 1079 m2/g), but the cerium compounds had excellent performances for CO2 adsorption as well as the CO2 desorption.

Retrofit implementation of Zernike phase plate imaging for cryo-TEM.

PubMed

Marko, Michael; Leith, Ardean; Hsieh, Chyongere; Danev, Radostin

2011-05-01

In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. Copyright © 2011 Elsevier Inc. All rights reserved.

CdSe nanorod/TiO2 nanoparticle heterojunctions with enhanced solar- and visible-light photocatalytic activity

PubMed Central

Laatar, Fakher; Moussa, Hatem; Alem, Halima; Balan, Lavinia; Girot, Emilien; Medjahdi, Ghouti; Ezzaouia, Hatem

2017-01-01

CdSe nanorods (NRs) with an average length of ≈120 nm were prepared by a solvothermal process and associated to TiO2 nanoparticles (Aeroxide® P25) by annealing at 300 °C for 1 h. The content of CdSe NRs in CdSe/TiO2 composites was varied from 0.5 to 5 wt %. The CdSe/TiO2 heterostructured materials were characterized by XRD, TEM, SEM, XPS, UV–visible spectroscopy and Raman spectroscopy. TEM images and XRD patterns show that CdSe NRs with wurtzite structure are associated to TiO2 particles. The UV–visible spectra demonstrate that the narrow bandgap of CdSe NRs serves to increase the photoresponse of CdSe/TiO2 composites until ≈725 nm. The CdSe (2 wt %)/TiO2 composite exhibits the highest photocatalytic activity for the degradation of rhodamine B in aqueous solution under simulated sunlight or visible light irradiation. The enhancement in photocatalytic activity likely originates from CdSe sensitization of TiO2 and the heterojunction between these materials which facilitates electron transfer from CdSe to TiO2. Due to its high stability (up to ten reuses without any significant loss in activity), the CdSe/TiO2 heterostructured catalysts show high potential for real water decontamination. PMID:29354345

CdSe nanorod/TiO2 nanoparticle heterojunctions with enhanced solar- and visible-light photocatalytic activity.

PubMed

Laatar, Fakher; Moussa, Hatem; Alem, Halima; Balan, Lavinia; Girot, Emilien; Medjahdi, Ghouti; Ezzaouia, Hatem; Schneider, Raphaël

2017-01-01

CdSe nanorods (NRs) with an average length of ≈120 nm were prepared by a solvothermal process and associated to TiO 2 nanoparticles (Aeroxide ® P25) by annealing at 300 °C for 1 h. The content of CdSe NRs in CdSe/TiO 2 composites was varied from 0.5 to 5 wt %. The CdSe/TiO 2 heterostructured materials were characterized by XRD, TEM, SEM, XPS, UV-visible spectroscopy and Raman spectroscopy. TEM images and XRD patterns show that CdSe NRs with wurtzite structure are associated to TiO 2 particles. The UV-visible spectra demonstrate that the narrow bandgap of CdSe NRs serves to increase the photoresponse of CdSe/TiO 2 composites until ≈725 nm. The CdSe (2 wt %)/TiO 2 composite exhibits the highest photocatalytic activity for the degradation of rhodamine B in aqueous solution under simulated sunlight or visible light irradiation. The enhancement in photocatalytic activity likely originates from CdSe sensitization of TiO 2 and the heterojunction between these materials which facilitates electron transfer from CdSe to TiO 2 . Due to its high stability (up to ten reuses without any significant loss in activity), the CdSe/TiO 2 heterostructured catalysts show high potential for real water decontamination.

Structural, mechanical, electrical and wetting properties of ZrNx films deposited by Ar/N2 vacuum arc discharge: Effect of nitrogen partial pressure

NASA Astrophysics Data System (ADS)

Abdallah, B.; Naddaf, M.; A-Kharroub, M.

2013-03-01

Non-stiochiometric zirconium nitride (ZrNx) thin films have been deposited on silicon substrates by vacuum arc discharge of (N2 + Ar) gas mixtures at different N2 partial pressure ratio. The microstructure, mechanical, electrical and wetting properties of these films are studied by means of X-ray diffraction (XRD), micro-Raman spectroscopy, Rutherford back scattering (RBS) technique, conventional micro-hardness testing, electrical resistivity, atomic force microscopy (AFM) and contact angle (CA) measurements. RBS results and analysis show that the (N/Zr) ratio in the film increases with increasing the N2 partial pressure. A ZrNx film with (Zr/N) ratio in the vicinity of stoichiometric ZrN is obtained at N2 partial pressure of 10%. XRD and Raman results indicate that all deposited films have strained cubic crystal phase of ZrN, regardless of the N2 partial pressure. On increasing the N2 partial pressure, the relative intensity of (1 1 1) orientation with respect to (2 0 0) orientation is seen to decrease. The effect of N2 partial pressure on micro-hardness and the resistivity of the deposited film is revealed and correlated to the alteration of grain size, crystallographic texture, stoichiometry and residual stress developed in the film. In particular, it is found that residual stress and nitrogen incorporation in the film play crucial role in the alteration of micro-hardness and resistivity respectively. In addition, CA and AFM results demonstrate that as N2 partial pressure increases, both the surface hydrophobicity and roughness of the deposited film increase, leading to a significant decrease in the film surface free energy (SFE).

Properties of Gd{sub 2}O{sub 3} nanoparticles studied by hyperfine interactions and magnetization measurements

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

Correa, E. L., E-mail: eduardo.correa@usp.br; Bosch-Santos, B.; Cavalcante, F. H. M.

2016-05-15

The magnetic behavior of Gd{sub 2}O{sub 3} nanoparticles, produced by thermal decomposition method and subsequently annealed at different temperatures, was investigated by magnetization measurements and, at an atomic level, by perturbed γ − γ angular correlation (PAC) spectroscopy measuring hyperfine interactions at {sup 111}In({sup 111}Cd) probe nuclei. Nanoparticle structure, size and shape were characterized by X-ray diffraction (XRD) and Transmission Electron Microscopy (TEM). Magnetization measurements were carried out to characterize the paramagnetic behavior of the samples. XRD results show that all samples crystallize in the cubic-C form of the bixbyite structure with space group Ia3. TEM images showed that particlesmore » annealed at 873 K present particles with highly homogeneous sizes in the range from 5 nm to 10 nm and those annealed at 1273 K show particles with quite different sizes from 5 nm to 100 nm, with a wide size distribution. PAC and magnetization results show that samples annealed at 873 and 1273 K are paramagnetic. Magnetization measurements show no indication of blocking temperatures for all samples down to 2 K and the presence of antiferromagnetic correlations.« less

Structure and Dynamics of Domains in Ferroelectric Nanostructures. In-situ TEM Studies

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

Pan, Xiaoqing

2015-06-30

The goal of this project was to explore the structure and dynamic behaviors of ferroelectric domains in ferroelectric thin films and nanostructures by advanced transmission electron microscopy (TEM) techniques in close collaboration with phase field modeling. The experimental techniques used include aberration-corrected sub-Å resolution TEM and in-situ TEM using a novel scanning tunneling microscopy (STM) - TEM holder that allows the direct observation of nucleation and dynamic evolution of ferroelectric domains under applied electric field. Specifically, this project was aimed to (1) to study the roles of static electrical boundary conditions and electrical charge in controlling the equilibrium domain structuresmore » of BiFeO 3 thin films with controlled substrate constraints, (2) to explore the fundamental mechanisms of ferroelectric domain nucleation, growth, and switching under an applied electric field in both uniform thin films and nanostructures, and to understand the roles of crystal defects such as dislocations and interfaces in these processes, (3) to understand the physics of ferroelectric domain walls and the influence of defects on the electrical switching of ferroelectric domains.« less

TEM in situ cube-corner indentation analysis using ViBe motion detection algorithm

NASA Astrophysics Data System (ADS)

Yano, K. H.; Thomas, S.; Swenson, M. J.; Lu, Y.; Wharry, J. P.

2018-04-01

Transmission electron microscopic (TEM) in situ mechanical testing is a promising method for understanding plasticity in shallow ion irradiated layers and other volume-limited materials. One of the simplest TEM in situ experiments is cube-corner indentation of a lamella, but the subsequent analysis and interpretation of the experiment is challenging, especially in engineering materials with complex microstructures. In this work, we: (a) develop MicroViBE, a motion detection and background subtraction-based post-processing approach, and (b) demonstrate the ability of MicroViBe, in combination with post-mortem TEM imaging, to carry out an unbiased qualitative interpretation of TEM indentation videos. We focus this work around a Fe-9%Cr oxide dispersion strengthened (ODS) alloy, irradiated with Fe2+ ions to 3 dpa at 500 °C. MicroViBe identifies changes in Laue contrast that are induced by the indentation; these changes accumulate throughout the mechanical loading to generate a "heatmap" of features in the original TEM video that change the most during the loading. Dislocation loops with b = ½ <111> identified by post-mortem scanning TEM (STEM) imaging correspond to hotspots on the heatmap, whereas positions of dislocation loops with b = <100> do not correspond to hotspots. Further, MicroViBe enables consistent, objective quantitative approximation of the b = ½ <111> dislocation loop number density.

[Infrared spectroscopy and XRD studies of coral fossils].

PubMed

Chen, Quan-li; Zhou, Guan-min; Yin, Zuo-wei

2012-08-01

Coral fossil is an old remain of multicellular animal on the earth, and formed by various geological processes. The structural characteristics and compositions of the coral fossils with different color and radial texture on the surface were studied by infrared absorption spectroscopy and X-ray powder diffraction analyses. The results show that the studied coral fossils mainly are composed of SiO2, and the radial microstructure characterized by the calcareous coral cross-section is preserved. It is formed by metasomatism by SiO2. The infrared absorption spectra of the coral fossil with different color and texture are essentially the same, showing typical infrared absorption spectra of the quartz jade. XRD analysis shows that the main components of the coral fossils with different color and texture are consistent and mainly composed of SiO2 with a trace amount of other minerals and without CaCO3.

Facile hydrothermal synthesis of mesoporous In2O3 nanoparticles with superior formaldehyde-sensing properties

NASA Astrophysics Data System (ADS)

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

2018-03-01

Mesoporous In2O3 nanoparticles were successfully synthesized via a facile, template free, and low-cost hydrothermal method. Their morphology and structure were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal and thermogravimetry analysis (DSC-TG), and N2 adsorption-desorption analyses. The results reveal that mesoporous In2O3 nanoparticles with a size range of 40-60 nm, possess plenty of pores, and average pore size is about 5 nm. Importantly, the mesoporous structure, large specific surface area, and small size endow the mesoporous In2O3 nanoparticles with highly sensing performance for formaldehyde detection. The response value to 10 ppm HCHO is 20 at an operating temperature of 280 °C, and the response and recovery time are 4 and 8 s, respectively. It is expected that the mesoporous In2O3 nanoparticles with large specific surface area and excellent sensing properties will become a promising functional material in monitoring and detecting formaldehyde.

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

NASA Astrophysics Data System (ADS)

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

2016-01-01

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

cisTEM, user-friendly software for single-particle image processing.

PubMed

Grant, Timothy; Rohou, Alexis; Grigorieff, Nikolaus

2018-03-07

We have developed new open-source software called cis TEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cis TEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k - 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cis TEM is available for download from cistem.org. © 2018, Grant et al.

cisTEM, user-friendly software for single-particle image processing

PubMed Central

2018-01-01

We have developed new open-source software called cisTEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cisTEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k – 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cisTEM is available for download from cistem.org. PMID:29513216

Structural, magnetic and transport properties of 2D structured perovskite oxychalcogenides

NASA Astrophysics Data System (ADS)

Berthebaud, David; Lebedev, Oleg I.; Pelloquin, Denis; Maignan, Antoine

2014-10-01

We have been looking for new potential thermoelectric materials in the family of 2D structured perovskite oxychalcogenides containing [Cu2Ch2]2- blocks (Ch = S or Se). Using high temperature syntheses, a new oxyselenide Sr2CuFeO3Se has been isolated and its structure has been compared to the isotypes sulfides, Ca2CuFeO3S and Sr2CuFeO3S, prepared by the same technique. By combining powder XRD and TEM analyses their composition and structure were analyzed. They all three crystallize in the Sr2CuGaO3S-type structure, with only the oxyselenide showing a Fe deficiency which is related to the stacking faults evidenced by high resolution TEM. Transport and magnetic properties of the samples have been studied; especially their electrical resistivity is characterized by high values in the range from 1 to 10 kΩ cm at 300 K. Thermoelectric potential of these materials is also discussed.

Metal-Insulator Transition in W-doped VO2 Nanowires

NASA Astrophysics Data System (ADS)

Long, Gen; Parry, James; Whittaker, Luisa; Banerjee, Sarbajit; Zeng, Hao

2010-03-01

We report a systematic study of the metal-insulator transition in W-doped VO2 nanowires. Magnetic susceptibility were measured for a bulk amount of VO2 nanowire powder. The susceptibility shows a sharp drop with decreasing temperature corresponding to the metal-insulator transition. The transition shows large temperature hysteresis for cooling and heating. With increasing doping concentration, the transition temperatures decreases systematically from 320 K to 275K. Charge transport measurements on the same nanowires showed similar behavior. XRD and TEM measurements were taken to further determine the structure of the materials in study.

Metal organic framework g-C3N4/MIL-53(Fe) heterojunctions with enhanced photocatalytic activity for Cr(VI) reduction under visible light

NASA Astrophysics Data System (ADS)

Huang, Wenyuan; Liu, Ning; Zhang, Xiaodong; Wu, Minghong; Tang, Liang

2017-12-01

In this study, hybrid nanocomposites based on Fe-based MOF and graphitic carbon nitride (g-C3N4) were developed by a facile solvothermal method. The as-prepared materials were characterized by XRD, FESEM, TEM, XPS and PL analysis. It was showed that the introduction of a certain amount of g-C3N4 on the surface of MIL-53(Fe) would improve the separation and migration rate of photo-induced charges, consequently resulting in the boost of photocatalytic efficiency. Compared with g-C3N4 and MIL-53(Fe), the CMFe composites displayed more excellent visible light-resposive photocatalytic activity for the reduction of Cr(VI). The optimal doping content of g-C3N4 in g-C3N4/MIL-53(Fe) composite was determined to be 3.0 wt%, and it showed about 2.1 and 2.0 times as high photocatalytic efficiency for the reduction of Cr(VI) as that of pure g-C3N4 and MIL-53(Fe), respectively. Meanwhile, the composite exhibited good reusability and stability in the process of cyclic experiments. A possible photocatalytic reaction mechanism was also investigated in detail by the related electrochemical analysis.

Removal of Cd2+ and Cu2+ ions from aqueous solution by using Fe-Fe3O4/graphene oxide as a novel and efficient adsorbent

NASA Astrophysics Data System (ADS)

Le, Giang H.; Ha, Anh Q.; Nguyen, Quang K.; Nguyen, Kien T.; Dang, Phuong T.; Tran, Hoa T. K.; Vu, Loi D.; Nguyen, Tuyen V.; Lee, Gun D.; Vu, Tuan A.

2016-10-01

The nano Fe-Fe3O4/graphene oxide (GO) was successfully synthesized by the precipitation method and followed by chemical reduction using FeCl3 as iron sources and NaBH4 as reducing agent. The products were characterized by x-ray diffraction (XRD), Fourier transform infrared spectroscopy, transmission electron microscopy (TEM), BET, x-ray photoelectron spectroscopy (XPS) and VMS. From the obtained XRD and XPS results, it revealed the formation of both Fe and Fe3O4 nano particles on GO surface. TEM images showed that both Fe3O4/GO and Fe-Fe3O4/GO had small particle size of 10-20 nm and uniform size distribution. Fe3O4/GO and Fe-Fe3O4/GO were used as adsorbents for removal of Cd2+ and Cu2+ ions from aqueous solution. Maximum adsorption capacity (Q max) of Fe-Fe3O4/GO for Cu2+ and Cd2+ are 90.0 mg g-1 and 108.6 mg g-1, respectively. These values are much higher as compared to those of Fe3O4/GO as well as those reported in the literature. Additionally, this novel adsorbent can be reused by washing with diluted Hcl solution and easily recovered by applying the magnetic field. The Cd2+ adsorption isotherm fits better for the Langmuir model that of the Freundlich model and it obeys the pseudo-second order kinetic equation.

Thermal behavior of polyhalite: a high-temperature synchrotron XRD study

DOE PAGES

Xu, Hongwu; Guo, Xiaofeng; Bai, Jianming

2016-09-17

As an accessory mineral in marine evaporites, polyhalite, K 2MgCa 2(SO 4) 4·2H 2O, coexists with halite (NaCl) in salt formations, which have been considered as potential repositories for permanent storage of high-level nuclear wastes. However, because of the heat generated by radioactive decays in the wastes, polyhalite may dehydrate, and the released water will dissolve its neighboring salt, potentially affecting the repository integrity. Thus, studying the thermal behavior of polyhalite is important. In this paper, a polyhalite sample containing a small amount of halite was collected from the Salado formation at the WIPP site in Carlsbad, New Mexico. Tomore » determine its thermal behavior, in situ high-temperature synchrotron X-ray diffraction was conducted from room temperature to 1066 K with the sample powders sealed in a silica-glass capillary. At about 506 K, polyhalite started to decompose into water vapor, anhydrite (CaSO 4) and two langbeinite-type phases, K 2Ca x Mg 2-x (SO 4) 3, with different Ca/Mg ratios. XRD peaks of the minor halite disappeared, presumably due to its dissolution by water vapor. With further increasing temperature, the two langbeinite solid solution phases displayed complex variations in crystallinity, composition and their molar ratio and then were combined into the single-phase triple salt, K 2CaMg(SO 4) 3, at ~919 K. Rietveld analyses of the XRD data allowed determination of structural parameters of polyhalite and its decomposed anhydrite and langbeinite phases as a function of temperature. Finally, from the results, the thermal expansion coefficients of these phases have been derived, and the structural mechanisms of their thermal behavior been discussed.« less

RBS Depth Profiling Analysis of (Ti, Al)N/MoN and CrN/MoN Multilayers.

PubMed

Han, Bin; Wang, Zesong; Devi, Neena; Kondamareddy, K K; Wang, Zhenguo; Li, Na; Zuo, Wenbin; Fu, Dejun; Liu, Chuansheng

2017-12-01

(Ti, Al)N/MoN and CrN/MoN multilayered films were synthesized on Si (100) surface by multi-cathodic arc ion plating system with various bilayer periods. The elemental composition and depth profiling of the films were investigated by Rutherford backscattering spectroscopy (RBS) using 2.42 and 1.52 MeV Li 2+ ion beams and different incident angles (0°, 15°, 37°, and 53°). The microstructures of (Ti, Al)N/MoN multilayered films were evaluated by X-ray diffraction. The multilayer periods and thickness of the multilayered films were characterized by scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HR-TEM) and then compared with RBS results.

Binding of TEM-1 beta-lactamase to beta-lactam antibiotics by frontal affinity chromatography.

PubMed

Chen, Xiu; Li, Yuhua; Zhang, Yan; Yang, Jianting; Bian, Liujiao

2017-04-15

TEM-1 beta-lactamases can accurately catalyze the hydrolysis of the beta-lactam rings in beta-lactam antibiotics, which make beta-lactam antibiotics lose its activity, and the prerequisite for the hydrolysis procedure in the binding interaction of TEM-1 beta-lactamases with beta-lactam antibiotics is the beta-lactam rings in beta-lactam antibiotics. Therefore, the binding of TEM-1 beta-lactamase to three beta-lactam antibiotics including penicillin G, cefalexin as well as cefoxitin was explored here by frontal affinity chromatography in combination with fluorescence spectra, adsorption and thermodynamic data in the temperature range of 278-288K under simulated physiological conditions. The results showed that all the binding of TEM-1 beta-lactamase to the three antibiotics were spontaneously exothermic processes with the binding constants of 8.718×10 3 , 6.624×10 3 and 2.244×10 3 (mol/L), respectively at 288K. All the TEM-1 beta-lactamases were immobilized on the surface of the stationary phase in the mode of monolayer and there existed only one type of binding sites on them. Each TEM-1 beta-lactamase bound with only one beta-lactam antibiotic and hydrogen bond interaction and Van der Waals force were the main forces between them. This work provided an insight into the binding interactions between TEM-1 beta-lactamases and beta-lactam antibiotics, which may be beneficial for the designing and developing of new substrates resistant to TEM-1 beta-lactamases. Copyright © 2017 Elsevier B.V. All rights reserved.

Studies on the self-catalyzed Knoevenagel condensation, characterization, DPPH radical scavenging activity, cytotoxicity, and molecular properties of 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones using single crystal XRD and DFT techniques

NASA Astrophysics Data System (ADS)

Suresh Kumar, G. S.; Antony Muthu Prabhu, A.; Bhuvanesh, N.

2014-10-01

We have studied the self-catalyzed Knoevenagel condensation, spectral characterization, DPPH radical scavenging activity, cytotoxicity, and molecular properties of 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones using single crystal XRD and DFT techniques. In the absence of any catalyst, a series of novel 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones were synthesized using Meldrum’s acid and formylphenoxyaliphatic acid(s) in water. These molecules are arranged in the dimer form through intermolecular H-bonding in the single crystal XRD structure. Compounds have better DPPH radical scavenging activity and cytotoxicity against A431 cancer cell line. The optimized molecular structure, natural bond orbital analysis, electrostatic potential map, HOMO-LUMO energies, molecular properties, and atomic charges of these molecules have been studied by performing DFT/B3LYP/3-21G(*) level of theory in gas phase.

Synthesis and structural characterization of a novel Sillén - Aurivillius bismuth oxyhalide, PbBi3VO7.5Cl, and its derivatives

NASA Astrophysics Data System (ADS)

Charkin, Dmitri O.; Plokhikh, Igor V.; Kazakov, Sergey M.; Kalmykov, Stepan N.; Akinfiev, Victor S.; Gorbachev, Anatoly V.; Batuk, Maria; Abakumov, Artem M.; Teterin, Yury A.; Maslakov, Konstantin I.; Teterin, Anton Yu; Ivanov, Kirill E.

2018-01-01

A new Sillén - Aurivillius family of layered bismuth oxyhalides has been designed and successfully constructed on the basis of PbBiO2X (X = halogen) synthetic perites and γ-form of Bi2VO5.5 solid electrolyte. This demonstrates, for the first time, the ability of the latter to serve as a building block in construction of mixed-layer structures. The parent compound PbBi3VO7.5-δCl (δ ≤ 0.05) has been investigated by powder XRD, TEM, XPS methods and magnetic susceptibility measurements. An unexpected but important condition for the formation of the mixed-layer structure is partial (ca. 5%) reduction of VV into VIV which probably suppresses competitive formation of apatite-like Pb - Bi vanadates. This reduction also stabilizes the γ polymorphic form of Bi2VO5.5 not only in the intergrowth structure, but in Bi2V1-xMxO5.5-y (M = Nb, Sb) solid solutions.

Surface structural evolution of AuAg/TiO2 catalyst in the transformation of benzyl alcohol to sodium benzoate

NASA Astrophysics Data System (ADS)

Cui, Yuanyuan; Wang, Ying; Fan, Kangnian; Dai, Wei-Lin

2013-08-01

A series of AuAg/TiO2 catalysts calcined at different temperatures were used for single-pot, solvent-free synthesis of sodium benzoate and benzoic acid through the green oxidation of benzyl alcohol. The best catalytic performance, which produced a sodium benzoate yield of up to 85%, was obtained over the AuAg/TiO2 catalyst calcined at 623 K. Systematic characterizations including BET, XRD, TEM, XPS, and UV-vis DRS and ICP were carried out to investigate the influence of calcined temperature on the structural evolution of the bimetallic AuAg/TiO2 catalysts. TEM images showed that both low (473 K) and high calcinations temperatures (973 K) resulted in larger particles. The smallest particles (8.2 nm) were obtained at 623 K. This decrease in particle size may have been induced by the re-dispersion and interaction of the bimetallic species. XRD and XPS results showed that proper calcination temperature (623 K) could promote interactions between the bimetallic particles and the TiO2 support as well as the dispersion of active bimetallic species. The higher catalytic performance of the 623 K calcined catalyst could be attributed to the smaller particle size and the synergetic interaction between nano-bimetallic gold and silver species.

Coexistence of SHV-4- and TEM-24-Producing Enterobacter aerogenes Strains before a Large Outbreak of TEM-24-Producing Strains in a French Hospital

PubMed Central

Mammeri, H.; Laurans, G.; Eveillard, M.; Castelain, S.; Eb, F.

2001-01-01

In 1996, a monitoring program was initiated at the teaching hospital of Amiens, France, and carried out for 3 years. All extended-spectrum β-lactamase (ESBL)-producing Enterobacter aerogenes isolates recovered from clinical specimens were collected for investigation of their epidemiological relatedness by pulsed-field gel electrophoresis and enterobacterial repetitive intergenic consensus PCR (ERIC-PCR) and determination of the type of ESBL harbored by isoelectric focusing and DNA sequencing. Molecular typing revealed the endemic coexistence, during the first 2 years, of two clones expressing, respectively, SHV-4 and TEM-24 ESBLs, while an outbreak of the TEM-24-producing strain raged in the hospital during the third year, causing the infection or colonization of 165 patients. Furthermore, this strain was identified as the prevalent clone responsible for outbreaks in many French hospitals since 1996. This study shows that TEM-24-producing E. aerogenes is an epidemic clone that is well established in the hospital's ecology and able to spread throughout wards. The management of the outbreak at the teaching hospital of Amiens, which included the reinforcement of infection control measures, failed to obtain complete eradication of the clone, which has become an endemic pathogen. PMID:11376055

Synthesis and characterization of a mixed phase of anatase TiO2 and TiO2(B) by low pressure chemical vapour deposition (LPCVD) for high photocatalytic activity

NASA Astrophysics Data System (ADS)

Chimupala, Y.; Hyett, G.; Simpson, R.; Brydson, R.

2014-06-01

This project is concerned with enhancing photocatalytic activity by preparing a mixed phase of nano-sized TiO2. TiO2 thin films were synthesized by using Low Pressure Chemical Vapour Deposition (LPCVD). Titanium isopropoxide and N2 gas were used as the precursor and carrier gas respectively. The effects of reaction temperature, carrier gas flow rate and deposited area were studied. TiO2 thin films with nano-sized TiO2 particles were obtained under suitable conditions and SEM, TEM, powder XRD and Raman spectroscopy were employed to characterize the phase and physical appearance of synthesized materials. Preliminary results show that a dual phase (TiO2(B) and anatase) thin film nanopowder was successfully prepared by LPCVD with needle- and polygonal plate-shape crystallites respectively. This thin film deposit produced a preferred orientation of TiO2(B) needles in the [001] direction of average crystallite size 50-80 nm in length and 5-10 nm in width, whilst the crystallite size of anatase polygonal-plates was around 200 nm. The optimal LPCVD condition for preparing this mixed phase of TiO2 was 600°C with a 1 mL/s N2 flow rate.

Rapid synthesis of Fe-doped CuO-Ce0.8Zr0.2O2 catalysts for CO preferential oxidation in H2-rich streams: Effect of iron source and the ratio of Fe/Cu

NASA Astrophysics Data System (ADS)

Wang, Jing; Han, Caiyun; Gao, Xiaoya; Lu, Jichang; Wan, Gengpin; He, Dedong; Chen, Ran; Chen, Kezhen; He, Sufang; Luo, Yongming

2017-03-01

A facile route (urea grind combustion method) is described for the rapid synthesis of Fe-doped Cu-Ce-Zr catalysts within 30 min through simple grinding and combustion. The effects of iron source and Fe/Cu mass ratio on the performances of the catalysts for CO preferential oxidation (CO-PROX) are evaluated. The influences of H2O, CO2, and their mixture on the activity as well as stability of the catalysts are also investigated. The samples are characterized by XRD, N2 adsorption-desorption, H2-TPR, TEM, Raman and XPS. Fe(NO3)3 is found to be superior to FeCl3 and Fe2(SO4)3 as the iron source for Fe-CuCZ catalyst. Among the different synthesized catalysts, 1/10Fe(N)-CuCZ is found to be the most active catalyst, indicating that the optimal Fe/Cu mass ratio is 1/10. The influences of H2O, CO2, and H2O + CO2 on the catalytic performance of 1/10Fe(N)-CuCZ are in the order of CO2 < CO2 + H2O < H2O. 1/10Fe(N)-CuCZ exhibits excellent stability during a 228 h time-on-stream test. 1/10Fe(N)-CuCZ shows the highest catalytic activity and excellent stability even in the presence of H2O and CO2. The excellent catalytic performance can be attributed to the synergy between the highly dispersed copper species and ceria, as well as the formation of more oxygen vacancies and reduced copper species.

Preparation of W and N, S-codoped titanium dioxide with enhanced photocatalytic activity under visible light irradiation

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

Huo, Rui; Yang, Jing-Yu; Liu, You-Qin

2016-04-15

Highlights: • W, N, S codoped TiO{sub 2} nanoparticles were synthesized by precipitation-impregnation method. • New linkages N–Ti–O, Ti–O–S and Ti–O–W were formed. • The activity of 0.011W, 0.030(N,S)-TiO{sub 2} is 10 times higher than that of TiO{sub 2}. • The doping enhanced visible light absorbance and accelerated the charge carrier separation. - Abstract: In this work, the preparation and physiochemical characterization of tungsten, nitrogen and sulfur codoping TiO{sub 2} photocatalysts (W, N, S-TiO{sub 2}) was undertaken. W, N, S-TiO{sub 2} nanoparticles were synthesized via the precipitation-impregnation method. To investigate the structural, optical, and electronic properties, the as-prepared W, N,more » S-TiO{sub 2} photocatalysts were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS), and ultraviolet-visible diffuse reflection spectrum (DRS). W, N, S-TiO{sub 2} samples showed photo-absorption in the visible light region and higher visible light photocatalytic activity than TiO{sub 2}. 0.011W, 0.030(N, S)-TiO{sub 2} exhibited the highest visible light photocatalytic activity, and the photocatalyic degradation activity of 0.011W,0.030(N,S)-TiO{sub 2} is nearly 10 times higher than that of TiO{sub 2}. Compared with the undoped TiO{sub 2}, the improved photocatalytic activity of W, N, S-TiO{sub 2} samples under visible light irradiation is attributed to the increase of the visible light absorption and the reduction in photogenerated electron-hole recombination.« less

Synchronizing flash-melting in a diamond cell with synchrotron X ray diffraction (XRD)

NASA Astrophysics Data System (ADS)

Karandikar, Amol; Boehler, Reinhard; Meng, Yue; Rod, Eric; Shen, Guoyin

2013-06-01

The major challenges in measuring melting temperatures in laser heated diamond cells are sample instability, thermal runaway and chemical reactions. To circumvent these problems, we developed a ``flash heating'' method using a modulated CW fiber laser and fast X ray detection capability at APS (Pilatus 1M detector). As an example, Pt spheres of 5 micron diameter were loaded in a single crystal sapphire encapsulation in the diamond cell at 65 GPa and heated in a single flash heating event for 20 ms to reach a desired temperature. A CCD spectrometer and the Pilatus were synchronized to measure the temperature and the XRD signal, respectively, when the sample reached the thermal steady state. Each successive flash heating was done at a higher temperature. The integrated XRD pattern, collected during and after (300 K) each heating, showed no chemical reaction up to 3639 K, the highest temperature reached in the experiment. Pt111 and 200 peak intensity variation showed gradual recrystalization and complete diminishing at about 3600 K, indicating melting. Thus, synchronized flash heating with novel sample encapsulation circumvents previous notorious problems and enables accurate melting temperature measurement in the diamond cell using synchrotron XRD probe. Affiliation 2: Geowissenschaeften, Goethe-Universitaet, Altenhoeferallee 1, D-60438 Frankfurt a.M., Germany.

TEM studies of III-V MOSFETs for ultimate CMOS

NASA Astrophysics Data System (ADS)

Longo, Paolo

Over the past half-century electronic industry has enormously grown changing the way people live their lives. Such growth has been driven by the miniaturisation and development of the transistors which are the main components in an integrated circuit (IC) commonly referred as a chip. Until today electronic industry has been based on the use of Si and its native oxide SiO2 in transistors. However, the performance limit of conventional Si based transistors is rapidly being approached and alternatives will soon be required. One of the proposed alternatives is GaAs. n-type GaAs has a mobility 5 times higher than Si. This makes it a suitable candidate for MOSFETs devices. So far, GaAs has not been used for practical MOSFETs because of the difficulties of making a good dielectric oxide layer in terms of leakage current and unpinned Fermi Level. Using processes pioneered by Passlack et al, dielectric gate stacks consisting of a template layer of amorphous Ga2O3 followed by amorphous GdGaO have been grown on GaAs substrates. Careful deposition of Ga2O3 can leave the Fermi Level unpinned. The introduction of Gd is important in order to decrease the leakage of current. The electrical properties of the Ga2O3/Gd[x]Ga[0.4-x]O[0.6] dielectric stack are related to the Gd concentration and the quality of the GaAs/Ga2O3 interface. Over the past years in a unique partnership several research groups from the Physics and the Electronic and Electrical engineering Department have collaboratively worked for the realisation and development of such new generation of GaAs based transistors using the technology described above. The properties of such devices depend on structures at the nanoscale which is only few atoms across. Thus the characterization using the transmission electron microscope (TEM) becomes essential. In this project TEM has been used to study several MBE grown III-V semiconductor nanostructures. In particular most of the thesis is focussed on the chemical characterisation

Controllable fabrication of Bi2O3/TiO2 heterojunction with excellent visible-light responsive photocatalytic performance

NASA Astrophysics Data System (ADS)

Huang, Yunfang; Wei, Yuelin; Wang, Jing; Luo, Dan; Fan, Leqing; Wu, Jihuai

2017-11-01

Three-dimensional Bi2O3/TiO2 hierarchical composites have been successfully prepared by a two-step hydrothermal method and subsequent calcination. The samples were characterized using XRD, SEM, TEM, EDS, BET and DRS. The measurement results signified that heterojunctions of various morphologies β-Bi2O3 growing on the three-dimensional hierarchical anatase TiO2 nanorods arrays on FTO glass were apparently formed. The morphology of Bi2O3 changed from three-dimension flower-like microstructures to the sphere-like nanoparticles as the Li(OH) dosage increased. The photocatalytic results showed that all samples exhibited much higher photocatalytic activities than that of pure Bi2O3 and TiO2 (P25) in photocatalytic degradation of methyl blue (MB) under visible-light irradiation. Whereas BTL4 sample exhibited the highest photoactivity with increasing the dosage of Li(OH) to 2 mmol. Furthermore, the absorption edge of the Bi2O3/TiO2 series composites displayed a broad-spectrum photoabsorption from UV to visible-light compared with the individual component. The as-synthesized Bi2O3/TiO2 composites possessed excellent photocatalytic activity and outstanding recyclability. The enhanced photocatalytic efficiency was mainly attributed to the Bi2O3/TiO2p-n heterojunctions and hierarchical nanostructure. The recombination of photogenerated electron-hole pairs was efficiently suppressed by the Bi2O3/TiO2p-n heterojunctions.

Optimization of process parameters in the RF-DC plasma N2-H2 for AISI420 molds and dies

NASA Astrophysics Data System (ADS)

Herdianto, Hengky; Djoko, D. J.; Santjojo, H.; Masruroh

2017-11-01

The RF-DC plasma N2-H2 was used to make precise AISI420 molds and dies have complex textured geometry. The quality of the molds and dies directly affect the quality of the produced parts. The excellent examples of molds were used for injection molding lenses and dies used for the precision forging of automotive drive train components. In this study, a temperature, DC bias, and duration as process parameters of the RF-DC plasma N2-H2 have been optimized for molds and dies fabrication. The mask-less micro-patterned method was utilized to draw the initial 2D micro patterns directly onto the AISI420 substrate surface. The unprinted substrate surfaces were selectively nitrided by the RF-DC plasma N2-H2 at 673 K for 5400 s by 70 Pa with hollow cathode device. Energy Dispersive X-ray was utilized to describe the nitrogen content distribution at the vicinity of the border between the unprinted surfaces. This exclusive nitrogen mapping proves that only the unprinted parts of the substrate have high content nitrogen solutes. XRD analysis was performed to investigate whether the iron nitrides were precipitated by RF-DC plasma N2-H2 in the AISI420.

Nonfouling NTA-PEG-Based TEM Grid Coatings for Selective Capture of Histidine-Tagged Protein Targets from Cell Lysates.

PubMed

Benjamin, Christopher J; Wright, Kyle J; Hyun, Seok-Hee; Krynski, Kyle; Yu, Guimei; Bajaj, Ruchika; Guo, Fei; Stauffacher, Cynthia V; Jiang, Wen; Thompson, David H

2016-01-19

We report the preparation and performance of TEM grids bearing stabilized nonfouling lipid monolayer coatings. These films contain NTA capture ligands of controllable areal density at the distal end of a flexible poly(ethylene glycol) 2000 (PEG2000) spacer to avoid preferred orientation of surface-bound histidine-tagged (His-tag) protein targets. Langmuir-Schaefer deposition at 30 mN/m of mixed monolayers containing two novel synthetic lipids-1,2-distearoyl-sn-glycero-3-phosphoethanolamine-N-[(5-amido-1-carboxypentyl)iminodiacetic acid]polyethylene glycolamide 2000) (NTA-PEG2000-DSPE) and 1,2-(tricosa-10',12'-diynoyl)-sn-glycero-3-phosphoethanolamine-N-(methoxypolyethylene glycolamide 350) (mPEG350-DTPE)-in 1:99 and 5:95 molar ratios prior to treatment with a 5 min, 254 nm light exposure was used for grid fabrication. These conditions were designed to limit nonspecific protein adsorption onto the stabilized lipid coating by favoring the formation of a mPEG350 brush layer below a flexible, mushroom conformation of NTA-PEG2000 at low surface density to enable specific immobilization and random orientation of the protein target on the EM grid. These grids were then used to capture His6-T7 bacteriophage and RplL from cell lysates, as well as purified His8-green fluorescent protein (GFP) and nanodisc solubilized maltose transporter, His6-MalFGK2. Our findings indicate that TEM grid supported, polymerized NTA lipid monolayers are capable of capturing His-tag protein targets in a manner that controls their areal densities, while efficiently blocking nonspecific adsorption and limiting film degradation, even upon prolonged detergent exposure.

Synthesis of CeO2 nanoparticles: Photocatalytic and antibacterial activities

NASA Astrophysics Data System (ADS)

Reddy Yadav, L. S.; Lingaraju, K.; Daruka Prasad, B.; Kavitha, C.; Banuprakash, G.; Nagaraju, G.

2017-05-01

We have successfully synthesized CeO2 nanoparticles (Nps) via the solution combustion method using sugarcane juice as a novel combustible fuel. The structural features, optical properties and morphology of the nanoparticles were characterized using XRD, FTIR, and Raman spectroscopy, UV-Vis, SEM and TEM. Structural characterization of the product shows cubic phase CeO2 . FTIR and Raman spectrum show characteristic peaks due to the presence of Ce-O vibration. SEM images show a porous structure and, from TEM images, the size of the nanoparticles were found to be ˜ 50 nm. The photocatalytic degradation of the methylene blue (MB) dye was examined using CeO2 Nps under solar irradiation as well as UV light irradiation and we studied the effect of p H, catalytic load and concentration on the degradation of the MB dye. Furthermore, the antibacterial properties of CeO2 Nps were investigated against Gram+ve and Gram- ve pathogenic bacterial strains using the agar well diffusion method.

Catalytic performance of V2O5-MoO3/γ-Al2O3 catalysts for partial oxidation of n-hexane1

NASA Astrophysics Data System (ADS)

Mahmoudian, R.; Khodadadi, Z.; Mahdavi, Vahid; Salehi, Mohammed

2016-01-01

In the current study, a series of V2O5-MoO3 catalyst supported on γ-Al2O3 with various V2O5 and MoO3 loadings was prepared by wet impregnation technique. The characterization of prepared catalysts includes BET surface area, powder X-ray diffraction (XRD), and oxygen chemisorptions. The partial oxidation of n-hexane by air over V2O5-MoO3/γ-Al2O3 catalysts was carried out under flow condition in a fixed bed glass reactor. The effect of V2O5 loading, temperature, MoO3 loading, and n-hexane LHSV on the n-hexane conversion and the product selectivity were investigated. The partial oxygenated products of n-hexane oxidation were ethanol, acetic anhydride, acetic acid, and acetaldehyde. The 10% V2O5-1%MoO3/γ-Al2O3 was found in most active and selective catalyst during partial oxidation of n-hexane. The results indicated that by increasing the temperature, the n-hexane conversion increases as well, although the selectivity of the products passes through a maximum by increasing the temperature.

Understanding the Magnesiothermic Reduction Mechanism of TiO2 to Produce Ti

NASA Astrophysics Data System (ADS)

Choi, Kyunsuk; Choi, Hanshin; Sohn, Il

2017-04-01

Titanium dioxide (TiO2) powders in the mineral form of rutile were reduced to metallic and an intermediate phase via a magnesiothermic reaction in molten Mg at temperatures between 973 K and 1173 K (700 °C and 900 °C) under high-purity Ar atmosphere. The reaction behavior and pathway indicated intermediate phase formation during the magnesiothermic reduction of TiO2 using XRD (X-ray diffraction), SEM (scanning electron microscope), and TEM (transmission electron microscope). Mg/TiO2 = 2 resulted in various intermediate phases of oxygen containing titanium, including Ti6O, Ti3O, and Ti2O, with metallic Ti present. MgTi2O4 ternary intermediate phases could also be observed, but they were dependent on the excess Mg present in the sample. Nevertheless, even with excessive amounts of Mg at Mg/TiO2 = 10, complete reduction to metallic Ti could not be obtained and some Ti6O intermediate phases were present. Although thermodynamics do not predict the formation of the MgTi2O4 spinel phase, detailed phase identification through XRD, SEM, and TEM showed significant amounts of this intermediate ternary phase even at excess Mg additions. Considering the stepwise reduction of TiO2 by Mg and the pronounced amounts of MgTi2O4 phase observed, the rate-limiting reaction is likely the reduction of MgTi2O4 to the TitO phase. Thus, an additional reduction step beyond thermodynamic predictions was developed.

Sulfur Nanoparticles Synthesis and Characterization from H2S Gas, Using Novel Biodegradable Iron Chelates in W/O Microemulsion

PubMed Central

2008-01-01

Sulfur nanoparticles were synthesized from hazardous H2S gas using novel biodegradable iron chelates in w/o microemulsion system. Fe3+–malic acid chelate (0.05 M aqueous solution) was studied in w/o microemulsion containing cyclohexane, Triton X-100 andn-hexanol as oil phase, surfactant, co-surfactant, respectively, for catalytic oxidation of H2S gas at ambient conditions of temperature, pressure, and neutral pH. The structural features of sulfur nanoparticles have been characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), energy dispersive spectroscopy (EDS), diffused reflectance infra-red Fourier transform technique, and BET surface area measurements. XRD analysis indicates the presence of α-sulfur. TEM analysis shows that the morphology of sulfur nanoparticles synthesized in w/o microemulsion system is nearly uniform in size (average particle size 10 nm) and narrow particle size distribution (in range of 5–15 nm) as compared to that in aqueous surfactant systems. The EDS analysis indicated high purity of sulfur (>99%). Moreover, sulfur nanoparticles synthesized in w/o microemulsion system exhibit higher antimicrobial activity (against bacteria, yeast, and fungi) than that of colloidal sulfur.

Dopant concentration dependent growth of Fe:ZnO nanostructures

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

Sahai, Anshuman; Goswami, Navendu, E-mail: navendugoswami@gmail.com

2016-05-23

Systematic investigations of structural properties of 1-10% Fe doped ZnO nanostructure (Fe:ZnO NS) prepared via chemical precipitation method have been reported. Structural properties were probed thoroughly employing scanning electron microscope (SEM) and transmission electron microscope (TEM), energy dispersive X-ray (EDAX) analysis and X-ray diffraction (XRD). Morphological transformation of nanostructures (NS) with Fe incorporation is evident in SEM/TEM images. Nanoparticles (NP) obtained with 1% Fe, evolve to nanorods (NR) for 3% Fe; NR transform to nanocones (NC) (for 5% and 7% Fe) and finally NC transform to nanoflakes (NF) at 10% Fe. Morover, primary phase of Zn{sub 1-x}Fe{sub x}O along withmore » secondary phases of ZnFe{sub 2}O{sub 4} and Fe{sub 2}O{sub 3} were also revealed through XRD measurements. Based on collective XRD, SEM, TEM, and EDAX interpretations, a model for morphological evolution of NS was proposed and the pivotal role of Fe dopant was deciphered.« less

Fabrication of mesoporous cerium dioxide films by cathodic electrodeposition.

PubMed

Kim, Young-Soo; Lee, Jin-Kyu; Ahn, Jae-Hoon; Park, Eun-Kyung; Kim, Gil-Pyo; Baeck, Sung-Hyeon

2007-11-01

Mesoporous cerium dioxide (Ceria, CeO2) thin films have been successfully electrodeposited onto ITO-coated glass substrates from an aqueous solution of cerium nitrate using CTAB (Cetyltrimethylammonium Bromide) as a templating agent. The synthesized films underwent detailed characterizations. The crystallinity of synthesized CeO2 film was confirmed by XRD analysis and HR-TEM analysis, and surface morphology was investigated by SEM analysis. The presence of mesoporosity in fabricated films was confirmed by TEM and small angle X-ray analysis. As-synthesized film was observed from XRD analysis and HR-TEM image to have well-crystallized structure of cubic phase CeO2. Transmission electron microscopy and small angle X-ray analysis revealed the presence of uniform mesoporosity with a well-ordered lamellar phase in the CeO2 films electrodeposited with CTAB templating.

Single-step uncalcined N-TiO2 synthesis, characterizations and its applications on alachlor photocatalytic degradations

NASA Astrophysics Data System (ADS)

Suwannaruang, Totsaporn; Wantala, Kitirote

2016-09-01

The aims of this research were to synthesize nitrogen doped TiO2 (N-TiO2) photocatalysts produced by hydrothermal technique and to test the degradation performance of alachlor by photocatalytic process under UV irradiations in the effect of aging temperature and time in the preparation process. The characterizations of synthesized TiO2 such as specific surface area, particle size, phase structure and elements were analyzed by using the Brunauer-Emmett-Teller (BET) technique, Transmission Electron Microscopy (TEM), X-ray Diffractometer (XRD) and Energy Dispersive X-ray spectrometer (EDX), respectively. The Central Composite Design (CCD) was used to design the experiment to determine the optimal condition, main effects and their interactions by using specific surface area, percent alachlor removal and observed first-order rate constant as responses. The kinetic reactions of alachlor degradation were explained by using Langmuir-Hinshelwood expression to confirm the reaction took place on the surface of photocatalyst. The results showed that the effect of aging temperatures was significant on surface area, whereas aging time was insignificant. Additionally, the square term of aging temperature and interaction term were shown significant on the specific surface area as well. The highest specific surface area from response surface at aging temperature between 150-175 °C and aging time between 6-13 h was found in a range of 100-106 m2/g. The average particle size of TiO2 was similar to crystallite size. Therefore, it can be concluded that one particle has only one crystal. The element analysis has shown 10% of nitrogen in TiO2 structure that the energy band-gap about 2.95 eV was found. Although, the effects of aging temperature and time on percent alachlor removal and observed first-order rate constants were insignificant, both terms were significant in term of the square for alachlor photocatalytic degradation. The optimal condition of both responses was achieved at an

The effect of PVP on morphology, optical properties and electron paramagnetic resonance of Zn0.5Co0.5Fe2-xPrxO4 nanoparticles

NASA Astrophysics Data System (ADS)

Bitar, Z.; El-Said Bakeer, D.; Awad, R.

2017-07-01

Zinc Cobalt nano ferrite doped with Praseodymium, Zn0.5Co0.5Fe2-xPrxO4 (0 ≤ x ≤ 0.2), were prepared by co-precipitation method from an aqueous solution containing metal chlorides and two concentrations of poly(vinylpyrrolidone) (PVP) 0 and 30g/L as capping agent. The samples were characterized using X-ray powder diffraction (XRD), Transmission Electron Microscope (TEM), UV-visible optical spectroscopy, Fourier transform infrared (FTIR) and Electron Paramagnetic Resonance (EPR). XRD results display the formation of cubic spinel structure with space group Fd3m and the lattice parameter (a) is slightly decreased for PVP capping samples. The particle size that determined by TEM, decreases for PVP capping samples. The optical band energy Eg increases for PVP capping samples, confirming the variation of energy gap with the particle size. The FTIR results indicate that the metal oxide bands were shifted for the PVP capping samples. EPR data shows that the PVP addition increases the magnetic resonance field and hence decreases the g-factor.

Synthesis and structural stability of Cr-doped Li2MnSiO4/C cathode materials by solid-state method

NASA Astrophysics Data System (ADS)

Cheng, Hong-Mei; Zhao, Shi-Xi; Wu, Xia; Zhao, Jian-Wei; Wei, Lei; Nan, Ce-Wen

2018-03-01

The crystal structure of the Li2MnSiO4 cathode material would collapse during the charge and discharge process because of that the Mn-O coordination polyhedron changed from [MnO4] into [MnO6] in the process of Mn+2 to Mn+4, but the Cr element could remain [CrO4] crystal ligand from Cr+2 to Cr+4, so Cr element substitution was used to improve the structural stability of the Li2MnSiO4 cathode material. In this work, Li2Mn1-xCrxSiO4/C nanocomposites were synthesized by solid-state method. XRD, SEM and TEM observations show that the as-prepared Li2Mn1-xCrxSiO4/C materials presents an orthorhombic crystal structure (S.G. Pmn21), the particle size of Li2Mn1-xCrxSiO4/C powder ranges from 50 to 100 nm. The XRD and XPS results indicate that Cr+2 is successfully doped into Li2MnSiO4 lattice and has well compatibility with Li2MnSiO4. The electrochemical results display that Li2Mn92.5%Cr7.5%SiO4/C exhibits significantly enhanced cycle stability and discharge capability. The initial discharge capacity of the Li2Mn92.5%Cr7.5%SiO4/C sample is 255 mAh g-1, and the discharge capacity was still about 60 mAh g-1 after 50 cycles. Furthermore, the XRD patterns, TEM images and Raman analysis reveal that the Cr doping enhances the structural stability of Li2Mn1-xCrxSiO4/C and improves the electrochemical activity of the cathode. Thus, the Li2Mn92.5%Cr7.5%SiO4/C have shown potential applications for lithium ion batteries.

Synthesis of porous g-C{sub 3}N{sub 4}/La and enhanced photocatalytic activity for the degradation of phenol under visible light irradiation

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

Rong, Xinshan; Qiu, Fengxian, E-mail: fxqiu@ujs.edu.cn; Rong, Jian

2015-10-15

A series of porous g-C{sub 3}N{sub 4}/La (PGCN/La) materials used as photocatalyst for the degradation of phenol were prepared by two steps. The photocatalysts were characterized by X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy (DRS), thermogravimetry (TG), Brunauer–Emmett–Teller (BET), Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). From the TEM morphology, the porous structure of g-C{sub 3}N{sub 4} could be successfully controlled; from BET results, BET specific surface area of porous g-C{sub 3}N{sub 4} (PGCN) sample increases with the increasing of urea mass ratio. Compared with PGCN material (PGCN-50), PGCN/La sample (PGCN-50/La-5) could exhibit anmore » enhanced photocatalytic activity and has the best degradation efficiency of 98.6% within 50 min under visible light irradiation. Photocatalytic reaction follows the first-order model kinetics; and PGCN-50/La-5 photocatalyst shows the largest reaction rate among all samples which is nearly 2.96 times higher than that of pure PGCN-50. The present work illustrates that the photocatalytic activity of porous g-C{sub 3}N{sub 4} was improved by the addition of La and PGCN-50/La-5 has potential application in the removal of phenol or other organic molecular from wastewater. - Graphical abstract: Porous g-C{sub 3}N{sub 4}/La photocatalyst is synthesized and its removal of phenol application has been explored. - Highlights: • Porous PGCN/La photocatalyst was prepared successfully by hydrothermal method. • PGCN/La has a highest degradation efficiency of 98.6% for phenol within 50 min. • The reaction rate of is nearly 2.96 times higher than that of pure PGCN. • As prepared material has potential application in removal of phenol from wastewater.« less

The decomposition of mixed oxide Ag2Cu2O3: Structural features and the catalytic properties in CO and C2H4 oxidation

NASA Astrophysics Data System (ADS)

Svintsitskiy, Dmitry A.; Kardash, Tatyana Yu.; Slavinskaya, Elena M.; Stonkus, Olga A.; Koscheev, Sergei V.; Boronin, Andrei I.

2018-01-01

The mixed silver-copper oxide Ag2Cu2O3 with a paramelaconite crystal structure is a promising material for catalytic applications. The as-prepared sample of Ag2Cu2O3 consisted of brick-like particles extended along the [001] direction. A combination of physicochemical techniques such as TEM, XPS and XRD was applied to investigate the structural features of this mixed silver-copper oxide. The thermal stability of Ag2Cu2O3 was investigated using in situ XRD under different reaction conditions, including a catalytic CO + O2 mixture. The first step of Ag2Cu2O3 decomposition was accompanied by the appearance of ensembles consisting of silver nanoparticles with sizes of 5-15 nm. Silver nanoparticles were strongly oriented to each other and to the surface of the initial Ag2Cu2O3 bricks. Based on the XRD data, it was shown that the release of silver occurred along the a and b axes of the paramelaconite structure. Partial decomposition of Ag2Cu2O3 accompanied by the formation of silver nanoparticles was observed during prolonged air storage under ambient conditions. The high reactivity is discussed as a reason for spontaneous decomposition during Ag2Cu2O3 storage. The full decomposition of the mixed oxide into metallic silver and copper (II) oxide took place at temperatures higher than 300 °C regardless of the nature of the reaction medium (helium, air, CO + O2). Catalytic properties of partially and fully decomposed samples of mixed silver-copper oxide were measured in low-temperature CO oxidation and C2H4 epoxidation reactions.

High-Resolution AES Mapping and TEM Study of Cu(In,Ga)Se2 Thin Film Growth: Preprint

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

Perkins, C. L.; Yan, Y.; Jones, K.

2001-10-01

Presented at 2001 NCPV Program Review Meeting: TEM and high-resolution AES mapping data on CIGS samples. The chalcopyrite Cu(In,Ga)Se{sub 2} (CIGS) shows promise as an absorber layer in thin polycrystalline solar cells, however, details of the PVD growth of this complicated material remain in a developing stage. Previous workers have postulated the existence of a thin film of liquid Cu{sub x}Se on the growing CIGS film, and that this layer acts as a reservoir of copper as well as a layer in which rapid mass transport is possible. In this paper we present transmission electron microscopy (TEM) and high resolutionmore » Auger electron spectroscopy (AES) mapping data taken on samples that had their growth interrupted at a stage when Cu{sub x}Se was expected to be present. The AES maps show CIGS grains which are highly enriched in copper relative to the rest of the CIGS film, and that these same areas contain almost no indium, results consistent with the presence of CuxSe. Small-area diffraction analysis and energy dispersive spectroscopy (EDS) performed on these same samples independently confirm the presence of Cu{sub x}Se at the surface of growing CIGS films.« less

Rapid synthesis of rutile TiO2 nano-flowers by dealloying Cu60Ti30Y10 metallic glasses

NASA Astrophysics Data System (ADS)

Wang, Ning; Pan, Ye; Wu, Shikai; Zhang, Enming; Dai, Weiji

2018-01-01

The 3D nanostructure rutile TiO2 photocatalyst was rapidly synthesized by dealloying method using Cu60Ti30Y10 amorphous ribbons as precursors. The preparation period was kept down to just 3 h, which is much shorter than those of the samples by dealloying Cu60Ti30Al10, Cu70Ti30 and Cu60Ti30Sn10. The synthesized sample was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). XRD and XPS reveal the successful synthesis of rutile TiO2. The SEM and TEM images show that the synthesized rutile TiO2 nano-material presents homogeneous distributed 3D nanoflowers structure, which is composed of large quantities of fine rice-like nanorods (40-150 nm in diameter and 100-250 nm in length). BET specific surface areas of the samples were investigated by N2 adsorption-desorption isotherms, the fabricated rutile TiO2 exhibits very high specific surface area (194.08 m2/g). The photocatalytic activities of the samples were evaluated by degrading rhodamine B (RhB) dye (10 mg/L) under the irradiation of both simulated visible light (λ > 420 nm) and ultraviolet (UV) light (λ = 365 nm). The results show that the photocatalytic activity of rutile TiO2 prepared by dealloying Cu60Ti30Y10 amorphous ribbons is higher than those of commercial rutile and the sample synthesized by dealloying Cu70Ti30 precursors. The advantages of both short preparation period and superior photocatalytic activity suggest that Cu60Ti30Y10 metallic glasses are really a kind of perfect titanium source for rapidly fabricating high efficient TiO2 nano-materials. In addition, the influence of chemical composition of the amorphous precursors on preparation period of the rutile TiO2 nano-material was investigated from the point of view of standard electrode potentials.