Structure and surface morphology studies of cerium oxide system using XRD and SEM analysis

International Nuclear Information System (INIS)

Ahmad Jais Alimin; Farid Nasir Ani; Wan Azelee Wan Abu Bakar

2000-01-01

Conventional Precious Group Materials (PGM) catalyst systems have been using CeO 2 as an Oxygen Storage Capacity component in the catalyst washcoat. Due to the limitations of the PGM catalyst, researches are now focusing on improving or replacing this conventional system. In a previous work, the potential of a copper-ceria (Cu-Ce) oxide as a catalyst system has been identified. In this paper, the morphology and characterisation of Cu-Ce oxides analysed using XRD and SEM will be described. The Cu-Ce samples were prepared at a fixed ratio under temperatures of 400 o C and 800 o C. XRD diffractograms showed CeO 2 is in a cubic phase at 400 o C and 800 o C. At 800 o C, the CuO particle is visible, presumably has incorporated with the lattice structure of ceria, indicating an absent of solid state condition between copper and ceria. Analysis by SEM revealed significant increase in particle sizes with increasing calcination temperatures. (Author)

Morphologic characterization for XRD and TEM of polyamide 6 and 66 nanocomposites with bentonite regional clay

International Nuclear Information System (INIS)

Leite, Amanda M.D.; Medeiros, Vanessa da N.; Maia, Larissa F.; Araujo, Edcleide M.; Lira, Helio L.

2009-01-01

Polyamide 6 and 66 nanocomposites with clay consisting of silicates layer from Paraiba were produced. The clay was modified being used the quaternary salt of ammonium Cetremide, this so there is a better interaction of the clay with polymeric matrix. The clay without treatment (MMT) and treated clay was evaluated by XRD that showed the insertion of the salt molecules into silicates layer. The nanocomposites were obtained from polyamide 6 and 66 were verified that these presented morphological structure composed of exfoliated/partially exfoliated, analyzed by XRD and TEM. (author)

Application of SEM/EBSD and FEG-TEM/CBED to determine eutectic solidification mechanisms

International Nuclear Information System (INIS)

Nogita, K.; Dahle, A.K.; Drennan, J.

2002-01-01

Full text: This study shows the application of electron backscatter diffraction (EBSD) in SEM and convergent beam electron diffraction (CBED) in FEG-TEM to determine eutectic nucleation and growth in hypoeutectic Al-Si foundry alloys. Because the eutectic reaction is often the final stage of solidification it can be expected to have a significant impact on the formation of casting defects, particularly porosity. Previous EBSD work by Nogita and Dahle (2001), Dahle et al (2001), has shown that the eutectic nucleates on the primary phase in the unmodified alloy, and eutectic grains are nucleated in the intergranular liquid, instead of filling the dendrite envelopes, when Sr or Sb is added. However, the orientation relationship between silicon and aluminium in the eutectic has so far not been determined because of difficulties with sample preparation for EBSD and also detection limitations of Kikuchi refraction of silicon and aluminium, particularly in modified alloys with a refined eutectic. The combination of the EBSD technique in SEM and CBED in TEM analyses can provide crystallographic orientation relationships between primary aluminium dendrites, eutectic aluminium and silicon, which are important to explicitly define the solidification mode of the eutectic in hypoeutectic Al-Si alloys. These relationships are influenced, and altered, by the addition of certain elements. This paper also describes the sample preparation techniques for SEM and TEM for samples with different eutectic structures. The advantages the techniques are discussed. Copyright (2002) Australian Society for Electron Microscopy Inc

Graphene oxide and reduced graphene oxide studied by the XRD, TEM and electron spectroscopy methods

International Nuclear Information System (INIS)

Stobinski, L.; Lesiak, B.; Malolepszy, A.; Mazurkiewicz, M.; Mierzwa, B.; Zemek, J.; Jiricek, P.; Bieloshapka, I.

2014-01-01

Highlights: • Graphene oxide (FL-GOc) and reduced graphene oxide (FL-RGOc): XRD, TEM, XPS, REELS. • FL-GOc: stacking nanostructure—22 × 6 nm (DxH), 0.9 nm layers separation (XRD). • FL-RGOc: stacking nanostructure—8 × 1 nm (DxH), 0.4 nm layers separation (XRD). • Reduction: oxygen group degradation, decreasing distance between graphene layers. • Number of graphene layers in stacking nanostructure: 6–7 (FL-GOc), 2–3 (FL-RGOc). - Abstract: The commercial and synthesised few-layer graphene oxide, prepared using oxidation reactions, and few-layer reduced graphene oxide samples were structurally and chemically investigated by the X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron spectroscopy methods, i.e. X-ray photoelectron spectroscopy (XPS) and reflection electron energy loss spectroscopy (REELS). The commercial graphene oxide (FL-GOc) shows a stacking nanostructure of about 22 × 6 nm average diameter by height with the distance of 0.9 nm between 6-7 graphene layers, whereas the respective reduced graphene oxide (FL-RGOc)—about 8 × 1 nm average diameter by height stacking nanostructure with the distance of 0.4 nm between 2-3 graphene layers (XRD). The REELS results are consistent with those by the XRD indicating 8 (FL-GOc) and 4 layers (FL-RGOc). In graphene oxide and reduced graphene oxide prepared from the graphite the REELS indicates 8–11 and 7–10 layers. All graphene oxide samples show the C/O ratio of 2.1–2.3, 26.5–32.1 at% of C sp 3 bonds and high content of functional oxygen groups (hydroxyl—C-OH, epoxy—C-O-C, carbonyl—C=O, carboxyl—C-OOH, water) (XPS). Reduction increases the C/O ratio to 2.8–10.3, decreases C sp 3 content to 11.4–20.3 at% and also the content of C-O-C and C=O groups, accompanied by increasing content of C-OH and C-OOH groups. Formation of additional amount of water due to functional oxygen group reduction leads to layer delamination. Removing of functional oxygen groups

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

International Nuclear Information System (INIS)

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

2013-01-01

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. - Highlights: • XRD and FTIR crystallinity indices for tooth enamel and synthetic HAP were obtained. • SEM and TEM images were more correlated with (CI) XRD than with (CI) FTIR . • Regardless of the temperature, (CI) XRD and (CI) FTIR showed similar behavior. • XRD and FTIR crystallinity indices resulted in a fast and qualitative measurement

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

Energy Technology Data Exchange (ETDEWEB)

Reyes-Gasga, José, E-mail: jreyes@fisica.unam.mx [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Martínez-Piñeiro, Esmeralda L., E-mail: esmemapi@gmail.com [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Rodríguez-Álvarez, Galois, E-mail: galoisborre@yahoo.com [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Tiznado-Orozco, Gaby E., E-mail: gab0409@yahoo.com.mx [Unidad Académica de Odontología, Universidad Autónoma de Nayarit, Edificio E7, Ciudad de la Cultura “Amado Nervo”, C.P. 63190 Tepic, Nayarit (Mexico); García-García, Ramiro, E-mail: ramiro@fisica.unam.mx [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); and others

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){sub XRD} index is related to the crystal structure of the samples and the (CI){sub 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){sub XRD} value indicated that enamel is more crystalline than synthetic HAP, while (CI){sub FTIR} indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. - Highlights: • XRD and FTIR crystallinity indices for tooth enamel and synthetic HAP were obtained. • SEM and TEM images were more correlated with (CI){sub XRD} than with (CI){sub FTIR}. • Regardless of the temperature, (CI){sub XRD} and (CI){sub FTIR} showed similar behavior. • XRD and FTIR crystallinity indices resulted in a fast and qualitative measurement.

MICROORGANISMS FOUND IN SECONDARY CATARACT MATERIAL OF ECCE PATIENTS, A STUDY WITH SEM AND TEM

NARCIS (Netherlands)

KALICHARAN, D; JONGEBLOED, WL; LOS, LI; WORST, JGF

1993-01-01

Globular secondary cataract material, removed from 24 patients with ECCE after ophthalmic cleaning of the anterior capsule, were investigated with SEM and TEM. Besides spherical, somewhat oval shaped bodies of various shape and size comparable with those found in cataractous lenses, (an)aerobic

A novel approach to TEM preparation with a (7-axis stage) triple-beam FIB-SEM system

Science.gov (United States)

Clarke, Jamil J.

2015-10-01

Preparation of lamellae from bulk to grid for Cs-corrected Transmission Electron Microscope (TEM) observation has mostly become routine work on the latest FIB-SEM systems, with standardized techniques that often are left to automation for the initial steps. The finalization of lamellae however, has mostly become, non-routine, non-repeatable and often driven by user experience level in most cases to produce high quality damage-less cross section. Materials processing of the latest technologies, with ever-shrinking Nano-sized structures pose challenges to modern FIB-SEM systems. This can often lead to specialized techniques and hyper-specific functions for producing ultra-thin high quality lamellae that often are lab specific, preventing practical use of such techniques across multiple materials and applications. Several factors that should be incorporated in processing fine structured materials successfully include how the use of electron and ion scan conditions can affect a thin section during ion milling, the type of ion species applied for material processing during the finalization of lamellae with gallium ions or of a smaller ion species type such as Ar/Xe, sample orientation of the lamella during the thinning process which is linked to ion beam incident angle as a direct relationship in the creation of waterfall effects or curtain effects, and how software can be employed to aid in the reduction of these artifacts with reproducible results regardless of FIB-SEM experience for site-specific lift outs. A traditional TEM preparation was performed of a fine structure specimen in pursuit of a process technique to produce a high quality TEM lamella which would address all of the factors mentioned. These new capabilities have been refined and improved upon during the FIB-SEM design and development stages with an end result of a new approach that yields an improvement in quality by the reduction of common ion milling artifacts such as curtain effects, amorphous

Mössbauer, XRD and TEM Study on the Intercalation and the Release of Drugs in/from Layered Double Hydroxides

Directory of Open Access Journals (Sweden)

E. Kuzmann

2015-12-01

Full Text Available Layered double hydroxides (LDHs are one of the very important nano-carriers for drug delivery, due to their many advantageous features, such as the ease and low-cost of preparation, low cytotoxicity, good biocompatibility, protection for the intercalated drugs, and the capacity to facilitate the uptake of the loaded drug in the cells. In our previous studies, Mössbauer spectroscopy was applied to monitor structural changes occurring during the incorporation of Fe(III in MgFe- and CaFe-LDHs, and the intercalation of various organic compounds in anionic form. Recently, we have successfully elaborated a protocol for the intercalation and release of indol-2-carboxylate and L-cysteinate in CaFe-LDH. The corresponding structural changes in the LDH samples were studied by XRD, HR-TEM and 57Fe Mössbauer spectroscopy. The Mössbauer spectra reflected small but significant changes upon both the intercalation and the release of drugs. The changes in the basal distances could be followed by XRD measurements, and HR-TEM images made these changes visible.

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

Science.gov (United States)

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

2014-09-01

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

Moessbauer, TEM/SAED and XRD investigation on waste dumps of the Valea lui Stan gold mines

Energy Technology Data Exchange (ETDEWEB)

Constantinescu, Serban Grigore, E-mail: sconst@infim.ro [National Institute of Materials Physics, Bucharest-Magurele (Romania); Udubasa, Sorin S.; Udubasa, Gheorghe [University of Bucharest, Fac. of Geology and Geophysics (Romania); Kuncser, Victor; Popescu-Pogrion, Nicoleta; Mercioniu, Ionel; Feder, Marcel [National Institute of Materials Physics, Bucharest-Magurele (Romania)

2012-03-15

The complementary investigation techniques, Moessbauer spectroscopy, transmission electron microscopy with selected area electron diffraction (TEM/SAED), X-ray diffraction (XRD) have been used to investigate the fate of the Valea lui Stan, Romania, gold-ore nanoscale-minerals during the long time of residence in the waste dumps. The preliminary investigations showed such waste dumps to contain significant amount of metals which cannot be identified by conventional methods. An intense research activity started up in order to evaluate the possibilities to recycle Valea lui Stan waste dumps and to recover metals by chemical or phytoextraction procedures. The waste dumps naturally show different mineral constituents with clay minerals as major phases, observed by XRD-technique. Although the waste dumps materials have whitish-yellowish colours, MOeSSBAUER technique evidences the presence of the finely dispersed iron bearing minerals. The authors are focusing to inspect and analyze Fe-compounds in the samples collected from Valea lui Stan's waste dumps in order to identify the magnetic phases by Moessbauer technique.

Synthesis, XRD, TEM, EPR, and Optical Absorption Spectral Studies of CuZnO2 Nanocompound

Directory of Open Access Journals (Sweden)

T. Ravindra Reddy

2014-01-01

Full Text Available Synthesis of nano CuZnO2 compound is carried out by thermal decomposition method. The crystalline phase of the material is characterized by XRD. The calculated unit cell constants are a=3.1 Å and c=3.4786 Å and are of tetragonal structure. The unit cell constants are different from wurtzite (hexagonal which indicate that a nanocompound is formed. Further TEM images reveal that the metal ion is in tetragonal structure with oxygen ligands. The prepared CuZnO2 is then characterized for crystallite size analysis by employing transmission electron microscopy (TEM. The size is found to be 100 nm. Uniform bright rings are noticed in the TEM picture suggesting that the nanocrystals have preferential instead of random orientations. The selected-area electron diffraction (SAED pattern clearly indicates the formation of CuO-ZnO nanocompound. The nature of bonding is studied by electron paramagnetic resonance (EPR. The covalency character is about 0.74 and thus the compound is electrically less conductive. Optical absorption spectral studies suggest that Cu(II is placed in tetragonal elongation crystal field. The spin-orbit coupling constant, λ, is calculated using the EPR and optical absorption spectral results suggest some covalent bond between metal and ligand. Near infrared (NIR spectra are due to hydroxyl and water fundamentals.

XRD, SEM and infrared study into the intercalation of sodium hexadecyl sulfate (SHS) into hydrocalumite.

Science.gov (United States)

Zhang, Ping; Wang, Tianqi; Zhang, Longlong; Wu, Daishe; Frost, Ray L

2015-12-05

Hydrocalumite (CaAl-LDH-Cl) interacted with a natural anionic surfactant, sodium hexadecyl sulfate (SHS), was performed using an intercalation method. To understand the intercalation behavior and characterize the resulting products, powder X-ray diffraction (XRD), scan electron microscopy (SEM) and mid-infrared (MIR) spectroscopy combined with near-infrared (NIR) spectroscopy technique were used. The XRD analysis indicated that SHS was intercalated into CaAl-LDH-Cl successfully, resulting in an expansion of the interlayer (from 0.78 nm to 2.74 nm). The bands of C-H stretching vibrations of SHS were observed in the near-infrared spectra, which indicated that the resulting products were indeed CaAl-LDH-SHS. In addition, the bands of water stretching vibrations and OH groups shifted to higher wavenumbers when SHS was intercalated into CaAl-LDH-Cl interlayer space. Copyright © 2015 Elsevier B.V. All rights reserved.

A detailed TEM and SEM study of Ni-base alloys oxide scales formed in primary conditions of pressurized water reactor

International Nuclear Information System (INIS)

Sennour, Mohamed; Marchetti, Loic; Martin, Frantz; Perrin, Stephane; Molins, Regine; Pijolat, Michele

2010-01-01

The oxide film formed on nickel-based alloys in pressurized water reactors (PWR) primary coolant conditions (325 o C, aqueous media) is very thin, in the range of 1-100 nm thick, depending on the surface state and on the corrosion test duration. The nature and the structure of this scale have been investigated by Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). TEM observations revealed an oxide layer divided in two parts. The internal layer was mainly composed of a continuous spinel layer, identified as a mixed iron and nickel chromite (Ni (1-x) Fe x Cr 2 O 4 ). Moreover, nodules of Cr 2 O 3 , with a size about 5 nm, were present at the interface between this spinel and the alloy. No chromium depletion was observed in the alloy, at the alloy/oxide interface. The external layer is composed of large crystallites corresponding to a spinel structure rich in iron (Ni (1-z) Fe (2+z) O 4 ) resulting from precipitation phenomena. SEM and TEM observations showed a link between the nucleation and/or the growth of crystallites of nickel ferrite and the crystallographic orientation of the substrate. A link between the presence of surface defects and the nucleation of the crystallites was also underlined by SEM observations. Partially hydrated nickel hydroxide, was also observed by TEM in the external scale. Based on these results, some considerations about the mechanism of formation of this oxide layer are discussed.

Polycrystalline oxides formation during transient oxidation of (001) Cu-Ni binary alloys studied by in situ TEM and XRD

International Nuclear Information System (INIS)

Yang, J.C.; Li, Z.Q.; Sun, L.; Zhou, G.W.; Eastman, J.A.; Fong, D.D.; Fuoss, P.H.; Baldo, P.M.; Rehn, L.E.; Thompson, L.J.

2009-01-01

The nucleation and growth of Cu 2 O and NiO islands due to oxidation of Cu x Ni 1-x (001) films were monitored, at various temperatures, by in situ ultra-high vacuum (UHV) transmission electron microscopy (TEM) and in situ synchrotron X-ray diffraction (XRD). In remarkable contrast to our previous observations of Cu and Cu-Au oxidation, irregular-shaped polycrystalline oxide islands formed with respect to the Cu-Ni alloy film, and an unusual second oxide nucleation stage was noted. In situ XRD experiments revealed that NiO formed first epitaxially, then other orientations appeared, and finally polycrystalline Cu 2 O developed as the oxidation pressure was increased. The segregation of Ni and Cu towards or away, respectively, from the alloy surface during oxidation could disrupt the surface and cause polycrystalline oxide formation.

Characterization of ash pond ashes from 3rd thermal power plant by SEM/EDX and XRD methods

OpenAIRE

A Minjigmaa; Ts Zolzaya; E Bayanjargal; B Davaabal; J Temuujin

2014-01-01

  Coal combustion by products from ash pond of 3rdthermal power plant of Ulaanbaatar city have been collected in 2010 and 2013 years. The ash samples have been characterized by XRD, XRF and SEM-EDX methods in order to evaluate their chemical and mineralogical composition changes with disposed times. The mineralogical composition of ash varies with time though the chemical composition of the ashes were close each other. Possibly, inefficient operating condition of the TPS shows influence on th...

Characterization of mineral particles in winter fog of Beijing analyzed by TEM and SEM.

Science.gov (United States)

Li, Weijun; Shao, Longyi

2010-02-01

Aerosol samples were collected during winter fog and nonfog episodes in Beijing. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were applied to study morphologies, sizes, and compositions of aerosol particles. TEM observation indicates that most mineral particles collected in fog episode are scavenged in fog droplets. Number-size distributions of mineral particles collected in fog and nonfog episodes show two main peaks at the ranges of 0.1-0.3 and 1-2.5 microm, respectively. Based on their major compositions, mineral particles mainly include Si-rich, Ca-rich, and S-rich. Average S/Ca ratio of mineral particles collected in fog episode is 6.11, being eight times higher than that in nonfog episodes. Development mechanism of individual mineral particles in fog droplets is proposed. It is suggested that mineral particles with abundant alkaline components (e.g., "Ca-rich" particles) occurred in air should alleviate acidic degree of fog and contribute to complexity of fog droplets in Beijing.

Characterization of ceramics from the archaeological site of San Miguel Ixtapan, Mexico State, Mexico, using NAA, SEM, XRD and PIXE techniques

International Nuclear Information System (INIS)

Tenorio, D.; Monroy-Guzman, F.; Longoria, L.C.; Almazan-Torres, M.G.; Universidad Autonoma del Estado de Mexico, Toluca; Rodriguez-Garcia, N.L.

2005-01-01

Ceramic samples found in San Miguel Ixtapan, Mexico State, Mexico, were analyzed by means of NAA, PIXE, SEM and XRD. Statistical treatments such as bivariate cluster and principal-components analysis were applied to the data set. The origins of these ceramic samples were classified as local, regional and foreign. (author)

Effect of interparticle interactions on size determination of zirconia and silica based systems – A comparison of SAXS, DLS, BET, XRD and TEM

Science.gov (United States)

Pabisch, Silvia; Feichtenschlager, Bernhard; Kickelbick, Guido; Peterlik, Herwig

2012-01-01

The aim of this work is a systematic comparison of size characterisation methods for two completely different model systems of oxide nanoparticles, i.e. amorphous spherical silica and anisotropic facet-shaped crystalline zirconia. Size and/or size distribution were determined in a wide range from 5 to 70 nm using small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), nitrogen sorption (BET), X-ray diffraction (XRD) and transmission electron microscopy (TEM). A nearly perfect coincidence was observed only for SAXS and TEM for both types of particles. For zirconia nanoparticles considerable differences between different measurement methods were observed. PMID:22347721

TEM/SEM investigation of microstructural changes within the white etching area under rolling contact fatigue and 3-D crack reconstruction by focused ion beam

International Nuclear Information System (INIS)

Grabulov, A.; Ziese, U.; Zandbergen, H.W.

2007-01-01

The white etching area (WEA) surrounding the cracks formed under high-cycle rolling contact fatigue was investigated by transmission electron microscopy (TEM) and Dual Beam (scanning electron microscopy (SEM)/focused ion beam). SEM revealed the initiation of cracks formed around artificially introduced Al 2 O 3 inclusions in the model steel (composition similar to SAE 52100). TEM investigations showed a microstructural difference between the WEA (formation of nanocrystalline ferrite) and the steel matrix (tempered martensitic structure). A three-dimensional image of the crack reconstructed from ∼400 Dual Beam cross-section images is reported

Variations in fixation techniques for field emission SEM and TEM of zebrafish (Branchydanio rerio) embryo inner and outer membranes

NARCIS (Netherlands)

Kalicharan, D; Jongebloed, WL; Rawson, DM; Zhang, TT

1998-01-01

The morphology of embryos of the fresh water teleost, Brachydania rerio (zebrafish), was examined in a parallel FE-SEM/TEM study, after various pre- and post-fixation regimes. Special attention was paid to the chorion, the contents of the peri-vitelline space, the plasma membrane, the syncytial

XRD, TEM, IR, Raman and NMR Spectroscopy of In Situ Crystallization of Lithium Disilicate Glass

Science.gov (United States)

Fuss, T.; Mogus-Milankovic, A.; Ray, C. S.; Lesher, C. E.; Youngman, R.; Day, D. E.

2006-01-01

The structure of a Li2O-2SiO2 (LS2) glass was investigated as a function of pressure and temperature up to 6 GPa and 750 C respectively, using XRD, TEM, IR, Raman and NMR spectroscopy. Glass densified at 6 GPa has an average Si-O-Si bond angle approx.7deg lower than that found in glass processed at 4.5 GPa. At 4.5 GPa, lithium disilicate crystallizes from the glass, while at 6 GPa a new high pressure form of lithium metasilicate crystallizes. The new phase, while having lithium metasilicate crystal symmetry, contains at least 4 different Si sites. NMR results for 6 GPa sample indicate the presence of Q4 species with (Q(sup 4))Si-O-Si(Q(sup 4)) bond angles of approx.157deg. This is the first reported occurrence of Q(sup 4) species with such large bond angles in alumina free alkali silicate glass. No five- or six- coordinated Si are found.

XRD and SEM study on the phase separation and crystallization behavior for an amorphous Cu+ conductor

International Nuclear Information System (INIS)

Yang Yuan; Hou Jianguo; Yu Wenhai

1990-01-01

The X-ray diffraction (XRD) and scanning electron microscopy (SEM) study was carried out for an amorphous Cu + conductor 0.4 CuI-0.3 Cu 2 O-0.3 P 2 O 5 with the simultaneous conductivity measurement in the isothermal heat treament process. The results indicated that the initial amorphous material was phase-separated. In the course of time the separated amorphous phase disappeared, the crystalline γ-CuI and Cu 2 P 2 O 7 formed in sequence and grew up gradually. The correlation of the phase separation and crystallization behavior with the conductivity anomaly confirmed again the interface effect between different phases in amorphous fast ionic conductors and its universality

Characterization of ash pond ashes from 3rd thermal power plant by SEM/EDX and XRD methods

Directory of Open Access Journals (Sweden)

A Minjigmaa

2014-10-01

Full Text Available   Coal combustion by products from ash pond of 3rdthermal power plant of Ulaanbaatar city have been collected in 2010 and 2013 years. The ash samples have been characterized by XRD, XRF and SEM-EDX methods in order to evaluate their chemical and mineralogical composition changes with disposed times. The mineralogical composition of ash varies with time though the chemical composition of the ashes were close each other. Possibly, inefficient operating condition of the TPS shows influence on the mineralogical composition.DOI: http://dx.doi.org/10.5564/mjc.v14i0.201Mongolian Journal of Chemistry 14 (40, 2013, p61-65

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

Energy Technology Data Exchange (ETDEWEB)

Gao, Jie [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); School of Physical Sciences, University of Chinese Academy of Sciences, Beijing 100049 (China); Bao, Liangman [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Huang, Hefei, E-mail: huanghefei@sinap.ac.cn [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Li, Yan, E-mail: liyan@sinap.ac.cn [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Lei, Qiantao [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Institute of Modern Physics, Fudan University, Shanghai 200433 (China); Deng, Qi [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Liu, Zhe; Yang, Guo [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); School of Physical Sciences, University of Chinese Academy of Sciences, Beijing 100049 (China); Shi, Liqun [Institute of Modern Physics, Fudan University, Shanghai 200433 (China)

2017-05-15

Hastelloy N alloy was implanted with 30 keV, 5 × 10{sup 16} ions/cm{sup 2} 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.

Characterization of wet precipitation by X-ray diffraction (XRD) and scanning electron microscopy (SEM) in the metropolitan area of Porto Alegre, Brazil

Energy Technology Data Exchange (ETDEWEB)

Montanari Migliavacca, Daniela [Instituto de Biociencias, Programa de Pos-Graduacao em Ecologia, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91509-900 Porto Alegre, RS (Brazil); Fundacao Estadual de Protecao Ambiental Henrique Luis Roessler, RS. Rua Carlos Chagas 55/802, 90030-020 Porto Alegre, RS (Brazil); Calesso Teixeira, Elba, E-mail: gerpro.pesquisa@fepam.rs.gov.br [Fundacao Estadual de Protecao Ambiental Henrique Luis Roessler, RS. Rua Carlos Chagas 55/802, 90030-020 Porto Alegre, RS (Brazil); Gervasoni, Fernanda; Vieira Conceicao, Rommulo [Instituto de Geociencias, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91509-900 Porto Alegre, RS (Brazil); Raya Rodriguez, Maria Teresa [Instituto de Biociencias, Programa de Pos-Graduacao em Ecologia, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91509-900 Porto Alegre, RS (Brazil)

2009-11-15

The purpose of this study is to assess the composition of wet precipitation in three sites of the metropolitan area of Porto Alegre. Besides the variables usually considered, such as pH, conductivity, major ions (Cl{sup -}, NO{sub 3}{sup -}, F{sup -}, SO{sub 4}{sup 2-}, Na{sup +}, K{sup +}, Mg{sup 2+}, NH{sub 4}{sup +} and Ca{sup 2+}) and metallic elements (Cd, Co, Cr, Cu, Fe, Mn and Ni), the suspended matter was examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM), with energy dispersive system (EDS), for better identification of possible anthropogenic material in this wet precipitation. Results showed an alkaline pH in the samples analyzed and higher concentrations for Na{sup +}, Cl{sup -} and SO{sub 4}{sup 2-}. The acidification and neutralization potential between anions (SO{sub 4}{sup 2-} + NO{sub 3}{sup -}) and cations (Ca{sup 2+} + Mg{sup 2+} + K{sup +} + NH{sub 4}{sup +}) showed a good correlation (0.922). The metallic elements with highest values were Zn, Fe and Mn. Results of XRD identified the presence of some minerals such as quartz, feldspar, mica, clay, carbonates and sulfates. In samples analyzed with SEM, we detected pyroxene, biotite, amphibole and oxides. Cluster analysis (CA) was applied to the data matrix to identify potential pollution sources of metals (natural or anthropogenic) and the association with minerals found in the analysis of SEM.

Extensive FE-SEM/EDS, HR-TEM/EDS and ToF-SIMS studies of micron- to nano-particles in anthracite fly ash

Energy Technology Data Exchange (ETDEWEB)

Ribeiro, Joana [Centro de Geologia, Universidade do Porto, Rua do Campo Alegre, 687, 4169-007 Porto (Portugal); DaBoit, Kátia [Institute of Environmental Research and Human Development, IPADHC, Capivari de Baixo, Santa Catarina (Brazil); Flores, Deolinda [Centro de Geologia, Universidade do Porto, Rua do Campo Alegre, 687, 4169-007 Porto (Portugal); Departamento de Geociências, Ambiente e Ordenamento do Território, Faculdade de Ciências, Universidade do Porto, Rua do Campo Alegre, 687, 4169-007 Porto (Portugal); Kronbauer, Marcio A. [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Victor Barreto, 2288 Centro 92010-000, Canoas, RS (Brazil); Silva, Luis F.O., E-mail: felipeqma@hotmail.com [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Victor Barreto, 2288 Centro 92010-000, Canoas, RS (Brazil); Environmental Science and Nanotechnology Department, Catarinense Institute of Environmental Research and Human Development, IPADHC, Capivari de Baixo, Santa Catarina (Brazil)

2013-05-01

The generation of anthropogenic carbonaceous matter and mixed crystalline/amorphous mineral ultrafine/nano-particles in the 1 to 100 nm size range by worldwide coal power plants represents serious environmental problems due to their potential hazards. Coal fly ash (CFA) that resulted from anthracite combustion in a Portuguese thermal power plant was studied in this work. The physico-chemical characterization of ultrafine/nano-particles present in the CFA samples and their interaction with environment are the aim of this study. The methodologies applied for this work were field emission scanning electron microscopy (FE-SEM) with energy dispersive X-ray spectroscopy (EDS), high-resolution transmission electron microscopy with energy dispersive X-ray spectroscopy (HR-TEM/EDS) and time of flight secondary ion mass spectrometry (ToF-SIMS). Some hazardous volatile elements, C, N, S and Hg contents were also determined in the studied samples. Generally, the CFA samples comprise carbonaceous, glassy and metallic solid spheres with some containing mixed amorphous/crystalline phases. The EDS analysis coupled with the FE-SEM and HR-TEM observations of the fly ash particles with 100 to 0.1 nm demonstrates that these materials contain a small but significant proportion of encapsulated HVEs. In addition, the presence of abundant multi-walled carbon nanotubes (MWCNTs) and amorphous carbon particles, both containing hazardous volatile elements (HVEs), was also evidenced by the FE-SEM/EDS and HR-TEM/EDS analysis. A wide range of organic and inorganic compounds was determined by chemical maps obtained in ToF-SIMS analysis. - Highlights: ► We examine changes in the level of ultrafine and nanoparticles of coal mining. ► Increasing geochemical information will increase human health information in this area. ► Electron bean and Tof-SIMS increase area information.

In situ TEM/SEM electronic/mechanical characterization of nano material with MEMS chip

International Nuclear Information System (INIS)

Wang Yuelin; Li Tie; Zhang Xiao; Zeng Hongjiang; Jin Qinhua

2014-01-01

Our investigation of in situ observations on electronic and mechanical properties of nano materials using a scanning electron microscope (SEM) and a transmission electron microscope (TEM) with the help of traditional micro-electro-mechanical system (MEMS) technology has been reviewed. Thanks to the stability, continuity and controllability of the loading force from the electrostatic actuator and the sensitivity of the sensor beam, a MEMS tensile testing chip for accurate tensile testing in the nano scale is obtained. Based on the MEMS chips, the scale effect of Young's modulus in silicon has been studied and confirmed directly in a tensile experiment using a transmission electron microscope. Employing the nanomanipulation technology and FIB technology, Cu and SiC nanowires have been integrated into the tensile testing device and their mechanical, electronic properties under different stress have been achieved, simultaneously. All these will aid in better understanding the nano effects and contribute to the designation and application in nano devices. (invited papers)

Infrared spectra, Raman laser, XRD, DSC/TGA and SEM ...

Indian Academy of Sciences (India)

Administrator

cussed and the X-ray diffraction, scanning electron microscopy (SEM) and atomic force microscope (AFM) ... acetamide as a simple organic compound at high tempera- ture has less ..... properties of selenium surface, AFM-microscopy tapping.

Site specific SEM/FIB/TEM for analysis of lubricated sliding wear of aluminium alloy composites

International Nuclear Information System (INIS)

Walker, J C; Jones, H; Rainforth, W M

2006-01-01

Although extensive research has been undertaken into the dry sliding wear of aluminium alloys, only limited work has been reported on lubricated wear. In this paper, the lubricated sliding wear of some powder derived aluminium alloy composites is reported. Stereo pairs of the worn surface were obtained in the SEM and digitally reconstructed to give an accurate projection of the surface topography. Analysis of the average surface roughness (R a ) along chosen sections provided quantitative information about the wear mechanism. Following this, dual beam focused ion beam (FIB) was undertaken to further explore the features revealed by the SEM surface reconstructions, with TEM sections removed from selected regions. Surface deformation was confined to a narrow layer, typically 1μm thick. Subgrain size within the subsurface layer was comparable to that found in dry sliding wear tests. Reinforcement fracture occurred in the surface particles only. The resultant fragments were often incorporated back into the surface following detachment, such that the total volume fraction reinforcement at the surface was greater than in the bulk. Thus, the dynamic surface topography was a result of three factors: surface deformation, local detachment of reinforcement and re-incorporation of the fragments back into the surface

The luminal surface of thyroid cysts in SEM

DEFF Research Database (Denmark)

Zelander, T; Kirkeby, S

1978-01-01

Four of the five kinds of cells constituting the walls of thyroid cysts can be identified in the SEM. These are cuboidal cells, mucous cells, cells with large granules and ciliated cells. A correlation between SEM and TEM observations is attempted.......Four of the five kinds of cells constituting the walls of thyroid cysts can be identified in the SEM. These are cuboidal cells, mucous cells, cells with large granules and ciliated cells. A correlation between SEM and TEM observations is attempted....

Is the TEM obsolescent?

International Nuclear Information System (INIS)

Williams, D.B.

2002-01-01

Full text: The TEM has undergone many revolutions since its invention 70 years ago, but is now a very mature instrument. The major functions of imaging, diffraction and analysis were invented decades ago. Much of the instrument development in the last 20 years has come in peripheral improvements such as ease of operation and computer control which, nevertheless, have made no substantial differences to basic operational methods. The TEM remains a predominantly manual instrument, still providing analog viewing and recording, well into the digital age. Indeed any operator of a Siemens Elmiskop 1 TEM from the 1950s would be more than skilled enough to operate a modern FEG TEM, with little more than a few minutes of training. It is arguable that no other cutting-edge scientific instrument is so basically unchanged in its method of operation over the last five decades, as the TEM. This state of affairs is a recipe for obsolescence. Students today are not interested in mastering the complexities of balancing potentiometers (which are still necessary for good centered dark-field operation) or manipulating sets of tilt controls to move from to , while fighting to maintain eucentricity and a recognizable image on the screen at 200 kX. Students are already masters of the mouse, keyboard or joystick and expect information to be generated, stored, processed and analyzed rapidly and efficiently under full computer control. We need to provide today's students with an instrument to challenge their skills, not those of their parents. There is nothing preventing the creation of a TEM that is under full computer control, except perhaps the notion that the TEM is an instrument worthy of mastery per se, rather than being simply a tool for the characterization of materials. In contrast, the SEM has never been seen as a 'real' electron microscope and consequently has found its way into many more research, education and commercial operations than the TEM. The SEM has also evolved

Chemical and structural analysis of the bone-implant interface by TOF-SIMS, SEM, FIB and TEM: Experimental study in animal

International Nuclear Information System (INIS)

Palmquist, Anders; Emanuelsson, Lena; Sjövall, Peter

2012-01-01

Although bone-anchored implants are widely used in reconstructive medicine, the mechanism of osseointegration is still not fully understood. Novel analytical tools are needed to further understand this process, where both the chemical and structural aspects of the bone-implant interface are important. The aim of this study was to evaluate the advantages of combining time-of-flight secondary ion mass spectroscopy (TOF-SIMS) with optical (LM), scanning (SEM) and transmission electron microscopy (TEM) techniques for studying the bone-implant interface of bone-anchored implants. Laser-modified titanium implants with surrounded bone retrieved after 8 weeks healing in rabbit were dehydrated and resin embedded. Three types of sample preparation were studied to evaluate the information gained by combining TOF-SIMS, SEM, FIB and TEM. The results show that imaging TOF-SIMS can provide detailed chemical information, which in combination with structural information from microscopy methods provide a more complete characterization of anatomical structures at the bone-implant interface. By investigating various sample preparation techniques, it is shown that grinded cross section samples can be used for chemical imaging using TOF-SIMS, if careful consideration of potential preparation artifacts is taken into account. TOF-SIMS analysis of FIB-prepared bone/implant cross section samples show distinct areas corresponding to bone tissue and implant with a sharp interface, although without chemical information about the organic components.

Investigation of the agglomeration and amorphous transformation effects of neutron irradiation on the nanocrystalline silicon carbide (3C-SiC) using TEM and SEM methods

Energy Technology Data Exchange (ETDEWEB)

Huseynov, Elchin M., E-mail: elchin.h@yahoo.com [Department of Nanotechnology and Radiation Material Science, National Nuclear Research Center, Inshaatchilar pr. 4, AZ 1073 Baku (Azerbaijan); Institute of Radiation Problems of Azerbaijan National Academy of Sciences, B.Vahabzade 9, AZ 1143 Baku (Azerbaijan)

2017-04-01

Nanocrystalline 3C-SiC particles irradiated by neutron flux during 20 h in TRIGA Mark II light water pool type research reactor. Silicon carbide nanoparticles were analyzed by Scanning Electron Microscope (SEM) and Transmission Electron Microscopy (TEM) devices before and after neutron irradiation. The agglomeration of nanoparticles was studied comparatively before and after neutron irradiation. After neutron irradiation the amorphous layer surrounding the nanoparticles was analyzed in TEM device. Neutron irradiation defects in the 3C-SiC nanoparticles and other effects investigated by TEM device. The effect of irradiation on the crystal structure of the nanomaterial was studied by selected area electron diffraction (SAED) and electron diffraction patterns (EDP) analysis.

Phosphorus Sorption Characteristics in Aluminum-based Water Treatment Residuals Reacted with Dairy Wastewater: 1. Isotherms, XRD, and SEM-EDS Analysis.

Science.gov (United States)

Zohar, Iris; Massey, Michael S; Ippolito, James A; Litaor, M Iggy

2018-05-01

We examined P sorption characteristics in Al-based water treatment residuals (Al-WTR) generated from slightly alkaline surface water and in an organic residual composite (WW-Al/O-WTR), produced by using the Al-WTR to treat organic-rich and high P concentration dairy wastewater. Solids from both residuals were examined using scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and X-ray diffraction (XRD), and exposed to P additions of 0 to 4000 mg L in a sorption experiment. The Al-WTR removed ∼97% of the added P, whereas WW-Al/O-WTR removed only 78% of the added P in the addition range of 0 to 100 mg P L. With P additions of ≥100 mg L, the removal rate declined to XRD indicated that the major mineral was calcite, with some silica and poorly crystalline Al hydroxides. Analysis by SEM-EDS, which used three-element overlay maps of the residual surfaces, indicated that P was sparsely sorbed on both calcic and Al (hydr)oxide surfaces, along with a few clusters, even at low P concentrations of the treated waters. Ternary clusters of P, Al, and Ca were more abundant on the WW-Al/O-WTR. Carbon distribution suggested that organic substances covered Al surfaces. Sorption of P onto WW-Al/O-WTR may be reversible due to relatively weak Ca-P and Al-P bonds induced by the slight alkaline nature and in the presence of organic moieties, enhancing the WW-Al/O-WTR potential to act as a P source, rather than a P sink, in agricultural applications. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

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

Science.gov (United States)

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.

Investigation of structural resorption behavior of biphasic bioceramics with help of gravimetry, μCT, SEM, and XRD.

Science.gov (United States)

de Wild, Michael; Amacher, Fabienne; Bradbury, Christopher R; Molenberg, Aart

2016-04-01

Resorbable bone substitute materials are widely used for bone augmentation after tumor resection, parallel to implant placement, or in critical size bone defects. In this study, the structural dissolution of a biphasic calcium phosphate bone substitute material with a hydroxyapatite (HA)/tricalcium phosphate (β-TCP) ratio of 60/40 was investigated by repeatedly placing porous blocks in EDTA solution at 37 °C. At several time points, the blocks were investigated by SEM, µCT, and gravimetry. It was found that always complete 2-3 µm sized grains were removed from the structure and that the β-TCP is dissolved more rapidly. This selective dissolution of the β-TCP grains was confirmed by XRD measurements. The blocks were eroded from the outside toward the center. The structure remained mechanically stable because the central part showed a delayed degradation and because the slower dissolving HA grains preserved the integrity of the structure. © 2015 Wiley Periodicals, Inc.

Identification of the silver state in the framework of Ag-containing zeolite by XRD, FTIR, photoluminescence, 109Ag NMR, EPR, DR UV-vis, TEM and XPS investigations.

Science.gov (United States)

Popovych, Nataliia; Kyriienko, Pavlo; Soloviev, Sergiy; Baran, Rafal; Millot, Yannick; Dzwigaj, Stanislaw

2016-10-26

Silver has been identified in the framework of Ag x SiBEA zeolites (where x = 3-6 Ag wt%) by the combined use of XRD, 109 Ag MAS NMR, FTIR, diffuse reflectance UV-visible, EPR and XPS spectroscopy. The incorporation of Ag ions into the framework of SiBEA zeolite has been evidenced by XRD. The consumption of OH groups as a result of their reaction with the silver precursor has been monitored by FTIR and photoluminescence spectroscopy. The changes in the silver state as a function of Ag content and thermal and hydrogen treatment at 573 K have been identified by 109 Ag MAS NMR, EPR, DR UV-visible, TEM and XPS investigations. The acidity of AgSiBEA has been investigated by FTIR spectroscopy of adsorbed CO and pyridine used as probe molecules.

FE-SEM, FIB and TEM Study of Surface Deposits of Apollo 15 Green Glass Volcanic Spherules

Science.gov (United States)

Ross, Daniel K.; Thomas-Keprta, K. L.; Rahman, Z.; Wentworth, S. J.; McKay, D. S.

2011-01-01

Surface deposits on lunar pyroclastic green (Apollo 15) and orange (Apollo 17) glass spherules have been attributed to condensation from the gas clouds that accompanied fire-fountain eruptions. The fire fountains cast molten lava high above the lunar surface and the silicate melt droplets quenched before landing producing the glass beads. Early investigations showed that these deposits are rich in sulfur and zinc. The deposits are extremely fine-grained and thin, so that it was never possible to determine their chemical compositions cleanly by SEM/EDX or electron probe x-ray analysis because most of the excited volume was in the under-lying silicate glass. We are investigating the surface deposits by TEM, using focused ion beam (FIB) microscopy to extract and thin the surface deposits. Here we report on chemical mapping of a FIB section of surface deposits of an Apollo green glass bead 15401using the ultra-high resolution JEOL 2500 STEM located at NASA Johnson Space Center.

Shocked quartz in the SEM: Distinction between amorphous and healed PDFs

NARCIS (Netherlands)

Hamers, M.F.; Pennock, G.M.; Drury, M.R.

2012-01-01

Combined SEM techniques show that different CL signatures of PDFs are related to fresh and healed microstructures of PDFs and host quartz. This is confirmed by TEM results. A combination of SEM techniques can give the same type of information as TEM

Vacancy ordered γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanohydroxyapatite: XRD, FTIR, TEM, XPS and Mössbauer studies

Energy Technology Data Exchange (ETDEWEB)

Ramos Guivar, Juan A., E-mail: juan.ramos5@unmsm.edu.pe [Faculty of Physical Sciences, National University of San Marcos, P. O. Box 14- 0149, Lima 14 (Peru); Sanches, Edgar A., E-mail: sanches.ufam@gmail.com [Federal University of Amazonas, Department of Physics, Manaus/AM (Brazil); Bruns, Florian, E-mail: f.bruns@tu-braunschweig.de [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Sadrollahi, Elaheh, E-mail: elahe.sadrollahi@gmail.com [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Morales, M.A., E-mail: marco.moralestorres@gmail.com [Department of Theoretical and Experimental Physics, UFRN, Natal, RN 59078- 970 (Brazil); López, Elvis O., E-mail: lopmezel@gmail.com [Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil); Litterst, F. Jochen, E-mail: litterst@cbpf.br [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil)

2016-12-15

Graphical abstract: Possible bonding configuration in the γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanoHAp. - Highlights: • Coprecipitation in alkaline medium for the synthesis of vacancy ordered γ-Fe{sub 2}O{sub 3}@HAp nanocomposite. • Samples were characterized by XRD, FTIR, XPS, TEM, VSM and Mössbauer spectroscopy. • The functionalization is explained with the binding of two oxygens of chemisorbed H{sub 2}O molecules at the common interface of HAp/C{sub 6}H{sub 8}O{sub 7}/γ-Fe{sub 2}O{sub 3}. - Abstract: Vacancy ordered maghemite (γ-Fe{sub 2}O{sub 3}) nanoparticles functionalized with nanohydroxyapatite (HAp – Ca{sub 10}(PO{sub 4}) {sub 6}(OH){sub 2}) have been successfully synthesized using an inexpensive co-precipitation chemical route. Evidence for the presence of vacancy order in maghemite was shown by the superstructure lines observed in X-ray diffraction. The adsorption of carboxyl groups of citric acid (C{sub 6}H{sub 8}O{sub 7}) onto γ-Fe{sub 2}O{sub 3} nanoparticles was investigated by FTIR, XPS and Mössbauer spectroscopy. From XPS surface analysis, two binding energies related to oxygen were attributed to bindings between C{sub 6}H{sub 8}O{sub 7}/γ- Fe{sub 2}O{sub 3} and C{sub 6}H{sub 8}O{sub 7}/HAp from an interfacial reaction promoted by strongly adsorbed H{sub 2}O molecules at the surface of these nanomaterials. Le Bail refinement of the XRD patterns showed the formation of well-crystallized pure tetragonal maghemite before and after functionalization with nanoHAp. The temperature dependence of hyperfine parameters of pure and functionalized γ-Fe{sub 2}O{sub 3} nanoparticles was investigated via Mössbauer spectroscopy. TEM revealed the formation of quasi-spherical γ- Fe{sub 2}O{sub 3} nanoparticles with an average diameter of ca. 12 nm and 16 nm before and after functionalization with nanoHAp in agreement with Le Bail refinement. Magnetometry measurements showed a saturation magnetization of 12 emu/g and a blocking

In situ oxidation of zirconium binary alloys by environmental SEM and analysis by AFM, FIB, and TEM

International Nuclear Information System (INIS)

Proff, C.; Abolhassani, S.; Dadras, M.M.; Lemaignan, C.

2010-01-01

Binary Zr-alloys containing 1%Fe and 1% Ni (large precipitates) and 1% Cr and 0.6% Nb (small precipitates), as well as a pure Zr sample were exposed in situ at 130 Pa water vapour pressure at 415 o C in an environmental SEM. The surface topography and composition of each sample was characterised before in situ experiments, during and after oxidation. After oxidation the surface was characterised by SEM and EDS, AFM and TEM combined with EDS. Focused ion beam was used to prepare cross sections of the metal-oxide interface and for the preparation of TEM thin foils. The oxidation behaviour of precipitates for these alloying elements can be characterised into two large families, those which show a rapid oxidation and those which induce a delayed oxidation in comparison with the Zr-matrix. At 415 o C after 1 h of oxidation for Zr1%Fe and Zr1%Ni, the formation of protrusions could be detected at the surface, being related to underlying SPP in the oxide. On Zr1%Cr and Zr0.6%Nb unoxidised SPPs were observed in the oxide, close to the metal-oxide interface. These SPPs were, however, oxidised close to the outer surface of the oxide. The surface roughness was increased for all materials after in situ oxidation, however, only for Zr1%Fe and Zr1%Ni protrusions appeared on the surface during oxidation. It was subsequently demonstrated that these latter correspond to the position of SPPs. For Zr1%Fe the surface roughness increased more than in the other materials and on these protrusions small iron oxide crystals have been observed at the surface. These observations confirm that Fe has a different behaviour compared to the other SPP forming elements, and it diffuses out to the free surface of the material. These alloying elements being the constituents of the commercial alloys (Fe and Cr for Zircaloy-4; Fe, Cr and Ni for Zircaloy-2 and Nb for all Nb-containing alloys), this study allows to separate their individual influence and can allow a subsequent comparison to the behaviour

TEM and SEM observation of uranium induced renal necrosis and the result of chelates treatment on rats

International Nuclear Information System (INIS)

Sun Shiquan; Li Baoxing; Lai Chixiang; You Zhanyun

1987-01-01

The TEM (transmission electron microscope) and SEM (scanning electron microscope) observation of uranium induced renal necrosis and the result of chelates treatment on rats are reported. Ultrastructural changes in kidney related with the impairment of intracellular fluid transportation can be found after acute uranium intoxication in rats, such as: condensation and swelling of mitochondria, matrix edema, dilatation of intercellular space, disappearance of basal folds, thickening of basal web, intensification of basal lamina of the proximal convoluted tubule epithelium cells, and foot processes swelling, diminishing of endothelium fenestrae of the renal glomerulus. Heavy metal chelates DTPA and H-73-10 treatment may result in intracellular fluid accumulation and condensed grannule formation in lysosome. Treatment with these chelates in the critical stage of uranium intoxication may accelerate the necrosis instead of diminishing. This may be related to the augment of the load of lysosome and intracellular system of fluid transportation

SEM, TEM, and IHC Analysis of the Sinus Node and Its Implications for the Cardiac Conduction System

Directory of Open Access Journals (Sweden)

D. Mandrioli

2013-01-01

Full Text Available More than 100 years after the discovery of the sinus node (SN by Keith and Flack, the function and structure of the SN have not been completely established yet. The anatomic architecture of the SN has often been described as devoid of an organized structure; the origin of the sinus impulse is still a matter of debate, and a definite description of the long postulated internodal specialized tract conducting the impulse from the SN to the atrioventricular node (AVN is still missing. In our previously published study, we proposed a morphologically ordered structure for the SN. As a confirmation of what was presented then, we have added the results of additional observations regarding the structural particularities of the SN. We investigated the morphology of the sinus node in the human hearts of healthy individuals using histochemical, immunohistochemical, optical, and electron microscopy (SEM, TEM. Our results confirmed that the SN presents a previously unseen highly organized architecture.

Bone matrix calcification during embryonic and postembryonic rat calvarial development assessed by SEM-EDX spectroscopy, XRD, and FTIR spectroscopy.

Science.gov (United States)

Henmi, Akiko; Okata, Hiroshi; Anada, Takahisa; Yoshinari, Mariko; Mikami, Yasuto; Suzuki, Osamu; Sasano, Yasuyuki

2016-01-01

Bone mineral is constituted of biological hydroxyapatite crystals. In developing bone, the mineral crystal matures and the Ca/P ratio increases. However, how an increase in the Ca/P ratio is involved in maturation of the crystal is not known. The relationships among organic components and mineral changes are also unclear. The study was designed to investigate the process of calcification during rat calvarial bone development. Calcification was evaluated by analyzing the atomic distribution and concentration of Ca, P, and C with scanning electron microscopy (SEM)-energy-dispersive X-ray (EDX) spectroscopy and changes in the crystal structure with X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Histological analysis showed that rat calvarial bone formation started around embryonic day 16. The areas of Ca and P expanded, matching the region of the developing bone matrix, whereas the area of C became localized around bone. X-ray diffraction and FTIR analysis showed that the amorphous-like structure of the minerals at embryonic day 16 gradually transformed into poorly crystalline hydroxyapatite, whereas the proportion of mineral to protein increased until postnatal week 6. FTIR analysis also showed that crystallization of hydroxyapatite started around embryonic day 20, by which time SEM-EDX spectroscopy showed that the Ca/P ratio had increased and the C/Ca and C/P ratios had decreased significantly. The study suggests that the Ca/P molar ratio increases and the proportion of organic components such as proteins of the bone matrix decreases during the early stage of calcification, whereas crystal maturation continues throughout embryonic and postembryonic bone development.

SEM and TEM Characterization of As-Fabricated U-7Mo Disperson Fuel Plates

International Nuclear Information System (INIS)

Keiser, D.D. Jr.; Yao, B.; Perez, E.; Sohn, Y.H.

2009-01-01

The starting microstructure of a dispersion fuel plate can have a dramatic impact on the overall performance of the plate during irradiation. To improve the understanding of the as-fabricated microstructures of dispersion fuel plates, SEM and TEM analysis have been performed on RERTR-9A archive fuel plates, which went through an additional hot isostatic procsssing (HIP) step during fabrication. The fuel plates had depleted U-7Mo fuel particles dispersed in either Al-2Si or 4043 Al alloy matrix. For the characterized samples, it was observed that a large fraction of the ?-phase U-7Mo alloy particles had decomposed during fabrication, and in areas near the fuel/matrix interface where the transformation products were present significant fuel/matrix interaction had occurred. Relatively thin Si-rich interaction layers were also observed around the U-7Mo particles. In the thick interaction layers, (U)(Al,Si)3 and U6Mo4Al43 were identified, and in the thin interaction layers U(Al,Si)3, U3Si3Al2, U3Si5, and USi1.88-type phases were observed. The U3Si3Al2 phase contained some Mo. Based on the results of this work, exposure of dispersion fuel plates to relatively high temperatures during fabrication impacts the overall microstructure, particularly the nature of the interaction layers around the fuel particles. The time and temperature of fabrication should be carefully controlled in order to produce the most uniform Si-rich layers around the U-7Mo particles.

SEM and TEM characterization of microstructure of stainless steel composites reinforced with TiB2

International Nuclear Information System (INIS)

Sulima, Iwona; Boczkal, Sonia; Jaworska, Lucyna

2016-01-01

Steel-8TiB 2 composites were produced by two new sintering techniques, i.e. Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT) sintering. This study discusses the impact of these sintering methods on the microstructure of steel composites reinforced with TiB 2 particles. Scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), X-ray diffraction, electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used to analyze the microstructure evolution in steel matrix composites. The results of microscopic examinations revealed a close relationship between the composite microstructure and the methods and conditions of sintering. Substantial differences were observed in the grain size of materials sintered by HP-HT and SPS. It has been demonstrated that the composites sintered by HP-HT tend to form a chromium-iron-nickel phase in the steel matrix. In contrast, the microstructure of the composites sintered by SPS is characterized by the presence of complex borides and chromium-iron phase. - Highlights: •The steel-8TiB 2 composites were fabricated by Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT). •Sintering techniques has an important effect on changes in the microstructure of steel-8TiB 2 composites. •New phases of different size and morphology were identified.

stainless steel by SEM-XRD and image analysis

Directory of Open Access Journals (Sweden)

Robinson Constanzo-R.

2014-01-01

Full Text Available El objetivo de este trabajo fue realizar un análisis cualitativ o de la distribución de un electrodepósito de cobre en el inter ior de electrodos porosos (EP de acero inoxidable y carbono grafito. Para ello, se reali zaron pruebas de electrodepositación de cobre a nivel de labora torio, con un posterior análisis de cortes de muestras de acero y grafito vía Microscopía Estereoscópica, Microscopía SEM-DRX y Análisis de Imagen, los cuales mostraron que el cobre no se deposita en forma uniforme al interior del electrodo. En el electrodo de acero, la penetra ción del depósito en el espesor fue alrededor de 50%, mientras que para el grafito a lrededor de 90%. En forma general, se observó un aumento de la cantidad de depósito hacia el extremo frente al ánodo y con sitios de difer ente crecimiento en depósito de cobre. Esto demuestra una distr ibución de corriente y potencial, función de parámetros físicos de electrodo y de la s características fisicoquímicas e hidrodinámicos del electroli to.

Swelling induced by alpha decay in monazite and zirconolite ceramics: A XRD and TEM comparative study

Science.gov (United States)

Deschanels, X.; Seydoux-Guillaume, A. M.; Magnin, V.; Mesbah, A.; Tribet, M.; Moloney, M. P.; Serruys, Y.; Peuget, S.

2014-05-01

Zirconolite and monazite matrices are potential ceramics for the containment of actinides (Np, Cm, Am, Pu) which are produced over the reprocessing of spent nuclear fuel. Actinides decay mainly through the emission of alpha particles, which in turn causes most ceramics to undergo structural and textural changes (amorphization and/or swelling). In order to study the effects of alpha decays on the above mentioned ceramics two parallel approaches were set up. The first involved the use of an external irradiation source, Au, which allowed the deposited recoil energy to be simulated. The second was based on short-lived actinide doping with 238Pu, (i.e. an internal source), via the incorporation of plutonium oxide into both the monazite and zirconolite structures during synthesis. In both types of irradiation experiments, the zirconolite samples became amorphous at room temperature with damage close to 0.3 dpa; corresponding to a critical dose of 4 × 1018 α g-1 (i.e. ∼1.3 × 1021 keV cm-3). Both zirconolite samples also showed the same degree of macroscopic swelling at saturation (∼6%), with ballistic processes being the predominant damaging effect. In the case of the monazite however, the macroscopic swelling and amorphization were dependent on the nature of the irradiation. Externally, (Au), irradiated samples became amorphous while also demonstrating a saturation swelling of up to 8%. In contrast to this, the swelling of the 238Pu doped samples was much smaller at ∼1%. Also, unlike the externally (Au) irradiated monazite these 238Pu doped samples remained crystalline up to 7.5 × 1018 α g-1 (0.8 dpa). XRD, TEM and swelling measurements were used to fully characterize and interpret this behavior. The low swelling and the conservation of the crystalline state of 238Pu doped monazite samples indicates that alpha annealing took place within this material.

Quantitative XRD analysis of {110} twin density in biotic aragonites.

Science.gov (United States)

Suzuki, Michio; Kim, Hyejin; Mukai, Hiroki; Nagasawa, Hiromichi; Kogure, Toshihiro

2012-12-01

{110} Twin densities in biotic aragonite have been estimated quantitatively from the peak widths of specific reflections in powder X-ray diffraction (XRD) patterns, as well as direct confirmation of the twins using transmission electron microscopy (TEM). Influence of the twin density on the peak widths in the XRD pattern was simulated using DIFFaX program, regarding (110) twin as interstratification of two types of aragonite unit layers with mirrored relationship. The simulation suggested that the twin density can be estimated from the difference of the peak widths between 111 and 021, or between 221 and 211 reflections. Biotic aragonite in the crossed-lamellar microstructure (three species) and nacreous microstructure (four species) of molluscan shells, fish otoliths (two species), and a coral were investigated. The XRD analyses indicated that aragonite crystals in the crossed-lamellar microstructure of the three species contain high density of the twins, which is consistent with the TEM examination. On the other hand, aragonite in the nacre of the four species showed almost no difference of the peak widths between the paired reflections, indicating low twin densities. The results for the fish otoliths were varied between the species. Such variation of the twin density in biotic aragonites may reflect different schemes of crystal growth in biomineralization. Copyright © 2012 Elsevier Inc. All rights reserved.

Nickel oxide reduction studied by environmental TEM and in situ XRD

DEFF Research Database (Denmark)

Jeangros, Q.; Hansen, Thomas Willum; Wagner, Jakob Birkedal

2012-01-01

Paar furnace and a mass spectrometer to complement and extrapolate the ETEM data to higher pressures and gas flows. Diffraction peak intensities, crystallite sizes (obtained using the Scherrer formula) and H2/H2O mass spectrometer signals are monitored. The recorded images and diffraction patterns show...... that the presence and stagnation of H2O vapour created upon reduction blocks H2 access to the reactive sites, decreasing the reaction rate at a high conversion fraction. The gas flow is low and may not evacuate the product gas efficiently around the Ni(O) particles. Complementary XRD experiments point towards...... the same conclusion and underline the impact of the pressure and gas flow on the kinetics. It is possible to determine an approximate activation energy for NiO reduction inside the ETEM using the Kissinger method [8], which is based on measurements of the shift in the temperature at which the reaction rate...

Two novel approaches to study arthropod anatomy by using dualbeam FIB/SEM.

Science.gov (United States)

Di Giulio, Andrea; Muzzi, Maurizio

2018-03-01

Transmission Electron Microscopy (TEM) has always been the conventional method to study arthropod ultrastructure, while the use of Scanning Electron Microscopy (SEM) was mainly devoted to the examination of the external cuticular structures by secondary electrons. The new generation field emission SEMs are capable to generate images at sub-cellular level, comparable to TEM images employing backscattered electrons. The potential of this kind of acquisition becomes very powerful in the dual beam FIB/SEM where the SEM column is combined with a Focused Ion Beam (FIB) column. FIB uses ions as a nano-scalpel to slice samples fixed and embedded in resin, replacing traditional ultramicrotomy. We here present two novel methods, which optimize the use of FIB/SEM for studying arthropod anatomy. Copyright © 2017 Elsevier Ltd. All rights reserved.

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

Powder samples of Ag/ZnO nanocomposite containing different amounts of Ag were synthesized by co-precipitation method. The synthesized samples were characterized by XRD, SEM, EDX and TEM techniques. The XRD results revealed that all the samples show wurtzite hexagonal phase of ZnO. The TEM micrographs ...

Evaluation of the effects of biodegradable nanoparticles on a vaccine delivery system using AFM, SEM, and TEM.

Science.gov (United States)

Kim, Bum-Gil; Kang, Ik-Joong

2008-09-01

Hepatitis B is a deadly disease, and is carried by 30% of the world's population. Antibodies are produced through a series of three manual vaccinations during infancy and childhood. However, the current needle vaccination not only induces pain in patients, but also can be inconvenient to administer. This is particularly true for the case of newborn babies. Intranasal vaccination is emerging as an alternative parenteral drug delivery method that facilitates drug delivery without causing pain. Chitosan, which is obtained through the deacetylation of chitin from crustacea, is a cationic polymer that is biodegradable, avirulent, and highly absorptive. In this study, ionic gelation between chitosan and TPP was conducted to synthesize chitosan nanoparticles with sizes of 200-400 nm and a surface potential of 55-60 mV, and which can be used as Hepatitis B vaccine carriers. Then, Hepatitis B antigen protein was impregnated to manufacture chitosan-recombinant gene vaccine protein (RGVP) nanoparticles. AFM, SEM, TEM, and STEM were used to analyze the manufactured nanoparticles, whose function as drug carriers and whose usefulness for intranasal vaccination were confirmed through in vivo tests with SD rats.

Evaluation of dislocation density in copper and brass α deformed by XRD peak width analysis

International Nuclear Information System (INIS)

Sousa, Talita Gama de

2014-01-01

The determination of dislocation density in metallic materials has been available for many years in scientific environment. This is due to the fact that the dislocations are the main responsible for plastic deformation, which, thereafter, markedly influences the mechanical properties. In this work, the dislocation density was analyzed through peak broadening of Xray diffraction (XRD) using Convolutional Multiple Whole Profile (CMWP) program. The measurements obtained by XRD were compared with those obtained from images observed by transmission electronic microscopy (TEM). The materials used in this study were pure copper and brass α as alloy 268 (6 % Cu and 34 % Zn), deformed by rolling and ECA (equal channel angular extrusion) processes. The results indicate that the XRD is a powerful tool for the characterization of the microstructure in relation to the dislocation density, as they were consistent to the TEM measurements, and also showed good relationship with measurements of hardness. Furthermore, through the dislocation density it was possible to verify the influence of stacking fault energy (SFE) in the evolution of the copper samples deformation process and its alloy, and that the presence of texture in rolled samples did not impair the measurements obtained by XRD technique. (author)

Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury.

Science.gov (United States)

Li, Cen; Yang, Hongxia; Du, Yuzhi; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao; Wei, Lixin

2016-01-01

Zuotai ( gTso thal ) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100-800 nm, which commonly further aggregate into 1-30  μ m loosely amorphous particles. XRD test shows that β -HgS, S 8 , and α -HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai , and it would play a positive role in interpreting this mysterious Tibetan drug.

Phase analysis of nano-phase materials using selected area electron diffraction in the TEM

International Nuclear Information System (INIS)

Labar, J. L.

2002-01-01

In analogy to X-ray power diffraction (XRD), we are developing a method to help phase identification when examining a large number of grains simultaneously by electron diffraction. Although XRD is well established, it can not be used for small quantities of materials (volumes below 1 mm 3 ). Examining a usual TEM sample with thickness of 100 nm and using a selected area of 1 mm in diameter, the selected area electron diffraction pattern (SAED) carries information about several thousands of grains from a material with an average grain size of about 10 nm. The accuracy of XRD can not be attained by electron diffraction (ED). However, simultaneous visual observation of the nanostructure is an additional benefit of TEM (beside the small amount of needed material). The first step of the development project was the development of a computer program ('ProcessDiffraction') that processes digital versions of SAED patterns and presents them in an XRD-like form (intensity vs. scattering vector). In the present version (V2.0.3) phase identification is carried out by comparing the measured distribution to 'Markers', i.e. data of known phases. XRD data cards are used if the detailed structure of a phase is not known. Kinematic electron diffraction intensities are calculated for phases with known atomic positions (Author)

The effect of different growth media, carbon source and pgrs on dendrobium broga giant orchid's protocorm-like bodies (plbs) proliferation supported with sem and tem analysis

International Nuclear Information System (INIS)

Uddain, J.; Gnasekaran, P.; Zakaria, L.

2015-01-01

Dendrobium Broga Giant (Dendrobium Bobby Messina * Dendrobium Superbiens) is a new orchid hybrid in Malaysia. The aim of this study was to investigate the effect of different growth media, carbon sources and PGRs on Dendrobium Broga Giant orchid's protocorm-like bodies (PLBs) proliferation supported with SEM and TEM analysis. The PLBs were cultured on different strength of semi-solid and liquid MS medium and the proliferation rate was recorded based on the fresh weight basis. The maximum PLBs proliferation (12.31% 0.57) was obtained in MS semi-solid medium. PLBs were cultured on MS semi-solid media supplemented with different sucrose concentrations (0, 10, 20, 30 and 40 g L-1). The highest proliferation rate of PLBs (15.48% 1.20) was recorded from MS supplemented with 20 g L-1 sucrose. Different concentrations of BAP (0, 0.5, 1.0, 2.0 mg.L-1) and NAA (0, 0.5, 1.0, 2.0 mgL-1) were added to MS semi-solid medium. Combinations of 1.0 mg L-1 BAP and 0.5 mg.L-1 NAA produced higher PLBs proliferation. Micromorphological studies by SEM and TEM displayed trichome, leaf primordial, stomata, various sizes of mitochondria, vacuoles, different shapes of chloroplast were found in PLBs which ameliorated the slow proliferation nature of plantlets. (author)

Cassette-based in-situ TEM sample inspection in the dual-beam FIB

International Nuclear Information System (INIS)

Kendrick, A B; Moore, T M; Zaykova-Feldman, L; Amador, G; Hammer, M

2008-01-01

A novel method is presented, combining site-specific TEM sample preparation and in-situ STEM analysis in a dual-beam microscope (FIB/SEM) fitted with a chamber mounted nano-manipulator. TEM samples are prepared using a modified in-situ, lift-out method, whereby the samples are thinned and oriented for immediate in-situ STEM analysis using the tilt, translation, and rotation capabilities of a FIB/SEM sample stage, a nano-manipulator, and a novel cassette. This cassette can provide a second tilt axis, orthogonal to the stage tilt axis, so that the STEM image contrast can be optimized to reveal the structural features of the sample (true STEM imaging in the FIB/SEM). The angles necessary for stage rotation and probe shaft rotation are calculated based on the position of the nano-manipulator relative to the stage and door and the stage tilt angle. A FIB/SEM instrument, equipped with a high resolution scanning electron column, can provide sufficiently high image resolution to enable many failure analysis and process control applications to be successfully carried out without requiring the use of a separate dedicated TEM/STEM instrument. The benefits of this novel approach are increased throughput and reduced cost per sample. Comparative analysis of different sample preparation methods is provided, and the STEM images obtained are shown.

Automated transmission-mode scanning electron microscopy (tSEM for large volume analysis at nanoscale resolution.

Directory of Open Access Journals (Sweden)

Masaaki Kuwajima

Full Text Available Transmission-mode scanning electron microscopy (tSEM on a field emission SEM platform was developed for efficient and cost-effective imaging of circuit-scale volumes from brain at nanoscale resolution. Image area was maximized while optimizing the resolution and dynamic range necessary for discriminating key subcellular structures, such as small axonal, dendritic and glial processes, synapses, smooth endoplasmic reticulum, vesicles, microtubules, polyribosomes, and endosomes which are critical for neuronal function. Individual image fields from the tSEM system were up to 4,295 µm(2 (65.54 µm per side at 2 nm pixel size, contrasting with image fields from a modern transmission electron microscope (TEM system, which were only 66.59 µm(2 (8.160 µm per side at the same pixel size. The tSEM produced outstanding images and had reduced distortion and drift relative to TEM. Automated stage and scan control in tSEM easily provided unattended serial section imaging and montaging. Lens and scan properties on both TEM and SEM platforms revealed no significant nonlinear distortions within a central field of ∼100 µm(2 and produced near-perfect image registration across serial sections using the computational elastic alignment tool in Fiji/TrakEM2 software, and reliable geometric measurements from RECONSTRUCT™ or Fiji/TrakEM2 software. Axial resolution limits the analysis of small structures contained within a section (∼45 nm. Since this new tSEM is non-destructive, objects within a section can be explored at finer axial resolution in TEM tomography with current methods. Future development of tSEM tomography promises thinner axial resolution producing nearly isotropic voxels and should provide within-section analyses of structures without changing platforms. Brain was the test system given our interest in synaptic connectivity and plasticity; however, the new tSEM system is readily applicable to other biological systems.

(AN)AEROBIC BACTERIA FOUND IN SECONDARY-CATARACT MATERIAL - A SEM/TEM STUDY

NARCIS (Netherlands)

KALICHARAN, D; JONGEBLOED, WL; LOS, LI; WORST, JGF

1992-01-01

Twentyfour patients, who had marked reduction of vision due to secondary-cataract developed after an ECCE, were treated by surgical cleaning of the posterior lens capsule. During this procedure globular secondary-cataract material was removed and collected for morphological examination by SEM and

SEM and TEM characterization of the microstructure of post-compressed TiB2/2024Al composite.

Science.gov (United States)

Guo, Q; Jiang, L T; Chen, G Q; Feng, D; Sun, D L; Wu, G H

2012-02-01

In the present work, 55 vol.% TiB(2)/2024Al composites were obtained by pressure infiltration method. Compressive properties of 55 vol.% TiB(2)/2024Al composite under the strain rates of 10(-3) and 1S(-1) at different temperature were measured and microstructure of post-compressed TiB(2)/2024Al composite was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). No trace of Al(3)Ti compound flake was found. TiB(2)-Al interface was smooth without significant reaction products, and orientation relationships ( [Formula: see text] and [Formula: see text] ) were revealed by HRTEM. Compressive strength of TiB(2)/2024Al composites decreased with temperature regardless of strain rates. The strain-rate-sensitivity of TiB(2)/2024Al composites increased with the increasing temperature. Fracture surface of specimens compressed at 25 and 250°C under 10(-3)S(-1) were characterized by furrow. Under 10(-3)S(-1), high density dislocations were formed in Al matrix when compressed at 25°C and dynamic recrystallization occurred at 250°C. Segregation of Mg and Cu on the subgrain boundary was also revealed at 550°C. Dislocations, whose density increased with temperature, were formed in TiB(2) particles under 1S(-1). Deformation of composites is affected by matrix, reinforcement and strain rate. Copyright © 2011 Elsevier Ltd. All rights reserved.

XRD and SEM/EDS characterization of coconut fibers in raw and treated forms used in the treatment of strontium in aqueous solution

Energy Technology Data Exchange (ETDEWEB)

Fonseca, Heverton C.O.; Garcia, Rafael H.L.; Ferreira, Robson J.; Silva, Flavia R.O.; Potiens Junior, Ademar J.; Sakata, Solange K., E-mail: sksakata@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2015-07-01

{sup 90}Sr, a radioactive isotope of strontium, is one of the fission products and quite often present in the radioactive waste produced by nuclear power plants. Recently, the removal efficiency of strontium by treated coconut fibers was evaluated and reached up to 95% in an aqueous solution. This work presents the characterization of raw and treated coconut fibers with different concentrations of hydrogen peroxide in basic medium using X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy (SEM / EDS). The analysis of X-ray diffraction shows a crystallinity of 37.6% for raw coconut fiber and crystallinity of 45.4% and 50.6% for coconut fibers 1 and 2, respectively. These results showed that the different degrees of degradation of organic matter can affect the crystallinity of the treated. This study of morphology and crystallinity of theses biosorbent materials with strontium will help in comprehension of the effects of alkaline hydrogen peroxide treatment and it will demonstrate the potential of strontium uptake by coconut fibers. (author)

XRD and SEM/EDS characterization of coconut fibers in raw and treated forms used in the treatment of strontium in aqueous solution

International Nuclear Information System (INIS)

Fonseca, Heverton C.O.; Garcia, Rafael H.L.; Ferreira, Robson J.; Silva, Flavia R.O.; Potiens Junior, Ademar J.; Sakata, Solange K.

2015-01-01

90 Sr, a radioactive isotope of strontium, is one of the fission products and quite often present in the radioactive waste produced by nuclear power plants. Recently, the removal efficiency of strontium by treated coconut fibers was evaluated and reached up to 95% in an aqueous solution. This work presents the characterization of raw and treated coconut fibers with different concentrations of hydrogen peroxide in basic medium using X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy (SEM / EDS). The analysis of X-ray diffraction shows a crystallinity of 37.6% for raw coconut fiber and crystallinity of 45.4% and 50.6% for coconut fibers 1 and 2, respectively. These results showed that the different degrees of degradation of organic matter can affect the crystallinity of the treated. This study of morphology and crystallinity of theses biosorbent materials with strontium will help in comprehension of the effects of alkaline hydrogen peroxide treatment and it will demonstrate the potential of strontium uptake by coconut fibers. (author)

Radiometric, SEM and XRD investigation of the Chituc black sands, southern Danube Delta, Romania

International Nuclear Information System (INIS)

Margineanu, R.M.; Blebea-Apostu, Ana-Maria; Celarel, Aurelia; Gomoiu, Claudia-Mariana; Costea, C.; Dumitras, Delia; Ion, Adriana; Duliu, O.G.

2014-01-01

The black sand of the Chituc marine sand bank, northern of the city of Navodari (Romania), presents anomalous high radioactivity. Field measurements recorded in some places dose rate up to 200 nSv/h, significantly overpassing the average value of 44 ± 20 nSv/h along the entire Southern sector of Romanian Black Sea shore. Gamma ray spectrometry performed on both Slanic-Prahova Underground Low Background Laboratory and Geological Institute of Romania Radiometric Facilities showed with clarity the dominance of 228 Ac radioisotope in the 50 microns fraction together with the 226 Ra and traces of 40 K. No significant amount of anthropogenic 137 Cs was identified. Based on radiometric as well as on SEM–EDAX and XRD determinations we come to the conclusion that the evidenced radioactivity could be attributed to both uranium and thorium series in the zircon and monazite fractions and to a lesser extent to potassium in the feldspars. - Highlights: • High background radioactivity (up to 200 nSv/h) evidenced. • Radiometric measurements showed a maximum radioactivity of U and Th confined to 50–100 μm fraction. • XRD and SEM–EDAX data revealed the presence of k-feldspars, ilmenite, zircone, monazite and garnets

Removal of industrial dyes and heavy metals by Beauveria bassiana: FTIR, SEM, TEM and AFM investigations with Pb(II).

Science.gov (United States)

Gola, Deepak; Malik, Anushree; Namburath, Maneesh; Ahammad, Shaikh Ziauddin

2017-10-01

Presence of industrial dyes and heavy metal as a contaminant in environment poses a great risk to human health. In order to develop a potential technology for remediation of dyes (Reactive remazol red, Yellow 3RS, Indanthrene blue and Vat novatic grey) and heavy metal [Cu(II), Ni(II), Cd(II), Zn(II), Cr(VI) and Pb(II)] contamination, present study was performed with entomopathogenic fungi, Beauveria bassiana (MTCC no. 4580). High dye removal (88-97%) was observed during the growth of B. bassiana while removal percentage for heavy metals ranged from 58 to 75%. Further, detailed investigations were performed with Pb(II) in terms of growth kinetics, effect of process parameters and mechanism of removal. Growth rate decreased from 0.118 h -1 (control) to 0.031 h -1 , showing 28% reduction in biomass at 30 mg L -1 Pb(II) with 58.4% metal removal. Maximum Pb(II) removal was observed at 30 °C, neutral pH and 30 mg L -1 initial metal concentration. FTIR analysis indicated the changes induced by Pb(II) in functional groups on biomass surface. Further, microscopic analysis (SEM and atomic force microscopy (AFM)) was performed to understand the changes in cell surface morphology of the fungal cell. SEM micrograph showed a clear deformation of fungal hyphae, whereas AFM studies proved the increase in surface roughness (RSM) in comparison to control cell. Homogenous bioaccumulation of Pb(II) inside the fungal cell was clearly depicted by TEM-high-angle annular dark field coupled with EDX. Present study provides an insight into the mechanism of Pb(II) bioremediation and strengthens the significance of using entomopathogenic fungus such as B. bassiana for metal and dye removal.

First ultrastructural data on the human tapeworm Taenia asiatica eggs by scanning and transmission electron microscopy (SEM, TEM).

Science.gov (United States)

Galán-Puchades, M Teresa; Yang, Yichao; Marcilla, Antonio; Choe, Seongjun; Park, Hansol; Osuna, Antonio; Eom, Keeseon S

2016-09-01

Humans are definitive hosts of three species of the Taenia genus, namely Taenia solium, Taenia saginata and Taenia asiatica. The relative novelty of the latter explains the lack of knowledge concerning certain relevant aspects related to this parasite, such as its definite geographical distribution and whether its eggs can infect humans or not. So far, only the eggs of T. solium are known to be infective for humans, producing cysticercosis. Although eggs contain the infective stage, the oncosphere, there is a lack of research on the ultrastructure of eggs of human taeniids. We show, for the first time, the ultrastructure of eggs of T. asiatica by means of SEM and TEM analyses. We detected all the envelopes, namely the egg shell, vitelline layer, outer embryophoric membrane, embryophore, granular layer, basal membrane, oncospheral membrane and oncospheral tegument. Hooks surrounded by myofibrils and glycogen-like particles, the two types of secretory granules of the penetration glands, as well as several nuclei and mitochondria were also revealed in the oncospheres. In addition to the already known structures in eggs from other Taenia species, the presence of two types of small vesicles is described herein, possibly corresponding to exosomes and ectosomes because of their shape and size, which could participate in the host/parasite intercellular communication.

A TEM Study on the Ti-Alloyed Grey Iron

DEFF Research Database (Denmark)

Moumeni, Elham; Tiedje, Niels Skat; Grumsen, Flemming Bjerg

2014-01-01

The microstructure of graphite flakes in titanium alloyed cast iron is studied using electron microscopy techniques. Dual beam SEM/FIB has been used for TEM sample preparation. A TEM study has been carried out on graphite flakes in grey cast iron using selected area electron diffraction. Based...... and that there is a high proportion of twins in the fine grained graphite. It appears that twinning and stacking faults are involved in the fine grained structure of the graphite. It is discussed how Ti addition affect crystal growth and may lead to formation of superfine graphite....

Conservation of Moroccan manuscript papers aged 150, 200 and 800 years. Analysis by infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), and scanning electron microscopy energy dispersive spectrometry (SEM-EDS).

Science.gov (United States)

Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Lakhiari, Hamid; Kerbal, Abdelali; Doumenq, Pierre; Mille, Gilbert; De Carvalho, Maria Luisa

2015-02-05

The preservation of manuscripts and archive materials is a serious problem for librarians and restorers. Paper manuscript is subjected to numerous degradation factors affecting their conservation state. This research represents an attempt to evaluate the conservation restoration process applied in Moroccan libraries, especially the alkaline treatment for strengthening weakened paper. In this study, we focused on six samples of degraded and restored paper taken from three different Moroccan manuscripts aged 150, 200 and 800 years. In addition, the Japanese paper used in restoration has been characterized. A modern paper was also analyzed as reference. A three-step analytical methodology based on infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD) and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) analysis was developed before and after restoration in order to determine the effect of the consolidation treatment on the paper structure. The results obtained by XRD and ATR-FTIR disclosed the presence of barium sulfate (BaSO4) in all restored paper manuscripts. The presence of calcium carbonate (CaCO3) in all considered samples was confirmed by FTIR spectroscopy. The application of de-acidification treatment causes significant changes connected with the increase of intensity mostly in the region 1426 cm(-1), assigned to the asymmetric and symmetric CO stretching mode of calcite, indicating the effectiveness of de-acidification procedure proved by the rise of the alkaline reserve content allowing the long term preservation of paper. Observations performed by SEM magnify the typical paper morphology and the structure of fibbers, highlighting the effect of the restoration process, manifested by the reduction of impurities. Copyright © 2014 Elsevier B.V. All rights reserved.

Correlation of superconducting properties and microstructure in MgB{sub 2} using SEM, EPMA and TEM

Energy Technology Data Exchange (ETDEWEB)

Birajdar, Balaji I.

2008-04-14

This thesis can be subdivided as follows: (I) Development of the quantitative electron microscopy and spectroscopy methods essential for the microstructural analysis of MgB{sub 2} and thereby assess the performance of two energy-filtered TEMs. (II) Application of these methods to few selected samples: (a) Pure and Al-alloyed MgB{sub 2} bulk samples prepared by solid-state reaction or by mechanical alloying, (b) In-situ and ex-situ MgB{sub 2} wires and tapes with and without SiC additives prepared by different variants of the powder-in-tube technology. Quantitative B analysis by EDX spectroscopy was applied in the SEM and TEM, which is a major achievement. (III) Establishing a model which quantitatively explains the correlation between microstructure and critical current density as a function of magnetic field. The actual Al mole fraction in the MgB{sub 2} matrix was found to be less than the nominal Al mole fraction and the difference increased with increasing Al mole fraction. Al is incorporated into MgB{sub 2} grains of {approx}1{mu}m size by substitution of Mg atoms causing T{sub c} and c lattice parameter to decrease at a rate of 1.56 K and 1.15 pm per at.% of Al alloying. Precipitation of Al was not detected up to highest Al mole fractions but Al was inhomogeneously distributed in the sample, which explained the broadening of the superconducting transition width ({delta}T{sub c}) with increasing Al mole fraction. For wires and tapes, significant differences were observed in the microstructure of in-situ and ex-situ samples. This holds particularly if SiC was added and yielded Mg{sub 2}Si for in-situ samples annealed at 600 -650 C and Mg-Si-O phases for ex-situ samples annealed between 900 -1050 C. Four microstructural parameters were identified as relevant for the I{sub c} of wires and tapes and these were: 1) MgB{sub 2} grain size which lies in the range of 20-1000 nm, 2) colony size (colony is a dense arrangement of MgB{sub 2} grains) which lies in the range

Synthesis and characterization of nanocrystalline graphite from coconut shell with heating process

Energy Technology Data Exchange (ETDEWEB)

Wachid, Frischa M., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Perkasa, Adhi Y., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Prasetya, Fandi A., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Rosyidah, Nurul, E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Darminto, E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id [Department of Physics, Faculty of Mathematics and Natural Sciences, Institut Teknologi Sepuluh Nopember, Campus ITS Sukolilo, Surabaya 60111 (Indonesia)

2014-02-24

Graphite were synthesized and characterized by heating process of coconut shell with varying temperature (400, 800 and 1000°C) and holding time (3 and 5 hours). After heating process, the samples were characterized by X-ray diffraction (XRD) and analyzed by X'pert HighScore Plus Software, Scanning Electron Microcope-Energy Dispersive X-Ray (SEM-EDX) and Transmission Electron Microscope-Energy Dispersive X-Ray (TEM-EDX). Graphite and londsdaelite phase were analyzed by XRD. According to EDX analysis, the sample was heated in 1000°C got the highest content of carbon. The amorphous carbon and nanocrystalline graphite were observed by SEM-EDX and TEM-EDX.

Synthesis and characterization of nanocrystalline graphite from coconut shell with heating process

International Nuclear Information System (INIS)

Wachid, Frischa M.; Perkasa, Adhi Y.; Prasetya, Fandi A.; Rosyidah, Nurul; Darminto

2014-01-01

Graphite were synthesized and characterized by heating process of coconut shell with varying temperature (400, 800 and 1000°C) and holding time (3 and 5 hours). After heating process, the samples were characterized by X-ray diffraction (XRD) and analyzed by X'pert HighScore Plus Software, Scanning Electron Microcope-Energy Dispersive X-Ray (SEM-EDX) and Transmission Electron Microscope-Energy Dispersive X-Ray (TEM-EDX). Graphite and londsdaelite phase were analyzed by XRD. According to EDX analysis, the sample was heated in 1000°C got the highest content of carbon. The amorphous carbon and nanocrystalline graphite were observed by SEM-EDX and TEM-EDX

EBSD and TEM Characterization of High Burn-up Mixed Oxide Fuel

International Nuclear Information System (INIS)

Teague, Melissa C; Gorman, Brian P.; Miller, Brandon D; King, Jeffrey

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to approximately 1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken from the cooler rim region of the fuel pellet had approximately 2.5x higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice approximately 25 um cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel

3D imaging of cells and tissues by focused ion beam/scanning electron microscopy (FIB/SEM).

Science.gov (United States)

Drobne, Damjana

2013-01-01

Integration of a scanning electron microscope (SEM) and focused ion beam (FIB) technology into a single FIB/SEM system permits use of the FIB as a nano-scalpel to reveal site-specific subsurface microstructures which can be examined in great detail by SEM. The FIB/SEM technology is widely used in the semiconductor industry and material sciences, and recently its use in the life sciences has been initiated. Samples for FIB/SEM investigation can be either embedded in a plastic matrix, the traditional means of preparation of transmission electron microscopy (TEM) specimens, or simply dried as in samples prepared for SEM imaging. Currently, FIB/SEM is used in the life sciences for (a) preparation by the lift-out technique of lamella for TEM analysis, (b) tomography of samples embedded in a matrix, and (c) in situ site-specific FIB milling and SEM imaging using a wide range of magnifications. Site-specific milling and imaging has attracted wide interest as a technique in structural research of single eukaryotic and prokaryotic cells, small animals, and different animal tissue, but it still remains to be explored more thoroughly. In the past, preparation of samples for site-specific milling and imaging by FIB/SEM has typically adopted the embedding techniques used for TEM samples, and which have been very well described in the literature. Sample preparation protocols for the use of dried samples in FIB/SEM have been less well investigated. The aim of this chapter is to encourage application of FIB/SEM on dried biological samples. A detailed description of conventional dried sample preparation and FIB/SEM investigation of dried biological samples is presented. The important steps are described and illustrated, and direct comparison between embedded and dried samples of same tissues is provided. The ability to discover links between gross morphology of the tissue or organ, surface characteristics of any selected region, and intracellular structural details on the nanometer

Investigation of composition and structure of spongy and hard bone tissue using FTIR spectroscopy, XRD and SEM

Science.gov (United States)

Al-Akhras, M.-Ali H.; Hasan Qaseer, M. K.; Albiss, B. A.; Alebrhim, M. Anwar; Gezawa, Umar S.

2018-02-01

Valuable structural and chemical features can be obtained for spongy and hard bone by infrared spectroscopy and X-ray diffraction. A better understanding of chemical and structural differences between spongy and hard bone is a very important contributor to bone quality. Our data according to IR data showed that the collagen cross-links occurred to be higher in spongy bone, and crystallinity was lower in spongy bone. Deconvolution of the infrared band near 870 cm-1 reveals evidence for A2-type carbonate substitution on hydroxyapatite of spongy bone in addition to the A and B type carbonate substitution that are also found in hard bone. IR and XRD data confirmed the results of each other since full width at half maximum of 002-apatite pattern of XRD showed that the crystallinity was lower in spongy bone. The microstructure was examined by using scanning electron microscope and the result showed that the lattice of thin threads in spongy bone and is less dense than hard bone.

Composition and microstructure of MTA and Aureoseal Plus: XRF, EDS, XRD and FESEM evaluation.

Science.gov (United States)

Cianconi, L; Palopoli, P; Campanella, V; Mancini, M

2016-12-01

The aim of this study was to determine the chemical composition and the phases' microstructure of Aureoseal Plus (OGNA, Italy) and ProRoot MTA (Dentsply Tulsa Dental, USA) and to compare their characteristics. Study Design: Comparing Aureoseal Plus and ProRoot MTA microstructure by means of several analyses type. The chemical analysis of the two cements was assessed following the UNI EN ISO 196-2 norm. X-Ray fluorescence (XRF) was used to determine the element composition. The crystalline structure was analysed quantitatively using x-ray diffraction (XRD). Powders morphology was evaluated using a scanning electron microscope (SEM) with backscattering detectors, and a field emission scanning electron microscope (FESEM). Elemental analysis was performed by energy dispersive x-ray analysis (EDS). The semi-quantitative XRF analysis showed the presence of heavy metal oxides in both cements. The XRD spectra of the two cements reported the presence of dicalcium silicate, tricalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, bismuth oxide and gypsum. SEM analysis showed that ProRoot MTA powder is less coarse and more homogeneous than Aureoseal. Both powders are formed by particles of different shapes: round, prismatic and oblong. The EDS analysis showed that some ProRoot MTA particles, differently from Aureoseal, contain Ca, Si, Al and Fe. Oblong particles in ProRoot and Aureoseal are rich of bismuth. The strong interest in developing new Portland cement-based endodontic sealers will create materials with increased handling characteristics and physicochemical properties. A thorough investigation on two cement powders was carried out by using XRF, XRD, SEM and EDS analysis. To date there was a lack of studies on Aureoseal Plus. This cement is similar in composition to ProRoot MTA. Despite that it has distinctive elements that could improve its characteristics, resulting in a good alternative to MTA.

XRF, XRD and SEM facilities in the School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia

International Nuclear Information System (INIS)

Azmi Rahmat

1996-01-01

The School has acquired excellent facilities for elemental analysis by XRF and EDX and phase analysis by XRD. The type of research work carried out in the School is described. The school also assists the local industries in trying to solve their problems fully utilizing these facilities along with other testing units

Center for Electron Nanoscopy, CEN-DTU

DEFF Research Database (Denmark)

Horsewell, Andy

- The projects - The physics Field Emission Gun very intense, highly coherent, stable electron source TEM 80 – 300 keV SEM ~1 – 30 keV Monochromator S/TEM TEM) Cs correction E-cell in-situ TEM, T0, reactive gasses, mass spectrometer, XRD - The microscopes E-TEM, A-TEM......, TEM, FEGSEM, FIB/FEGSEM, LVSEM, ESEM E-TEM Environmental cell, gas-surface interactions, in-situ heating, tomography A-TEM Analytical high resolution microscopy, S/TEM, HREM, EFTEM, EDS, HAADF FIB/FEGSEM Microscopy, EDS, EBSD in 3-dimensions 3D image reconstruction for microstructure, composition...

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

Science.gov (United States)

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.

Structural, optical and photocatalytic properties of flower-like ZnO nanostructures prepared by a facile wet chemical method

Directory of Open Access Journals (Sweden)

Sini Kuriakose

2013-11-01

Full Text Available Flower-like ZnO nanostructures were synthesized by a facile wet chemical method. Structural, optical and photocatalytic properties of these nanostructures have been studied by X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, photoluminescence (PL and UV–vis absorption spectroscopy. SEM and TEM studies revealed flower-like structures consisting of nanosheets, formed due to oriented attachment of ZnO nanoparticles. Flower-like ZnO structures showed enhanced photocatalytic activity towards sun-light driven photodegradation of methylene blue dye (MB as compared to ZnO nanoparticles. XRD, UV–vis absorption, PL, FTIR and TEM studies revealed the formation of Zn(OH2 surface layer on ZnO nanostructures upon ageing. We demonstrate that the formation of a passivating Zn(OH2 surface layer on the ZnO nanostructures upon ageing deteriorates their efficiency to photocatalytically degrade of MB.

Some critical aspects of FT-IR, TGA, powder XRD, EDAX and SEM studies of calcium oxalate urinary calculi.

Science.gov (United States)

Joshi, Vimal S; Vasant, Sonal R; Bhatt, J G; Joshi, Mihir J

2014-06-01

Urinary calculi constitute one of the oldest afflictions of humans as well as animals, which are occurring globally. The calculi vary in shape, size and composition, which influence their clinical course. They are usually of the mixed-type with varying percentages of the ingredients. In medical management of urinary calculi, either the nature of calculi is to be known or the exact composition of calculi is required. In the present study, two selected calculi were recovered after surgery from two different patients for detailed examination and investigated by using Fourier-Transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA), powder X-ray diffraction (XRD), scanning electron microscopy and energy dispersive analysis of X-rays (EDAX) techniques. The study demonstrated that the nature of urinary calculi and presence of major phase in mixed calculi could be identified by FT-IR, TGA and powder XRD, however, the exact content of various elements could be found by EDAX only.

Evaluation of microstructural development in electron beam melted Ti-6Al-4V

International Nuclear Information System (INIS)

Safdar, A.; Wei, L.-Y.; Snis, A.; Lai, Z.

2012-01-01

In the current work an investigation of the microstructures of EBM built Ti-6Al-4V test bars has been performed using OM, SEM, TEM and XRD. It has been found that the prior β phase, that formed during the initial solidification, possesses a column shaped morphology with growing direction parallel to built direction. Typical (α + β) structures namely Widmanstätten α platelets with rod-like β phase formed on the interfaces of the fine α grains, have been observed in the columnar prior β grains. Grain boundary α phase was found to be formed around the boundaries of the columnar prior β grains. Different phases present in the parts, especially the BCC β phases have been characterized. The TEM/EDX results indicate very high V composition in the β phase. Results of TEM/SAED and XRD also revealed that a superlattice structure could be present in the β phase. Phase transformation sequence is discussed according to the processing history and the microstructures observed. - Highlights: ► α + β and individual β phase is observed and characterized by SEM, TEM and XRD. ► β-phase is identified as rod-like structure embedded in α matrix and platelets. ► Phase transformation sequence is discussed as per thermal history and microstructures.

Attempt of correlative observation of morphological synaptic connectivity by combining confocal laser-scanning microscope and FIB-SEM for immunohistochemical staining technique.

Science.gov (United States)

Sonomura, Takahiro; Furuta, Takahiro; Nakatani, Ikuko; Yamamoto, Yo; Honma, Satoru; Kaneko, Takeshi

2014-11-01

Ten years have passed since a serial block-face scanning electron microscopy (SBF-SEM) method was developed [1]. In this innovative method, samples were automatically sectioned with an ultramicrotome placed inside a scanning electron microscope column, and the block surfaces were imaged one after another by SEM to capture back-scattered electrons. The contrast-inverted images obtained by the SBF-SEM were very similar to those acquired using conventional TEM. SFB-SEM has made easy to acquire image stacks of the transmission electron microscopy (TEM) in the mesoscale, which is taken with the confocal laser-scanning microcopy(CF-LSM).Furthermore, serial-section SEM has been combined with the focused ion beam (FIB) milling method [2]. FIB-incorporated SEM (FIB-SEM) has enabled the acquisition of three-dimensional images with a higher z-axis resolution com- pared to ultramicrotome-equipped SEM.We tried immunocytochemistry for FIB-SEM and correlated this immunoreactivity with that in CF-LSM. Dendrites of neurons in the rat neostriatum were visualized using a recombinant viral vector. Moreover, the thalamostriatal afferent terminals were immunolabeled with Cy5 fluorescence for vesicular glutamate transporter 2 (VGluT2). After detection of the sites of terminals apposed to the dendrites by using CF-LSM, GFP and VGluT2 immunoreactivities were further developed for EM by using immunogold/silver enhancement and immunoperoxidase/diaminobenzidine (DAB) methods, respectively.We showed that conventional immuno-cytochemical staining for TEM was applicable to FIB-SEM. Furthermore, several synaptic contacts, which were thought to exist on the basis of CF-LSM findings, were confirmed with FIB-SEM, revealing the usefulness of the combined method of CF-LSM and FIB-SEM. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Electrodialytic soil remediation in a small pilot plant (Part II)

DEFF Research Database (Denmark)

Karlsmose, Bodil; Hansen, Lene

1999-01-01

-monia. Ammonia was chosen because it forms strong complexes with copper and to keep the soil basic, so that the carbonates were not dissolved. The bulk soil was treated by electrodialytic reme-dia-tion, and soil treated for seven months was investigated with XRD, TEM and SEM.Malachite was found by use of XRD...

Quantitative in situ TEM tensile testing of an individual nickel nanowire

International Nuclear Information System (INIS)

Lu Yang; Peng Cheng; Ganesan, Yogeeswaran; Lou Jun; Huang Jianyu

2011-01-01

In this paper, we have demonstrated the usage of a novel micro-mechanical device (MMD) to perform quantitative in situ tensile tests on individual metallic nanowires inside a transmission electron microscope (TEM). Our preliminary experiment on a 360 nm diameter nickel nanowire showed that the sample fractured at an engineering stress of ∼ 1.2 GPa and an engineering strain of ∼ 4%, which is consistent with earlier experiments performed inside a scanning electron microscope (SEM). With in situ high resolution TEM imaging and diffraction capabilities, this novel experimental set-up could provide unique opportunities to reveal the underlying deformation and damage mechanisms for metals at the nanoscale.

X-ray diffraction analysis of a severely plastically deformed aluminum alloy

International Nuclear Information System (INIS)

Ortiz, A.L.; Shaw, L.

2004-01-01

The crystallite size, lattice microstrain, lattice parameter, and formation of solid solutions of a nanocrystalline Al 93 Fe 3 Cr 2 Ti 2 alloy prepared via mechanical alloying (MA) starting from elemental powders have been investigated using the Rietveld method of X-ray diffraction (XRD) in conjunction with line-broadening analyses through the variance, Warren-Averbach, and Stokes and Wilson methods. Detailed analyses using transmission electron microscopy (TEM), scanning electron microscopy (SEM), and inductively coupled plasma-optical emission spectroscopy (ICP) have also been conducted in order to corroborate the formation of solid solutions and the grain size measurement determined from the XRD analyses. The results from the exhaustive XRD analyses are in excellent agreement with those derived from the investigation of TEM, SEM, and ICP. The lattice microstrains of the nanocrystalline Al solid solution determined from the XRD analyses are isotropic along different crystallographic directions and high, exhibiting the same order of magnitude as the ratio of the tensile strength to the elastic modulus of the Al crystal. Implications resulting from the comparison between the present study and the simplified XRD analyses are discussed

Nanoparticles of ZrPO4 for green catalytic applications

Science.gov (United States)

Sreenivasulu, Peta; Pendem, Chandrasekhar; Viswanadham, Nagabhatla

2014-11-01

Here we report the successful room temperature synthesis of zirconium phosphate nanoparticles (ZPNP) using the P123 tri-co-block polymer for the first time. The samples were characterized by SEM, TEM, XRD, TPD, and BET and were employed for fixation of CO2 on aniline to produce pharmaceutically important acetanilide under mild reaction conditions (150 °C and 150 Psi CO2 pressure).Here we report the successful room temperature synthesis of zirconium phosphate nanoparticles (ZPNP) using the P123 tri-co-block polymer for the first time. The samples were characterized by SEM, TEM, XRD, TPD, and BET and were employed for fixation of CO2 on aniline to produce pharmaceutically important acetanilide under mild reaction conditions (150 °C and 150 Psi CO2 pressure). Electronic supplementary information (ESI) available: Experimental details, wide angle XRD, EDX, IR spectra, GC data etc. See DOI: 10.1039/c4nr03209h

Study of the mechanisms involved in reactive silica

International Nuclear Information System (INIS)

Boinski, Frederic; Khouchaf, Lahcen; Tuilier, Marie-Helene

2010-01-01

The microstructure of a heterogeneous SiO 2 submitted to a depolymerisation process is studied using Transmission Electron Microscope (TEM), Environmental SEM (ESEM), and X-ray diffraction (XRD). With ESEM the formation of micro domain induced by the dissolution phenomena is shown. XRD shows the formation of a halo that is associated with the formation of amorphous phase. The parameters 'position and FWHM' of the halo, enabled us to show the evolution of the disorderly phase when the reaction progresses. The hypothesis of formation of nanoparticles with different structural states was confirmed by the TEM.

Synthesis, field emission properties and optical properties of ZnSe nanoflowers

Energy Technology Data Exchange (ETDEWEB)

Xue, S.L., E-mail: slxue@dhu.edu.cn [Department of Applied Physics, College of Science, Donghua University, Shanghai 201620 (China); Wu, S.X.; Zeng, Q.Z.; Xie, P.; Gan, K.X.; Wei, J.; Bu, S.Y.; Ye, X.N.; Xie, L. [Department of Applied Physics, College of Science, Donghua University, Shanghai 201620 (China); Zou, R.J. [State Key Laboratory for Modification and Chemical Fibers and Polymer Materials, Donghua University, Shanghai 201620 (China); Zhang, C.M.; Zhu, P.F. [Department of Physics, School of Fundamental Studies, Shanghai University of Engineering Science, Shanghai 201620 (China)

2016-03-01

Graphical abstract: Unique ZnSe nanoflowers have been successfully synthesized by reaction of Se powder with Zn substrates. They are characterized by XRD, SEM, TEM, XPS, EDS and Raman spectroscopy and were single crystals with cubic zinc blende (ZB) structure. They also have excellent field emission properties and optical properties. - Highlights: • Novel ZnSe nanoflowers are grown on Zn foils. • ZnSe nanoflowers are characterized by XRD, SEM, TEM, XPS and Raman spectra. • ZnSe nanoflowers on Zn foils as cathodes possess good FE properties. - Abstract: ZnSe nanoflowers have been synthesized by reaction of Se powder with Zn substrates at low temperature. The as-prepared ZnSe nanoflowers were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), X-ray energy dispersive spectroscope (EDS) and Raman spectroscopy measurements. It was found that the morphologies of the as-prepared samples highly depended on reaction time. ZnSe nanoclusters and nanoflowers formed at 573 K when the reaction time was 20 and 60 min, respectively. The as-prepared ZnSe nanoflowers were composed of radically aligned ZnSe nanorods with smooth surfaces. The results of XRD, XPS, EDS, TEM and Raman showed that the as-prepared ZnSe nanocrystals were single crystals with cubic zinc blende (ZB) structure. The formation mechanism of the as-prepared ZnSe nanoflowers was also discussed. In addition, the as-prepared ZnSe nanoflowers had excellent electron emission properties. The turn-on field of the as-prepared ZnSe nanoflowers was 3.5 V/μm and the enhancement factor was 3499. The optical properties of the as-prepared ZnSe nanoflowers were also investigated. The results demonstrated that the as-prepared ZnSe nanoflowers were potential candidates for optoelectronic devices.

Facile Synthesis of Yolk/Core-Shell Structured TS-1@Mesosilica Composites for Enhanced Hydroxylation of Phenol

KAUST Repository

Zou, Houbing; Sun, Qingli; Fan, Dongyu; Fu, Weiwei; Liu, Lijia; Wang, Runwei

2015-01-01

characterized by X-ray diffraction (XRD), N2 sorption, Fourier transform infrared spectoscopy (FT-IR) UV-Visible spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The characterization results showed that these samples

Fabrication and optical properties of TiO sub 2 nanowire arrays made by sol-gel electrophoresis deposition into anodic alumina membranes

CERN Document Server

Lin, Y; Yuan, X Y; Xie, T; Zhang, L D

2003-01-01

Ordered TiO sub 2 nanowire arrays have been successfully fabricated into the nanochannels of a porous anodic alumina membrane by sol-gel electrophoretic deposition. After annealing at 500 deg. C, the TiO sub 2 nanowire arrays and the individual nanowires were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and x-ray diffraction (XRD). SEM and TEM images show that these nanowires are dense and continuous with a uniform diameter throughout their entire length. XRD and SAED analysis together indicate that these TiO sub 2 nanowires crystallize in the anatase polycrystalline structure. The optical absorption band edge of TiO sub 2 nanowire arrays exhibits a blue shift with respect of that of the bulk TiO sub 2 owing to the quantum size effect.

Comparison of multilayered nanowire imaging by SEM and Helium Ion Microscopy

International Nuclear Information System (INIS)

Inkson, B J; Peng, Y; Jepson, M A E; Rodenburg, C; Liu, X

2010-01-01

The helium ion microscope (HeIM) is capable of probe sizes smaller than SEM and, with intrinsically small ion/sample interaction volumes, may therefore potentially offer higher spatial resolution secondary electron (SE) imaging of nanostructures. Here 55 nm diameter CoPt/Pt multilayered nanowires have been imaged by HeIM, SEM and TEM. It is found that there is an increased resolution of nanowire surface topography in HeIM SE images compared to SEM, however there is a reduction of materials contrast of the alternating Pt and CoPt layers. This can be attributed to the increased contribution of surface contamination layers to the ion-induced SE signal, and carbon is also observed to grow on the nanowires under prolonged HeIM scanning.

Synthesis, structural and magnetic characterization of soft magnetic nanocrystalline ternary FeNiCo particles

Energy Technology Data Exchange (ETDEWEB)

Toparli, Cigdem [Department of Metallurgical & Materials Eng., Istanbul Technical University, 34469 Istanbul (Turkey); Max-Planck-Institut für Eisenforschung GmbH, Düsseldorf (Germany); Ebin, Burçak [Department of Metallurgical & Materials Eng., Istanbul Technical University, 34469 Istanbul (Turkey); Nuclear Chemistry and Industrial Material Recycling, Department of Chemistry and Chemical Engineering, Chalmers University of Technology, S-412 96 Gothenburg (Sweden); Gürmen, Sebahattin, E-mail: gurmen@itu.edu.tr [Department of Metallurgical & Materials Eng., Istanbul Technical University, 34469 Istanbul (Turkey)

2017-02-01

The present study focuses on the synthesis, microstructural and magnetic properties of ternary FeNiCo nanoparticles. Nanocrystalline ternary FeNiCo particles were synthesized via hydrogen reduction assisted ultrasonic spray pyrolysis method in single step. The effect of precursor concentration on the morphology and the size of particles was investigated. The syntheses were performed at 800 °C. Structure, morphology and magnetic properties of the as-prepared products were characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM) studies. Scherer calculation revealed that crystallite size of the ternary particles ranged between 36 and 60 nm. SEM and TEM investigations showed that the particle size was strongly influenced by the precursor concentration and Fe, Ni, Co elemental composition of individual particles was homogeneous. Finally, the soft magnetic properties of the particles were observed to be a function of their size. - Highlights: • Ternary FeNiCo alloy nanocrystalline particles were synthesized in a single step. • Cubic crystalline structure and spherical morphology was observed by XRD, SEM and TEM investigations. • The analysis of magnetic properties indicates the soft magnetic features of particles.

Estimation of lattice strain for zirconia nanoparticles based on Williamson- Hall analysis

Energy Technology Data Exchange (ETDEWEB)

Aly, Kamal A., E-mail: kamalaly2001@gmail.com [Physics Department, Faculty of Science & Arts, Khullais, University of Jeddah, Jeddah (Saudi Arabia); Physics Department, Faculty of Science, Al-Azhar University, Assiut Branch, Assiut (Egypt); Khalil, N.M. [Chemistry Department, Faculty of Science & Arts, Khullais, University of Jeddah, Jeddah (Saudi Arabia); Refractories, Ceramics and Building Materials Department, National Research Centre, 12311, Cairo (Egypt); Algamal, Yousif [Chemistry Department, Faculty of Science & Arts, Khullais, University of Jeddah, Jeddah (Saudi Arabia); Saleem, Qaid M.A. [Chemistry Department, Faculty of Science & Arts, Khullais, University of Jeddah, Jeddah (Saudi Arabia); Aden University, Shabwa (Yemen)

2017-06-01

Nanoparticles of Zirconia were prepared (ZrO{sub 2}) by the neutralization of zirconium oxychloride octahydrate (ZrOCl{sub 2}-8H{sub 2}O) (2M) and ammonia solution (2M) at pH 8. The ZrO{sub 2} crystalline state was revealed by X-ray diffraction (XRD). The analysis of Scanning electron microscopy (SEM) and Transmission Electron microscope (TEM) images reveals that the as-synthesized ZrO{sub 2} particles at firing temperature of 800 °C are uniform and of range of 30 nm. Increasing of the temperature up to 1100 °C leads to the increase in particle size and alters the powders shape due to agglomeration arose from zirconia calcination as well as the increase in particle size. The X-ray peak broadening analysis (XRDBA) was used in the estimation of the crystalline size. Williamson-Hall (W-H) analysis was applied successfully to determine the energy density, stress, and the strain values via uniform deformation model (UDM), uniform deformation stress model (UDSM) and uniform deformation energy density model (UDEDM). The mean of the strain root square was calculated. The different strain values obtained from these models predicting the zirconia isotropic behavior. In addition to that, the W-H analysis results were discussed in terms of that obtained by Scherrer’s relationship, SEM and TEM images. - Graphical abstract: XRD patterns for zirconia nano-particles at different calcined temperature. - Highlights: • Nanoparticles of Zirconia (ZrO{sub 2}) were synthesized. • The ZrO{sub 2} crystalline state was revealed by XRD, SEM and TEM. • SEM and TEM images reveals that the ZrO{sub 2} particles are uniform and relatively small. • Both blocky particles and the powders shape are affected by the firing temperature. • The crystalline sizes were estimated using X-ray peak broadening analysis (XRDBA).

Facile charge transport in FeN x /Mo₂N/CNT nanocomposites for ...

Indian Academy of Sciences (India)

The nanocomposites were characterized using powder XRD, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), ElectronDiffraction, ThermogravimetricAnalysis and FTIRSpectroscopy. The electrochemical investigations suggest that the electrocatalytic activity of the composite increases with ...

High resolution SEM characterization of nano-precipitates in ODS steels.

Science.gov (United States)

Jóźwik, Iwona; Strojny-Nędza, Agata; Chmielewski, Marcin; Pietrzak, Katarzyna; Kurpaska, Łukasz; Nosewicz, Szymon

2018-05-01

The performance of the present-day scanning electron microscopy (SEM) extends far beyond delivering electronic images of the surface topography. Oxide dispersion strengthened (ODS) steel is on of the most promising materials for the future nuclear fusion reactor because of its good radiation resistance, and higher operation temperature up to 750°C. The microstructure of ODS should not exceed tens of nm, therefore there is a strong need in a fast and reliable technique for their characterization. In this work, the results of low-kV SEM characterization of nanoprecipitates formed in the ODS matrix are presented. Application of highly sensitive photo-diode BSE detector in SEM imaging allowed for the registration of single nm-sized precipitates in the vicinity of the ODS alloys. The composition of the precipitates has been confirmed by TEM-EDS. © 2018 Wiley Periodicals, Inc.

The use of micro-XRD for the study of glaze color decorations

Energy Technology Data Exchange (ETDEWEB)

Pradell, T.; Molina, G. [Universitat Politecnica de Catalunya, Dpt. Fisica i Enginyeria Nuclear, Castelldefels (Spain); Molera, J.; Pla, J. [Universitat de Vic, GRTD, Escola Politecnica Superior, Vic (Spain); Labrador, A. [BM16-ESRF, LLS, BP 220, Grenoble Cedex (France); Lund University, MAX IV Laboratory, Lund (Sweden)

2013-04-15

The compounds responsible for the colors and decorations in glass and glazed ceramics include: coloring agents (transition-metal ions), pigments (micro- and nanoprecipitates of compounds that either do not dissolve or recrystallize in the glassy matrix) and opacifiers (microcrystalline compounds with high light scattering capability). Their composition, structure and range of stability are highly dependent not only on the composition but also on the procedures followed to obtain them. Chemical composition of the colorants and crystallites may be obtained by means of SEM-EDX and WDX. Synchrotron radiation micro-X-ray diffraction (SR-micro-XRD) has a small beam size adequate (10 to 50 microns footprint size) to obtain the structural information of crystalline compounds and high brilliance, optimal for determining the crystallites even when present in low amounts. In addition, in glass decorations the crystallites often appear forming thin layers (from 10 to 100 micrometers thick) and they show a depth-dependent composition and crystal structure. Their nature and distribution across the glass/glaze decorations gives direct information on the technology of production and stability and may be related to the color and appearance. A selection of glass and glaze coloring agents and decorations are studied by means of SR-micro-XRD and SEM-EDX including: manganese brown, antimony yellow, red copper lusters and cobalt blue. The selection includes Medieval (Islamic, and Hispano Moresque) and Renaissance tin-glazed ceramics from the 10th to the 17th century AD. (orig.)

A.C. impedance, XRD, DSC, SEM and charge/discharge studies on Al2O3, TiO2, SiO2 dispersoid LiPF6/PVC/PVdF-co-HFP composite polymer electrolytes by phase inversion

Science.gov (United States)

Vickraman, P.; Gopukumar, S.

2017-07-01

The PVC/PVdF-co-HFP composite polymer electrolyte membranes (CPEMs) by varying blend ratios 1:1, 1:2, and 2:1 with fixed content of Al2O3, TiO2 and SiO2 having soaked in 0.5 M LiPF6 in EC/DEC (1:1) v/v) have been prepared by phase inversion. CPEMs of higher ionic conductivity (not dependent on electrolyte uptake as observed in our study) ASA4 (3.61×10-4 Scm-1), TSA3 (1.53×10-4 Scm-1), and SSA3 (4.81×10-4 Scm-1) have been only chosen for XRD, DSC, SEM and electrochemical studies. In XRD, crystalline peaks (phases) of PVdF have been noted with/without change in intensity as well as FWHM which correspond to type of filler interaction with host matrix. In DSC, it is observed that shifts in baseline, melting endotherms, and area under the endotherms indicating the thermal hist ory of PVC (Tg = 82 ° C) and melting of VdF crystallites varied with nature of the filler dispersoid. In SEM, the coagulated fibrils of the polymer coiled with the sponge like structure has been mapped. The charge/discharge studies are carried out on these CPEMs at C/10 rate in the voltage range 2.8 V - 4.2 V, and it is noted that the TSA3 showed better cycling performance with good capacity retention i.e., 50 cycles with 66% capacity retention than ASA4 of 28 cycles with 65% and SSA3 of 5 cycles with 56%. In the present study Coulombic efficiency is concerned only for first cycle and it is noted that the TSA3 showed 71% than 66% and 62% respectively for SSA3 and ASA4.

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

Science.gov (United States)

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

Morphology Characterization of PP/Clay Nanocomposites Across the Length Scales of the Structural Architecture

NARCIS (Netherlands)

Szazdi, Laszlo; Abranyi, Agnes; Pukansky Jr, Bela; Vancso, Gyula J.; Pukanszky, B.; Pukanszky, Bela

2006-01-01

The structure and rheological properties of a large number of layered silicate poly(propylene) nanocomposites were studied with widely varying compositions. Morphology characterization at different length scales was achieved by SEM, TEM, and XRD. Rheological measurements supplied additional

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

Science.gov (United States)

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.

Monolayer to MTS: using SEM, HIM, TEM and SERS to compare morphology, nanosensor uptake and redox potential in MCF7 cells

Science.gov (United States)

Jamieson, L. E.; Bell, A. P.; Harrison, D. J.; Campbell, C. J.

2015-06-01

Cellular redox potential is important for the control and regulation of a vast number of processes occurring in cells. When the fine redox potential balance within cells is disturbed it can have serious consequences such as the initiation or progression of disease. It is thought that a redox gradient develops in cancer tumours where the peripheral regions are well oxygenated and internal regions, further from vascular blood supply, become starved of oxygen and hypoxic. This makes treatment of these areas more challenging as, for example, radiotherapy relies on the presence of oxygen. Currently techniques for quantitative analysis of redox gradients are limited. Surface enhanced Raman scattering (SERS) nanosensors (NS) have been used to detect redox potential in a quantitative manner in monolayer cultured cells with many advantages over other techniques. This technique has considerable potential for use in multicellular tumour spheroids (MTS) - a three dimensional (3D) cell model which better mimics the tumour environment and gradients that develop. MTS are a more realistic model of the in vivo cellular morphology and environment and are becoming an increasingly popular in vitro model, replacing traditional monolayer culture. Imaging techniques such as transmission electron microscopy (TEM), scanning electron microscopy (SEM) and helium ion microscopy (HIM) were used to investigate differences in morphology and NS uptake in monolayer culture compared to MTS. After confirming NS uptake, the first SERS measurements revealing quantitative information on redox potential in MTS were performed.

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

Science.gov (United States)

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%).

One-Step Synthesis of Hollow Titanate (Sr/Ba Ceramic Fibers for Detoxification of Nerve Agents

Directory of Open Access Journals (Sweden)

Satya R. Agarwal

2012-01-01

Full Text Available Poly(vinyl pyrrolidone(PVP/(strontium/barium acetate/titanium isopropoxide composite fibers were prepared by electrospinning technique via sol-gel process. Diameters of fibers prepared by calcinations of PVP composite fibers were 80–140 nm (solid and 1.2-2.2 μm (hollow fibers prepared by core-shell method. These fibers were characterized using scanning electron microscope (SEM, X-ray diffraction (XRD, and transmission electron microscope (TEM analytical techniques. XRD results showed better crystalline nature of the materials when calcined at higher temperatures. SEM and TEM results clearly showed the formation of hollow submicrometer tubes. The surface area of the samples determined by BET analysis indicated that hollow fibers have ~20% higher surface area than solid fibers. The UV studies indicate better detoxification properties of the hollow fibers compared to solid fibers.

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

Directory of Open Access Journals (Sweden)

T. S. N. Sales

2017-05-01

Full Text Available 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%.

Study of the mechanisms involved in reactive silica

Energy Technology Data Exchange (ETDEWEB)

Boinski, Frederic [Univ Lille Nord of France, Ecole des Mines, 941, rue Charles Bourseul, BP 838, 59508 Douai (France); Khouchaf, Lahcen, E-mail: lahcenkho@live.fr [Univ Lille Nord of France, Ecole des Mines, 941, rue Charles Bourseul, BP 838, 59508 Douai (France); Tuilier, Marie-Helene [Universite de Haute-Alsace, LPMT (EA CNRS 4365), Universite de Haute Alsace, 61 rue Albert Camus, F-68093 Mulhouse (France)

2010-07-01

The microstructure of a heterogeneous SiO{sub 2} submitted to a depolymerisation process is studied using Transmission Electron Microscope (TEM), Environmental SEM (ESEM), and X-ray diffraction (XRD). With ESEM the formation of micro domain induced by the dissolution phenomena is shown. XRD shows the formation of a halo that is associated with the formation of amorphous phase. The parameters 'position and FWHM' of the halo, enabled us to show the evolution of the disorderly phase when the reaction progresses. The hypothesis of formation of nanoparticles with different structural states was confirmed by the TEM.

Friction stir processed Al–TiO₂ surface composites: Anodising behaviour and optical appearance

DEFF Research Database (Denmark)

Gudla, Visweswara Chakravarthy; Jensen, Flemming; Simar, Aude

2015-01-01

was investigated. Microstructural and morphological characterization was performed using scanning (SEM) and transmission electron microscopy (TEM), and X-ray diffraction (XRD). The surface appearance was analysed using an integrating sphere-spectrophotometer setup which measures the diffuse and total reflectance...

Microstructure study of AUC and UO2

International Nuclear Information System (INIS)

Pan Ying; Gao Dihua; Lu Huaichang

1992-01-01

The microstructures of AUC, UO 2 powder and pellets were investigated with metallo-scope, SEM, TEM, XRD, and image analyzer. The influence of the reduction conditions of AUC on the microstructures of UO 2 powder and pellet were studied

Laser cladding of Zr-based coating on AZ91D magnesium alloy for ...

Indian Academy of Sciences (India)

based coating made of Zr powder was fabricated on AZ91D magnesium alloy by laser cladding. The microstructure of the coating was characterized by XRD, SEM and TEM techniques. The wear resistance of the coating was evaluated under dry ...

Acetyl salicylic acid–ZnAl layered double hydroxide functional nanohybrid for skin care application

CSIR Research Space (South Africa)

Mosangi, Damodar

2016-10-01

Full Text Available In this study, a pharmaceutically active ingredient, acetyl salicylic acid (ASA), was intercalated into ZnAl layered double hydroxide (LDH). The LDH–ASA nanohybrid material was characterized by XRD, FTIR, SEM, ICP-MS, TEM and TGA. Successful...

Novel fabrication of silica nanotubes using multi-walled carbon ...

Indian Academy of Sciences (India)

Administrator

Abstract. Silica nanotubes were synthesized using multi-walled carbon nanotubes (MWCNTs) as template. The as-obtained samples were characterized by infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscope (FE–SEM) and photo-.

Synthesis of bio-inspired Ag–Au nanocomposite and its anti-biofilm ...

Indian Academy of Sciences (India)

Nanocomposite; biological method; anti-biofilm; SEM; TEM; XRD. 1. Introduction ... [13] and banana peel extract (BPE) [14] have been reported. ∗ ... gation at 10,000 rpm for 30 min and air-dried to obtain dry ... Further, 150 μl of ethanol.

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

Science.gov (United States)

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.

Palladium nanoparticles supported on layered hydroxide salts and their use in carbon-carbon coupling organic reactions

OpenAIRE

Martínez,Maby; Ocampo,Rogelio; Rios,Luz Amalia; Ramírez,Alfonso; Giraldo,Oscar

2011-01-01

Palladium nanoparticles supported on zinc hydroxide salts were prepared by intercalation of [PdCl6]2- and its further reduction with ethanol under reflux. All the materials were completely characterized by atomic absorption spectroscopy (AAS), X-ray diffraction (XRD), thermogravimetric/derivative thermogravimetric (TG/DTG) analyses, scanning electron microscopy (SEM), UV-Visible spectrometry and transmission electron microscopy (TEM). TEM analysis confirmed that the palladium nanoparticles we...

Rapid extra-/intracellular biosynthesis of gold nanoparticles by the fungus Penicillium sp.

Science.gov (United States)

Du, Liangwei; Xian, Liang; Feng, Jia-Xun

2011-03-01

In this work, the fungus Penicillium was used for rapid extra-/intracellular biosynthesis of gold nanoparticles. AuCl4 - ions reacted with the cell filtrate of Penicillium sp. resulting in extracellular biosynthesis of gold nanoparticles within 1 min. Intracellular biosynthesis of gold nanoparticles was obtained by incubating AuCl4 - solution with fungal biomass for 8 h. The gold nanoparticles were characterized by means of visual observation, UV-Vis absorption spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The extracellular nanoparticles exhibited maximum absorbance at 545 nm in UV-Vis spectroscopy. The XRD spectrum showed Bragg reflections corresponding to the gold nanocrystals. TEM exhibited the formed spherical gold nanoparticles in the size range from 30 to 50 nm with an average size of 45 nm. SEM and TEM revealed that the intracellular gold nanoparticles were well dispersed on the cell wall and within the cell, and they are mostly spherical in shape with an average diameter of 50 nm. The presence of gold was confirmed by EDX analysis.

Columnar structure of reactively sputtered aluminium nitride films

International Nuclear Information System (INIS)

Chen Chisan; Hwang Binghwai; Lu Hongyang; Hsu Tzuchien

2002-01-01

Columnar structure of thin aluminium nitride (AlN) films is examined by x-ray diffractometry (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The films were deposited on SiO 2 /Si(100) substrate using radiofrequency reactive sputtering method. Strong [0001] preferred orientation is observed by XRD and confirmed by selected area diffraction pattern of TEM. Columnar grains of ∼50-100 nm inclined at an angle of ∼10 deg. to the substrate normal are observed by SEM. As revealed by TEM, each columnar grain is composed of nano-grains of the order of 10 nm and no faceting is observed in the nano-grains and columns. The [0001] preferred orientation results as columnar grains are oriented at various azimuthal angles with their c-axes perpendicular to the substrate surface. A slight tilt of a few tenths of a degree between adjacent nano-grains within a column is also observed. The random azimuthal orientation of columnar grains and small tilt between nano-grains in the films are accommodated by the amorphous phase present in the grain boundaries

Fabrication of High Energy Density Tin/Carbon Anode Using Reduction Expansion Synthesis and Aerosol Through Plasma Techniques

Science.gov (United States)

2017-03-01

his assistance with the analysis of samples using the TEM, as well as teaching me the safe use of XRD and SEM. Special thanks also go out to Ryan Adams...from the energy and construct a greyscale image for display. Figure 19. Zeiss NEON 40 SEM. Setup of SEM. Left: SEM and movement of stage using...delithiation cycling,” J. Electrochem. Soc., vol. 161, no. 11, pp. 3019– 3024, Jun. 2014. [20] P. L. Walker, Chemistry and Physics of Carbon: A Series of

Synthesis of a hierarchically structured zeolite-templated carbon starting from fly ash-derived zeolite X

CSIR Research Space (South Africa)

Musyoka, Nicholas M

2014-05-01

Full Text Available A hierarchically structured zeolite derived from coal fly ash was used as a hard templating agent for the synthesis of a templated carbonaceous material. The samples were characterized using XRD, SEM, TEM, TGA, EDS and BET. The resulting carbon had...

Electrical and optical studies in polyaniline nanofibre–SnO 2 ...

Indian Academy of Sciences (India)

Polyaniline nanofibre–tin oxide (PAni-SnO2) nanocomposites are synthesized and mixed with polyvinyl alcohol (PVA) as stabilizer to cast free-standing films. Composite films are characterized by X-ray diffraction studies (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), ...

Synthesis, characterization and photocatalytic activity of WO3/TiO2 for NO removal under UV and visible light irradiation

NARCIS (Netherlands)

Luevano Hipolito, E.; Martínez-de la Cruz, A.; López-Cuellar, E.; Yu, Q.L.; Brouwers, H.J.H.

2014-01-01

Samples with different proportions WO3/TiO2 were prepared by co-precipitation method followed by a heat treatment. The samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS), and

Solid-State synthesis of POPD@AgNPs nanocomposites for electrochemical sensors

CSIR Research Space (South Africa)

Paulraj, P

2017-07-01

Full Text Available techniques. POPD and POPD@AgNPs were characterized using HR-TEM, FE-SEM, XRD, UV-Visible, FT-IR, Micro Raman spectroscopy and those results were confirmed their chemical purity, particle size, shape and its elemental compositions. Moreover, the DPV...

Synthesis of templated carbon from nanoclay and its zeolitic derivatives for hydrogen storage applications

CSIR Research Space (South Africa)

Musyoka, Nicholas M

2014-06-01

Full Text Available materials were thoroughly characterized using XRD, SEM, TGA, TEM, N2-BET and also tested for hydrogen storage capacity. The resulting templated carbons were found to be highly ordered and had mimicked the crystal morphology of the templating materials...

Effects of hydrothermal annealing on characteristics of CuInS{sub 2} thin films by SILAR method

Energy Technology Data Exchange (ETDEWEB)

Shi Yong, E-mail: sys-99@163.com [Key Laboratory of Industrial Ecology and Environmental Engineering and State Key Laboratory of Fine Chemical, School of Environmental Sciences and Technology, Dalian University of Technology, Dalian 116024 (China); Xue Fanghong [Key Laboratory of Industrial Ecology and Environmental Engineering and State Key Laboratory of Fine Chemical, School of Environmental Sciences and Technology, Dalian University of Technology, Dalian 116024 (China); Li Chunyan [School of Materials, Dalian University of Technology, Dalian 116024 (China); Zhao Qidong; Qu Zhenping; Li Xinyong [Key Laboratory of Industrial Ecology and Environmental Engineering and State Key Laboratory of Fine Chemical, School of Environmental Sciences and Technology, Dalian University of Technology, Dalian 116024 (China)

2012-07-15

CuInS{sub 2} thin films have been deposited by successive ionic layer absorption and reaction (SILAR) method, then annealed in a Na{sub 2}S solution (denoted as hydrothermal annealing) at 200 Degree-Sign C for different time. The effect of hydrothermal annealing on the properties of the films was studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and optical absorption spectroscopy. The XRD, TEM and SEM results indicate that well-crystallized CuInS{sub 2} films could be obtained after annealing in 0.1 mol/L Na{sub 2}S solution for 1.5 h. The annealed CuInS{sub 2} films were slightly S-rich and the direct band gap varied from 1.32 to 1.58 eV as the annealing time increased from 0.5 h to 2 h.

Sol-gel route of synthesis of nanoparticles of MgFe2O4 and XRD, FTIR and VSM study

International Nuclear Information System (INIS)

Pradeep, A.; Priyadharsini, P.; Chandrasekaran, G.

2008-01-01

Nanoparticles of MgFe 2 O 4 are synthesized using sol-gel autocombustion method. Structural studies are carried out using X-ray diffraction (XRD). The XRD pattern of MgFe 2 O 4 provides information about single-phase formation of spinel structure with cubic symmetry. The grain size and lattice constant are obtained using XRD data. The cation distribution is also proposed theoretically. The change in site preference of cations in nano-MgFe 2 O 4 is compared with its bulk counterpart. The structural morphology of the nanoparticles is studied using Scanning Electron Microscopy (SEM). Formation of spinel structure is conformed using Fourier transform infrared spectroscopy (FTIR), which also lends support for the cation distribution proposed using XRD data. The effect of nanoregime on parameters such as bond length, vibration frequency and force constant are discussed with the help of FTIR data. The M-H loop of MgFe 2 O 4 has been traced using the Vibrating Sample Magnetometer (VSM) and magnetic parameters such as saturation magnetization (M S ), coercivity (H C ) and retentivity (M R ) are obtained from VSM data

High-performance towards removal of toxic hexavalent chromium from aqueous solution using graphene oxide-alpha cyclodextrin-polypyrrole nanocomposites

CSIR Research Space (South Africa)

Chauke, VP

2015-07-01

Full Text Available toxic Cr(VI) from water. The prepared GO-aCD-PPY NCs were successfully characterised with AT-FTIR, FE-SEM, HR-TEM, BET and XRD techniques. Adsorption experiments were performed in batch mode to determine optimum conditions that include temperature, p...

Fabrication of mesoporous cerium dioxide films by cathodic electrodeposition.

Science.gov (United States)

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.

Morphology of Poly lactide/Polycaprolactone (PLA/PCL) Nano composite by Scanning Electron Microscopy (SEM)

International Nuclear Information System (INIS)

Siti Zulaiha Hairaldin; Wan Md Zin Wan Yunus; Norazowa Ibrahim

2011-01-01

In this study, Octadecylamine Modified Montmorillonites (ODAMMT) were used to prepare Poly lactide/ Polycaprolactone (PLA/ PCL) nano composites. PLA and PCL mix in 90:10 ratios, using an internal mixer by melt blending technique. The other sample was blend with Natrium Montmorillonite (NaMMT) and Octadecylamine Modified Montmorillonite (ODA-MMT) to produce PLA/ PCL-NaMMT and PLA/ PCL ODAMMT. To characterize the polymer nano composites, X-ray diffraction (XRD), FTIR and SEM analysis were conducted. Comparison of morphology were made up between PLA/ PCL, PLA/ PCL with presence of 7 % of Na-MMT and 7 % ODA-MMT respectively based on SEM micrograph by calculate the number-average diameter. (author)

A low-cost, environment-friendly and solvent-free route for synthesis of AgBr nanoparticles

Czech Academy of Sciences Publication Activity Database

Shahsavani, E.; Khalaji, A.D.; Feizi, N.; Das, D.; Matalobos, J.S.; Kučeráková, Monika; Dušek, Michal

2015-01-01

Roč. 82, Jun (2015), s. 18-25 ISSN 0749-6036 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : AgBr * nanoparticles * thiosemicarbazone * XRD * SEM * TEM Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.117, year: 2015

DNA-assisted synthesis of chitosan/ α -Fe 2 O 3 nanocomposites for ...

Indian Academy of Sciences (India)

The FDnanoparticles were prepared by co-precipitation method using DNA as the capping agent. The samples were characterizedby XRD, EDAX, SEM and TEM. The hematite nanoparticles that were prepared using DNA were compared withthe samples prepared using EDTA and CTAB as capping agents. The effect of ...

Substrate integrated Lead-Carbon hybrid ultracapacitor with flooded ...

Indian Academy of Sciences (India)

The electrode and silica-gel electrolyte materials are characterized by XRD, XPS, SEM, TEM, Rheometry, BET surface area, and FTIR spectroscopy in conjunction with electrochemistry. Electrochemical performance of SI-PbO2 and carbon electrodes is studied using cyclic voltammetry with constant-current charge and ...

Synthesis of Mn-doped CeO 2 nanorods and their application as ...

Indian Academy of Sciences (India)

Mn-doped CeO2 nanorods have been prepared from CeO2 particles through a facile compositehydroxide-mediated (CHM) approach. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The analysis from the X-ray photoelectron ...

Characterization of low alloy ferritic steel–Ni base alloy dissimilar metal weld interface by SPM techniques, SEM/EDS, TEM/EDS and SVET

Energy Technology Data Exchange (ETDEWEB)

Wang, Siyan; Ding, Jie; Ming, Hongliang; Zhang, Zhiming; Wang, Jianqiu, E-mail: wangjianqiu@imr.ac.cn

2015-02-15

The interface region of welded A508–Alloy 52 M is characterized by scanning probe microscope (SPM) techniques, scanning electron microscopy (SEM)/energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM)/Energy Dispersive Spectroscopy (EDS) and scanning vibrate electrode technique (SVET). The regions along the welded A508–Alloy 52 M interface can be categorized into two types according to their different microstructures. In the type-I interface region, A508 and Alloy 52 M are separated by the fusion boundary, while in the type-II interface region, A508 and Alloy 52 M are separated by a martensite zone. A508, martensite zone and grain boundaries in Alloy 52 M are ferromagnetic while the Alloy 52 M matrix is paramagnetic. The Volta potentials measured by scanning Kelvin probe force microscopy (SKPFM) of A508, martensite zone and Alloy 52 M follow the order: V{sub 52} {sub M} > V{sub A508} > V{sub martensite}. The corrosion behavior of A508–Alloy 52 M interface region is galvanic corrosion, in which Alloy 52 M is cathode while A508 is anode. The martensite dissolves faster than Alloy 52 M, but slower than A508 in the test solution. - Highlights: • The A508–Alloy 52 M interface regions can be categorized into two types. • The chromium depleted region is observed along the Alloy 52 M grain boundary. • The Alloy 52 M grain boundaries which are close to the interface are ferromagnetic. • Martensite zone has lower Volta potential but higher corrosion resistance than A508.

Low Temperature Ferromagnetism and Optical Properties of Fe Doped ZnO Nanoparticles Synthesized by Sol-Gel Method

Directory of Open Access Journals (Sweden)

B. Sathya

2017-06-01

Full Text Available In this present investigation, pure and Fe doped Zinc oxide nanoparticles were successfully synthesized by sol gel method.The structural and optical properties were examined by using X-ray diffraction (XRD, Scanning electron microscope (SEM, Transmission electron microscope (TEM, Ultraviolet spectroscopy and Photoluminescence (PL techniques.The structural characterization of XRD analysis confirmed the phase purity of the samples and crystallite size can be decreased with increasing doping concentrations.SEM image show that nanoparticles in spherical shape. The optical band gap calculated through UV-visible spectroscopy is found to be increasing from 3.48 to 3.57eV. TEM analysis depicted the crystallinity of nanoparticles prepared and chemical composition conformed the EDAX analysis. The PL spectra reveal that, Fe doped ZnO exhibit a decrease in intensity of the band edge emission peak while the intensity of the deep level emission peak increases.The enhancement of low temperature ferromagnetism in ZnO: Fe was achieved.

Synthesis Structural and Optical Properties Of (Co, Al) co-doped ZnO Nano Particles

Science.gov (United States)

Swapna, P.; Venkatramana Reddy, S.

2018-02-01

We prepared (Co, Al) co-doped ZnO nanostructures using the method chemical co-precipitation successfully, at room temperature using PEG (Poly ethylene glycol) as stabilizing agent. Samples are prepared with different concentrations by keeping aluminium at 5 mol percent constant and varying the concentration of cobalt from 1 to 5 mol percent. After the preparation all the samples are carefully subjected to characterizations such as XRD, SEM with EDS, TEM, PL and UV-VIS-NIR. XRD pattern shows that all the samples possess hexagonal wurtzite crystal structure having no secondary phases pertaining to Al or cobalt, which shows successful dissolution of the dopents. TEM results shows the accurate size of particles and is confirmed the XRD data. SEM images of all the samples shows that particles are in nearly spherical shape, EDS spectrum reveals that incorporation of cobalt and aluminum in host lattice. PL spectrum shows that all the samples containing two prominent peaks centered at 420 nm and 446 nm. UV-VIS-NIR spectra has shown three absorptions peaks in the range of wavelength 550 nm to 700 nm, which are ascribed as typical d-d transitions of cobalt ions.

Effect of capping agent on the morphology, size and optical properties of In{sub 2}O{sub 3} nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Latha, Ch. Kanchana; Aparna, Y. [Department of Physics, Jawaharlal Nehru Technological University Hyderabad (JNTUH), College of Engineering Hyderabad (CEH), Telangana (India); Raghasudha, Mucherla; Veerasomaiah, P., E-mail: raghasudha_m@yahoo.co.in [Department of Chemistry, University College of Science, Osmania University, Hyderabad, Telangana (India); Ramchander, M. [Department of Bio Chemistry, Mahatma Gandhi University, Nalgonda, Telangana (India); Ravinder, D. [Department of Physics, Osmania University, Hyderabad, Telangana (India); Jaipal, K. [Inorganic & Physical Chemistry Division, Indian Institute of Chemical Technology (IICT), Hyderabad, Telangana (India); Shridhar, D. [Department of Physics, Khairatabad Government Degree College, Hyderabad, Telangana (India)

2017-01-15

The Indium Oxide (In{sub 2}O{sub 3}) nanoparticles were synthesized through Acacia gum mediated method with the surfactants CTAB (Cetyl Trimethyl Ammonium Bromide) and SDBS (Sodium Docecyl Benzene Sulfonate). The characterization of the synthesized In{sub 2}O{sub 3} nanoparticles was carried out by XRD, FTIR, RAMAN, TEM, SEM, EDAX, UV-Vis and PL techniques. TG-DTA analysis was performed to know the calcination temperature of In{sub 2}O{sub 3} nanoparticles. XRD analysis confirmed the crystalline nature of the synthesized In{sub 2}O{sub 3} nanoparticles. The morphology and chemical composition were characterized by TEM, SEM and EDAX respectively. It was observed that morphology and size of synthesized nanoparticles measured by TEM and SEM analysis were dependent on the type of capping agent (surfactant) used. Raman and UV-Vis spectral analysis confirmed that the band gap value of CTAB capped In{sub 2}O{sub 3} particles were larger than the SDBS capped In{sub 2}O{sub 3} particles. FTIR analysis indicated that the bands were stretched in In{sub 2}O{sub 3} particles capped by SDBS than by CTAB. From the photoluminescence studies (PL technique), a blue shift in the emission peaks of CTAB and SDBS capped In{sub 2}O{sub 3} particles was observed that indicates larger optical band gap than the bulk. (author)

Green synthesis and characterization of graphene nanosheets

Energy Technology Data Exchange (ETDEWEB)

Tavakoli, Farnosh [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Badiei, Alireza [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Mohandes, Fatemeh [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of)

2015-03-15

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.

Green synthesis and characterization of graphene nanosheets

International Nuclear Information System (INIS)

Tavakoli, Farnosh; Salavati-Niasari, Masoud; Badiei, Alireza; Mohandes, Fatemeh

2015-01-01

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products

Structural, magnetic and electronic structure properties of Co doped ZnO nanoparticles

International Nuclear Information System (INIS)

Kumar, Shalendra; Song, T.K.; Gautam, Sanjeev; Chae, K.H.; Kim, S.S.; Jang, K.W.

2015-01-01

Highlights: • XRD and HR-TEM results show the single phase nature of Co doped ZnO nanoparticles. • XMCD and dc magnetization results indicate the RT-FM in Co doped ZnO nanoparticles. • Co L 3,2 NEXAFS spectra infer that Co ions are in 2+ valence state. • O K edge NEXAFS spectra show that O vacancy increases with Co doping in ZnO. - Abstract: We reported structural, magnetic and electronic structure studies of Co doped ZnO nanoparticles. Doping of Co ions in ZnO host matrix has been studied and confirmed using various methods; such as X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersed X-ray (EDX), high resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, magnetic hysteresis loop measurements and X-ray magnetic circular dichroism (XMCD). From the XRD and HR-TEM results, it is observed that Co doped ZnO nanoparticles have single phase nature with wurtzite structure and exclude the possibility of secondary phase formation. FE-SEM and TEM micrographs show that pure and Co doped nanoparticles are nearly spherical in shape. O K edge NEXAFS spectra indicate that O vacancies increase with Co doping. The Co L 3,2 edge NEXAFS spectra revealed that Co ions are in 2+ valence state. DC magnetization hysteresis loops and XMCD results clearly showed the intrinsic origin of temperature ferromagnetism in Co doped ZnO nanoparticles

Synthesis and characterization of nanocomposites based on poly(3 ...

Indian Academy of Sciences (India)

The structure and morphologies of LNMO/P3HT- g -CNTs nanocomposites have also been performed by SEM, XRD and TEM. The electrochemical performance of LNMO/P3HT- g -CNTs nanocomposites as cathode materials of lithium-ion batteries were investigated by cyclic voltammetry and electrochemical impedance ...

A Kinetic Insight into the Activation of n -Octane with Alkaline-Earth ...

African Journals Online (AJOL)

Alkaline-earth metal hydroxyapatites are prepared by the co-precipitation method and characterized using XRD, ICP,NH3-TPD, SEM-EDX, TEM and N2 physisorption analysis. The metal present in the hydroxyapatite influences the acidity of the catalyst. Oxidative dehydrogenation reactions carried out in a continuous flow ...

PREPARATION AND CHARACTERIZATION OF SOY PROTEIN ISOLATE(SPI)/MONTMORILLONITE(MMT) BIONANOCOMPOSITES

Institute of Scientific and Technical Information of China (English)

傅强

2009-01-01

The bionanocomposites of soy protein isolate(SPI)/montmorillonite(MMT) have been prepared successfully via simple melt mixing,in which MMT was used as nanofiller and glycerol was used as plasticizer.Their structures and properties were characterized with X-ray diffraction(XRD),differential scanning calorimetry(DSC),scanning electron microscopy(SEM),thermogravimetric analysis and tensile testing.XRD、TEM and SEM results indicated that the MMT layers could be easily intercalated by the SPI matrix even by si...

TEM microstructural analysis of creep deformed CM186LC single crystal Ni-base superalloy

Energy Technology Data Exchange (ETDEWEB)

Dubiel, B.; Czyrska-Filemonowicz, A. [AGH Univ. of Science and Technology, Krakow (Poland); Blackler, M. [Howmet Ltd., Exeter (United Kingdom); Barnard, P.M. [ALSTOM Power Turbo-Systems Technology Centre, Rugby (United Kingdom)

2006-07-01

The nickel based single crystal superalloy CM186LC was extensively investigated as a potential low cost material for industrial gas turbine vanes within the COST522 programme. The alloy exhibits inhomogeneous structure consisting of dendritic regions and eutectic colonies. In the present work attention is focused on microstructural changes observed in single crystal CM186LC following creep deformation at 750 C. Creep tests were conducted at 750 C with an applied stress of 560 or 675 MPa for up to 11440 hours. The microstructure o ruptured and terminated specimens was investigated by scanning (SEM) and transmission (TEM) electron microscopy. TEM analysis revealed the microstructural changes in the CM186LC at primary and secondary creep as well as after creep rupture. (orig.)

Combined XRD and XAS

International Nuclear Information System (INIS)

Ehrlich, S.N.; Hanson, J.C.; Lopez Camara, A.; Barrio, L.; Estrella, M.; Zhou, G.; Si, R.; Khalid, S.; Wang, Q.

2011-01-01

X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS) are complementary techniques for investigating the structure of materials. XRD probes long range order and XAFS probes short range order. We have combined the two techniques at one synchrotron beamline, X18A at the NSLS, allowing samples to be studied in a single experiment. This beamline will allow for coordinated measurements of local and long range structural changes in chemical transformations and phase transitions using both techniques.

Characterisation of rust surfaces formed on mild steel exposed to marine atmospheres using XRD and SEM/Micro-Raman techniques

International Nuclear Information System (INIS)

Fuente, D. de la; Alcántara, J.; Chico, B.; Díaz, I.; Jiménez, J.A.; Morcillo, M.

2016-01-01

Highlights: • SEM/Micro-Raman is very useful for characterizing rust phases morphologies. • SEM/Micro-Raman enables unequivocal rust phases identification. • γ-FeOOH basically presents two types of morphologies: globular and laminar. • Fe 3 O 4 presents two morphologies: flat patches and black doughnut-type formations. • β-FeOOH presents highly porous morphologies comprised by fine prismatic crystals. - Abstract: The exposure of mild steel to marine atmospheres gives rise to the formation of various corrosion products, mainly lepidocrocite, goethite, magnetite and akaganeite. In this study, Grazing Incidence X-Ray Diffraction, Micro-X-Ray Diffraction and Scanning Electron Microscopy/Micro-Raman are used to characterise rust layer surfaces and to identify the principal component rust phases and their morphology. The main conclusion reached is that lepidocrocite is preferentially located on the outermost surface while magnetite and akaganeite form mostly close to base steel. The Scanning Electron Microscopy/Micro-Raman technique has been very useful for characterising (identifying) the wide variety of morphologies presented by the rust phases.

SEM-EDS and XRD study of a NiCrAlU alloy at temperatures from 800 celsius degree to 1300 celsius degree

International Nuclear Information System (INIS)

Al-Badairy, H.; Fox, P.

2004-01-01

Full text.The oxidation behaviour of a 74.5wt%Ni, 20wt%Cr, 5wt%Al and 0.5wt%U alloy was examined using Scanning Electron Microscopy with X-ray Energy Dispersive Spectroscopy (SEM-EDS) and X-ray Diffractometry (XRD). The oxidation temperature ranged from 800 to 1300 celsius degree in laboratory air with oxidation times up to 120h. Analysis showed that during short term oxidation (40h) at the lower temperatures there was evidence of the formation of Cr, Ni and Al oxides. With increasing oxidation time, the Cr-rich oxide became predominant with the presence of islands of Ni-rich oxide, but no uranium was detected at the outermost layer of the scale. The scale was of flat topography with spallation occurring after 40h oxidation at 900 celsius degree and increasing with increasing temperature and time. Cross-sectional investigations indicated the presence of an internal oxidation zone comprising an Al-rich oxide beneath the outer Cr-rich scale with significant amounts of uranium. The depth of this zone varied from 1 micron to 60 microns and increased with increasing the oxidation temperature and time. At higher temperatures (above 1000 celsius degree), the internal oxidation zone ceased to grow due to the formation of a complete layer of alumina which protected the metal substrate from further degradation. The constituents of the scales formed reflect the selective oxidation of Cr and Al as a result of the higher reactivity of aluminium and chromium compared to nickel and the greater stability of Al 2 O 3 and Cr 2 O 3 compared to NiO. This study showed that Al-rich oxide was not the predominant protective oxide and the presence of uranium was restricted to the grain boundaries of the metal substrate and to within the internal oxidation zone. It appeared that the Cr-rich scale formed on this alloy does not to convolute. This may be due to the influence of uranium since Cr-rich scales forming on NiCrAl containing no uranium are often convoluted

Investigations into the Surface Strain/Stress State in a Single-Crystal Superalloy via XRD Characterization

Directory of Open Access Journals (Sweden)

Haodong Duan

2018-05-01

Full Text Available The present study was aimed at determining the surface strain/stress state in an Ni-based single-crystal (SC superalloy that was subjected to two different cooling rates from solid solution temperature through using the X-ray diffraction (XRD method. The normal stresses σ 11 s and σ 22 s were determined, then the Von Mises stresses ( σ V M s were derived from them. Field emission gun scanning electron microscope (FEG-SEM and transmission electron microscope (TEM micrographs were taken to illustrate the strain/stress state change. The precipitation of the secondary γ′ phases in the γ phase and the formation of the dislocation in the interphase upon a slower cooling rate caused the γ phase lattice distortion to increase, so a larger σ V M s of the γ phase was realized in comparison to the faster cooling sample. For both of the two cooling modes, we found that the σ V M s of the γ′ phase increased due to the growth of the γ′ phase during the aging process. Also, the aging process led to pronouncedly anisotropic lattice mismatches in the {331} and {004} planes. In addition, the surface strain/stress states of a cylinder sample and a tetragonal sample were also studied using a faster cooling rate, and σ 11 s and σ 22 s were analyzed to explain the influence of the shape factor on the stress anisotropy in the [001] and [ 1 1 ¯ 0 ] orientations. The strain in the [001] orientation of the γ phase is more sensitive to the shape change.

FIB/SEM technology and high-throughput 3D reconstruction of dendritic spines and synapses in GFP-labeled adult-generated neurons

Directory of Open Access Journals (Sweden)

Carles eBosch

2015-05-01

Full Text Available The fine analysis of synaptic contacts is usually performed using transmission electron microscopy (TEM and its combination with neuronal labeling techniques. However, the complex 3D architecture of neuronal samples calls for their reconstruction from serial sections. Here we show that focused ion beam/scanning electron microscopy (FIB/SEM allows efficient, complete, and automatic 3D reconstruction of identified dendrites, including their spines and synapses, from GFP/DAB-labeled neurons, with a resolution comparable to that of TEM. We applied this technology to analyze the synaptogenesis of labeled adult-generated granule cells (GCs in mice. 3D reconstruction of spines in GCs aged 3–4 and 8–9 weeks revealed two different stages of spine development and unexpected features of synapse formation, including vacant and branched spines and presynaptic terminals establishing synapses with up to 10 spines. Given the reliability, efficiency, and high resolution of FIB/SEM technology and the wide use of DAB in conventional EM, we consider FIB/SEM fundamental for the detailed characterization of identified synaptic contacts in neurons in a high-throughput manner.

Preparation of a novel breviscapine-loaded halloysite nanotubes complex for controlled release of breviscapine

Science.gov (United States)

Gao, Min; Lu, Liqian; Wang, Xiaoyue; Lin, Houke; Zhou, Qingsong

2017-11-01

For sustain the release rate and prolong half-life of breviscapine in vivo, the breviscapine-loaded halloysite nanotubes complex was prepared. The breviscapine was encapsulated into halloysite nanotubes (HNTs) using a vacuum process. The complex were investigated by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electron microscope (TEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy(FT-IR). The formation of breviscapine-loaded HNTs complex was proved by the test results of SEM, DSC, TEM and IR analysise. The results confirmed that breviscapine was successfully loaded in the halloysite nanotubes. Additionally, the in vitro drug release of breviscapine from breviscapine-loaded HNTs complex was investigated, the result indicated this complex has apparent sustained-release effect.

Characterization of synthesized polyurethane/montmorillonite nanocomposites foams

International Nuclear Information System (INIS)

Ansari, Farahnaz; Njuguna, James; Sachse, Sophia; Kavosh, Masoud; Michalowski, S; Pielichowski, Krzysztof

2014-01-01

Nanophased hybrid composites based on polyurethane/montmorillonite (PU/MMT) have been fabricated. The nanocomposite which was formed by the addition of a polyol premix with 4,4'-diphenylmethane diisocyanate to obtain nanophased polyurethane foams which were then used for fabrication of nanocomposite panels has been shown to have raised strength, stiffness and thermal insulation properties. The nanophased polyurethane foam was characterized by means of scanning electron microscope (SEM), transmission electron microscope (TEM) measurements and X-ray diffraction (XRD). TEM and SEM analysis indicated that nanophased particles are dispersed homogeneously in the polyurethane matrix on the nanometer scale indicating that PU/MMT is an intercalated nanocomposite with a 2-3 nm nanolayer thickness

Electrospun polyacrylonitrile nanofibers loaded with silver nanoparticles by silver mirror reaction

International Nuclear Information System (INIS)

Shi, Yongzheng; Li, Yajing; Zhang, Jianfeng; Yu, Zhongzhen; Yang, Dongzhi

2015-01-01

The silver mirror reaction (SMR) method was selected in this paper to modify electrospun polyacrylonitrile (PAN) nanofibers, and these nanofibers loaded with silver nanoparticles showed excellent antibacterial properties. PAN nanofibers were first pretreated in AgNO 3 aqueous solution before the SMR process so that the silver nanoparticles were distributed evenly on the outer surface of the nanofibers. The final PAN nanofibers were characterized by scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), transmission electron microscopy (TEM), TEM-selected area electron diffraction (SAED), X-ray diffraction (XRD) and thermogravimetric analysis (TGA). SEM, TEM micrographs and SAED patterns confirmed homogeneous dispersion of the silver nanoparticles which were composed of monocrystals with diameters 20–30 nm. EDS and XRD results showed that these monocrystals tended to form face-centered cubic single silver. TGA test indicated that the nanoparticles loaded on the nanofibers reached above 50 wt.%. This material was also evaluated by the viable cell-counting method. The results indicated that PAN nanofibers loaded with silver nanoparticles exhibited excellent antimicrobial activities against gram-negative Escherichia coli (E. coli), gram-positive Staphylococcus aureus (S. aureus) and the fungus Monilia albicans. Thus, this material had many potential applications in biomedical fields. - Highlights: • Silver mirror reaction was used to prepare nanofibers loaded with silver nanoparticles. • The SAED patterns demonstrated the monocrystallinity of silver nanocrystals. • The XRD results showed nanoparticles tended to be face-centered cubic single silver. • The material showed excellent antimicrobial activities against bacteria and fungi

Developing 3D SEM in a broad biological context

Science.gov (United States)

Kremer, A; Lippens, S; Bartunkova, S; Asselbergh, B; Blanpain, C; Fendrych, M; Goossens, A; Holt, M; Janssens, S; Krols, M; Larsimont, J-C; Mc Guire, C; Nowack, MK; Saelens, X; Schertel, A; Schepens, B; Slezak, M; Timmerman, V; Theunis, C; Van Brempt, R; Visser, Y; GuÉRin, CJ

2015-01-01

When electron microscopy (EM) was introduced in the 1930s it gave scientists their first look into the nanoworld of cells. Over the last 80 years EM has vastly increased our understanding of the complex cellular structures that underlie the diverse functions that cells need to maintain life. One drawback that has been difficult to overcome was the inherent lack of volume information, mainly due to the limit on the thickness of sections that could be viewed in a transmission electron microscope (TEM). For many years scientists struggled to achieve three-dimensional (3D) EM using serial section reconstructions, TEM tomography, and scanning EM (SEM) techniques such as freeze-fracture. Although each technique yielded some special information, they required a significant amount of time and specialist expertise to obtain even a very small 3D EM dataset. Almost 20 years ago scientists began to exploit SEMs to image blocks of embedded tissues and perform serial sectioning of these tissues inside the SEM chamber. Using first focused ion beams (FIB) and subsequently robotic ultramicrotomes (serial block-face, SBF-SEM) microscopists were able to collect large volumes of 3D EM information at resolutions that could address many important biological questions, and do so in an efficient manner. We present here some examples of 3D EM taken from the many diverse specimens that have been imaged in our core facility. We propose that the next major step forward will be to efficiently correlate functional information obtained using light microscopy (LM) with 3D EM datasets to more completely investigate the important links between cell structures and their functions. Lay Description Life happens in three dimensions. For many years, first light, and then EM struggled to image the smallest parts of cells in 3D. With recent advances in technology and corresponding improvements in computing, scientists can now see the 3D world of the cell at the nanoscale. In this paper we present the

Synthesis of MoS 2 Inorganic Fullerene-like Nanoparticles by a ...

African Journals Online (AJOL)

MoS2 nanoparticles with fullerene-like structure (IF-MoS2) were successfully obtained at heating temperature higher than 840 °C by a chemical vapour deposition method usingMoO3 and sulfur powders as raw materials. The synthesized samples were characterized by XRD, SEM, TEM, EDX and Raman spectrometry, ...

Asian conference on x-rays and related techniques in research and industry. Proceedings

International Nuclear Information System (INIS)

1996-01-01

This proceedings compile the paper presented at the conference. The papers for presentation are from wide spectrum stressing the interdisciplinary nature of the conference i.e. x-ray fluorescence spectrometry (XRF), x-ray diffraction (XRD), TEM, scanning electron microscope (SEM), energy dispersive x-ray (EDX), auger electron microscopy, electron back scatter diffraction (EBSD)

Nonlinear entropy transfer in ETG-TEM turbulence via TEM driven zonal flows

International Nuclear Information System (INIS)

Asahi, Yuuichi; Tsutsui, Hiroaki; Tsuji-Iio, Shunji; Ishizawa, Akihiro; Sugama, Hideo; Watanabe, Tomohiko

2015-01-01

Nonlinear interplay of the electron temperature gradient (ETG) modes and the trapped electron modes (TEMs) was investigated by means of gyrokinetic simulation. Focusing on the situation where both TEMs and ETG modes are linearly unstable, the effects of TEM-driven zonal flows on ETG turbulence were examined by means of entropy transfer analysis. In a statistically steady turbulence where the TEM driven zonal flows are dominant, it turned out that the zonal flows meditate the entropy transfer of the ETG modes from the low to high radial wavenumber regions. The successive entropy transfer broadens the potential fluctuation spectrum in the radial wavenumber direction. In contrast, in the situation where ETG modes are unstable but TEMs are stable, the pure ETG turbulence does not produce strong zonal flows, leading to a rather narrow spectrum in the radial wavenumber space and a higher transport level. (author)

Preparation, characterization and catalytic effects of copper oxalate nanocrystals

International Nuclear Information System (INIS)

Singh, Gurdip; Kapoor, Inder Pal Singh; Dubey, Reena; Srivastava, Pratibha

2012-01-01

Graphical abstract: Prepared copper oxalate nanocrystals were characterized by FE-SEM and bright field TEM micrographs. Its catalytic activity was evaluated on the thermal decomposition of ammonium perchlorate using TG and TG-DSC techniques. Highlights: ► Preparation of nanocrystals (∼9.0 nm) of copper oxalate using Cu(NO 3 ) 2 ·2H 2 O, oxalic acid and acetone under thermal conditions. ► Method is simple and novel. ► Characterization using XRD, SEM, TEM, HRTEM and ED pattern. ► Catalytic activity of copper oxalate nanocrystals on AP thermal decomposition using thermal techniques (TG, TG-DSC and ignition delay). ► Kinetics of thermal decomposition of AP + CONs using isoconversional and model fitting kinetic approaches. - Abstract: Recent work has described the preparation and characterization of copper oxalate nanocrystals (CONs). It was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and electron diffraction pattern (ED). The catalytic activity of CONs on the thermal decomposition of ammonium perchlorate (AP) and composite solid propellants (CSPs) has been done by thermogravimetry (TG), differential scanning calorimetry (DSC) and ignition delay measurements. Burning rate of CSPs was also found to be enhanced in presence of copper oxalate nanocrystals. Kinetics of thermal decomposition of AP with and without CONs has also been investigated. The model free (isoconversional) and model-fitting kinetic approaches have been applied to data for isothermal TG decomposition.

Preparation and characterization of the nanoparticle and nanocomposite by gamma irradiation

International Nuclear Information System (INIS)

Lee, K.P.; Choi, S.H.

2002-01-01

Complete text of publication follows. Nanometer metal particle-organic polymer composites have attracted considerable interests in recent years. These composites not only combine the advantageous properties of metals and polymers but also exhibit many new characters that single-phase materials do not have. They have a wide range of applications including electromagnetic inferences shielding, heat conduction, discharge static electricity, conversion of mechanical to electrical signals, and like. In order to obtain nanocomposite, silver nanoparticle was prepared by γ-irradiation. The obtained Ag nanoparticle was characterized by UV, FT-IR, XRD, SEM, TEM, and etc. The ethylacetate-Ag nanocomposite was prepared by emulsion polymerization. The obtained nanocomposites were characterized by SEM, XRD, and thermal (TGA/DSC) analysis. Furthermore, the CdS nanocomposite was prepared using CdSO 4 and Na 2 SO 4 by γ-irradiation method. The ethylacetate-CdS nanocomposite was also prepared by emulsion polymerization, and characterized by SEM, XRD, and thermal (TGA/DSC) analysis. The application of such prepared metal particle-organic polymer composites in the field of anti-bacterial film, semiconductor film, and fluorescence film may be of interest

Distinction between amorphous and healed planar deformation features in shocked quartz using composite color scanning electron microscope cathodoluminescence (SEM-CL) imaging

Science.gov (United States)

Hamers, Maartje F.; Pennock, Gill M.; Herwegh, Marco; Drury, Martyn R.

2016-10-01

Planar deformation features (PDFs) in quartz are one of the most reliable and most widely used forms of evidence for hypervelocity impact. PDFs can be identified in scanning electron microscope cathodoluminescence (SEM-CL) images, but not all PDFs show the same CL behavior: there are nonluminescent and red luminescent PDFs. This study aims to explain the origin of the different CL emissions in PDFs. Focused ion beam (FIB) thin foils were prepared of specific sample locations selected in composite color SEM-CL images and were analyzed in a transmission electron microscope (TEM). The FIB preparation technique allowed a direct, often one-to-one correlation between the CL images and the defect structure observed in TEM. This correlation shows that composite color SEM-CL imaging allows distinction between amorphous PDFs on one hand and healed PDFs and basal Brazil twins on the other: nonluminescent PDFs are amorphous, while healed PDFs and basal Brazil twins are red luminescent, with a dominant emission peak at 650 nm. We suggest that the red luminescence is the result of preferential beam damage along dislocations, fluid inclusions, and twin boundaries. Furthermore, a high-pressure phase (possibly stishovite) in PDFs can be detected in color SEM-CL images by its blue luminescence.

Studies the alterations of biochemical and mineral contents in bone tissue of mus musculus due to aluminum toxicity and the protective action of desferrioxamine and deferiprone by FTIR, ICP-OES, SEM and XRD techniques.

Science.gov (United States)

Sivakumar, S; Khatiwada, Chandra Prasad; Sivasubramanian, J

2014-05-21

The present study has attempt to analyze the changes in the biochemical and mineral contents of aluminum intoxicated bone and determine the protective action of desferrioxamine (DFO) and deferiprone (DFP) by using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), inductively coupled plasma optical emission spectroscopy (ICP-OES), and scanning electron microscopy (SEM) techniques for four groups of animals such as control (Group I), aluminum intoxicated (Group II), Al+DFP (Group III) and Al+DFO+DFP (Group IV) treated groups respectively. The FTIR spectra of the aluminum intoxicated bone showed significant alteration in the biochemical constituents. The bands ratio at I1400/I877 significantly decreased from control to aluminum, but enhanced it by Al+DFP to Al+DFO+DFP treated bone tissue for treatments of 16 weeks. This result suggests that DFO and DFP are the carbonate inhibitor, recovered from chronic growth of bone diseases and pathologies. The alteration of proteins profile indicated by Amide I and Amide II, where peak area values decreased from control to aluminum respectively, but enhanced by treated with DFP (p.o.) and DFO+DFP (i.p.) respectively. The XRD analysis showed a decrease in crystallinity due to aluminum toxicity. Further, the Ca, Mg, and P contents of the aluminum exposed bone were less than those of the control group, and enhanced by treatments with DFO and DFP. The concentrations of trace elements were found by ICP-OES. Therefore, present study suggests that due to aluminum toxicity severe loss of bone minerals, decrease in the biochemical constituents and changes in the surface morphology. Copyright © 2014 Elsevier B.V. All rights reserved.

Direct synthesis and structure characterization of ultrafine CeO2 nanoparticles

International Nuclear Information System (INIS)

Hu Chenguo; Zhang Zuwei; Liu Hong; Gao Puxian; Wang Zhonglin

2006-01-01

A new method to directly synthesize single-crystalline CeO 2 nanoparticles has been developed. The advantages of the method are rapid synthesis, at normal atmosphere, 100% productive ratio and low cost, with a great potential for scale-up. X-ray diffraction (XRD) spectra showed unusual peak width versus particle size, compared with Scherrer equation predictions. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), electron diffraction and ultraviolet (UV) absorption were used to examine the particle size and microstructure to find out the cause. As a result, ultrafine particles with a size less than 6 nm were found to be self-assembled into a 'coherent interface', so that a large group of particles behave like a large single particle in XRD

Sol-gel synthesis of 8 nm magnetite (Fe 3O 4) nanoparticles and their magnetic properties

KAUST Repository

Lemine, O. M.; Omri, Karim; Zhang, Bei; El Mir, Lassaad; Sajieddine, Mohammed; Alyamani, Ahmed Y.; Bououdina, M.

2012-01-01

Magnetite (Fe 3O 4) nanoparticles were successfully synthesized by a sol-gel method. The obtained nanoparticles were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive analysis by X-ray (EDAX), transmission electron microscopy (TEM), superconducting quantum interference device (SQUID) and Mössbauer spectrometry. XRD and Mössbauer measurements indicate that the obtained nanoparticles are single phase. TEM analysis shows the presence of spherical nanoparticles with homogeneous size distribution of about 8 nm. Room temperature ferromagnetics behavior was confirmed by SQUID measurements. The mechanism of nanoparticles formation and the comparison with recent results are discussed. Finally, the synthesized nanoparticles present a potential candidate for hyperthermia application given their saturation magnetization. © 2012 Elsevier Ltd. All rights reserved.

Sol-gel synthesis of 8 nm magnetite (Fe 3O 4) nanoparticles and their magnetic properties

KAUST Repository

Lemine, O. M.

2012-10-01

Magnetite (Fe 3O 4) nanoparticles were successfully synthesized by a sol-gel method. The obtained nanoparticles were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive analysis by X-ray (EDAX), transmission electron microscopy (TEM), superconducting quantum interference device (SQUID) and Mössbauer spectrometry. XRD and Mössbauer measurements indicate that the obtained nanoparticles are single phase. TEM analysis shows the presence of spherical nanoparticles with homogeneous size distribution of about 8 nm. Room temperature ferromagnetics behavior was confirmed by SQUID measurements. The mechanism of nanoparticles formation and the comparison with recent results are discussed. Finally, the synthesized nanoparticles present a potential candidate for hyperthermia application given their saturation magnetization. © 2012 Elsevier Ltd. All rights reserved.

Decoration of Multi-walled Carbon Nanotubes by Metal ...

African Journals Online (AJOL)

The powder patterns of the as-prepared and acid treated MWCNTs are shown by the XRD spectra. The TEM results show the microstructure of the multi-walled carbon nanotubes well decorated with metal nanoparticles (Cu, Fe, Ni) and metal oxides (CuO, Fe2O3, NiO), while the SEM show the surface morphology.

Exploration of shallow subsurface resistivity structure using a portable TEM system: TEM-FAST prosystem; Kan`igata TEM ho sochi TEM-FAST prosystem ni yoru senbu hiteiko chosa

Energy Technology Data Exchange (ETDEWEB)

Miura, Y; Kumekawa, Y; Takasugi, S [GERD Geothermal Energy Research and Development Co. Ltd., Tokyo (Japan)

1997-05-27

Discussions were given on effectiveness of the TEM-FAST ProSystem which is a portable TEM system developed recently for use in exploration of shallow subsurface resistivity. The system consists of a loop type antenna, the TEM-FAST as the main equipment, and a host computer, the host computer controlling the entire system. The system acquires transient response data in secondary induced magnetic fields lasting 4 {mu} sec to 1 m sec. The number of data is 5490 stacks in one measurement, and the data acquisition time is about three minutes. Measurements were carried out by using the TEM-FAST in the vicinity of a well, whose results were compared with those of electric logging, and discussions were given on them. Although the electric logging results had no data available for depths shallower than 35 m, the measurement results from the TEM-FAST were found highly harmonious with those of the electric logging. In addition, there were transmission and telephone lines in locations about 10 m away from the well during the measurement, but extremely high data quality was discovered. 6 refs., 7 figs., 1 tab.

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

Science.gov (United States)

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

2018-01-01

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

Structural, optical, and magnetic properties of Mn and Fe-doped Co3O4 nanoparticles

Directory of Open Access Journals (Sweden)

C. Stella

2015-08-01

Full Text Available Mn and Fe-doped Co3O4 nanoparticles were prepared by a simple precipitation method. The synthesized particles were characterized by X-ray diffraction (XRD, scanning electron microscope (SEM, transmission electron microscope (TEM, UV-Vis absorption spectroscopy, Fourier transform infrared spectroscopy (FTIR, Raman spectroscopy, and vibrating sample magnetometer (VSM techniques. XRD analysis showed the cubic structure of Co3O4. SEM and TEM images confirmed the formation of interconnected nanoparticles. Mn and Fe-doped Co3O4 showed broad absorption in the visible region compared to undoped sample and the band gap values are red shifted. Five Raman active modes were observed from the Raman spectra. FTIR spectra confirmed the spinel structure of Co3O4 and the doping of Mn and Fe shifts the vibrational modes to lower wave number region. The magnetic measurements confirmed that Fe-doped Co3O4 shows a little ferromagnetic behavior compared to undoped and Mn-doped Co3O4, which could be related to the uncompensated surface spins and the finite size effects.

Graphite to Graphene via Graphene Oxide: An Overview on Synthesis, Properties, and Applications

Science.gov (United States)

Hansora, D. P.; Shimpi, N. G.; Mishra, S.

2015-12-01

This work represents a state-of-the-art technique developed for the preparation of graphene from graphite-metal electrodes by the arc-discharge method carried out in a continuous flow of water. Because of continuous arcing of graphite-metal electrodes, the graphene sheets were observed in water with uniformity and little damage. These nanosheets were subjected to various purification steps such as acid treatment, oxidation, water washing, centrifugation, and drying. The pure graphene sheets were analyzed using Raman spectrophotometry, x-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), and tunneling electron microscopy (TEM). Peaks of Raman spectra were recorded at (1300-1400 cm-1) and (1500-1600 cm-1) for weak D-band and strong G-band, respectively. The XRD pattern showed 85.6% crystallinity of pure graphite, whereas pure graphene was 66.4% crystalline. TEM and FE-SEM micrographs revealed that graphene sheets were overlapped to each other and layer-by-layer formation was also observed. Beside this research work, we also reviewed recent developments of graphene and related nanomaterials along with their preparations, properties, functionalizations, and potential applications.

Titanium Dioxide Supported on Different Porous Materials as Photocatalyst for the Degradation of Methyl Green in Wastewaters

Directory of Open Access Journals (Sweden)

Haithem Bel Hadjltaief

2015-01-01

Full Text Available TiO2 nanoparticles were immobilized on two porous materials used as catalyst supports, namely, activated carbon (AC and natural clay (NC, through an impregnation process using TiO2 (P25 as precursor. The so-prepared composite materials were characterized by X-ray diffraction (XRD, scanning electron microscopy (SEM, transition electron microscopy (TEM, and nitrogen physisorption, that is, Brunauer-Emmett-Teller (BET surface area determination. SEM and TEM observation evidenced that TiO2 was deposited on AC and NC surface. XRD results confirmed that TiO2 existed in a mixture of anatase and rutile phases. The specific surface area of photocatalysts decreased drastically in comparison with the original materials. The photocatalytic activity of these materials was assayed in the oxidation of Methyl Green (MG dye in aqueous medium under UV irradiation. TiO2/AC exhibited higher photocatalytic oxidation activity than TiO2 at neutral pH. Total mineralization of MG was confirmed by means of COD analysis, pointing to these materials as an efficient, cost-effective, and environment friendly alternative for water treatment.

Preparation and electrocatalytic property of WC/carbon nanotube composite

International Nuclear Information System (INIS)

Li Guohua; Ma Chunan; Tang Junyan; Sheng Jiangfeng

2007-01-01

Tungsten carbide/carbon nanotube composite was prepared by surface decoration and in situ reduction-carbonization. The samples were characterized by XRD, SEM, EDS, TEM, HRTEM and BET, respectively. The XRD results show that the sample is composed of carbon nanotube, tungsten carbide and tungsten oxide. The EDS results show that the distribution of tungsten oxide is consistent with that of tungsten carbide. SEM, TEM and HRTEM results show that the tungsten carbide nanoparticle with irregular granule grows on the outside surface of carbon nanotube homogenously. The electrocatalytic activity of the sample for p-nitrophenol reduction was tested by a powder microelectrode in a basic solution. The results show that the electrocatalytic activity of the sample is higher than that of granular tungsten carbide, hollow globe tungsten carbide with mesoporosity and carbon nanotube purified. The improvement of the electrocatalytic activity of the sample can be attributed to its components and composite structure. These results indicate that tungsten carbide/carbon nanotube composite is one of the effective ways to improve the electrocatalytic activity of tungsten carbide

Helical polyurethane-attapulgite nanocomposite: Preparation, characterization and study of optical activity

International Nuclear Information System (INIS)

Wang Zhiqiang; Zhou Yuming; Sun Yanqing; Fan Kai; Guo Xingxing; Jiang Xiaolei

2009-01-01

Helical polyurethane-attapulgite (BM-ATT) based on R-1,1'-binaphthyl-2',2-diol (R-BINOL) composite was prepared after the surface modification of attapulgite (ATT). BM-ATT was characterized by Fourier-transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HTEM) and vibrational circular dichroism (VCD) spectroscopy. FT-IR and XRD analyses indicate that the helical polyurethane has been successfully grafted onto the surfaces of the modified ATT without destroying the original crystalline structure of ATT. BM-ATT exhibits the rod-like structure by SEM, TEM, and HTEM photographs. BM-ATT displays obvious Cotton effect for some absorbance in VCD spectrum, and its optical activity results from the singlehanded conformation of helical polyurethane. - Graphical Abstract: Helical polyurethane-attapulgite (BM-ATT) based on R-1,1'-binaphthyl-2',2-diol (R-BINOL) nanocomposite was prepared after surface modification of attapulgite (ATT). This rod-like composite is coated by the optically active polyurethane shell on the surfaces.

Fe_3O_4@B-MCM-41: A new magnetically recoverable nanostructured catalyst for the synthesis of polyhydroquinolines

International Nuclear Information System (INIS)

Abdollahi-Alibeik, Mohammad; Rezaeipoor-Anari, Ali

2016-01-01

Boron modified MCM-41 with magnetite core (Fe_3O_4@B-MCM-41) as a new magnetically recoverable heterogeneous catalyst was prepared and characterized by SEM, TEM, BET, XRD, VSM and FT-IR techniques. The catalytic activity of Fe_3O_4@B-MCM-41 was investigated in the four-component reaction of aldehyde, dimedone, active methylene compounds and ammonium acetate for the synthesis of polyhydroquinolines. According to optimization and characterization results the catalyst with Si:B:Fe_3O_4 mole composition of 40:4:1 has the best activity. The catalyst could be recovered easily by external magnet and has excellent reusability many times without significant decrease of activity. - Highlights: • Core–shell Fe_3O_4@MCM-41 nanoparticles modified by boron (Fe_3O_4@B-MCM-41). • Fe_3O_4@B-MCM-41 as reusable catalyst for the synthesis of polyhydroquinolines. • Characterization of Fe_3O_4@B-MCM-41 using SEM, TEM, BET, XRD and FT-IR techniques.

Fabrication and Characteristics of Macroporous TiO2 Photocatalyst

Directory of Open Access Journals (Sweden)

Guiyun Yi

2014-01-01

Full Text Available Macroporous TiO2 photocatalyst was synthesized by a facile nanocasting method using polystyrene (PS spherical particles as the hard template. The synthesized photocatalyst was characterized by transmission electron microscope (TEM, scanning electron microscopy (SEM, thermogravimetry-differential thermogravimetry (TG-DTG, X-ray diffraction (XRD, and N2-sorption. TEM, SEM, and XRD characterizations confirmed that the macroporous TiO2 photocatalyst is composed of anatase phase. The high specific surface area of 87.85 m2/g can be achieved according to the N2-sorption analysis. Rhodamine B (RhB was chosen as probe molecule to evaluate the photocatalytic activity of the TiO2 catalysts. Compared with the TiO2 materials synthesized in the absence of PS spherical template, the macroporous TiO2 photocatalyst sintered at 500°C exhibits much higher activity on the degradation of RhB under the UV irradiation, which can be assigned to the well-structured macroporosity. The macroporous TiO2 material presents great potential in the fields of environmental remediation and energy conversion and storage.

Effect of processing routes on microstructure, electrical and dielectric behavior of Mg-doped CaCu3Ti4O12 electro-ceramic

Science.gov (United States)

Singh, Laxman; Rai, U. S.; Mandal, K. D.; Rai, Alok Kumar

2013-09-01

In the present communication, data on magnesium-doped calcium copper titanate CaCu2.90Mg0.10Ti4O12 (CCMTO) electro-ceramic, synthesized by the semi-wet route (SWR), ball-milled route (BMR) and solid-state route (SSR), is characterized by TG-DTA, XRD, SEM, EDX and TEM techniques. XRD confirmed the formation of single phase in CCMTO ceramic. The CuO phase present at grain boundaries in SWR ceramic was shown by the SEM micrograph, which was verified by EDX. The TEM image of SWR ceramic shows nanocrystalline particles in the range 80±20 nm. The value of the dielectric constant of SWR ( ɛ r ˜20091) ceramic is higher than those of BMR and SSR ( ɛ r ˜1247) ceramics at 1 kHz at 450 K. A dielectric relaxation has been observed in the frequency range 100 Hz-100 kHz. The high-temperature dielectric dispersion shows one large low-frequency response and two Debye-type relaxations. The impedance and modulus studies show the highest grain-boundary resistance for BMR ceramic.

Synthesis of gold and silver nanoparticles by electron irradiation at 5-15 keV energy

Energy Technology Data Exchange (ETDEWEB)

Mahapatra, S K; Bogle, K A; Dhole, S D; Bhoraskar, V N [Microtron Accelerator Laboratory, Department of Physics, University of Pune, Pune-411007 (India)

2007-04-04

Thin coatings ({approx}10 {mu}m) made from a mixture of polyvinyl alcohol (PVA) and HAuCl{sub 4} or PVA and AgNO{sub 3} on quartz plates were irradiated with 5-15 keV electrons, at room temperature. The electron energy was varied from coating to coating in the range of 5-15 keV, but electron fluence was kept constant at {approx}10{sup 15} e cm{sup -2}. Samples were characterized by the UV-vis, XRD, SEM and TEM techniques. The plasmon absorption peaks at {approx}511 and {approx}442 nm confirmed the formation of gold and silver nanoparticles in the respective electron-irradiated coatings. The XRD, SEM and TEM measurements reveal that the average size of the particles could be tailored in the range of 130-50 nm for gold and from 150-40 nm for silver by varying the electron energy in the range of 5-15 keV. These particles of gold and silver embedded in the polymer could also be separated by dissolving the coatings in distilled water.

Green synthesis of magnetic chitosan nanocomposites by a new sol–gel auto-combustion method

Energy Technology Data Exchange (ETDEWEB)

Ansari, Fatemeh [Institute of Nano Science and Nano Technology, University of Kashan, P.O. Box. 87317–51167, Kashan, Islamic Republic of Iran (Iran, Islamic Republic of); Sobhani, Azam [Department of Chemistry, Kosar University of Bojnord, Bojnord, Islamic Republic of Iran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Institute of Nano Science and Nano Technology, University of Kashan, P.O. Box. 87317–51167, Kashan, Islamic Republic of Iran (Iran, Islamic Republic of)

2016-07-15

The Fe{sub 2}O{sub 3}/CuFe{sub 2}O{sub 4}/chitosan nanocomposites have been successfully synthesized via a new sol–gel auto-combustion route. To prepare the nanocomposites, copper ferrite (CuFe{sub 2}O{sub 4}) and iron (II) oxide (Fe{sub 2}O{sub 3}) nanostructures were first prepared utilizing onion as a green reductant for the first time, and characterized by SEM, TEM, XRD, IR and VSM. Then chitosan was added into the nanostructures dispersed in water. Chitosan was used to functionalize and modify the nanostructures and also to improve surface properties. The nanocomposites were also characterized by several techniques including SEM, TEM, XRD, IR and VSM. The effects of amount of onion and chitosan on the morphology and particle size of nanocomposites were evaluated. - Highlights: • Fe{sub 2}O{sub 3}/CuFe{sub 2}O{sub 4}/chitosan nanocomposites were synthesized for the first time. • A simple, low-cost and friendly route was used to synthesize the nanocomposites. • Effects of amount of onion and chitosan were investigated.

Ag loading induced visible light photocatalytic activity for pervoskite SrTiO3 nanofibers

Science.gov (United States)

Wu, Yeqiu; He, Tao

2018-06-01

The synthesis and photocatalytic activities of Ag-SrTiO3 nanofibers were reported in this work. The fabricated Ag-SrTiO3 nanofibers were characterized by TG-DSC, XRD, IR, XPS, SEM, TEM, DRS and ESR techniques. The XRD and IR results show that Ag-SrTiO3 nanofibers have a perovskite structure after the heat treatment at 700 °C. The XPS result shows that Ag element exists as Ag0 in the fabricated Ag-SrTiO3 nanofibers. The SEM and TEM images indicate the obtaining of nanofibers with porous structure. The photocatalytic activity of Ag-SrTiO3 nanofibers was evaluated by degrading RhB and MB under visible light irradiation. The Ag-SrTiO3 nanofibers show excellent photocatalytic activity under visible light irradiation because of the surface plasmon resonance effect of Ag0. In the photocatalysis process of RhB and MB, lots of hydroxyl radicals were generated, which plays the key role in the decomposition of organic pollutants.

Synthesis of cerium oxide (CeO{sub 2}) nanoparticles using simple CO-precipitation method

Energy Technology Data Exchange (ETDEWEB)

Farahmandjou, M.; Zarinkamar, M.; Firoozabadi, T. P., E-mail: farahamndjou@iauvaramin.ac.ir [Islamis Azad University, Varamin-Phisva Branch, Department of Physics, Varamin (Iran, Islamic Republic of)

2016-11-01

Synthesis of cerium oxide (CeO{sub 2}) nanoparticles was studied by new and simple co-precipitation method. The cerium oxide nanoparticles were synthesized using cerium nitrate and potassium carbonate precursors. Their physicochemical properties were characterized by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (Sem), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (Ftir) and UV-Vis spectrophotometer. XRD pattern showed the cubic structure of the cerium oxide nanoparticles. The average particle size of CeO{sub 2} was around 20 nm as estimated by XRD technique and direct HRTEM observations. The surface morphological studies from Sem and Tem depicted spherical particles with formation of clusters. The sharp peaks in Ftir spectrum determined the existence of CeO{sub 2} stretching mode and the absorbance peak of UV-Vis spectrum showed the bandgap energy of 3.26 eV. (Author)

XRF, μ-XRD and μ-spectroscopic techniques for revealing the composition and structure of paint layers on polychrome sculptures after multiple restorations.

Science.gov (United States)

Franquelo, M L; Duran, A; Castaing, J; Arquillo, D; Perez-Rodriguez, J L

2012-01-30

This paper presents the novel application of recently developed analytical techniques to the study of paint layers on sculptures that have been restored/repainted several times across centuries. Analyses were performed using portable XRF, μ-XRD and μ-Raman instruments. Other techniques, such as optical microscopy, SEM-EDX and μ-FTIR, were also used. Pigments and other materials including vermilion, minium, red lac, ivory black, lead white, barium white, zinc white (zincite), titanium white (rutile and anatase), lithopone, gold and brass were detected. Pigments from both ancient and modern times were found due to the different restorations/repaintings carried out. μ-Raman was very useful to characterise some pigments that were difficult to determine by μ-XRD. In some cases, pigments identification was only possible by combining results from the different analytical techniques used in this work. This work is the first article devoted to the study of sculpture cross-section samples using laboratory-made μ-XRD systems. Copyright © 2011 Elsevier B.V. All rights reserved.

The Effect of Nonnormality on CB-SEM and PLS-SEM Path Estimates

OpenAIRE

Z. Jannoo; B. W. Yap; N. Auchoybur; M. A. Lazim

2014-01-01

The two common approaches to Structural Equation Modeling (SEM) are the Covariance-Based SEM (CB-SEM) and Partial Least Squares SEM (PLS-SEM). There is much debate on the performance of CB-SEM and PLS-SEM for small sample size and when distributions are nonnormal. This study evaluates the performance of CB-SEM and PLS-SEM under normality and nonnormality conditions via a simulation. Monte Carlo Simulation in R programming language was employed to generate data based on the theoretical model w...

Effect of tempering temperature on microstructure and sliding wear property of laser quenched 4Cr13 steel

NARCIS (Netherlands)

Ouyang, J.H.; Pei, Y.T.; Li, X.D.; Lei, T.C.

1994-01-01

4Cr13 martensite stainless steel was quenched by a CO2 laser and tempered for 2 h at different temperatures in the range 200 °C to 550 °C. The microstructure of treated layer was observed by SEM, XRD and TEM. Tempering leads to the decomposition of a large number of retained austenites in laser

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

... 1:1, 1:3 and 0:1) by a facile in situ one-step reduction in the absence of any capping agent. SEM, EDS, TEM, FTIR, XRD, ICP-AES, XPS and nitrogen adsorption/desorption analysis were employed to systematically investigate the morphology and structure of the obtained SiO2 microspheres and SiO₂/PtNi nanocatalysts.

Experimental study of the synthesis and characterisation of silica nanoparticles via the sol-gel method

International Nuclear Information System (INIS)

Tabatabaei, S; Shukohfar, A; Aghababazadeh, R; Mirhabibi, A

2006-01-01

Silica nano-particles were synthesised by chemical methods from tetraethylorthosilicate (TEOS), ethanol (C 2 H 5 OH) and deionized water in the presence of ammonia as catalyst at room temperature. The morphology and structure of colloidal silica particles formed depend on the molar ratio of reagents. The formation of silica particles has been investigated using different solvents: ethanol and ethanol-glycerol. The nature and morphology of particles was investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD)

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.

Science.gov (United States)

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.

XRD, DRS, and SEM stundies of the effects of metal dopants (Pt and Au) on the structural and optical properties of TiO2

CSIR Research Space (South Africa)

Moloantoa, JR

2011-07-01

Full Text Available Au and Pt doped TiO2 nanocrystlas were prepared using the sol gel method. Diffuse Reflectance Spectroscopy (DRS) was used to study the characteristics of these precious metals and X-ray diffraction (XRD) with calculated lattice parameters was used...

Influences of Co doping on the structural and optical properties of ZnO nanostructured

Science.gov (United States)

Majeed Khan, M. A.; Wasi Khan, M.; Alhoshan, Mansour; Alsalhi, M. S.; Aldwayyan, A. S.

2010-07-01

Pure and Co-doped ZnO nanostructured samples have been synthesized by a chemical route. We have studied the structural and optical properties of the samples by using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), field-emission transmission electron microscope (FETEM), energy-dispersive X-ray (EDX) analysis and UV-VIS spectroscopy. The XRD patterns show that all the samples are hexagonal wurtzite structures. Changes in crystallite size due to mechanical activation were also determined from X-ray measurements. These results were correlated with changes in particle size followed by SEM and TEM. The average crystallite sizes obtained from XRD were between 20 to 25 nm. The TEM images showed the average particle size of undoped ZnO nanostructure was about 20 nm whereas the smallest average grain size at 3% Co was about 15 nm. Optical parameters such as absorption coefficient ( α), energy band gap ( E g ), the refractive index ( n), and dielectric constants ( σ) have been determined using different methods.

Electrospun polyacrylonitrile nanofibers loaded with silver nanoparticles by silver mirror reaction

Energy Technology Data Exchange (ETDEWEB)

Shi, Yongzheng; Li, Yajing; Zhang, Jianfeng; Yu, Zhongzhen; Yang, Dongzhi, E-mail: yangdz@mail.buct.edu.cn

2015-06-01

The silver mirror reaction (SMR) method was selected in this paper to modify electrospun polyacrylonitrile (PAN) nanofibers, and these nanofibers loaded with silver nanoparticles showed excellent antibacterial properties. PAN nanofibers were first pretreated in AgNO{sub 3} aqueous solution before the SMR process so that the silver nanoparticles were distributed evenly on the outer surface of the nanofibers. The final PAN nanofibers were characterized by scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), transmission electron microscopy (TEM), TEM-selected area electron diffraction (SAED), X-ray diffraction (XRD) and thermogravimetric analysis (TGA). SEM, TEM micrographs and SAED patterns confirmed homogeneous dispersion of the silver nanoparticles which were composed of monocrystals with diameters 20–30 nm. EDS and XRD results showed that these monocrystals tended to form face-centered cubic single silver. TGA test indicated that the nanoparticles loaded on the nanofibers reached above 50 wt.%. This material was also evaluated by the viable cell-counting method. The results indicated that PAN nanofibers loaded with silver nanoparticles exhibited excellent antimicrobial activities against gram-negative Escherichia coli (E. coli), gram-positive Staphylococcus aureus (S. aureus) and the fungus Monilia albicans. Thus, this material had many potential applications in biomedical fields. - Highlights: • Silver mirror reaction was used to prepare nanofibers loaded with silver nanoparticles. • The SAED patterns demonstrated the monocrystallinity of silver nanocrystals. • The XRD results showed nanoparticles tended to be face-centered cubic single silver. • The material showed excellent antimicrobial activities against bacteria and fungi.

Platinum boride nanowires: Synthesis and characterization

International Nuclear Information System (INIS)

Ding Zhanhui; Qiu Lixia; Zhang Jian; Yao Bin; Cui Tian; Guan Weiming; Zheng Weitao; Wang Wenquan; Zhao Xudong; Liu Xiaoyang

2012-01-01

Highlights: ► Platinum boride nanowires have been synthesized via the direct current arc discharge method. ► XRD, TEM and SAED indicate that the nanowires are single-crystal PtB. ► Two broad photoluminescence emission peaks at about 586 nm and 626 nm have been observed in the PL spectroscopy of PtB nanowires. - Abstract: Platinum boride (PtB) nanowires have been successfully fabricated with direct current arc discharge method using a milled mixture of platinum (Pt) and boron nitride (BN) powders. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the compositions, morphology, and structures of the samples. The results show that PtB nanowires are 30–50 nm thick and 20–30 μm long. TEM and selected area electron diffraction (SAED) patterns identify that the PtB nanowires are single-crystalline in nature. A growth mechanism based on vapor–liquid–solid (VLS) process is proposed for the formation of nanowires.

Mass synthesis of yttrium oxide nano-powders using radio frequency (RF) plasma

International Nuclear Information System (INIS)

Ghorui, S.; Sahasrabudhe, S.N.; Chakravarthy, Y.; Nagaraj, A.; Das, A.K.; Dhamale, G.

2014-01-01

Mass synthesis of nano-phase Yttrium Oxide (Y 2 O 3 ) from commercially available coarse grain powder is reported. Nano-sized high purity Y 2 O 3 is an important and critical constituent of ceramics like YAG (Yttrium aluminum garnet: Y 3 Al 5 O 12 ) for laser applications. The system is characterized in terms of its thermal and electrical behavior. Boltzmann plot technique is used to measure axial variation of temperature of the generated plasma. The synthesized particles are characterized in terms of XRD, SEM, TEM and BET analyses for qualification of the developed system. Major features observed are efficient conversion into nanometer-sized highly spherical particles, narrow size distribution, highly crystallite nature and highly pure phases. The particle distribution (from TEM) peaks within 20-30 nm. Average particle sizes determined from different methods like XRD, TEM and BET are very close to each other and point toward particle sizes within 20 to 30 nm

Applications of Real Space Crystallography in Characterization of Dislocations in Geological Materials in a Scanning Electron Microscope (SEM)

Science.gov (United States)

Kaboli, S.; Burnley, P. C.

2017-12-01

Imaging and characterization of defects in crystalline materials is of significant importance in various disciplines including geoscience, materials science, and applied physics. Linear defects such as dislocations and planar defects such as twins and stacking faults, strongly influence many of the properties of crystalline materials and also reflect the conditions and degree of deformation. Dislocations have been conventionally imaged in thin foils in a transmission electron microscope (TEM). Since the development of field emission scanning electron microscopes (FE-SEM) with high gun brightness and small spot size, extensive efforts have been dedicated to the imaging and characterization of dislocations in semi-conductors using electron channeling contrast imaging (ECCI) in the SEM. The obvious advantages of using SEM over TEM include easier and non-destructive sample preparation and a large field of view enabling statistical examination of the density and distribution of dislocations and other defects. In this contribution, we extend this technique to geological materials and introduce the Real Space Crystallography methodology for imaging and complete characterization of dislocations based on bend contour contrast obtained by ECCI in FE-SEM. Bend contours map out the distortion in the crystal lattice across a deformed grain. The contrast of dislocations is maximum in the vicinity of bend contours where crystal planes diffract at small and positive deviations from the Bragg positions (as defined by Bragg's law of electron diffraction). Imaging is performed in a commercial FE-SEM equipped with a standard silicon photodiode backscattered (BSE) detector and an electron backscatter diffraction (EBSD) system for crystal orientation measurements. We demonstrate the practice of this technique in characterization of a number of geological materials in particular quartz, forsterite olivine and corundum, experimentally deformed at high pressure-temperature conditions. This

Preparation of meta-stable phases of barium titanate by Sol-hydrothermal method

Directory of Open Access Journals (Sweden)

Mahalakshmi Selvaraj

2015-11-01

Full Text Available Two low-cost chemical methods of sol–gel and the hydrothermal process have been strategically combined to fabricate barium titanate (BaTiO3 nanopowders. This method was tested for various synthesis temperatures (100 °C to 250 °C employing barium dichloride (BaCl2 and titanium tetrachloride (TiCl4 as precursors and sodium hydroxide (NaOH as mineralizer for synthesis of BaTiO3 nanopowders. The as-prepared BaTiO3 powders were investigated for structural characteristics using x-ray diffraction (XRD, scanning electron microscopy (SEM and transmission electron microscopy (TEM. The overall analysis indicates that the hydrothermal conditions create a gentle environment to promote the formation of crystalline phase directly from amorphous phase at the very low processing temperatures investigated. XRD analysis showed phase transitions from cubic - tetragonal - orthorhombic - rhombohedral with increasing synthesis temperature and calculated grain sizes were 34 – 38 nm (using the Scherrer formula. SEM and TEM analysis verified that the BaTiO3 nanopowders synthesized by this method were spherical in shape and about 114 - 170 nm in size. The particle distribution in both SEM and TEM shows that as the reaction temperature increases from 100 °C to 250 °C, the particles agglomerate. Selective area electron diffraction (SAED shows that the particles are crystalline in nature. The study shows that choosing suitable precursor and optimizing pressure and temperature; different meta-stable (ferroelectric phases of undoped BaTiO3 nanopowders can be stabilized by the sol-hydrothermal method.

New constraints on deformation processes in serpentinite from sub-micron Raman Spectroscopy and TEM

Science.gov (United States)

Smith, S. A. F.; Tarling, M.; Rooney, J. S.; Gordon, K. C.; Viti, C.

2017-12-01

Extensive work has been performed to characterize the mineralogical and mechanical properties of the various serpentine minerals (i.e. antigorite, lizardite, chrysotile, polyhedral and polygonal serpentine). However, correct identification of serpentine minerals is often difficult or impossible using conventional analytical techniques such as optical- and SEM-based microscopy, X-ray diffraction and infrared spectroscopy. Transmission Electron Microscopy (TEM) is the best analytical technique to identify the serpentine minerals, but TEM requires complex sample preparation and typically results in very small analysis areas. Sub-micron confocal Raman spectroscopy mapping of polished thin sections provides a quick and relatively inexpensive way of unambiguously distinguishing the main serpentine minerals within their in-situ microstructural context. The combination of high spatial resolution (with a diffraction-limited system, 366 nm), large-area coverage (up to hundreds of microns in each dimension) and ability to map directly on thin sections allows intricate fault rock textures to be imaged at a sample-scale, which can then form the target of more focused TEM work. The potential of sub-micron Raman Spectroscopy + TEM is illustrated by examining sub-micron-scale mineral intergrowths and deformation textures in scaly serpentinites (e.g. dissolution seams, mineral growth in pressure shadows), serpentinite crack-seal veins and polished fault slip surfaces from a serpentinite-bearing mélange in New Zealand. The microstructural information provided by these techniques has yielded new insights into coseismic dehydration and amorphization processes and the interplay between creep and localised rupture in serpentinite shear zones.

Composite nanofibers/water photosplitting and photocatalytic degradation of dairy effluent

DEFF Research Database (Denmark)

Kanjwal, Muzafar A.; Leung, Wallace W.F.; Chronakis, Ioannis S.

2018-01-01

Photocatalytic removal of Dairy effluent (DE) was studied by using TiO2-GeO2 and TiO2-CdO nanofibers (NFs), produced by electrospinning method. These NFs were characterized by SEM, TEM and XRD studies. The TiO2-GeO2 and TiO2-CdO NFs were smooth and continuous, with an average diameter of about 27...

Hydroxyapatite-Functionalized Graphene: A New Hybrid Nanomaterial

OpenAIRE

Rodríguez-González, C.; Cid-Luna, H. E.; Salas, P.; Castaño, V. M.

2014-01-01

Graphene oxide sheets (GO) were functionalized with hydroxyapatite nanoparticles (nHAp) through a simple and effective hydrothermal treatment and a novel physicochemical process. Microstructure and crystallinity were investigated by Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray diffraction (XRD), ultraviolet-visible (UV-Vis) absorption spectroscopy, and thermogravimetric analysis (TGA). Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) ...

Construcción de la microestructura y macroestructura semántica en textos expositivos producidos por estudiantes universitarios de LUZ

OpenAIRE

Fuenmayor, Gloria; Villasmil, Yeriling; Rincón, María

2008-01-01

El objetivo de esta investigación es analizar la construcción de la microestructura y macroestructura semántica  en textos expositivos producidos por estudiantes universitarios, a partir del uso de  procedimientos gramaticales como las proformas. La teoría se sustenta en los conceptos: Microestructrura y Macroestructura semántica, (van Dijk y Kintsch 1983, 1992); Mecanismos de cohesión y progresión temática (Calsamiglia y Tusón, 1999); El texto expositivo (Álvarez, 1996, 2001); Carácter socia...

Study of copper deposit on a porous electrode of carbon and stainless steel by sem-xrd and image analysis

OpenAIRE

Constanzo-R., Robinson; Pagliero-N., Antonio; Vergara-G., Froilán

2014-01-01

El objetivo de este trabajo fue realizar un análisis cualitativ o de la distribución de un electrodepósito de cobre en el inter ior de electrodos porosos (EP) de acero inoxidable y carbono grafito. Para ello, se reali zaron pruebas de electrodepositación de cobre a nivel de labora torio, con un posterior análisis de cortes de muestras de acero y grafito vía Microscopía Estereoscópica, Microscopía SEM-DRX y Análisis de Imagen, los cuales mostraron que el cobre no se deposita en forma uniforme ...

Three dimensional rock microstructures: insights from FIB-SEM tomography

Science.gov (United States)

Drury, Martyn; Pennock, Gill; de Winter, Matthijs

2016-04-01

Most studies of rock microstructures investigate two-dimensional sections or thin slices of three dimensional grain structures. With advances of X-ray and electron tomography methods the 3-D microstructure can be(relatively) routinely investigated on scales from a few microns to cm. 3D studies are needed to investigate the connectivity of microstructures and to test the assumptions we use to calculate 3D properties from 2D sections. We have used FIB-SEM tomography to study the topology of melts in synthetic olivine rocks, 3D crystal growth microstructures, pore networks and subgrain structures. The technique uses a focused ion beam to make serial sections with a spacing of tens to hundreds of nanometers. Each section is then imaged or mapped using the electron beam. The 3D geometry of grains and subgrains can be investigated using orientation contrast or EBSD mapping. FIB-SEM tomography of rocks and minerals can be limited by charging of the uncoated surfaces exposed by the ion beam. The newest generation of FIB-SEMs have much improved low voltage imaging capability allowing high resolution charge free imaging. Low kV FIB-SEM tomography is now widely used to study the connectivity of pore networks. In-situ fluids can also be studied using cryo-FIB-SEM on frozen samples, although special freezing techniques are needed to avoid artifacts produced by ice crystallization. FIB-SEM tomography is complementary, in terms of spatial resolution and sampled volume, to TEM tomography and X-ray tomography, and the combination of these methods can cover a wide range of scales. Our studies on melt topology in synthetic olivine rocks with a high melt content show that many grain boundaries are wetted by nanometre scale melt layers that are too thin to resolve by X-ray tomography. A variety of melt layer geometries occur consistent with several mechanisms of melt layer formation. The nature of melt geometries along triple line junctions and quadruple points can be resolved

In Situ TEM Electrical Measurements

DEFF Research Database (Denmark)

Canepa, Silvia; Alam, Sardar Bilal; Ngo, Duc-The

2016-01-01

understanding of complex physical and chemical interactions in the pursuit to optimize nanostructure function and device performance. Recent developments of sample holder technology for TEM have enabled a new field of research in the study of functional nanomaterials and devices via electrical stimulation...... influence the sample by external stimuli, e.g. through electrical connections, the TEM becomes a powerful laboratory for performing quantitative real time in situ experiments. Such TEM setups enable the characterization of nanostructures and nanodevices under working conditions, thereby providing a deeper...... and measurement of the specimen. Recognizing the benefits of electrical measurements for in situ TEM, many research groups have focused their effort in this field and some of these methods have transferred to ETEM. This chapter will describe recent advances in the in situ TEM investigation of nanostructured...

Determination of the activation energy in a cast aluminium alloy by TEM and DSC

International Nuclear Information System (INIS)

Ovono Ovono, D.; Guillot, I.; Massinon, D.

2007-01-01

The precipitation behaviour and microstructure development of the A319 alloy during ageing were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM and STEM). During T5 treatment, θ' precipitates with an average size of about 18 nm were observed by TEM. The precipitate sizes increased with ageing temperature and attained an average size of 107 nm. In addition, there was a linear relationship between precipitate growth temperature and the cube of the precipitate size. This indicates that precipitate growth of the A319 alloy belongs to a thermal activated process of the Arrhenius type. The activation energy for the precipitate growth was calculated to be 140.4 ± 13.3 kJ/mol. However, under continuous heating conditions, the activation energy for the precipitate growth obtained by Kissinger plot was determined to be 119.5 ± 8.3 kJ/mol. Allowing for experimental error, both values are comparable and are related to the diffusion of Cu and/or Si in Al

Characterisation of the coke formed during metal dusting of iron in CO-H2-H2O gas mixtures

International Nuclear Information System (INIS)

Zhang, J.; Schneider, A.; Inden, G.

2003-01-01

Carbon deposits formed on the surface of iron samples during carburisation at 700 deg. C in a gas mixture of 75%CO-24.81%H 2 -0.19%H 2 O were characterised by using scanning electron microscopy (SEM), X-ray diffraction (XRD), Moessbauer spectroscopy and transmission electron microscopy (TEM). Cross-section observation of the iron sample by light optical microscopy revealed the formation of cementite after only 10 min reaction, together with a thin layer of graphite. After 4 h reaction, a thick coke layer was formed on top of the cementite surface. SEM surface observation indicated the formation of filamentous carbon in the coke layer. Further analysis of the coke by XRD and Moessbauer showed the presence of mainly Fe 3 C and small amount of Fe 2 C but no metallic iron in the carbon deposit. TEM analysis of the coke detected very convoluted filaments with iron-containing particles at the tip or along their length. These particles were identified to be cementite by selected area diffraction. Carbon deposits produced at the same temperature but with other gas compositions were also analysed by using XRD. It was found that with a low content of CO, e.g. 5%, both α-Fe and Fe 3 C were detected in the coke. Increasing CO content to more than 30%, iron carbide was the only iron-containing phase

Synthesis and characterization of advanced high capacity cathode active nanomaterials with three integrated spinel-layered phases for Li-ion batteries

Energy Technology Data Exchange (ETDEWEB)

Bulut, Emrah, E-mail: ebulut@sakarya.edu.tr [Department of Chemistry, Sakarya University, 54187 Serdivan, Sakarya (Turkey); Can, Mustafa, E-mail: mstfacan@gmail.com [Vocational School of Arifiye, Sakarya University, 54580 Arifiye, Sakarya (Turkey); Özacar, Mahmut, E-mail: nmozacart@hotmail.com [Department of Chemistry, Sakarya University, 54187 Serdivan, Sakarya (Turkey); Akbulut, Hatem, E-mail: akbulut@Sakarya.edu.tr [Department of Metallurgical and Materials Engineering, Sakarya University, 54187 Serdivan, Sakarya (Turkey)

2016-06-15

Mesoporous cathode active materials that included undoped and separated Cu{sup 2+} and Co{sup 3+} doped spinels were prepared. The “doped spinel-Layered-Li-rich spinel” composite nanoparticles within the three integrated phased (LiM{sub 0,02}Mn{sub 1,98}O{sub 4}–Li{sub 2}MnO{sub 3}–Li{sub 1,27}Mn{sub 1,73}O{sub 4}; where M is Cu{sup 2+} and Co{sup 3+}) were synthesized by a microwave assisted hydrothermal synthesis. These materials were investigated with X-Ray powder Diffraction spectroscopy (XRD), Scanning Electron Microscopy (SEM and FE-SEM), High Resolution Transmission Electron Microscopy (HR-TEM), galvanostatic cycling at 0.1C and 0.5C rates, Cyclic Voltammetry (CV), and Electrochemical Impedance Spectroscopy (EIS). The effects of the calcination temperature and the partial substitution of Mn{sup 3+} in the spinel by Cu{sup 2+} and Co{sup 3+}, and onto the spinel structure were investigated with XRD. The lattice parameters of the spinel structured compounds were calculated from the XRD data using the Williamson-Hall equation. However, the morphological changes, which depended on the calcination temperature, were examined by SEM, FE-SEM and HRTEM. Furthermore, the two other phases which were different from LiM{sub 0,02}Mn{sub 1,98}O{sub 4} had a great impact on the electrochemical performance over the potential range of the 3–5 V. At the 0.1C rate, the first discharge capacities of undoped and Cu{sup 2+}, Co{sup 3+} doped materials were 577, 285, 560 mAh/g respectively. After 50 cycles at 0.5C rate, we achieved 96.2%; 52.5%; 95.4% capacity retention for the undoped and Cu{sup 2+}, Co{sup 3+} doped materials respectively. - Highlights: • Mesoporous cathode active nanomaterials with three integrated phase were synthesized. • The materials were characterized structurally by XRD, FE-SEM, HR-TEM. • Integrated phases provide an additional 400 mAh/g discharge capacity at low rate. • Higher specific capacities than literature values were achieved at 0

XRD and HRTEM characterization of mechanosynthesized Ti{sub 0.9}W{sub 0.1}C cermet

Energy Technology Data Exchange (ETDEWEB)

Bandyopadhyay, S. [Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India); Dutta, H. [Department of Physics, Vivekananda College, Burdwan 713103, West Bengal (India); Pradhan, S.K., E-mail: skp_bu@yahoo.com [Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India)

2013-12-25

Highlights: •Cubic Ti{sub 0.9}W{sub 0.1}C is formed after 50 min of milling of α-Ti, W and graphite powders. •Nanocrystalline Ti{sub 0.9}W{sub 0.1}C with particle size ∼11 nm is obtained after 8 h milling. •Average particle size of Ti{sub 0.9}W{sub 0.1}C from XRD analysis and HRTEM is very close. •Formation of Ti{sub 0.9}W{sub 0.1}C is hindered as compared with TiC. -- Abstract: Elemental powder mixture of titanium, tungsten and graphite is milled by high energy planetary ball mill at a fixed ball to powder mass ratio (BPMR) for different duration to produce nanosized particles of Ti{sub 0.9}W{sub 0.1}C hard metal. Microstructure characterization in terms of lattice imperfections and phase quantification of ball-milled samples has been done primarily by analyzing the XRD pattern and employing Rietveld method of structure and microstructure refinement. After 8 h of ball-milling full formation of Ti{sub 0.9}W{sub 0.1}C is noticed without any contamination of other phase or milling media. TEM study of 8 h ball-milled sample gives direct supportive evidence of structural and microstructural evaluation by XRD pattern analysis. A comparative study of microstructural changes between TiC and Ti{sub 0.9}W{sub 0.1}C helps to understand the effect of addition of W as solute in Ti–C metal matrix.

Synthesis and Characterization of Cadmium Sulfide Nanoparticles by Chemical Precipitation Method.

Science.gov (United States)

Devi, R Aruna; Latha, M; Velumani, S; Oza, Goldie; Reyes-Figueroa, P; Rohini, M; Becerril-Juarez, I G; Lee, Jae-Hyeong; Yi, Junsin

2015-11-01

Cadmium sulfide (CdS) nanoparticles were synthesized by chemical precipitation method using cadmium chloride (CdCl2), sodium sulfide (Na2S) and water as a solvent by varying temperatures from 20-80 degrees C. The nanoparticles were characterized by X-ray diffraction (XRD), Raman spectroscopy, field emission scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), High-resolution transmission electron microscopy (HR-TEM) and UV-Visible spectroscopy. XRD pattern revealed cubic crystal structure for all the synthesized CdS nanoparticles. Raman spectra showed first and second order longitudinal optical (LO) phonon vibrational modes of CdS. The size of CdS nanoparticles was found to be in the range of 15-80 nm by FE-SEM analysis, in all cases. The atomic percentage of cadmium and sulfur was confirmed to be 1:1 from EDS analysis. TEM micrograph depicts the spherical shape of the particles and the size is in the range of 15-85 nm while HR-TEM images of CdS nanoparticles exhibit well-resolved lattice fringes of the cubic structure of CdS. The optical properties of CdS were examined by UV-Visible spectroscopy which showed variation in absorption band from 460-480 nm. The band gap was calculated from the absorption edge and found to be in the range of 3.2-3.5 eV which is greater than the bulk CdS.

Synthesis of Carbon Nanotubes and Nanospheres from Coconut Fibre and the Role of Synthesis Temperature on Their Growth

Science.gov (United States)

Adewumi, Gloria A.; Inambao, Freddie; Eloka-Eboka, Andrew; Revaprasadu, Neerish

2018-04-01

Carbon nanotubes (CNT) and carbon nanospheres were successfully synthesized from coconut fibre-activated carbon. The biomass was first carbonized then physically activated, followed by treatment using ethanol vapor at 700°C to 1100°C at 100°C intervals. The effect of synthesis temperature on the formation of the nanomaterials was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectrometry, x-ray diffraction (XRD), Fourier transform infrared microscopy (FTIR) and thermogravimetric analysis. SEM analysis revealed that nanospheres were formed at higher temperatures of 1000°C and 1100°C, while lower temperatures of 800°C and 900°C favored the growth of CNT. At 700°C, however, no tubes or spheres were formed. TEM and FTIR were used to observe spectral features, such as the peak positions, intensity and bandwidth, which are linked to some structural properties of the samples investigated. All these observations provided facts on the nanosphere and nanotube dimensions, vibrational modes and the degree of purity of the obtained samples. The TEM results show spheres of diameter in the range 50 nm to 250 nm while the tubes had diameters between 50 nm to 100 nm. XRD analysis reveals the materials synthesized are amorphous in nature with a hexagonal graphite structure.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

Science.gov (United States)

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

A developed wedge fixtures assisted high precision TEM samples pre-thinning method: Towards the batch lamella preparation

Directory of Open Access Journals (Sweden)

Dandan Wang

2017-04-01

Full Text Available Ion milling, wedge cutting or polishing, and focused ion beam (FIB milling are widely-used techniques for the transmission electron microscope (TEM sample preparation. Especially, the FIB milling provides a site-specific analysis, deposition, and ablation of materials in the micrometer and nanometer scale. However, the cost of FIB tools has been always a significant concern. Since it is inevitable to use the FIB technique, the improvement of efficiency is a key point. Traditional TEM sample preparation with FIB was routinely implemented on a single sample each time. Aiming at cost efficiency, a new pre-thinning technique for batch sample preparation was developed in this paper. The present proposal combines the sample preparation techniques with multi-samples thinning, cross-section scanning electron microscopy (SEM, wedge cutting, FIB and other sample pre-thinning techniques. The new pre-thinning technique is to prepare an edge TEM sample on a grinding and polishing fixture with a slant surface. The thickness of the wedges sample can be measured to 1∼2 μm under optical microscope. Therefore, this fixture is superior to the traditional optical method of estimating the membrane thickness. Moreover, by utilizing a multi-sample holding fixture, more samples can be pre-thinned simultaneously, which significantly improved the productivity of TEM sample preparation.

Template-free synthesis of ZnWO{sub 4} powders via hydrothermal process in a wide pH range

Energy Technology Data Exchange (ETDEWEB)

Hojamberdiev, Mirabbos, E-mail: mirabbos_uz@yahoo.com [Shaanxi Key Laboratory of Nano-materials and Technology, Xi' an University of Architecture and Technology, Xi' an 710055 (China); Zhu, Gangqiang [School of Physics and Information Technology, Shaanxi Normal University, Xi' an 710062 (China); Xu, Yunhua [Shaanxi Key Laboratory of Nano-materials and Technology, Xi' an University of Architecture and Technology, Xi' an 710055 (China)

2010-12-15

ZnWO{sub 4} powders with different morphologies were fabricated through a template-free hydrothermal method at 180 {sup o}C for 8 h in a wide pH range. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible and luminescence spectrophotometers were applied to study the effects of pH values on crystallinity, morphology, optical and luminescence properties. The XRD results showed that the WO{sub 3} + ZnWO{sub 4}, ZnWO{sub 4}, and ZnO phases could form after hydrothermal processing at 180 {sup o}C for 8 h with the pH values of 1, 3-11, and 13, respectively. The SEM and TEM observation revealed that the morphological transformation of ZnWO{sub 4} powders occurred with an increase in pH values as follows: star anise-, peony-, and desert rose-like microstructures and soya bean- and rod-like nanostructures. The highest luminescence intensity was found to be in sample consisting of star anise-like crystallites among all the samples due to the presence of larger particles with high crystallinity resulted from the favorable pH under the current hydrothermal conditions.

Size-controlled synthesis of chalcogen and chalcogenide nanoparticles using protic ionic liquids with imidazolium cation

International Nuclear Information System (INIS)

Meenatchi, Boominathan; Renuga, Velayutham; Manikandan, Ayyar

2016-01-01

Green synthesis of selenium (chalcogen) nanoparticles (SeNPs) has been successfully attained by simple wet chemical method that involves the reaction of six different protic ionic liquids with imidazolium cations and sodium hydrogen selenide (NaHSe) in the presence of poly ethylene glycol-600 (PEG-600) as an additional stabilizer. The obtained SeNPs were characterized using UV spectral (UV), Fourier transform infra-red (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential thermal analysis (DTA), scanning electron microscope (SEM) with energy dispersive X-ray (EDX) and high resolution transmission electron microscope (TEM) analysis. The results illustrate that the synthesized SeNPs are spherical in shape with size ranging 19-24 nm and possess good optical property with greater band gap energy, high thermal stability up to 330 .deg. C, low melting point of 218-220 .deg. C comparing to precursor selenium. Using the synthesized SeNPs, two chalcogenides such as ZnSe and CdSe semiconductor nanoparticles were synthesized and characterized using XRD, SEM with EDX and TEM analysis. The fabricated CdSe and ZnSe nanoparticles appeared like pebble and cluster structure with particle size of 29.97 nm and 22.73 nm respectively.

Enhanced electrochemical properties of vanadium-doped titanium niobate as a new anode material for lithium-ion batteries

International Nuclear Information System (INIS)

Wen, Xiaoyan; Ma, Chenxiang; Du, Chenqiang; Liu, Jie; Zhang, Xinhe; Qu, Deyang; Tang, Zhiyuan

2015-01-01

The Vanadium-doped TiNb 2 O 7 (TNO) samples have been investigated as novel anode active materials for application in lithium-ion batteries. The samples are characterized by X-ray diffraction patterns (XRD), raman spectrum, scanning electron microscopy (SEM), transmission electron microscopy (TEM), galvanostatic charge-discharge tests, and cyclic voltammetry (CV) tests. The XRD results indicate that V-doping expands the lattice parameters of TiNb 2 O 7 samples and facilitates the enhanced lithium ion diffusion. SEM and TEM results show that lattice expansion caused by V-doping doesn’t significantly change the particle size distribution of TiNb 2 O 7 samples. The electrochemical measurements indicate that the TiNb 1.98 V 0.02 O 7 anode material displays a highly reversible capacity and excellent cycling stability. The initial discharge capacities of TiNb 1.98 V 0.02 O 7 are 298.48 mAh g −1 and 171.99 mAh g −1 at 0.3C and 10C, respectively, indicating that the TiNb 1.98 V 0.02 O 7 material can be utilized as a promising anode material for lithium-ion batteries.

Biosynthesis, characterization and antimicrobial studies of green synthesized silver nanoparticles from fruit extract of Syzygium alternifolium (Wt.) Walp. an endemic, endangered medicinal tree taxon

Science.gov (United States)

Yugandhar, P.; Savithramma, N.

2016-02-01

In nanotechnology, the plant mediated synthesis of nanoparticles has terrific application in biomedicine due to its novel properties and its eco-friendly nature. The present study deals with the biosynthesis of stable silver nanoparticles (SNPs) from aqueous fruit extract of S. alternifolium an endemic medicinal plant to Eastern Ghats. The synthesized nanoparticles are characterized by UV-VIS spectroscopy, FTIR, XRD, AFM, SEM with EDAX and TEM. Colour change from brown to grey indicates the formation of nanoparticles and UV-VIS surface plasmon resonance spectroscopy observed at 442 nm further confirms the synthesized nanoparticles are SNPs. FTIR studies reveal that the phenols and primary amines of proteins are main responsible for reduction, stabilization and capping agents towards these SNPs. The XRD data show crystalline nature of nanoparticles and EDAX measurements reveal the (12.74 %) percentage presence of Ag metal. AFM, SEM and TEM microscopic analyses revealed that the size of synthesized SNPs ranging from 5 to 68 nm has spherical shape and they are in polydispersed condition. Further, the antimicrobial studies of synthesized SNPs show high toxicity towards different bacterial and fungal isolates. This is the first report on fruit mediated synthesis of silver nanoparticles from S. alternifolium.

Synthesis, Optical and Structural Properties of Copper Sulfide Nanocrystals from Single Molecule Precursors

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Peter A. Ajibade

2017-02-01

Full Text Available We report the synthesis and structural studies of copper sulfide nanocrystals from copper (II dithiocarbamate single molecule precursors. The precursors were thermolysed in hexadecylamine (HDA to prepare HDA-capped CuS nanocrystals. The optical properties of the nanocrystals studied using UV–visible and photoluminescence spectroscopy showed absorption band edges at 287 nm that are blue shifted, and the photoluminescence spectra show emission curves that are red-shifted with respect to the absorption band edges. These shifts are as a result of the small crystallite sizes of the nanoparticles leading to quantum size effects. The structural studies were carried out using powder X-ray diffraction (XRD, transmission electron microscopy (TEM, scanning electron microscopy (SEM, energy dispersive X-ray spectroscopy (EDS, and atomic force microscopy. The XRD patterns indicates that the CuS nanocrystals are in hexagonal covellite crystalline phases with estimated particles sizes of 17.3–18.6 nm. The TEM images showed particles with almost spherical or rod shapes, with average crystallite sizes of 3–9.8 nm. SEM images showed morphology with ball-like microspheres on the surfaces, and EDS spectra confirmed the presence of CuS nanoparticles.

The synthesis of Ba2+ doped multiferroic BiFeO3 nanoparticles by using a hydrothermal approach in the presence of different surface activators and the investigation of structural and magnetic features

Science.gov (United States)

Mardani, Reza

2017-05-01

In this work, Bi1-x Ba x FeO3 nanoparticles were synthesized by a hydrothermal method in the presence of various surface activators, and different amounts of barium were inserted in a bismuth ferrite (x  =  0.1, 0.15, 0.2) structure instead of bismuth. The structural and magnetic properties, morphology, and size of the synthesized nanoparticles were investigated by XRD, FT-IR, FE-SEM, TEM, DLS and VSM. The XRD analysis results reveal that the synthetic nanoparticles have a single phase. A phase shift from a rhombohedral structure to a tetragonal structure occurs due to the enhanced barium amount in the bismuth ferrite structure. The SEM analysis exhibits a uniform shape of the Bi0.85Ba0.15FeO3 particles and the image observed by TEM clarifies the size of the particles as 11 nm. Furthermore, the effect of the diverse surfaces of activators in the synthesis of Bi0.85Ba0.15FeO3 nanoparticles was studied, revealing that when sugar was used as a surfactant, the particle size reduced and the magnetic properties increased notably.

Size-controlled synthesis of chalcogen and chalcogenide nanoparticles using protic ionic liquids with imidazolium cation

Energy Technology Data Exchange (ETDEWEB)

Meenatchi, Boominathan [Cauvery College for Women, Tamilnadu (India); Renuga, Velayutham [National College, Tamilnadu (India); Manikandan, Ayyar [Bharath Institute of Higher Education and Research, Bharath University, Tamilnadu (India)

2016-03-15

Green synthesis of selenium (chalcogen) nanoparticles (SeNPs) has been successfully attained by simple wet chemical method that involves the reaction of six different protic ionic liquids with imidazolium cations and sodium hydrogen selenide (NaHSe) in the presence of poly ethylene glycol-600 (PEG-600) as an additional stabilizer. The obtained SeNPs were characterized using UV spectral (UV), Fourier transform infra-red (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential thermal analysis (DTA), scanning electron microscope (SEM) with energy dispersive X-ray (EDX) and high resolution transmission electron microscope (TEM) analysis. The results illustrate that the synthesized SeNPs are spherical in shape with size ranging 19-24 nm and possess good optical property with greater band gap energy, high thermal stability up to 330 .deg. C, low melting point of 218-220 .deg. C comparing to precursor selenium. Using the synthesized SeNPs, two chalcogenides such as ZnSe and CdSe semiconductor nanoparticles were synthesized and characterized using XRD, SEM with EDX and TEM analysis. The fabricated CdSe and ZnSe nanoparticles appeared like pebble and cluster structure with particle size of 29.97 nm and 22.73 nm respectively.

Synthesis and structural characterization of CdS nanoparticles using nitrogen adducts of mixed diisopropylthiourea and dithiolate derivatives of Cd(II) complexes

Science.gov (United States)

Osuntokun, Jejenija; Ajibade, Peter A.

2015-07-01

[Cd(diptu)2(ced)], [Cd(diptu)2(ced)(bpy)], [Cd(diptu)2(ced)(phen)], (where diptu = diisopropyl thiourea; ced = 1-cyano-1-carboethoxylethylene-2,2‧-dithiolate; bpy = 2,2‧-bipyridine and phen = 1,10-phenanthroline) have been prepared and used as single source precursors for the preparation of hexadecylamine capped CdS nanoparticles. The precursor complexes were characterized by elemental analysis, FTIR and TGA. The structural properties of the nanoparticles were investigated using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy techniques (SEM). The optical properties of the nanoparticles were studied using UV-Visible and photoluminescence spectroscopy. The XRD analysis showed that the nanoparticles were indexed to the hexagonal phase of CdS and the TEM results showed CdS nanoparticles with average crystallite sizes of 4.00-8.80 nm.

Morphological Study on Room-Temperature-Cured PMMA-Grafted Natural Rubber-Toughened Epoxy/Layered Silicate Nanocomposite

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N. Y. Yuhana

2012-01-01

Full Text Available A morphological study was conducted on ternary systems containing epoxy, PMMA-grafted natural rubber, and organic chemically modified montmorillonite (Cloisite 30B. Optical microscopy, transmission electron microscopy (TEM, scanning electron microscopy (SEM, energy dispersive X-ray (EDX, and wide-angle X-ray diffraction (WAXD analysis were used. The following four materials were prepared at room temperature: cured unmodified epoxy, cured toughened epoxy, cured unmodified epoxy/Cloisite 30B nanocomposites, and cured toughened epoxy/Cloisite 30B nanocomposites. Mixing process was performed by mechanical stirring. Poly(etheramine was used as the curing agent. The detailed TEM images revealed co-continuous and dispersed spherical rubber in the epoxy-rubber blend, suggesting a new proposed mechanism of phase separation. High-magnification TEM analysis showed good interactions between rubber and Cloisite 30B in the ternary system. Also, it was found that rubber particles could enhance the separation of silicates layers. Both XRD and TEM analyses confirmed that the intercalation of Cloisite 30B was achieved. No distinct exfoliated silicates were observed by TEM. Aggregates of layered silicates (tactoids were observed by SEM and EDX, in addition to TEM at low magnification. EDX analysis confirmed the presence of organic and inorganic elements in the binary and ternary epoxy systems containing Cloisite 30B.

ZnS, CdS and HgS Nanoparticles via Alkyl-Phenyl Dithiocarbamate Complexes as Single Source Precursors

OpenAIRE

Onwudiwe, Damian C.; Ajibade, Peter A.

2011-01-01

The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescen...

Characterization of structural properties of U and Pu in model systems by advanced synchrotron based X-ray spectroscopy

International Nuclear Information System (INIS)

Pidchenko, Ivan

2016-01-01

This dissertation presents the investigations of different U and Pu model systems relevant for safety assessment studies of nuclear waste repositories using the X-ray based synchrotron techniques: U and Pu L_3/M_4_,_5 edges HR-XANES, L_3 edge EXAFS and 3d4f RIXS as well as other complementary techniques, including XPS, XRD, SEM, TEM and UV-Vis-NIR techniques.

Microstructural characterization of nuclear-waste ceramics

International Nuclear Information System (INIS)

Ryerson, F.J.; Clarke, D.R.

1982-01-01

Characterization of nuclear waste ceramics requires techniques possessing high spatial and x-ray resolution. XRD, SEM, electron microprobe, TEM and analytical EM techniques are applied to ceramic formulations designed to immobilize both commercial and defense-related reactor wastes. These materials are used to address the strengths and limitations of the techniques above. An iterative approach combining all these techniques is suggested. 16 figures, 2 tables

New 'chimie douce' approach to the synthesis of hybrid nanosheets of MoS2 on CNT and their anti-friction and anti-wear properties.

Science.gov (United States)

Altavilla, Claudia; Sarno, Maria; Ciambelli, Paolo; Senatore, Adolfo; Petrone, Vincenzo

2013-03-29

Hybrid organic-inorganic oleylamine@MoS2-CNT nanocomposites with different compositions were obtained by thermal decomposition of tetrathiomolybdate in the presence of oleylamine and high quality multiwalled carbon nanotubes (CNTs) previously prepared by the CCVD technique. The nanocomposite samples were characterized by the TEM, SEM TG-MS, Raman and XRD techniques and successfully tested as anti-friction and anti-wear additives for grease lubricants.

Thioglycolic acid (TGA) assisted hydrothermal synthesis of SnS nanorods and nanosheets

International Nuclear Information System (INIS)

Biswas, Subhajit; Kar, Soumitra; Chaudhuri, Subhadra

2007-01-01

Nanorods and nanosheets of tin sulfide (SnS) were synthesized by a novel thioglycolic acid (TGA) assisted hydrothermal process. The as prepared nanostructures were characterized by X-ray diffraction (XRD) study, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). XRD study reveals the formation of well-crystallized orthorhombic structure of SnS. Diameter of the SnS nanorods varied within 30-100 nm. High-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) patterns identify the single crystalline nature for the SnS nanocrystals. The mechanism for the TGA assisted growth for the nanosheets and nanorods have been discussed

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

Science.gov (United States)

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.

Applications of the rotating orientation XRD method to oriented materials

International Nuclear Information System (INIS)

Guo Zhenqi; Li Fei; Jin Li; Bai Yu

2009-01-01

The rotating orientation x-ray diffraction (RO-XRD) method, based on conventional XRD instruments by a modification of the sample stage, was introduced to investigate the orientation-related issues of such materials. In this paper, we show its applications including the determination of single crystal orientation, assistance in crystal cutting and evaluation of crystal quality. The interpretation of scanning patterns by RO-XRD on polycrystals with large grains, bulk material with several grains and oriented thin film is also presented. These results will hopefully expand the applications of the RO-XRD method and also benefit the conventional XRD techniques. (fast track communication)

Evaluation of poly (vinyl alcohol) based cryogel–zinc oxide nanocomposites for possible applications as wound dressing materials

Energy Technology Data Exchange (ETDEWEB)

Chaturvedi, Archana [Bose Memorial Research Laboratory, Department of Chemistry, Government Autonomous Science College Jabalpur (India); Bajpai, Anil K., E-mail: akbmrl@yahoo.co.in [Bose Memorial Research Laboratory, Department of Chemistry, Government Autonomous Science College Jabalpur (India); Bajpai, Jaya [Bose Memorial Research Laboratory, Department of Chemistry, Government Autonomous Science College Jabalpur (India); Singh, Sunil K. [Department of Chemistry, Guru Ghasidas University, Bilaspur, CG (India)

2016-08-01

In this investigation cryogels composed of poly (vinyl alcohol) (PVA) were prepared by repeated freeze thaw method followed by in situ precipitation of zinc oxide nanoparticles within the cryogel networks. Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD), Energy dispersive X-ray spectroscopy (EDX) were used to characterize the nanocomposites. The morphologies of native PVA cryogels and PVA cryogel-ZnO nanocomposites were observed by scanning electron microscopy (SEM), transmission electron microscopy (TEM) techniques. The SEM analysis suggested that cryogels show a well-defined porous morphology whereas TEM micrographs revealed the presence of nearly spherical and well separated zinc oxide nanoparticles with diameter < 100 nm. XRD results showed all relevant Bragg's reflections for crystal structure of zinc oxide nanoparticles. Thermo gravimetric-differential thermal analysis (TG-DTA) was conducted to evaluate thermal stability of the nanocomposites. Mechanical properties of nanocomposites were determined in terms of tensile strength and percent elongation. Biocompatible nature was ascertained by anti-haemolytic activity, bovine serum albumin (blood protein) adsorption and in vitro cytotoxicity tests. The prepared nanocomposites were also investigated for swelling and deswelling behaviours. The results revealed that both the swelling and deswelling process depend on the chemical composition of the nanocomposites, number of freeze-thaw cycles, pH and temperature of the swelling medium. The developed biocompatible PVA cryogel-ZnO nanocomposites were also tested for antibacterial activities against both Gram-negative and Gram-positive bacteria. - Highlights: • PVA–zinc oxide nanocomposites have been prepared with no chemical crosslinking. • The nanocomposites are completely biocompatible. • They also show antibacterial property. • The nanocomposites

Global gyrokinetic simulations of TEM microturbulence

Science.gov (United States)

Vernay, T.; Brunner, S.; Villard, L.; McMillan, B. F.; Jolliet, S.; Bottino, A.; Görler, T.; Jenko, F.

2013-07-01

Global gyrokinetic simulations of electrostatic temperature-gradient-driven trapped-electron-mode (TEM) turbulence using the δf particle-in-cell code ORB5 are presented. The electron response is either fully kinetic or hybrid, i.e. considering kinetic trapped and adiabatic passing electrons. A linear benchmark in the TEM regime against the Eulerian-based code GENE is presented. Two different methods for controlling the numerical noise, based, respectively, on a Krook operator and a so-called coarse-graining approach, are discussed and successfully compared. Both linear and non-linear studies are carried out for addressing the issue of finite-ρ*-effects and finite electron collisionality on TEM turbulence. Electron collisions are found to damp TEMs through the detrapping process, while finite-ρ*-effects turn out to be important in the non-linear regime but very small in the linear regime. Finally, the effects of zonal flows on TEM turbulence are briefly considered as well and shown to be unimportant in the temperature-gradient-driven TEM regime. Consistently, basically no difference is found between linear and non-linear critical electron temperature gradients in the TEM regime.

Synthesis of nano-sized ceria (CeO2 particles via a cerium hydroxy carbonate precursor and the effect of reaction temperature on particle morphology

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Majid Farahmandjou

2015-06-01

Full Text Available Cerium oxide (CeO2 or ceria has been shown to be an interesting support material for noble metals in catalysts designed for emission control, mainly due to its oxygen storage capacity. Ceria nanoparticles were prepared by precipitation method. The precursor materials used in this research were cerium nitrate hexahydrate (as a basic material, potassium carbonate and potassium hydroxide (as precipitants. The morphological properties were characterized by high resolution transmission electron microscopy (HRTEM, scanning electron microscopy (SEM and X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR and UV-Vis spectrophotometer. XRD results showed face centered cubic CeO2 nanoparticles for annealed nanoparticles at 1000°C. SEM measurement showed that by increasing the calcinations temperature from 200 to 600°C, the crystallite size decreased from 90 to 28 nm. The SEM results showed that the size of the CeO2 nanoparticles decreased with increasing temperature. The particle size of CeO2 was around 25 nm as estimated by XRD technique and direct HRTEM observation. SEM and TEM studies showed that the morphology of the prepared powder was sphere-like with a narrow size distribution. The sharp peaks in FTIR spectrum determined the purity of CeO2 nanoparticles and absorbance peak of UV-Vis spectrum showed the small band gap energy of 3.26 ev.

Characterization, Antibacterial and Antioxidant Properties of Silver Nanoparticles Synthesized from Aqueous Extracts of Allium sativum, Zingiber officinale, and Capsicum frutescens.

Science.gov (United States)

Otunola, Gloria Aderonke; Afolayan, Anthony Jide; Ajayi, Emmanuel Olusegun; Odeyemi, Samuel Wale

2017-07-01

Herbal drug delivery is limited by poor solubility and bioavailability which can be overcome with suitable nanomaterials that will enhance their pharmacokinetics and performance. This study aimed to analyze the synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from three spices. AgNPs were prepared using 0.1 M silver nitrate and aqueous extracts of Allium sativum L. (garlic), Zingiber officinale Rosc. (ginger), and Capsicum frutescens L. (cayenne pepper). The AgNPs were characterized using ultraviolet-visible (UV-Vis) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray, X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. The AgNPs were formed within an hour of the reaction and showed maximum UV-Vis absorption in the 375-480 nm range. SEM and TEM revealed well-dispersed spherical particles with little agglomeration, average sizes of 3-6 nm, 3-22 nm, and 3-18 nm for garlic, ginger, and cayenne pepper, respectively. FTIR showed that amine, protein, phenolic, aromatic, and alkynes groups contributed to AgNP synthesis and XRD confirmed their crystalline and face-centered cubic nature. Antibacterial action of the AgNPs was in the following order: ginger (minimum inhibitory concentration [MIC] garlic> cayenne pepper (MIC 125 μg/mL). Antioxidant action showed cayenne pepper > ginger > garlic (inhibitory concentration 50% [IC50]: 40, 240, and 250 μg/mL, respectively) against 2,2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid) and garlic > cayenne pepper > ginger (IC50: <31.25, 40, and 120 μg/mL, respectively) against 1,1-diphenyl-2-picrylhydrazyl. Optimization of this green synthesis would support the production of AgNPs with great therapeutic potentials. The synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from garlic, ginger and cayenne pepper were evaluatedThe AgNPs formed were characterized using UV

Three-dimensional intracellular structure of a whole rice mesophyll cell observed with FIB-SEM.

Science.gov (United States)

Oi, Takao; Enomoto, Sakiko; Nakao, Tomoyo; Arai, Shigeo; Yamane, Koji; Taniguchi, Mitsutaka

2017-07-01

Ultrathin sections of rice leaf blades observed two-dimensionally using a transmission electron microscope (TEM) show that the chlorenchyma is composed of lobed mesophyll cells, with intricate cell boundaries, and lined with chloroplasts. The lobed cell shape and chloroplast positioning are believed to enhance the area available for the gas exchange surface for photosynthesis in rice leaves. However, a cell image revealing the three-dimensional (3-D) ultrastructure of rice mesophyll cells has not been visualized. In this study, a whole rice mesophyll cell was observed using a focused ion beam scanning electron microscope (FIB-SEM), which provides many serial sections automatically, rapidly and correctly, thereby enabling 3-D cell structure reconstruction. Rice leaf blades were fixed chemically using the method for conventional TEM observation, embedded in resin and subsequently set in the FIB-SEM chamber. Specimen blocks were sectioned transversely using the FIB, and block-face images were captured using the SEM. The sectioning and imaging were repeated overnight for 200-500 slices (each 50 nm thick). The resultant large-volume image stacks ( x = 25 μm, y = 25 μm, z = 10-25 μm) contained one or two whole mesophyll cells. The 3-D models of whole mesophyll cells were reconstructed using image processing software. The reconstructed cell models were discoid shaped with several lobes around the cell periphery. The cell shape increased the surface area, and the ratio of surface area to volume was twice that of a cylinder having the same volume. The chloroplasts occupied half the cell volume and spread as sheets along the cell lobes, covering most of the inner cell surface, with adjacent chloroplasts in close contact with each other. Cellular and sub-cellular ultrastructures of a whole mesophyll cell in a rice leaf blade are demonstrated three-dimensionally using a FIB-SEM. The 3-D models and numerical information support the hypothesis that rice mesophyll

SEM Anthology

Science.gov (United States)

Rodgers, Michelle; Zimar, Heather

2004-01-01

The "SEM Anthology" is a compilation of articles by more than 30 enrollment management professionals from a variety of institutions across the country. This collection, which has appeared in SEM Monthly over the past year, chronicles Strategic Enrollment Management efforts at campuses nationwide. The book illustrates the successes and challenges…

Hybrid Organometallic-Inorganic Nanomaterial: Acetyl Ferrocene Schiff base Immobilized on Silica Coated Magnetite Nanoparticles

Directory of Open Access Journals (Sweden)

M. Masteri-Farahani

2015-10-01

Full Text Available In  this  work,  a  new  hybrid  organometallic-inorganic  hybrid nanomaterial was prepared by immobilization of acetyl ferrocene on the  surface  of magnetite  nanoparticles. Covalent  grafting of silica coated magnetite nanoparticles (SCMNPs with 3-aminopropyl triethoxysilane gave aminopropyl-modified magnetite nanoparticles (AmpSCMNPs. Then, Schiff base condensation  of AmpSCMNPs with acetyl  ferrocene resulted in the preparation of acferro-SCMNPs hybrid nanomaterial. Characterization of the prepared nanomaterial was performed with different physicochemical methods such as Fourier transform infrared spectroscopy (FT-IR, X-ray diffraction (XRD, vibrating sample magnetometry (VSM, thermogravimetric analysis (TGA, scanning electron microscopy (SEM, and transmission electron microscopy (TEM. VSM analysis showed superparamagnetic properties of the prepared nanomaterial and TEM and SEM analyses indicated the relatively spherical nanoparticles with 15 nm average size.

Functionalized SiC nanocrystals for tuning of optical, thermal, mechanical and electrical properties of polyvinyl alcohol

DEFF Research Database (Denmark)

Saini, Isha; Sharma, Annu; Dhiman, Rajnish

2017-01-01

 MPa for PVA to 45 MPa for PVA-SiC nanocomposite film containing 0.023 wt% f-SiC nanocrystals at an applied load of 9.8 mN indicating improved interfacial interaction. Current-voltage analysis indicated an increase in conductivity of PVA with the introduction of f-SiC nanocrystals. The conduction......Polyvinyl alcohol (PVA)-SiC nanocomposite films were prepared by incorporating functionalized Silicon Carbide (f-SiC) nanocrystals in PVA matrix. Structural characterization of SiC nanocrystals before and after the functionalization was carried out using Fourier transform infrared spectroscopy...... (FTIR), X-ray diffraction (XRD) and Thermogravimetric analysis (TGA). Transmission electron microscopy (TEM) and Scanning Electron Microscopy (SEM) were used to study the morphology and size distribution of f-SiC nanocrystals in PVA-SiC nanocomposite films. TEM and SEM images depict an improved...

Rod-like zinc oxide constructed by nanoparticles: synthesis, characterization and optical properties

Energy Technology Data Exchange (ETDEWEB)

Jia Zhigang [Chemisty Department, Zhejiang University, Hangzhou 310027 (China); Yue Linhai [Chemisty Department, Zhejiang University, Hangzhou 310027 (China)], E-mail: zjchem_yue@126.com; Zheng Yifan [College of Chemical Engineering and Materials, Zhejiang University of Technology, Hangzhou 310014 (China); Xu Zhude [Chemisty Department, Zhejiang University, Hangzhou 310027 (China)

2008-01-15

One-dimensional (1D) rod-like structure of znic oxide constructed by nanoparticles was synthesized by the thermal treatment of zinc oxalate sub-micron rods, which were obtained via alcohol thermal process. The samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) and photoluminescence (PL) spectrum. SEM and TEM show that the morphology of zinc oxalate dihydrate precursor is rod-like, about 400 nm in average diameter and 3 {mu}m in average length. The zinc oxide obtained by annealing zinc oxalate exhibits 1D rod-like structure constructed by ZnO nanoparticles in original direction of the precursor. The room-temperature photoluminescence spectrum of as-prepared ZnO shows UV emission around 398 nm and a diverse visible emission peaks indicating that there are deep level defects in ZnO nanoparticles.

Rod-like zinc oxide constructed by nanoparticles: synthesis, characterization and optical properties

International Nuclear Information System (INIS)

Jia Zhigang; Yue Linhai; Zheng Yifan; Xu Zhude

2008-01-01

One-dimensional (1D) rod-like structure of znic oxide constructed by nanoparticles was synthesized by the thermal treatment of zinc oxalate sub-micron rods, which were obtained via alcohol thermal process. The samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) and photoluminescence (PL) spectrum. SEM and TEM show that the morphology of zinc oxalate dihydrate precursor is rod-like, about 400 nm in average diameter and 3 μm in average length. The zinc oxide obtained by annealing zinc oxalate exhibits 1D rod-like structure constructed by ZnO nanoparticles in original direction of the precursor. The room-temperature photoluminescence spectrum of as-prepared ZnO shows UV emission around 398 nm and a diverse visible emission peaks indicating that there are deep level defects in ZnO nanoparticles

TEM turbulence optimisation in stellarators

Science.gov (United States)

Proll, J. H. E.; Mynick, H. E.; Xanthopoulos, P.; Lazerson, S. A.; Faber, B. J.

2016-01-01

With the advent of neoclassically optimised stellarators, optimising stellarators for turbulent transport is an important next step. The reduction of ion-temperature-gradient-driven turbulence has been achieved via shaping of the magnetic field, and the reduction of trapped-electron mode (TEM) turbulence is addressed in the present paper. Recent analytical and numerical findings suggest TEMs are stabilised when a large fraction of trapped particles experiences favourable bounce-averaged curvature. This is the case for example in Wendelstein 7-X (Beidler et al 1990 Fusion Technol. 17 148) and other Helias-type stellarators. Using this knowledge, a proxy function was designed to estimate the TEM dynamics, allowing optimal configurations for TEM stability to be determined with the STELLOPT (Spong et al 2001 Nucl. Fusion 41 711) code without extensive turbulence simulations. A first proof-of-principle optimised equilibrium stemming from the TEM-dominated stellarator experiment HSX (Anderson et al 1995 Fusion Technol. 27 273) is presented for which a reduction of the linear growth rates is achieved over a broad range of the operational parameter space. As an important consequence of this property, the turbulent heat flux levels are reduced compared with the initial configuration.

Kinetic and morphological differentiation of ettringites in plain and blended Portland cements with metakaolin and the ASTM C 452-68 test. Part II: Morphological differentiation by SEM and XRD analysis

Directory of Open Access Journals (Sweden)

Talero, R.

2009-03-01

Full Text Available The same cementitious materials (OPCs, SRPCs and matekaolin, MK, the same blended cements and the same ASTM C 452-68 test than in Part I, were used. Other complementary determinations were: chemical analysis of cementing materials, SEM and XRD analysis of ettringites and specific properties of some cement tested and of their pastes.The experimental results have also demonstrated that when 7.0% SO3, equivalent to 15.05% of gypsum, was added to the M pozzolan-containing Portland cement and tested with the ASTM C 452-68 method, it was not found to behave aggressively but rather as “setting regulator ”, because the increase in mechanical strengths over time and setting times in these mixes were, therefore, similar to the pattern observed in any PC. However, when the gypsum content was raised to triple than that amount (21.0% SO3, it behaved aggressively. In both cases, logically, ettringite from both origins were involved in the resulting beneficial or adverse behavior.En esta Parte II se utilizaron los mismos materiales cementíceos (CPO, CPRS, y metakaolín, MK, los mismos cementos de mezcla y el mismo método de ensayo ASTM C 452-68 que en la Parte I. Otras determinaciones complementarias fueron: análisis químico de los materiales cementíceos, análisis por DRX y SEM de ettringitas y propiedades específicas de algunos cementos ensayados y de sus pastas.Los resultados experimentales obtenidos han demostrado también que, el 7.0% de SO3 presente en los 30 cementos de mezcla con MK, ensayados conforme el método ASTM C 452-68, no se comporta como agresivo sino como ”regulador de fraguado”, porque los tiempos de fraguado y el aumento de resistencias mecánicas fueron como los de cualquier CP. De aquí que algunos de esos cementos de mezcla puedan ser considerados “cementos hidráulicos expansivos”, el resto, no. Sin embargo, cuando la cantidad de yeso aportada fue el triple (21,0% SO3, se comportó como agresivo, motivo por el cual

Fabrication of an Electrically-Resistive, Varistor-Polymer Composite

Directory of Open Access Journals (Sweden)

Sanaz A. Mohammadi

2012-11-01

Full Text Available This study focuses on the fabrication and electrical characterization of a polymer composite based on nano-sized varistor powder. The polymer composite was fabricated by the melt-blending method. The developed nano-composite was characterized by X-ray diffraction (XRD, transmission electron microscopy (TEM, field emission scanning electron microscopy (FeSEM, and energy-dispersive X-ray spectroscopy (EDAX. The XRD pattern revealed the crystallinity of the composite. The XRD study also showed the presence of secondary phases due to the substitution of zinc by other cations, such as bismuth and manganese. The TEM picture of the sample revealed the distribution of the spherical, nano-sized, filler particles throughout the matrix, which were in the 10–50 nm range with an average of approximately 11 nm. The presence of a bismuth-rich phase and a ZnO matrix phase in the ZnO-based varistor powder was confirmed by FeSEM images and EDX spectra. From the current-voltage curves, the non-linear coefficient of the varistor polymer composite with 70 wt% of nano filler was 3.57, and its electrical resistivity after the onset point was 861 KΩ. The non-linear coefficient was 1.11 in the sample with 100 wt% polymer content. Thus, it was concluded that the composites established a better electrical non-linearity at higher filler amounts due to the nano-metric structure and closer particle linkages.

Pre-concentration of pesticide residues in environmental water samples using Silica nanoparticles and identification of residues By GC-MS method

OpenAIRE

Tentu. Nageswara Rao; A. Muralidhar Reddy; SNVS. Murthy; Prathipati Revathi; K. Suneel Kumar

2016-01-01

The silica nanoparticles prepared by stober’s mechanism by reaction of tetraethylorthosilicate (TEOS) with ammonia was tested for their adsorption capacity in the pre-concentration of residues of pesticides in water. The synthesized nanoparticles were characterized by Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and X-Ray Diffraction (XRD). The size of the silica nanoparticles were 50 to 250 nm. The solid phase extraction (SPE) cartridges were prepared by filling...

Advanced SEM imaging

International Nuclear Information System (INIS)

Joy, D. C.; Newbury, D. E.

1998-01-01

The scanning electron microscope (SEM) represents the most promising tool for metrology, defect review, and for the analysis of ULSI structures, but both fundamental problems such as electron-solid interactions, and practical considerations such as electron-optical constraints, are now setting a limit to performance. This paper examines the directions in which an advanced SEM might be developed to overcome these constraints. The SEM also offers considerable promise as a tool for the high spatial resolution X-ray microanalysis, especially for those situations where a thin cross-section is not practical and first surface analysis is required. The ways in which this capability can be incorporated in an advanced SEM are examined

Advanced SEM imaging

International Nuclear Information System (INIS)

Joy, D.C.; Newbury, D.E.; Newbury, D.E.

1998-01-01

The scanning electron microscope (SEM) represents the most promising tool for metrology, defect review, and for the analysis of ULSI structures, but both fundamental problems such as electron-solid interactions, and practical considerations such as electron-optical constraints, are now setting a limit to performance. This paper examines the directions in which an advanced SEM might be developed to overcome these constraints. The SEM also offers considerable promise as a tool for the high spatial resolution X-ray microanalysis, especially for those situations where a thin cross-section is not practical and first surface analysis is required. The ways in which this capability can be incorporated in an advanced SEM are examined. copyright 1998 American Institute of Physics

Stability of mineral fibres in contact with human cell cultures. An in situ μXANES, μXRD and XRF iron mapping study.

Science.gov (United States)

Pollastri, Simone; Gualtieri, Alessandro F; Vigliaturo, Ruggero; Ignatyev, Konstantin; Strafella, Elisabetta; Pugnaloni, Armanda; Croce, Alessandro

2016-12-01

Relevant mineral fibres of social and economic importance (chrysotile UICC, crocidolite UICC and a fibrous erionite from Jersey, Nevada, USA) were put in contact with cultured diploid human non-tumorigenic bronchial epithelial (Beas2B) and pleural transformed mesothelial (MeT5A) cells to test their cytotoxicity. Slides of each sample at different contact times up to 96 h were studied in situ using synchrotron XRF, μ-XRD and μ-XAS (I18 beamline, Diamond Light Source, UK) and TEM investigations. XRF maps of samples treated for 96 h evidenced that iron is still present within the chrysotile and crocidolite fibres and retained at the surface of the erionite fibres, indicating its null to minor mobilization in contact with cell media; this picture was confirmed by the results of XANES pre-edge analyses. μ-XRD and TEM data indicate greater morphological and crystallinity modifications occurring in chrysotile, whereas crocidolite and erionite show to be resistant in the biological environment. The contact of chrysotile with the cell cultures seems to lead to earlier amorphization, interpreted as the first dissolution step of these fibres. The formation of such silica-rich fibre skeleton may prompt the production of HO in synergy with surface iron species and could indicate that chrysotile may be much more reactive and cytotoxic in vitro in the (very) short term whereas the activity of crocidolite and erionite would be much more sluggish but persistent in the long term. Copyright © 2016 Elsevier Ltd. All rights reserved.

Deuterium-induced nanostructure formation on tungsten exposed to high-flux plasma

Energy Technology Data Exchange (ETDEWEB)

Xu, H.Y., E-mail: donaxu@163.com [Key Laboratory of Advanced Materials, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Science and Technology on Surface Physics and Chemistry Laboratory, Mianyang, Sichuan 621907 (China); De Temmerman, G. [FOM Institute DIFFER, Dutch Institute For Fundamental Energy Research, Ass. EURATOM-FOM, Trilateral Euregio Cluster, Postbus 1207, 3430BE Nieuwegein (Netherlands); ITER Organization, Route de Vinon-sur-Verdon CS 90046-13067, St Paul Lez Durance Cedex (France); Luo, G.-N. [Institute of Plasma Physics, Chinese Academy of Sciences, Hefei, Anhui 230031 (China); Jia, Y.Z.; Yuan, Y.; Fu, B.Q.; Godfrey, A. [Key Laboratory of Advanced Materials, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Liu, W., E-mail: liuw@mail.tsinghua.edu.cn [Key Laboratory of Advanced Materials, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China)

2015-08-15

Surface topography of polycrystalline tungsten (W) have been examined after exposure to a low-energy (38 eV/D), high-flux (∼1.1–1.5 × 10{sup 24} m{sup −2} s{sup −1}) deuterium plasma in the Pilot-PSI linear plasma device. The methods used were scanning electron microscopy (SEM), transmission electron microscopy (TEM), positron annihilation Doppler broadening (PADB) and grazing incident X-ray diffraction (GI-XRD). After exposure to high flux D plasma, blisters and nanostructures are formed on the W surface. Generation of defects was evidenced by PADB, while high stress and mixture of phases were detected in depth of 50 nm by GI-XRD. TEM observation revealed fluctuations and disordered microstructure on the outmost surface layer. Based on these results, surface reconstruction is considered as a possible mechanism for the formation of defects and nanostructures.

Accelerator-tem interface facility and application

International Nuclear Information System (INIS)

Li Ming; He Jun; Yang Zheng; Zhou Lin; Liu Chuansheng; Guo Liping; Jiang Changzhong; Yang Shibo; Fu Dejun; Fan Xiangjun; Liu Jiarui; Lee, J.C.

2010-01-01

An accelerator-TEM interface facility has been established at Wuhan University. The system consists of an H800 TEM linked to a 200 kV ion implanter and a 2 x 1.7 MV tandetron accelerator. Measures were taken to isolate the TEM from mechanical vibration transmitted from the ion beam lines and good resolution was maintained with the TEM machine when operated under high zoom modes during the ion implantation. Nitrogen ions at 115 keV were successfully transported from the implanter into the TEM chamber through the interface system, and the ion currents measured at the entrance of the TEM column were between 20 and 180 nA. Structural evolution caused by ion irradiation in Si, GaAs, nanocrystal Ag were observed in situ. The TEM sample could be tilted by 52 degree and for low energy ion irradiation, real time observation was realized. The in situ observation showed that the critical implant dose for amorphization of Si is 2 x 10 14 cm -2 and it became fully amorphized at 3 x 10 15 cm -2 . Amorphization of GaAs started at 1 x 10 14 cm -2 , whereas for nanocrystal Ag, the starting dose was 6 x 10 14 cm -2 . The nuclear material C276 samples implanted with 115 keV Ar+ was also studied and dislocation loops with sizes of 3-12 nm were clearly observed after implantation to doses higher than 1 x 10 15 cm -2 . The density of the loops increased with the increase in the implant dose and evolution to polycrystalline and amorphous structures were observed at 5 x 10 15 cm -2 and 3 x 10 16 cm -2 , respectively. An in situ RBS/C chamber has been installed on the transport line of the accelerator-TEM interface system. This makes it possible to in situ measure composition and location of impurities in the lattice of the implanted samples. In addition, a 50 kV low-energy gaseous ion generator was installed close to the TEM chamber, which facilitates in situ TEM observation of helium bubbles formed in materials by helium implantation. (authors)

Recent advances in FIB-TEM specimen preparation techniques

International Nuclear Information System (INIS)

Li Jian; Malis, T.; Dionne, S.

2006-01-01

Preparing high-quality transmission electron microscopy (TEM) specimens is of paramount importance in TEM studies. The development of the focused ion beam (FIB) microscope has greatly enhanced TEM specimen preparation capabilities. In recent years, various FIB-TEM foil preparation techniques have been developed. However, the currently available techniques fail to produce TEM specimens from fragile and ultra-fine specimens such as fine fibers. In this paper, the conventional FIB-TEM specimen preparation techniques are reviewed, and their advantages and shortcomings are compared. In addition, a new technique suitable to prepare TEM samples from ultra-fine specimens is demonstrated

Influence of smectite suspension structure on sheet orientation in dry sediments: XRD and AFM applications.

Science.gov (United States)

Zbik, Marek S; Frost, Ray L

2010-06-15

The structure-building phenomena within clay aggregates are governed by forces acting between clay particles. Measurements of such forces are important to understand in order to manipulate the aggregate structure for applications such as dewatering of mineral processing tailings. A parallel particle orientation is required when conducting XRD investigation on the oriented samples and conduct force measurements acting between basal planes of clay mineral platelets using atomic force microscopy (AFM). To investigate how smectite clay platelets were oriented on silicon wafer substrate when dried from suspension range of methods like SEM, XRD and AFM were employed. From these investigations, we conclude that high clay concentrations and larger particle diameters (up to 5 microm) in suspension result in random orientation of platelets in the substrate. The best possible laminar orientation in the clay dry film, represented in the XRD 001/020 intensity ratio of 47 was obtained by drying thin layers from 0.02 wt.% clay suspensions of the natural pH. Conducted AFM investigations show that smectite studied in water based electrolytes show very long-range repulsive forces lower in strength than electrostatic forces from double-layer repulsion. It was suggested that these forces may have structural nature. Smectite surface layers rehydrate in water environment forms surface gel with spongy and cellular texture which cushion approaching AFM probe. This structural effect can be measured in distances larger than 1000 nm from substrate surface and when probe penetrate this gel layer, structural linkages are forming between substrate and clay covered probe. These linkages prevent subsequently smooth detachments of AFM probe on way back when retrieval. This effect of tearing new formed structure apart involves larger adhesion-like forces measured in retrieval. It is also suggested that these effect may be enhanced by the nano-clay particles interaction. 2010 Elsevier Inc. All

TEMS: results of a specialist centre.

Science.gov (United States)

Flexer, S M; Durham-Hall, A C; Steward, M A; Robinson, J M

2014-06-01

Transanal endoscopic microsurgery (TEMS) is becoming more widespread due to the increasing body of evidence to support its role. Previous published data has reported recurrence rates in excess of 10% for benign polyps after TEMS. Bradford Royal Infirmary is a tertiary referral centre for TEMS and early rectal cancer in the UK. Data for all TEMS operations were entered into a prospective database over a 7-year period. Demographic data, complications and recurrence rates were recorded. Both benign adenomas and malignant lesions were included. A total of 164 patients (65% male), with a mean age of 68 years were included; 114 (70%) of the lesions resected were benign adenomas, and 50 (30%) were malignant lesions. Median polyp size was 4 (range 0.6-14.5) cm. Mean length of operation was 55 (range 10-120) min. There were no recurrences in any patients with a benign adenoma resected; two patients with malignant lesions developed recurrences. Three intra-operative complications were recorded, two rectal perforations (repaired primarily, one requiring defunctioning stoma), and a further patient suffered a blood loss of >300 ml requiring transfusion. Six patients developed strictures requiring dilation either endoscopically or under anaesthetic in the post-operative period. We have demonstrated that TEMS procedures performed in a specialist centre provide low rates of both recurrence and complication. Within a specialist centre, TEMS surgery should be offered to all patients for rectal lesions, both benign and malignant, that are amenable to TEMS.

Investigation on by-products of bioenergy systems (anaerobic digestion and gasification) as potential crop nutrient using FTIR, XRD, SEM analysis and phyto-toxicity test.

Science.gov (United States)

Kataki, Sampriti; Hazarika, Samarendra; Baruah, D C

2017-07-01

Success and acceptability of the bio energy conversion technology to a large extent depend upon management of the inevitable by-products generated during the conversion process. By-products can be considered favourable as organic fertilizer as they retain nutrients with varying composition depending upon input biomass. However, characteristics of these heterogeneous resources with respect to feedstock and processing conditions have to be assessed to state on their agricultural and environmental benefits. Therefore, 3 types of anaerobic digestion by-products (digestate) from surplus biomass viz. cow dung, Ipomoea carnea:cow dung (60:40 dry weight basis) and rice straw:green gram stover:cow dung (30:30:40 dry weight basis) and one gasification by-product (biochar) from rice husk are considered to understand the fertilizer prospects. Considering 3 potential application options, digestate from each feedstock option was further processed as separated solid, separated liquid and ash from solid digestates. Thus, a total of 10 by-products were investigated for understanding their prospects as fertilizer using Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive X ray Spectroscopy (EDX) and phyto-toxicity test to have a broad insight in terms of their organic, mineral, elemental composition, morphological feature and potential phyto-toxicity. In general, irrespective of origin of feedstock, solid digestate, ash digestate and char showed similarity in terms of composition of functional groups with some degree of variation in relative content as reflected by FTIR analysis. Dominance of organic functional groups in separated solid digestates compared to liquid fraction indicated the former as favourable organic amendments. Quartz was the prevalent mineral phase in all separated solid, ash digestate and rice husk char. Digestates in ash phase represent more concentrated plant nutrient source with

First oxygen from lunar basalt

Science.gov (United States)

Gibson, M. A.; Knudsen, C. W.; Brueneman, D. J.; Kanamori, H.; Ness, R. O.; Sharp, L. L.; Brekke, D. W.; Allen, C. C.; Morris, R. V.; Keller, L. P.

1993-01-01

The Carbotek/Shimizu process to produce oxygen from lunar soils has been successfully demonstrated on actual lunar samples in laboratory facilities at Carbotek with Shimizu funding and support. Apollo sample 70035 containing approximately 25 percent ilmenite (FeTiO3) was used in seven separate reactions with hydrogen varying temperature and pressure: FeTiO3 + H2 yields Fe + TiO2 + H2O. The experiments gave extremely encouraging results as all ilmenite was reduced in every experiment. The lunar ilmenite was found to be about twice as reactive as terrestrial ilmenite samples. Analytical techniques of the lunar and terrestrial ilmenite experiments performed by NASA Johnson Space Center include iron Mossbauer spectroscopy (FeMS), optical microscopy, SEM, TEM, and XRD. The Energy and Environmental Research Center at the University of North Dakota performed three SEM techniques (point count method, morphology determination, elemental mapping), XRD, and optical microscopy.

Synthesis and characterization of silver nanoparticle composite with poly(p-Br-phenylsilane).

Science.gov (United States)

Kim, Myoung-Hee; Lee, Jun; Mo, Soo-Yong; Woo, Hee-Gweon; Yang, Kap Seung; Kim, Bo-Hye; Lee, Byeong-Gweon; Sohn, Honglae

2012-05-01

The one-pot synthesis and characterization of silver nanoparticle-poly(p-Br-phenylsilane) composites have been carried out. The conversion of silver(+1) salt to stable silver(0) nanoparticles is promoted by poly(p-Br-phenylsilane), Br-PPS possessing both possible reactive Si-H bonds in the polymer backbone and C-Br bonds in the substituents. The composites were characterized using XRD, TEM, FE-SEM, and solid-state UV-vis analytical techniques. TEM and FE-SEM data show the formation of the composites where large number of silver nanoparticles (less than 30 nm of size) are well dispersed throughout the Br-PPS matrix. XRD patterns are consistent with that for fcc-typed silver. The elemental analysis for Br atom and the polymer solubility confirm that the cleavage of C-Br bond and the Si-Br dative bonding were not occurred appreciably at ambient temperature. Nonetheless, TGA data suggest that some sort of cross-linking was occurred at high temperature. The size and processability of such nanoparticles depend on the ratio of metal to Br-PPS. In the absence of Br-PPS, most of the silver particles undergo macroscopic aggregation, which indicates that the polysilane is necessary for stabilizing the silver nanoparticles.

Influence of Ce Doping on the Electrical and Optical Properties of TiO2 and Its Photocatalytic Activity for the Degradation of Remazol Brilliant Blue R

Directory of Open Access Journals (Sweden)

Aisha Malik

2013-01-01

Full Text Available Nanocrystalline TiO2 particles doped with different concentrations of Cerium (Ce, 1–10% have been synthesized using sol-gel method. The prepared particles were characterized by standard analytical techniques such as X-ray diffraction (XRD, FTIR and Scanning Electron Microscopy (SEM, and Transmission Electron Microscopy (TEM. The XRD analysis shows no change in crystal structure of TiO2 after doping with different concentrations of Ce, which indicates the single-phase polycrystalline material. The SEM analysis shows the partial crystalline nature of undoped, and doped TiO2 and TEM analysis shows the particle sizes were in the range of 9–14 nm in size. The a.c. analysis shows that the dielectric constant ε and dielectric loss tan δ decrease with the increase in frequency. The dielectric property decreases with the increase in dopant concentration. It is also observed that the impedance increases with an increase in dopant concentration. The photocatalytic activity of the synthesized particles (Ce-doped TiO2 with dopant concentration of 9% (Ce showed the highest photocatalytic activity for the degradation of the dye derivative Remazol Brilliant Blue R in an immersion well photochemical reactor with 500 W halogen linear lamp in the presence of atmospheric oxygen.

Steam-assisted crystallization of TPA+-exchanged MCM-41 type mesoporous materials with thick pore walls

International Nuclear Information System (INIS)

Chen, Hong Li; Zhang, Kun; Wang, Yi Meng

2012-01-01

Highlights: ► Mesoporous Ti-containing silica with thicker pore walls was synthesized. ► Ion-exchange and steam-assisted crystallization led to MCM-41/MFI composite. ► The introduction of Ti inhibited the formation of separated MFI particles. ► Lower temperature favored retaining mesoporous characteristics and morphology. -- Abstract: Hierarchical MCM-41/MFI composites were synthesized through ion-exchange of as-made MCM-41 type mesoporous materials with tetrapropylammonium bromide and subsequent steam-assisted recrystallization. The obtained samples were characterized by powder X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis, FT-IR, 1 H– 13 C CP/MAS and nitrogen adsorption–desorption. The XRD patterns show that the MCM-41/MFI composite possesses both ordered MCM-41 phase and zeolite MFI phase. SEM and TEM images indicate that the recrystallized materials retained the mesoporous characteristics and the morphology of as-made mesoporous materials without the formation of bulky zeolite, quite different from the mechanical mixture of MCM-41 and MFI structured zeolite. Among others, lower recrystallization temperature and the introduction of the titanium to the parent materials are beneficial to preserve the mesoporous structure during the recrystallization process.

THERMAL EXPANSION BEHAVIOR OF THE Ba0.2Sr0.8Co0.8Fe0.2O3−δ (BSCF WITH Sm0.2Ce0.8O1.9

Directory of Open Access Journals (Sweden)

M. AHMADREZAEI

2014-03-01

Full Text Available Nanostructured perovskite oxides of Ba0.2Sr0.8Co0.8Fe0.2O3−δ (BSCF were synthesized through the co-precipitation method. The thermal decomposition, phase formation and thermal expansion behavior of BSCF were characterized by thermogravimetric analysis, X-ray diffraction (XRD, and dilatometry, respectively. XRD peaks were indexed to a cubic perovskite structure with a Pm3m (221 space group. All the combined oxides produced the desired perovskite-phase BSCF. The microstructures were characterized by scanning electron microscopy (SEM and transmission electron microscopy (TEM. The TEM analysis showed that BSCF powders had uniform nanoparticle sizes and high homogeneity. The cross-sectional SEM micrograph of BSCF exhibited a continuous and no delaminated layer from the electrolyte-supported cell. The thermal expansion coefficient (TEC of BSCF was 16.2×10-6 K-1 at a temperature range of 600°C to 800°C. Additional experiments showed that the TEC of BSCF is comparable to that of Sm0.2Ce0.8O1.9 (SDC within the same temperature range. The results demonstrate that BSFC is a promising cathode material for intermediate-temperature solid-oxide fuel cells.

Design of carbon nanofiber embedded conducting epoxy resin

International Nuclear Information System (INIS)

Gantayat, Subhra; Sarkar, Niladri; Rout, Dibyaranjan; Swain, Sarat K.

2017-01-01

Acid treated carbon nanofiber (t-CNF) reinforced epoxy nanocomposites were fabricated by hand lay-up method with various wt % of t-CNF loadings. Pristine or unmodified carbon nano fibers (u-CNFs) were made compatible with epoxy matrix by means of mixed acid treatment. Fabricated nanocomposites were characterized with Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) study, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM). Mechanical and thermal properties of the nanocomposites were measured as a function of t-CNF content. Effect of acid treated CNFs on to the mechanical properties of epoxy nanocomposites was justified by comparing the mechanical properties of epoxy/t-CNF and epoxy/u-CNF nanocomposites with same loading level. The electrical conductivity was achieved by epoxy resin with a threshold at 1 wt % of t-CNF. Substantial improvement in thermal, mechanical and electrical properties of the synthesized epoxy/t-CNF nanocomposites may be suitable for fabricating electronic devices. - Highlights: • Epoxy/t-CNF nanocomposites are characterized by XRD, FTIR, SEM, AFM and TEM. • Electrical conductivity was achieved by epoxy with a threshold at 1 wt% of t-CNF. • Tensile strength is enhanced by 40% due to dispersion of t-CNF. • Synthesized nanocomposites are suitable for fabricating electronic devises.

Flux Growth of Highly Crystalline Photocatalytic BaTiO3 Particle Layers on Porous Titanium Sponge Substrate and Insights into the Formation Mechanism

Science.gov (United States)

Wang, Q.; Li, B.

2017-09-01

A unique architecture of idiomorphic and highly crystalline BaTiO3 particle layers directly grown on a porous titanium sponge substrate was successfully achieved for the first time using a facile molten salt method at a relatively low temperature of 700 °C. Specifically, the low-melting KCl-NaCl eutectic salts and barium hydroxide octahydrate were employed as the reaction medium and barium source, respectively. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and UV-vis diffuse reflectance spectrophotometry were used to characterize the structure, morphology and optical property of the obtained samples. The results revealed that the flux-grown tetragonal BaTiO3 products had well-defined and uniform morphology with an average size of 300 nm and a band gap of ∼3.16 eV. Based on XRD, EDS, SEM, and TEM, the possible formation mechanism responsible for the well-developed architecture of BaTiO3 particle layers was proposed and discussed. Furthermore, the photocatalytic activity of the flux-grown BaTiO3 products for organic pollutant degradation under simulated sunlight irradiation was also investigated.

Design of carbon nanofiber embedded conducting epoxy resin

Energy Technology Data Exchange (ETDEWEB)

Gantayat, Subhra [Department of Chemistry, Veer Surendra Sai University of Technology, Burla, Sambalpur 768018, Odisha (India); School of Applied Sciences, KIIT University, Bhubaneswar 751024, Odisha (India); Sarkar, Niladri [Department of Chemistry, Veer Surendra Sai University of Technology, Burla, Sambalpur 768018, Odisha (India); Rout, Dibyaranjan [School of Applied Sciences, KIIT University, Bhubaneswar 751024, Odisha (India); Swain, Sarat K., E-mail: swainsk2@yahoo.co.in [Department of Chemistry, Veer Surendra Sai University of Technology, Burla, Sambalpur 768018, Odisha (India)

2017-01-15

Acid treated carbon nanofiber (t-CNF) reinforced epoxy nanocomposites were fabricated by hand lay-up method with various wt % of t-CNF loadings. Pristine or unmodified carbon nano fibers (u-CNFs) were made compatible with epoxy matrix by means of mixed acid treatment. Fabricated nanocomposites were characterized with Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) study, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM). Mechanical and thermal properties of the nanocomposites were measured as a function of t-CNF content. Effect of acid treated CNFs on to the mechanical properties of epoxy nanocomposites was justified by comparing the mechanical properties of epoxy/t-CNF and epoxy/u-CNF nanocomposites with same loading level. The electrical conductivity was achieved by epoxy resin with a threshold at 1 wt % of t-CNF. Substantial improvement in thermal, mechanical and electrical properties of the synthesized epoxy/t-CNF nanocomposites may be suitable for fabricating electronic devices. - Highlights: • Epoxy/t-CNF nanocomposites are characterized by XRD, FTIR, SEM, AFM and TEM. • Electrical conductivity was achieved by epoxy with a threshold at 1 wt% of t-CNF. • Tensile strength is enhanced by 40% due to dispersion of t-CNF. • Synthesized nanocomposites are suitable for fabricating electronic devises.

Solution combustion method for synthesis of nanostructured hydroxyapatite, fluorapatite and chlorapatite

Science.gov (United States)

Zhao, Junjie; Dong, Xiaochen; Bian, Mengmeng; Zhao, Junfeng; Zhang, Yao; Sun, Yue; Chen, JianHua; Wang, XuHong

2014-09-01

Hydroxyapatite (HAP), fluorapatite (Fap) and chlorapatite (Clap) were prepared by solution combustion method with further annealing at 800 °C. The characterization and structural features of the synthesized powders were evaluated by the powder X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and transmission electron microscopy (TEM) techniques. Characterization results from XRD and Rietveld analysis revealed that OH- in the HAP lattice were gradually substituted with the increase of F- and Cl- content and totally substituted at the molar concentration of 0.28 and 0.6, respectively. The results from FI-IR have also confirmed the incorporation of substituted anions in the apatite structure.

Synthesis and sintering of nanocrystalline hydroxyapatite powders by citric acid sol-gel combustion method

International Nuclear Information System (INIS)

Han Yingchao; Li Shipu; Wang Xinyu; Chen Xiaoming

2004-01-01

The citric acid sol-gel combustion method has been used for the synthesis of nanocrystalline hydroxyapatite (HAP) powder from calcium nitrate, diammonium hydrogen phosphate and citric acid. The phase composition of HAP powder was characterized by X-ray powder diffraction analysis (XRD). The morphology of HAP powder was observed by transmission electron microscope (TEM). The HAP powder has been sintered into microporous ceramic in air at 1200 deg. C with 3 h soaking time. The microstructure and phase composition of the resulting HAP ceramic were characterized by scanning electron microscope (SEM) and XRD, respectively. The physical characterization of open porosity and flexural strength have also been carried out

Influence of current density on surface morphology and properties of pulse plated tin films from citrate electrolyte

Energy Technology Data Exchange (ETDEWEB)

Sharma, Ashutosh; Bhattacharya, Sumit; Das, Siddhartha; Das, Karabi, E-mail: karabi@metal.iitkgp.ernet.in

2014-01-30

Bulk polycrystalline tin films have been processed by pulse electrodeposition technique from a simple solution containing triammonium citrate and stannous chloride. The cathodic investigations have been carried out by galvanostatic methods. As deposited samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). XRD analysis of the deposited films shows microcrystalline grains having β-Sn form. The surface morphology is very rough at lower current density, but becomes smooth at higher current density, and exhibits pyramid type morphology at all the current densities. The effect of current density on microhardness, melting behavior, and electrical resistivity are also reported here.

Microstructure and wear characterization of self-lubricating Al2O3 - MoS2 composite ceramic coatings

International Nuclear Information System (INIS)

Koshkarian, K.A.; Kriven, W.M.

1989-01-01

The authors report the results of composite ceramic coatings of alumina Al 2 O 3 containing some molybdenum disulfide MoS 2 electro-codeposited on to Al metal substrates by a combination of anodic sparks deposition of Al 2 O 3 and electrophoresis of MoS 2 . The microstructures were characterized by XRD, XPS, SEM, EDS, SNMS, TEM, SAD and relative wear resistance measurements. The coatings consisted mostly of Al 2 O 3 with some and present as well. The coatings were porous and microcracked. SEM showed them to consist of circular splats which had rapidly crystallized from the molten state in areas of dielectric breakdown in the coating. In the TEM the microstructure was seen to contain sets of parallel, elongated grains having a single crystallographic orientation. The grains were separated by dislocated, low angle grain boundaries or microcracks. The sets intersected at irregularly curved interfaces and were mechanically interlocked. Quantitative SNMS indicated that up to 26 wt% MoS 2 was incorporated in coatings fabricated from 5g/1 solutions. SEM/EDS as well as TEM/SAD/EDS identified 1-3 μ particles of MoS 2 incorporated into the 5g/1 solution derived coatings. These coatings exhibited 50% lower wear rate than pure alumina coatings deposited under the same condition

Implementação de sistemas eólicos para redes de sensores sem fios

OpenAIRE

Mendonça, Fábio Rúben Silva

2015-01-01

O trabalho tem por objetivo principal estudar a utilização de aerogeradores para microprodução de energia (menor que 1 W) de forma a poderem alimentar os nós das redes de sensores sem fios. Para tal, analisaram-se dois tipos de aerogeradores, os de eixo vertical e os de eixo horizontal, tendo-se efetuado simulações de CFD (Computational Fluid Dynamics) para verificar o desempenho das turbinas, de forma a determinar qual é o mais adequado. Foi realizado o projeto dos dois sistemas e anali...

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

Science.gov (United States)

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.

Quantifying Golgi structure using EM: combining volume-SEM and stereology for higher throughput.

Science.gov (United States)

Ferguson, Sophie; Steyer, Anna M; Mayhew, Terry M; Schwab, Yannick; Lucocq, John Milton

2017-06-01

Investigating organelles such as the Golgi complex depends increasingly on high-throughput quantitative morphological analyses from multiple experimental or genetic conditions. Light microscopy (LM) has been an effective tool for screening but fails to reveal fine details of Golgi structures such as vesicles, tubules and cisternae. Electron microscopy (EM) has sufficient resolution but traditional transmission EM (TEM) methods are slow and inefficient. Newer volume scanning EM (volume-SEM) methods now have the potential to speed up 3D analysis by automated sectioning and imaging. However, they produce large arrays of sections and/or images, which require labour-intensive 3D reconstruction for quantitation on limited cell numbers. Here, we show that the information storage, digital waste and workload involved in using volume-SEM can be reduced substantially using sampling-based stereology. Using the Golgi as an example, we describe how Golgi populations can be sensed quantitatively using single random slices and how accurate quantitative structural data on Golgi organelles of individual cells can be obtained using only 5-10 sections/images taken from a volume-SEM series (thereby sensing population parameters and cell-cell variability). The approach will be useful in techniques such as correlative LM and EM (CLEM) where small samples of cells are treated and where there may be variable responses. For Golgi study, we outline a series of stereological estimators that are suited to these analyses and suggest workflows, which have the potential to enhance the speed and relevance of data acquisition in volume-SEM.

Accelerator-TEM interface facility and application

International Nuclear Information System (INIS)

Liu Chuansheng; Li Ming; He Jun; Yang Zheng; Zhou Lin; Wang Zesong; Guo Liping; Jiang Changzhong; Yang Shibo; Fu Dejun; Fan Xiangjun; Liu Jiarui; Lee J C

2010-01-01

An accelerator-TEM interface facility has been established at Wuhan University in 2008. The system consists of an H800 TEM linked to a 200 kV ion implanter and a 2 x 1.7 MV tandem accelerator. Nitrogen ions at 115 keV were successfully transported from the implanter into the TEM chamber through the interface system, and the ion currents measured at the entrance of the TEM column were between 20 and 180 nA. Structural evolution caused by ion irradiation in Si, GaAs, nanocrystal Ag was observed in situ. The in situ observation showed that the critical implantation dose for amorphization of Si is 10 14 cm -2 . The nuclear material C276 samples implanted with 115 keV Ar + was also studied, and dislocation loops sized at 3-12 nm were clearly observed after implantation to doses of over 1 x 10 15 cm -2 . The density of the loops increased with the dose. Evolution to polycrystalline and amorphous structures were observed at 5 x l0 15 cm -2 and 3 x 10 16 cm -2 , respectively. An in situ RBS/C chamber was installed on the transport line of the accelerator-TEM interface system. This enables in situ measurement of composition and location of the implanted species in lattice of the samples. In addition, a 50 kV low-energy gaseous ion generator was installed close to the TEM chamber, which facilitates in situ TEM observation of helium bubbles formed in helium-implanted materials. (authors)

Hollow raspberry-like PdAg alloy nanospheres: High electrocatalytic activity for ethanol oxidation in alkaline media

Science.gov (United States)

Peng, Cheng; Hu, Yongli; Liu, Mingrui; Zheng, Yixiong

2015-03-01

Palladium-silver (PdAg) alloy nanospheres with unique structure were prepared using a one-pot procedure based on the galvanic replacement reaction. Their electrocatalytic activity for ethanol oxidation in alkaline media was evaluated. The morphology and crystal structure of the samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). Electrochemical characterization techniques, including cyclic voltammetry (CV) and chronoamperometry (CA) measurements were used to analyze the electrochemical performance of the PdAg alloy nanospheres. The SEM and TEM images showed that the PdAg alloy nanospheres exhibit a hierarchical nanostructure with hollow interiors and porous walls. Compared to the commercial Pd/C catalyst, the as-prepared PdAg alloy nanospheres exhibit superior electrocatalytic activity and stability towards ethanol electro-oxidation in alkaline media, showing its potential as a new non-Pt electro-catalyst for direct alcohol fuel cells (DAFCs).

Synthesis of Nanocrystalline CdS by SILAR and Their Characterization

Directory of Open Access Journals (Sweden)

Partha Protim Chandra

2014-01-01

Full Text Available A simple and cost effective chemical technique has been utilized to prepare cadmium sulphide (CdS nanoparticles at room temperature. The sample is characterized with XRD (X-ray diffractometer, SEM (scanning electron microscope, TEM (transmission electron microscope, FTIR (Fourier transform infrared, EDX (energy dispersive X-rays, and UV-VIS (ultraviolet visible spectrophotometer. The particle size estimated using X-ray line broadening method is ~21.5 nm. While particle size estimation, both instrumental and strain broadening was taken into account. The lattice strain was evaluated using Williamson-Hall equation. SEM illustrates formation of submicron size crystallites and TEM image gives a particle size of ~23.5 nm. The characteristic stretching vibration frequency of CdS was observed in the absorption band in FTIR spectrum. Optical absorption study exhibits a band gap energy value of about 2.44 eV.

Electrochemical lithium insertion in graphite containing dispersed tin-antimony alloys

Energy Technology Data Exchange (ETDEWEB)

Billaud, Denis; Nabais, Catarina; Mercier, Cedric [LCSM, Laboratoire de Chimie du Solide Mineral, Nancy University, BP 239, 54506 Vandoeuvre les Nancy Cedex (France); Schneider, Raphael [LCPME, Laboratoire de Chimie Physique et Microbiologie pour l' Environnement, Nancy University, Faculte de Pharmacie, BP 80 403, 54001 Nancy Cedex (France); Willmann, Patrick [CNES, Centre National d' Etudes Spatiales, 18, Avenue E. Belin, 31055 Toulouse Cedex (France)

2008-09-15

Graphite/SnSb composites were prepared by solution-phase reduction of SnCl{sub 2} and SbCl{sub 5} in the presence of graphite powder using either t-BuONa-activated NaH or t-BuOLi-activated LiH. Crude and washed materials were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and field emission gun-scanning electron microscopy (FEG-SEM). Electrochemical lithium insertion was carried out in both types of composites using voltammetry or galvanostatic charge/discharge techniques. It appeared that graphite-SnSb composites prepared using t-BuOLi-activated LiH as reductant displayed the highest reversible capacity (ca. 500 mA h g{sup -1}). This phenomenon is likely in relation with a better dispersion and grafting of metal particles on graphite, as suggested by FEG-SEM and TEM analyses. However, such dispersion appeared to increase significantly the irreversible capacity. (author)

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

Science.gov (United States)

Kale, R. B.; Sartale, S. D.; Ganesan, V.; Lokhande, C. D.; Lin, Yi-Feng; Lu, Shih-Yuan

2006-11-01

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH3COO)2 as Pb2+ and Na2SeSO3 as Se2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

International Nuclear Information System (INIS)

Kale, R.B.; Sartale, S.D.; Ganesan, V.; Lokhande, C.D.; Lin, Y.-F.; Lu, S.-Y.

2006-01-01

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH 3 COO) 2 as Pb 2+ and Na 2 SeSO 3 as Se 2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV

Single crystalline ZnO nanorods grown by a simple hydrothermal process

Energy Technology Data Exchange (ETDEWEB)

Pei, L.Z., E-mail: lzpei1977@163.com [School of Materials Science and Engineering, Institute of Molecular Engineering and Applied Chemistry, Key Lab of Materials Science and Processing of Anhui Province, Anhui University of Technology, Ma' anshan, Anhui 243002 (China); Zhao, H.S. [School of Materials Science and Engineering, Institute of Molecular Engineering and Applied Chemistry, Key Lab of Materials Science and Processing of Anhui Province, Anhui University of Technology, Ma' anshan, Anhui 243002 (China); Tan, W. [Henkel Huawei Electronics Co. Ltd., Lian' yungang, Jiangsu 222006 (China); Yu, H.Y. [School of Materials Science and Engineering, Institute of Molecular Engineering and Applied Chemistry, Key Lab of Materials Science and Processing of Anhui Province, Anhui University of Technology, Ma' anshan, Anhui 243002 (China); Chen, Y.W. [Department of Materials Science, Fudan University, Shanghai 200433 (China); Zhang Qianfeng [School of Materials Science and Engineering, Institute of Molecular Engineering and Applied Chemistry, Key Lab of Materials Science and Processing of Anhui Province, Anhui University of Technology, Ma' anshan, Anhui 243002 (China)

2009-09-15

Single crystalline ZnO nanorods with wurtzite structure have been prepared by a simple hydrothermal process. The microstructure and composition of the products were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM, energy dispersive X-ray spectrum (EDS) and Raman spectrum. The nanorods have diameters ranging from 100 nm to 800 nm and length of longer than 10 {mu}m. Raman peak at 437.8 cm{sup -1} displays the characteristic peak of wurtzite ZnO. Photoluminescence (PL) spectrum shows a blue light emission at 441 nm, which is related to radiative recombination of photo-generated holes with singularly ionized oxygen vacancies.

Single crystalline ZnO nanorods grown by a simple hydrothermal process

International Nuclear Information System (INIS)

Pei, L.Z.; Zhao, H.S.; Tan, W.; Yu, H.Y.; Chen, Y.W.; Zhang Qianfeng

2009-01-01

Single crystalline ZnO nanorods with wurtzite structure have been prepared by a simple hydrothermal process. The microstructure and composition of the products were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM, energy dispersive X-ray spectrum (EDS) and Raman spectrum. The nanorods have diameters ranging from 100 nm to 800 nm and length of longer than 10 μm. Raman peak at 437.8 cm -1 displays the characteristic peak of wurtzite ZnO. Photoluminescence (PL) spectrum shows a blue light emission at 441 nm, which is related to radiative recombination of photo-generated holes with singularly ionized oxygen vacancies.

A simple route to synthesize multiform structures of tin oxide nanobelts and optical properties investigation

International Nuclear Information System (INIS)

Cheng Chuanwei; Xu Guoyue; Zhang Haiqian; Li Yingying; Luo Yan; Zhang Peigen

2008-01-01

Multiform structures of SnO 2 nanobelts including of zigzag, branching and straight structures have been synthesized by a simple molten-salt assisted route. The obtained samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) and high resolution transmission electron microscope (HRTEM). The growth mechanism of zigzag nanobelts was proposed. A strong blue emission band centered in 425 nm was observed in the photoluminescence spectrum

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

International Nuclear Information System (INIS)

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

2017-01-01

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. (paper)

Micelle-template synthesis of hollow silica spheres for improving water vapor permeability of waterborne polyurethane membrane

OpenAIRE

Bao, Yan; Wang, Tong; Kang, Qiaoling; Shi, Chunhua; Ma, Jianzhong

2017-01-01

Hollow silica spheres (HSS) with special interior spaces, high specific surface area and excellent adsorption and permeability performance were synthesized via micelle-template method using cetyl trimethyl ammonium bromide (CTAB) micelles as soft template and tetraethoxysilane (TEOS) as silica precursor. SEM, TEM, FT-IR, XRD, DLS and BET-BJH were carried out to characterize the morphology and structure of as-obtained samples. The results demonstrated that the samples were amorphous with a hol...

Preparation and photocatalytic properties of YVO4 nanopowders

International Nuclear Information System (INIS)

Xu Haiyan; Wang Hao; Yan Hui

2007-01-01

YVO 4 photocatalysts with different grain sizes were obtained by annealing the YVO 4 nanopowders synthesized via microwave irradiation. The products were characterized by X-ray diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), surface area and porosity analyzer, and ultraviolet-visible (UV-vis) spectrophotometer. Photocatalytic measurements showed that the YVO 4 nanopowders with grain size of about 5 nm possess superior photocatalytic properties in decolorization of methyl orange solution

Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

Science.gov (United States)

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.

Recent improvement of a FIB-SEM serial-sectioning method for precise 3D image reconstruction - application of the orthogonally-arranged FIB-SEM.

Science.gov (United States)

Hara, Toru

2014-11-01

IntroductionWe installed the first "orthogonally-arranged" FIB-SEM in 2011. The most characteristic point of this instrument is that the FIB and SEM columns are perpendicularly mounted; this is specially designed to obtain a serial-sectioning dataset more accurately and precisely with higher contrast and higher spatial resolution compare to other current FIB-SEMs [1]. Since the installation in 2011, we have developed the hardware and methodology of the serial-sectioning based on this orthogonal FIB-SEM. In order to develop this technique, we have widely opened this instrument to every researcher of all fields. In the presentation, I would like to introduce some of application results that are obtained by users of this instrument. The characteristic points of the orthogonal systemFigure 1 shows a difference between the standard and the orthogonal FIB-SEM systems: In the standard system, shown in Fig.1(a), optical axes of a FIB and a SEM crosses around 60deg., while in the orthogonal system (Fig.1(b)), they are perpendicular to each other. The standard arrangement (a) is certainly suitable for TEM lamellae preparation etc. because the FIB and the SEM can see the same position simultaneously. However, for a serial-sectioning, it is not to say the best arrangement. One of the reasons is that the sliced plane by the FIB is not perpendicular to the electron beam so that the background contrast is not uniform and observed plane is distorted. On the other hand, in case of the orthogonally-arranged system,(b), these problems are resolved. In addition, spatial resolution can keep high enough even in a low accelerating voltage (e.g. 500V) because a working distance is set very small, 2mm. From these special design, we can obtain the serial-sectioning dataset from rather wide area (∼100um) with high spatial resolution (Max. 2×2×2nm). As this system has many kinds of detectors: SE, ET, Backscatter Electron(Energy-selective), EDS, EBSD, STEM(BF&ADF), with Ar+ ion-gun and a

Surface characterization of cottonseed meal products by SEM, SEM-EDS, XRD and XPS analysis

Science.gov (United States)

The utilization of cottonseed meal as a valuable industrial feedstock needs to be exploited. We have recently produced water-washed cottonseed meal, total cottonseed protein, sequentially extracted water- and alkali-soluble proteins, and two residues after the total and sequential protein extraction...

Synchrotron-based XRD from rat bone of different age groups.

Science.gov (United States)

Rao, D V; Gigante, G E; Cesareo, R; Brunetti, A; Schiavon, N; Akatsuka, T; Yuasa, T; Takeda, T

2017-05-01

Synchrotron-based XRD spectra from rat bone of different age groups (w, 56 w and 78w), lumber vertebra at early stages of bone formation, Calcium hydroxyapatite (HAp) [Ca 10 (PO 4 ) 6 (OH) 2 ] bone fill with varying composition (60% and 70%) and bone cream (35-48%), has been acquired with 15keV synchrotron X-rays. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15keV X-rays (λ=0.82666 A 0 ). Diffraction data were quantitatively analyzed using the Rietveld refinement approach, which allowed us to characterize the structure of these samples in their early stages. Hydroxyapatite, received considerable attention in medical and materials sciences, since these materials are the hard tissues, such as bone and teeth. Higher bioactivity of these samples gained reasonable interest for biological application and for bone tissue repair in oral surgery and orthopedics. The results obtained from these samples, such as phase data, crystalline size of the phases, as well as the degree of crystallinity, confirm the apatite family crystallizing in a hexagonal system, space group P6 3 /m with the lattice parameters of a=9.4328Å and c=6.8842Å (JCPDS card #09-0432). Synchrotron-based XRD patterns are relatively sharp and well resolved and can be attributed to the hexagonal crystal form of hydroxyapatite. All the samples were examined with scanning electron microscope at an accelerating voltage of 15kV. The presence of large globules of different sizes is observed, in small age groups of the rat bone (8w) and lumber vertebra (LV), as distinguished from, large age groups (56 and 78w) in all samples with different magnification, reflects an amorphous phase without significant traces of crystalline phases. Scanning electron microscopy (SEM) was used to characterize the morphology and crystalline properties of Hap, for all the samples, from 2 to 100μm resolution. Copyright © 2017 Elsevier B.V. All rights reserved.

Local behavior of an AISI 304 stainless steel submitted to in situ biaxial loading in SEM

Energy Technology Data Exchange (ETDEWEB)

Caër, C., E-mail: celia.caer@gmail.com; Pesci, R.

2017-04-06

The microstructural response of a coarse grained AISI 304 stainless steel submitted to biaxial tensile loading was investigated using SEM and X-ray diffraction. The specimen geometry was designed to allow for biaxial stress state and incipient crack in the center of the active part under biaxial tensile loading. This complex loading was performed step by step by a micromachine fitting into a SEM chamber. At each loading step FSD pictures and EBSD measurements were carried out to study the microstructural evolution of the alloy, namely grain rotations and misorientations, stress-induced martensite formation and crack propagation. According to their initial orientation, grains are found to behave differently under loading. Approximately 60% of grains are shown to reorient to the [110] Z orientation under biaxial tensile loading, whereas the 40% left undergo high plastic deformation. EBSD and XRD measurements respectively performed under loading and on the post mortem specimen highlighted the formation of about 4% of martensite.

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

Science.gov (United States)

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.

Synthesis of Uranium-di-Oxide nano-particles by pulsed laser ablation in ethanol and their characterisation

International Nuclear Information System (INIS)

Kumar, Aniruddha; Prasad, Manisha; Shail, Shailini

2015-01-01

The importance of actinide based nano-structures is well known in the area of biology, nuclear medicine, and nuclear industry. Pulsed laser ablation in liquid is recognised as an attractive technique for production of nano-structures of different metals and metal oxides with high purity. In this paper, we report synthesis of uranium-di-oxide nano particles by pulsed laser ablation in ethanol. The second harmonic emission of an electro- optically Q-switched nano-second Nd-YAG laser was used as the coherent source here. The structural and optical properties of the fabricated Uranium-di-oxide nano- particles were investigated by XRD, SEM, TEM, EDX and UV- Vis-NIR spectrophotometry. The mean size of the particles was found to be dependent on the laser ablation parameters. XRD and TEM analysis confirmed the phase of the synthesised material as pure crystalline Uranium-di- oxide with Face Centred Cubic structure. UV- Vis- NIR absorption spectra of the colloidal solution show high absorption in the UV regime. (author)

The investigation on electrochemical reaction mechanism of CuF2 thin film with lithium

International Nuclear Information System (INIS)

Cui Yanhua; Xue Mingzhe; Zhou Yongning; Peng Shuming; Wang Xiaolin; Fu Zhengwen

2011-01-01

Crystalline CuF 2 thin films were prepared by pulsed laser deposition under room temperature. The physical and electrochemical properties of the as-deposited thin films have been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), galvanostatic cycling and cyclic voltammetry (CV). Reversible capacity of 544 mAh g -1 was achieved in the potential range of 1.0-4.0 V. A reversible couple of redox peaks at 3.0 V and 3.7 V was firstly observed. By using ex situ XRD and TEM techniques, an insertion process followed by a fully conversion reaction to Cu and LiF was revealed in the lithium electrochemical reaction of CuF 2 thin film electrode. The reversible insertion reaction above 2.8 V could provide a capacity of about 125 mAh g -1 , which makes CuF 2 a potential cathode material for rechargeable lithium batteries.

Ultrafine ferromagnetic iron oxide nanoparticles: Facile synthesis by low temperature decomposition of iron glycerolate

Energy Technology Data Exchange (ETDEWEB)

Bartůněk, Vilém, E-mail: vilem.bartunek@vscht.cz [Department of Inorganic Chemistry, Faculty of Chemical Technology, University of Chemistry and Technology, Technická 5, 166 28 Prague 6 (Czech Republic); Průcha, David [Department of Inorganic Chemistry, Faculty of Chemical Technology, University of Chemistry and Technology, Technická 5, 166 28 Prague 6 (Czech Republic); Švecová, Marie [Department of Analytical Chemistry, Faculty of Chemical Engineering, University of Chemistry and Technology, Technická 5, 166 28 Prague 6 (Czech Republic); Ulbrich, Pavel [Department of Biochemistry and Microbiology, Faculty of Food and Biochemical Technology, University of Chemistry and Technology, Technická 3, 166 28 Prague 6 (Czech Republic); Huber, Štěpán; Sedmidubský, David; Jankovský, Ondřej [Department of Inorganic Chemistry, Faculty of Chemical Technology, University of Chemistry and Technology, Technická 5, 166 28 Prague 6 (Czech Republic)

2016-09-01

We synthesized dark colored ultrafine – sub 10 nm iron oxide nanoparticles by a facile and low temperature process based on thermal decomposition of an affordable precursor – iron glycerolate. Simultaneous thermal analysis (STA) was used to study the thermal behaviour during the decomposition. The iron glycerolate was thoroughly analysed by various methods. The size of the iron nanoparticles was determined from XRD patterns and by transmission electron microscopy (TEM) and their composition has been confirmed by XPS. Magnetic properties of the nanoparticles were studied by vibrating sample magnetometry. The prepared single phase material exhibiting ferromagnetic properties is usable in a wide range of applications and may be suitable even for large scale industrial applications. - Highlights: • Iron glycerolate prepared and characterised. • Iron oxide nanoparticles prepared by thermal decomposition of iron glycerolate. • STA used to study the decomposition. • Products characterised by XRD, XPS, FT-IR, SEM and TEM. • Magnetic behaviour of monophasic samples determined.

Templateless Synthesis and Characterization of Hollow Gadolinium Doped Cerium Oxide Nanofibers by Electrospinning

Directory of Open Access Journals (Sweden)

Chutima Thiabdokmai

2014-01-01

Full Text Available The hollow nanofibers of Ce0.8Gd0.2O2−δ (GDC20 were electrospun from the PVP and nitrate precursors. The evolution of hollow channel was investigated by TG-DTA and ex situ TEM for the fibers heated at 250–300°C for 1–5 h. The hollow cores were revealed during the crystallization of nano-GDC20 and the PVP decomposition stage. The structural and morphological properties of GDC20 fibers before and after being calcined at 500–900°C for 8 h were investigated by FTIR, FE-SEM, TEM, EDS, XRD, and Raman spectroscopy. The results from XRD and Raman scattering verify the successful doping of Gd3+ ions into the CeO2 host lattice. The conductivity of the cold-pressed GDC 20 pellet sintered at 1400°C is more than 0.01 S/cm at and above 600°C.

Microstructure and mechanical properties of Al-20Si-5Fe-2X (X = Cu, Ni, Cr) alloys produced by melt-spinning

International Nuclear Information System (INIS)

Rajabi, M.; Simchi, A.; Davami, P.

2008-01-01

Al-20Si-5Fe-2X (X = Cu, Ni and Cr) ribbons were produced by melt-spinning and consolidated by hot pressing at 400 deg. C for 60 min. The microstructure of the ribbons and the consolidated alloys was investigated using optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffractometry (XRD) method, and transmission electron microscopy (TEM). The hardness and compressive strength of the specimens at ambient and elevated temperatures were examined. The microstructure of the ribbons exhibited featureless and dendritic zones. Results of XRD and TEM showed formation of spherically shaped Si particles with an average diameter of 20 nm. Ultrafine Si (110-150 nm) and iron-containing intermetallic particles were noticed in the microstructure of the consolidated ribbons. An improved strength was achieved by alloying of Al-20Si-5Fe with Cu, Ni, and Cr. Nickel was found to be the most effective element in increasing the maximum stress, particularly at elevated temperatures

Effects of high-speed homogenization and high-pressure homogenization on structure of tomato residue fibers.

Science.gov (United States)

Hua, Xiao; Xu, Shanan; Wang, Mingming; Chen, Ying; Yang, Hui; Yang, Ruijin

2017-10-01

Tomato residue fibers obtained after derosination and deproteinization were processed by high-speed homogenization (HSH) and high-pressure homogenization (HPH), and their effects on fiber structure was investigated, respectively. Characterizations including particle size distribution, SEM, TEM and XRD were performed. HSH could break raw fibers to small particles of around 60μm, while HPH could reshape fibers to build network structure. Microfibrils were released and their nanostructure consisting of elementary fibrils was observed by TEM. XRD patterns indicated both HSH and HPH could hardly alter the nanostructure of the fibers. Physicochemical properties including expansibility, WHC and OHC were determined. Both HSH and HPH could increase the soluble fiber content by about 8%, but HSH-HPH combined processing did not show better result. Acid (4mol/L HCl) was used in replacement of water medium and the acidic degradation of fibers could be promoted by high speed shearing or high pressure processing. Copyright © 2017 Elsevier Ltd. All rights reserved.

Infrared spectra, Raman laser, XRD, DSC/TGA and SEM ...

Indian Academy of Sciences (India)

Ga2O3, Se metal, SnO, Sb2O3, HgO and PbCO3 are formed upon the reaction of acetamide aqueous solutions with Ga(NO3)3, SeO2, SnCl2, SbCl3, HgCl2 and Pb(NO3)2, respectively, at 90°C. Different amorphous or crystalline phases can be obtained depending upon the experimental conditions (molar ratios, metal salts ...

Characterization, Antibacterial and Antioxidant Properties of Silver Nanoparticles Synthesized from Aqueous Extracts of Allium sativum, Zingiber officinale, and Capsicum frutescens

Science.gov (United States)

Otunola, Gloria Aderonke; Afolayan, Anthony Jide; Ajayi, Emmanuel Olusegun; Odeyemi, Samuel Wale

2017-01-01

Background: Herbal drug delivery is limited by poor solubility and bioavailability which can be overcome with suitable nanomaterials that will enhance their pharmacokinetics and performance. Objective: This study aimed to analyze the synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from three spices. Materials and Methods: AgNPs were prepared using 0.1 M silver nitrate and aqueous extracts of Allium sativum L. (garlic), Zingiber officinale Rosc. (ginger), and Capsicum frutescens L. (cayenne pepper). The AgNPs were characterized using ultraviolet-visible (UV-Vis) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray, X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. Results: The AgNPs were formed within an hour of the reaction and showed maximum UV-Vis absorption in the 375–480 nm range. SEM and TEM revealed well-dispersed spherical particles with little agglomeration, average sizes of 3–6 nm, 3–22 nm, and 3–18 nm for garlic, ginger, and cayenne pepper, respectively. FTIR showed that amine, protein, phenolic, aromatic, and alkynes groups contributed to AgNP synthesis and XRD confirmed their crystalline and face-centered cubic nature. Antibacterial action of the AgNPs was in the following order: ginger (minimum inhibitory concentration [MIC] garlic> cayenne pepper (MIC 125 μg/mL). Antioxidant action showed cayenne pepper > ginger > garlic (inhibitory concentration 50% [IC50]: 40, 240, and 250 μg/mL, respectively) against 2,2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid) and garlic > cayenne pepper > ginger (IC50: <31.25, 40, and 120 μg/mL, respectively) against 1,1-diphenyl-2-picrylhydrazyl. Conclusion: Optimization of this green synthesis would support the production of AgNPs with great therapeutic potentials. SUMMARY The synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from garlic, ginger

Nanofibers obtained by electrospinning of BaTiO3 particles dispersed in polyvinyl alcohol and ethylcellulose

Energy Technology Data Exchange (ETDEWEB)

Avila, Humar A.; Reboredo, Maria M.; Castro, Miriam; Parra, Rodrigo, E-mail: havila@fi.mdp.edu.ar [Instituto de Investigaciones en Ciencia y Tecnologia de Materiales - INTEMA, Consejo Nacional de Investigaciones Cientificas y Tecnicas - CONICET, Universidad Nacional de Mar del Plata - UNMdP, Mar del Plata (Argentina)

2013-11-01

Barium titanate particles (100-300 nm) synthesized by hydrothermal method were dispersed in both polyvinyl alcohol (PVA) and ethylcellulose (EC) solutions. These suspensions were processed by electrospinning. When no particles were added, homogeneous polymeric nanofibers were obtained. Under certain conditions, polymeric suspensions of barium titanate particles were electrospun generating polymeric fibers with BT particles. The effect of a surfactant was also assessed over the formation of nanofibers. The BaTiO{sub 3} particles synthesized by hydrothermal method were characterized by X-Ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and Raman spectroscopy. Fibers were characterized by scanning electron microscopy (SEM). (author)

Behavior of W-based materials in hot helium gas

Directory of Open Access Journals (Sweden)

J. Matějíček

2016-12-01

A number of W-based materials (pure tungsten and some of its alloys prepared by powder metallurgy techniques was exposed to He atmosphere at 720ºC and 500kPa for 500h. Morphological surface changes were observed by SEM, chemical and phase composition was analyzed by EDS and XRD, respectively. The internal microstructure was observed by a combination of SEM, FIB and TEM techniques. Mechanical properties were determined by instrumented indentation. Some alloys developed a thin oxide layer, in some cases new morphological features were observed, while some samples remained mostly intact. The observed changes are correlated with specific compositions and microstructures.

Transreceptor de faixa larga baseado em impulso de rádio para sensor sem fios de curta distância implementado em tecnologia CMOS

OpenAIRE

Rodrigues, David Manuel Cardoso

2013-01-01

Dissertação para obtenção do Grau de Mestre em Engenharia Electrotécnica e de Computadores O rápido desenvolvimento da microtecnologia e microelectrónica tem vindo a contribuir de forma decisiva para uma crescente utilização de sensores, sejam eles com ou sem fios, o que permitirá interagir mais eficientemente com o meio envolvente, em consequência de mais e melhor medição e atuação. Neste contexto, as redes de sensores sem fios (WSNs) estão a emergir como uma das grandes e mais impo...

SEM analysis for irradiated materials

International Nuclear Information System (INIS)

Liu Xiaosong; Yao Liang

2008-06-01

A radiation-proof Scanning Electron Microscope (SEM) system is introduced. It has been widely used in various areas. For analyzing radioactive samples, normal SEM system needs lots of alterations. Based on KYKY-2800B SEM, the sample room, belt line, operating table and aerator were updated. New radiation-proof SEM system has used to analytic surface contaminated samples and RPV materials samples. An elementary means of SEM analysis for radioactive samples was studied, and this examination supported some available references for further irradiated fuel researches. (authors)

Characterization of Yeast Biofilm by Cryo-SEM and FIB-SEM

Czech Academy of Sciences Publication Activity Database

Hrubanová, Kamila; Nebesářová, Jana; Růžička, F.; Dluhoš, J.; Krzyžánek, Vladislav

2013-01-01

Roč. 19, S2 (2013), s. 226-227 ISSN 1431-9276 R&D Projects: GA MŠk EE.2.3.20.0103; GA TA ČR TE01020118; GA ČR GAP205/11/1687 Institutional support: RVO:68081731 ; RVO:60077344 Keywords : yeast biofilm * cryo-SEM * FIB-SEM Subject RIV: BH - Optics, Masers, Lasers Impact factor: 1.757, year: 2013

Ag{sub 2}CdI{sub 4}: Synthesis, characterization and investigation the strain lattice and grain size

Energy Technology Data Exchange (ETDEWEB)

Ghanbari, Mojgan [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P.O. Box 87317-51167, I.R. (Iran, Islamic Republic of); Gholamrezaei, Sousan [Young Researchers Club, Arak Branch, Islamic Azad University, Arak (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P.O. Box 87317-51167, I.R. (Iran, Islamic Republic of)

2016-05-15

In this work the Ag{sub 2}CdI{sub 4} nanostructures have been synthesized via a solid state reaction from reaction of AgI and CdI{sub 2} as precursors. The effect of the mole ratio of precursors, time and temperature of reaction has been optimized to achieve the best product on morphology and purity. Nanostructures have been characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman (FT-IR) techniques, X-ray energy dispersive spectroscopy (EDS) and Ultraviolet spectroscopy (UVvis). The XRD patterns of nanostructures have been used to estimate the grain sizes and strain lattice. Grain size of nanostructures is in range of 5–17 nm and the strain of lattice is changed in range of 0.0024–0.014. The band gap of these nanostructures has been estimated by DRS spectrum about 5.4 eV. Raman spectroscopy has been confirmed the XRD results and show that the Ag{sub 2}CdI{sub 4} nanostructures have been synthesized. SEM and TEM images have been used for investigation of morphology of product. Results show that the best morphology and purity have been achieved in 12 h and 200 °C in 1:1 mol ratio of precursors. - Highlights: • Ag{sub 2}CdI{sub 4} nanostructures have been synthesized by low temperature solid state method. • The reaction has been optimized for purity, morphology, and grain size and strain lattice. • Effective parameters have been optimized such as time, temperature and mole ratio.

Parametric investigations on the influence of nano-second Nd{sup 3+}:YAG laser wavelength and fluence in synthesizing NiTi nano-particles using liquid assisted laser ablation technique

Energy Technology Data Exchange (ETDEWEB)

Patra, Nandini, E-mail: nandinipatra2007@gmail.com [Centre for Material Science and Engineering, Indian Institute of Technology, Indore, Madhya Pradesh, Pin-453441 (India); Akash, K.; Shiva, S.; Gagrani, Rohit; Rao, H. Sai Pranesh; Anirudh, V.R. [Mechatronics and Instrumentation lab, Discipline of Mechanical Engineering, Indian Institute of Technology, Indore, Madhya Pradesh, Pin-453441 (India); Palani, I.A., E-mail: palaniia@iiti.ac.in [Centre for Material Science and Engineering, Indian Institute of Technology, Indore, Madhya Pradesh, Pin-453441 (India); Mechatronics and Instrumentation lab, Discipline of Mechanical Engineering, Indian Institute of Technology, Indore, Madhya Pradesh, Pin-453441 (India); Singh, Vipul [Centre for Material Science and Engineering, Indian Institute of Technology, Indore, Madhya Pradesh, Pin-453441 (India)

2016-03-15

Graphical abstract: - Highlights: • Influence of laser wavelengths (1064 nm, 532 nm and 355 nm) and fluences (40 J/cm{sup 2}, 30 J/cm{sup 2} and 20 J/cm{sup 2}) on generation of underwater laser ablated NiTi nanoparticles. • Particle size range of 140–10 nm was generated at varying laser wavelengths. • The alloy formation of NiTi nanoparticles was confirmed from XRD and TEM analysis where the crystalline peaks of NiTi, Ni{sub 4}Ti{sub 3} and Ni{sub 3}Ti were observed from XRD. • Formation efficiency of NiTi nanoparticles was maximum at 1064 nm wavelength and 40 J/cm{sup 2} fluence. - Abstract: This paper investigates the influence of laser wavelengths and laser fluences on the size and quality of the NiTi nanoparticles, generated through underwater solid state Nd:YAG laser ablation technique. The experiments were performed on Ni55%–Ti45% sheet to synthesize NiTi nano-particles at three different wavelengths (1064 nm, 532 nm and 355 nm) with varying laser fluences ranging from 20 to 40 J/cm{sup 2}. Synthesized NiTi nano-particles were characterized through SEM, DLS, XRD, FT-IR, TEM and UV–vis spectrum. It was observed that, maximum particle size of 140 nm and minimum particle size of 10 nm were generated at varying laser wavelengths. The crystallinity and lattice spacing of NiTi alloy nanoparticles were confirmed from the XRD analysis and TEM images, respectively.

Cadmium sulfide quantum dots stabilized by castor oil and ricinoleic acid

Science.gov (United States)

Kyobe, Joseph William; Mubofu, Egid Beatus; Makame, Yahya M. M.; Mlowe, Sixberth; Revaprasadu, Neerish

2016-02-01

Castor oil and ricinoleic acid (an isolate of castor oil) are environmentally friendly bio-based organic surfactants that have been used as capping agents to prepare nearly spherical cadmium sulfide quantum dots (QDs) at 230, 250 and 280 °C. The prepared quantum dots were characterized by Ultra violet-visible (UV-vis), Photoluminescence (PL), Transmission Electron Microscopy (TEM), High Resolution Transmission Electron Microscopy (HRTEM) and X-ray diffraction (XRD) giving an overall CdS QDs average size of 5.14±0.39 nm. The broad XRD pattern and crystal lattice fringes in the HRTEM images showed a hexagonal phase composition of the CdS QDs. The calculated/estimated average size of the prepared castor oil capped CdS QDs for various techniques were 4.64 nm (TEM), 4.65 nm (EMA), 5.35 nm (UV-vis) and 6.46 nm (XRD). For ricinoleic acid capped CdS QDs, the average sizes were 5.56 nm (TEM), 4.78 nm (EMA), 5.52 nm (UV-vis) and 8.21 nm (XRD). Optical properties of CdS QDs showed a change of band gap energy from its bulk band gap of 2.42-2.82 eV due to quantum size confinement effect for temperature range of 230-280 °C. Similarly, a blue shift was observed in the photoluminescence spectra. Scanning electron microscope (SEM) observations show that the as-synthesized CdS QDs structures are spherical in shape. Fourier transform infra-red (FTIR) studies confirms the formation of castor oil and ricinoleic acid capped CdS QDs.

Blocos semânticos: o movimento argumentativo na construção do sentido no discurso

Directory of Open Access Journals (Sweden)

Ernani Cesar de FREITAS

2008-07-01

Full Text Available Este trabalho tem por objetivo sistematizar e aplicar conceitos da Semântica Argumentativa de Oswald Ducrot e Marion Carel, no que diz respeito ao modelo teórico dos Blocos Semânticos, de modo que dêem conta da construção do sentido de unidades mais complexas como o texto e o discurso. A tese concebida como norteadora deste estudo, seguindo a metodologia proposta por Ducrot (1987, pressupõe que o texto é um bloco semântico inscrito no nível teórico da produção e realizado pelo encadeamento argumentativo complexo que é o discurso, orientado argumentativamente pelo uso de conectores tipo DC e/ ou PT. As análises discursivas realizadas, neste trabalho, demonstram que os encadeamentos dos enunciados estão bem marcados pelos conectores donc e pourtant que dão sentido ao discurso complexo, pelas conexões semânticas produzidas em suas AI e AE. Esse movimento argumentativo resulta da interdependência dos segmentos argumentativos, dos encadeamentos e por conseqüência dos blocos semânticos, todos interconectados e interdependentes nas relações de sentido que estabelecem entre si, processo que culmina na realização linguística de nível complexo constituído pelo texto, entidade abstrata subjacente aos discursos realizados, e pelo discurso, como seqüência de enunciados interligados, por isso, também entendido como entidade concreta, ou seja, a manifestação e realização do texto.

Blocos semânticos: o movimento argumentativo na construção do sentido no discurso

Directory of Open Access Journals (Sweden)

Ernani Cesar de FREITAS

2013-10-01

Full Text Available Este trabalho tem por objetivo sistematizar e aplicar conceitos da Semântica Argumentativa de Oswald Ducrot e Marion Carel, no que diz respeito ao modelo teórico dos Blocos Semânticos, de modo que dêem conta da construção do sentido de unidades mais complexas como o texto e o discurso. A tese concebida como norteadora deste estudo, seguindo a metodologia proposta por Ducrot (1987, pressupõe que o texto é um bloco semântico inscrito no nível teórico da produção e realizado pelo encadeamento argumentativo complexo que é o discurso, orientado argumentativamente pelo uso de conectores tipo DC e/ ou PT. As análises discursivas realizadas, neste trabalho, demonstram que os encadeamentos dos enunciados estão bem marcados pelos conectores donc e pourtant que dão sentido ao discurso complexo, pelas conexões semânticas produzidas em suas AI e AE. Esse movimento argumentativo resulta da interdependência dos segmentos argumentativos, dos encadeamentos e por conseqüência dos blocos semânticos, todos interconectados e interdependentes nas relações de sentido que estabelecem entre si, processo que culmina na realização linguística de nível complexo constituído pelo texto, entidade abstrata subjacente aos discursos realizados, e pelo discurso, como seqüência de enunciados interligados, por isso, também entendido como entidade concreta, ou seja, a manifestação e realização do texto.

Zirconium-titanium-phosphate nanoparticles. Triton X-100 based size modification, characterization and application in radiochemical separation

Energy Technology Data Exchange (ETDEWEB)

Chakraborty, R.; Sen, B.; Chattopadhyay, P. [Burdwan Univ. (India). Dept. of Chemistry

2014-07-01

Zirconium-titanium-phosphate nanoparticles (ZTP) of different sizes were synthesized using tritron X-100 (polyethylene glycol-p-isooctylphenyl ether) surfactant. The materials were characterized by FTIR and powdered X-ray diffraction (XRD). The structural and morphological details of the material were obtained by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The SEM study was followed by energy dispersive spectroscopic analysis (EDS) for elemental analysis of the sample. The important peaks of the XRD spectra were analyzed to determine the probable composition of the material. The particle sizes were determined by dynamic light scattering (DLS) method. Ion exchange capacity was measured for different metal ions with sizes of the ZTP nanoparticles and size-dependent ion exchange property of the material was investigated thoroughly. The nanomaterial of the smallest size of around 5 nm was employed to separate carrier-free {sup 137m}Ba from {sup 137}Cs in column chromatographic technique using 1.0 M HNO{sub 3} as eluting agent at pH = 5. (orig.)

TEM analysis and wear resistance of the ceramic coatings on Q235 steel prepared by hybrid method of hot-dipping aluminum and plasma electrolytic oxidation

Energy Technology Data Exchange (ETDEWEB)

Lu Lihong [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Science and Research Department, Chinese People' s Armed Police Academy, Langfang 065000 (China); Zhang Jingwu [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Shen Dejiu, E-mail: sdj217@ysu.edu.cn [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Wu Lailei; Jiang Guirong [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Li Liang [State Key Laboratory of Automotive Safety and Energy, Tsinghua University, Beijing 100084 (China)

2012-01-25

Highlights: Black-Right-Pointing-Pointer Transmission electron microscopy (TEM) was firstly used to analyze the phase composition of the ceramic coatings. Black-Right-Pointing-Pointer The phase composition of the ceramic coatings is mainly amorphous phase and crystal Al{sub 2}O{sub 3} oxides. Black-Right-Pointing-Pointer The cross-section micro-hardness of the treated samples was investigated, the hardness of the ceramic coatings is about HV1300. Black-Right-Pointing-Pointer The wear resistance of the PEO samples is about 3 times higher than that of the heat treated 45 steel. - Abstract: The hybrid method of PEO and hot-dipping aluminum (HDA) was employed to deposit composite ceramic coatings on the surface of Q235 steel. The composition of the composite coatings was investigated with X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. The cross-section microstructure and micro-hardness of the treated specimens were investigated and analyzed with scanning electron microscopy (SEM) and microscopic hardness meter (MHM), respectively. The wear resistance of the ceramic coatings was investigated by a self-made rubbing wear testing machine. The results indicate that metallurgical bonding can be observed between the ceramic coatings and the steel substrate. There are many micro-pores and micro-cracks, which act as the discharge channels and result of quick and non-uniform cooling of melted sections in the plasma electrolytic oxidation ceramic coatings. The phase composition of the ceramic coatings is mainly composed of amorphous phase and crystal Al{sub 2}O{sub 3} oxides. The crystal Al{sub 2}O{sub 3} phase includes {kappa}-Al{sub 2}O{sub 3}, {theta}-Al{sub 2}O{sub 3} and {beta}-Al{sub 2}O{sub 3}. The grain size of the {kappa}-Al{sub 2}O{sub 3} crystal is quite non-uniform. The hardness of the ceramic coatings is about HV1300 and 10 times higher than that of the Q235 substrate, which was favorable to the better wear resistance of the ceramic

NiFe{sub 2}O{sub 4}/activated carbon nanocomposite as magnetic material from petcoke

Energy Technology Data Exchange (ETDEWEB)

Briceño, Sarah, E-mail: sbriceno@ivic.gob.ve [Laboratorio de Física de la Materia Condensada, Centro de Física, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Brämer-Escamilla, W., E-mail: wbramer@ivic.gob.ve [Laboratorio de Física de la Materia Condensada, Centro de Física, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Silva, P. [Laboratorio de Física de la Materia Condensada, Centro de Física, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); García, J.; Del Castillo, H.; Villarroel, M. [Laboratorio de Cinética y Catálisis, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes ULA, Mérida 5101-A (Venezuela, Bolivarian Republic of); Rodriguez, J.P. [Laboratorio de Microscopia Electrónica. Instituto de Estudios Científicos y Tecnológicos IDECYT. Apartado 47925 - Caracas 1041-A (Venezuela, Bolivarian Republic of); Ramos, M.A.; Morales, R. [Instituto Zuliano de Investigaciones Tecnológicas INZIT. Apdo. Postal 331. La Cañada-Maracaibo (Venezuela, Bolivarian Republic of); Diaz, Y. [Centro de Química, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of)

2014-06-01

Nickel ferrite (NiFe{sub 2}O{sub 4}) was supported on activated carbon (AC) from petroleum coke (petcoke). Potassium hydroxide (KOH) was employed with petcoke to produce activated carbon. NiFe{sub 2}O{sub 4} were synthesized using PEG-Oleic acid assisted hydrothermal method. The structural and magnetic properties were determined using thermogravimetric and differential thermal analysis (TGA–DTA), X-ray diffraction (XRD), Fourier Transform Infrared (IR-FT), surface area (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). XRD analysis revealed the cubic spinel structure and ferrite phase with high crystallinity. IR-FT studies showed that chemical modification promoted the formation of surface oxygen functionalities. Morphological investigation by SEM showed conglomerates of spherical nanoparticles with an average particle size of 72 nm and TEM showed the formation of NiFe{sub 2}O{sub 4}/carbon nanofibers. Chemical modification and activation temperature of 800 °C prior to activation dramatically increased the BET surface area of the resulting activated carbon to 842.4 m{sup 2}/g while the sulfur content was reduced from 6 to 1%. Magnetic properties of nanoparticles show strong dependence on the particle size. - Highlights: • TEM showed the formation of NiFe{sub 2}O{sub 4}/carbon nanofibers. • Nanoparticles were supported on the activated carbon from petcoke. • Activation dramatically increased the BET surface area to 842 m{sup 2}/g. • Magnetic properties show strong dependence on the particle size. • Sulphur content was reduced from 6 to 1% with the petcoke activation.

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

OpenAIRE

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

2017-01-01

This paper demonstrates an acetylene gas sensor based on an Ag-decorated tin dioxide/reduced graphene oxide (Ag–SnO2/rGO) nanocomposite film, prepared by layer-by-layer (LbL) self-assembly technology. The as-prepared Ag–SnO2/rGO nanocomposite was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectrum. The acetylene sensing properties were investigated using different working temperatures and gas concentrations. A...

A novel ZnO@Ag@Polypyrrole hybrid composite evaluated as anode material for zinc-based secondary cell

OpenAIRE

Jianhang Huang; Zhanhong Yang; Zhaobin Feng; Xiaoe Xie; Xing Wen

2016-01-01

A novel ZnO@Ag@Polypyrrole nano-hybrid composite has been synthesized with a one-step approach, in which silver-ammonia complex ion serves as oxidant to polymerize the pyrrole monomer. X-ray diffraction (XRD) and infrared spectroscopy (IR) show the existence of metallic silver and polypyrrole. The structure of nano-hybrid composites are characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM), which demonstrates that the surface of ZnO is decorated with n...

Synthesis of solid and hollow ATO spheres by carbothermal reduction of ATO nanoparticles

International Nuclear Information System (INIS)

Chai Chunfang; Huang Zaiyin; Liao Dankui; Tan Xuecai; Wu Jian; Yuan Aiqun

2007-01-01

Solid and hollow ATO spheres were fabricated by heating ATO nanoparticles and graphite mixture in a tube furnace. The as-synthesized samples were characterized by EDS, XRD, FE-SEM, TEM and HRTEM. The size of the solid spheres could be controlled by adjusting the rate of Ar flow and deposition positions. The hollow spheres were synthesized in an alumina tube system under conditions of a relatively high oxygen concentration. The growth mechanism of solid and hollow spheres was analysed

Studies on the antimicrobial properties of colloidal silver nanoparticles stabilized by bovine serum albumin.

Science.gov (United States)

Mathew, Thomas V; Kuriakose, Sunny

2013-01-01

Colloidal silver nanoparticles were synthesised using sol-gel method and these nanoparticles were stabilised by encapsulated into the scaffolds of bovine serum albumin. Silver nanoparticles and encapsulated products were characterised by FTIR, NMR, XRD, TG, SEM and TEM analyses. Silver nanoparticle encapsulated bovine serum albumin showed highly potent antibacterial activity towards the bacterial strains such as Staphylococcus aureus, Serratia marcescens, Pseudomonas aeruginosa, Escherichia coli and Klebsiella pneumoniae. Copyright © 2012 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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.

TEM sample preparation by femtosecond laser machining and ion milling for high-rate TEM straining experiments

Energy Technology Data Exchange (ETDEWEB)

Voisin, Thomas; Grapes, Michael D. [Dept. of Materials Science and Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States); Zhang, Yong [Dept. of Mechanical Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States); Lorenzo, Nicholas; Ligda, Jonathan; Schuster, Brian [US Army Research Laboratory, Aberdeen Proving Ground, Aberdeen, MD 21005 (United States); Weihs, Timothy P. [Dept. of Materials Science and Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States)

2017-04-15

To model mechanical properties of metals at high strain rates, it is important to visualize and understand their deformation at the nanoscale. Unlike post mortem Transmission Electron Microscopy (TEM), which allows one to analyze defects within samples before or after deformation, in situ TEM is a powerful tool that enables imaging and recording of deformation and the associated defect motion during mechanical loading. Unfortunately, all current in situ TEM mechanical testing techniques are limited to quasi-static strain rates. In this context, we are developing a new test technique that utilizes a rapid straining stage and the Dynamic TEM (DTEM) at the Lawrence Livermore National Laboratory (LLNL). The new straining stage can load samples in tension at strain rates as high as 4×10{sup 3}/s using two piezoelectric actuators operating in bending while the DTEM at LLNL can image in movie mode with a time resolution as short as 70 ns. Given the piezoelectric actuators are limited in force, speed, and displacement, we have developed a method for fabricating TEM samples with small cross-sectional areas to increase the applied stresses and short gage lengths to raise the applied strain rates and to limit the areas of deformation. In this paper, we present our effort to fabricate such samples from bulk materials. The new sample preparation procedure combines femtosecond laser machining and ion milling to obtain 300 µm wide samples with control of both the size and location of the electron transparent area, as well as the gage cross-section and length. - Highlights: • Tensile straining TEM specimens made by femtosecond laser machining and ion milling. • Accurate positioning of the electron transparent area within a controlled gauge region. • Optimization of femtosecond laser and ion milling parameters. • Fast production of numerous samples with a highly repeatable geometry.

Green synthesis of silver nanoparticles using tannins

Science.gov (United States)

Raja, Pandian Bothi; Rahim, Afidah Abdul; Qureshi, Ahmad Kaleem; Awang, Khalijah

2014-09-01

Colloidal silver nanoparticles were prepared by rapid green synthesis using different tannin sources as reducing agent viz. chestnut (CN), mangrove (MG) and quebracho (QB). The aqueous silver ions when exposed to CN, MG and QB tannins were reduced which resulted in formation of silver nanoparticles. The resultant silver nanoparticles were characterized using UV-Visible, X-ray diffraction (XRD), scanning electron microscopy (SEM/EDX), and transmission electron microscopy (TEM) techniques. Furthermore, the possible mechanism of nanoparticles synthesis was also derived using FT-IR analysis. Spectroscopy analysis revealed that the synthesized nanoparticles were within 30 to 75 nm in size, while XRD results showed that nanoparticles formed were crystalline with face centered cubic geometry.

Hydroxyapatite nanocrystals: Simple preparation, characterization and formation mechanism

International Nuclear Information System (INIS)

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-01-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ( 1 H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. - Highlights: • HAP nanobundles and nanoparticles have been prepared by a precipitation method. • Morphologies of HAP nanocrystals were controlled by different coordination ligands. • The formation mechanism of hydroxyapatite nanocrystals was also considered

Hydroxyapatite nanocrystals: Simple preparation, characterization and formation mechanism

Energy Technology Data Exchange (ETDEWEB)

Mohandes, Fatemeh [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Fathi, Mohammadhossein [Biomaterials Research Group, Department of Materials Engineering, Isfahan University of Technology, Isfahan 8415683111, Islamic Republic of Iran (Iran, Islamic Republic of); Dental Materials Research Center, Isfahan University of Medical Sciences, Isfahan, Islamic Republic of Iran (Iran, Islamic Republic of); Fereshteh, Zeinab [Biomaterials Research Group, Department of Materials Engineering, Isfahan University of Technology, Isfahan 8415683111, Islamic Republic of Iran (Iran, Islamic Republic of)

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ({sup 1}H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. - Highlights: • HAP nanobundles and nanoparticles have been prepared by a precipitation method. • Morphologies of HAP nanocrystals were controlled by different coordination ligands. • The formation mechanism of hydroxyapatite nanocrystals was also considered.

Influence of mineralizer agents on the growth of crystalline CeO{sub 2} nanospheres by the microwave-hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Deus, R.C. [Universidade Estadual Paulista-Unesp - Faculdade de Engenharia de Guaratingueta, Av. Dr. Ariberto Pereira da Cunha, 333 Bairro Portal das Colinas, CEP 12516-410 Guaratingueta-SP (Brazil); Cilense, M.; Foschini, C.R. [Universidade Estadual Paulista-Unesp - Instituto de Quimica - Laboratorio Interdisciplinar em Ceramica (LIEC), Rua Professor Francisco Degni s/n, CEP 14800-90 Araraquara, SP (Brazil); Ramirez, M.A. [Universidade Estadual Paulista-Unesp - Faculdade de Engenharia de Guaratingueta, Av. Dr. Ariberto Pereira da Cunha, 333 Bairro Portal das Colinas, CEP 12516-410 Guaratingueta-SP (Brazil); Longo, E. [Universidade Estadual Paulista-Unesp - Instituto de Quimica - Laboratorio Interdisciplinar em Ceramica (LIEC), Rua Professor Francisco Degni s/n, CEP 14800-90 Araraquara, SP (Brazil); Simoes, A.Z., E-mail: alezipo@yahoo.com [Universidade Estadual Paulista-Unesp - Faculdade de Engenharia de Guaratingueta, Av. Dr. Ariberto Pereira da Cunha, 333 Bairro Portal das Colinas, CEP 12516-410 Guaratingueta-SP (Brazil); Universidade Federal de Itajuba-Unifei - Campus Itabira, Rua Sao Paulo, 377 Bairro Amazonas, CEP 35900-37 Itabira, MG (Brazil)

2013-02-15

Cystalline ceria (CeO{sub 2}) nanoparticles have been synthesized by a simple and fast microwave-assisted hydrothermal (MAH) under NaOH, KOH, and NH{sub 4}OH mineralizers added to a cerium ammonium nitrate aqueous solution. The products were characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transformed-IR and Raman spectroscopies. Rietveld refinement reveals a cubic structure with a space group Fm3m while infrared data showed few traces of nitrates. Field emission scanning microcopy (FEG-SEM) revealed a homogeneous size distribution of nanometric CeO{sub 2} nanoparticles. The MAH process in KOH and NaOH showed most effective to dehydrate the adsorbed water and decrease the hydrogen bonding effect leaving a weakly agglomerated powder of hydrated ceria. TEM micrographs of CeO{sub 2} synthesized under MAH conditions reveal particles well-dispersed and homogeneously distributed. The MAH enabled cerium oxide to be synthesized at 100 Degree-Sign C for 8 min.

Influence of mineralizer agents on the growth of crystalline CeO2 nanospheres by the microwave-hydrothermal method

International Nuclear Information System (INIS)

Deus, R.C.; Cilense, M.; Foschini, C.R.; Ramirez, M.A.; Longo, E.; Simões, A.Z.

2013-01-01

Cystalline ceria (CeO 2 ) nanoparticles have been synthesized by a simple and fast microwave-assisted hydrothermal (MAH) under NaOH, KOH, and NH 4 OH mineralizers added to a cerium ammonium nitrate aqueous solution. The products were characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transformed-IR and Raman spectroscopies. Rietveld refinement reveals a cubic structure with a space group Fm3m while infrared data showed few traces of nitrates. Field emission scanning microcopy (FEG-SEM) revealed a homogeneous size distribution of nanometric CeO 2 nanoparticles. The MAH process in KOH and NaOH showed most effective to dehydrate the adsorbed water and decrease the hydrogen bonding effect leaving a weakly agglomerated powder of hydrated ceria. TEM micrographs of CeO 2 synthesized under MAH conditions reveal particles well-dispersed and homogeneously distributed. The MAH enabled cerium oxide to be synthesized at 100 °C for 8 min.

Synthesis and characterization of bovine femur bone hydroxyapatite containing silver nanoparticles for the biomedical applications

International Nuclear Information System (INIS)

Nirmala, R.; Sheikh, Faheem A.; Kanjwal, Muzafar A.; Lee, John Hwa; Park, Soo-Jin; Navamathavan, R.; Kim, Hak Yong

2011-01-01

Bovine femur bone hydroxyapatite (HA) containing silver (Ag) nanoparticles was synthesized by thermal decomposition method and subsequent reduction of silver nitrate with N,N-dimethylformamide (DMF) in the presence of poly(vinylacetate) (PVAc). The structural, morphological, and chemical properties of the HA–Ag nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). TEM images showed that the Ag nanoparticles with size ranging from 8 to 20 nm and were arranged at the periphery of HA crystals. Bactericidal activity of HA–Ag with different concentration of Ag nanoparticles immobilized on the surface of HA was investigated against gram-positive Staphylococcus aureus (S. aureus, non-MRSA), Methicillin resistant S. aureus (MRSA) and gram-negative Escherichia coli (E.coli) by the disc diffusion susceptibility test. The HA–Ag nanoparticles showed that broad spectrum activity against non-MRSA, MRSA, and E. coli bacterial strains.

In Situ Synthesis and Characterization of Polyethyleneimine-Modified Carbon Nanotubes Supported PtRu Electrocatalyst for Methanol Oxidation

Directory of Open Access Journals (Sweden)

Xi Geng

2015-01-01

Full Text Available PtRu bimetallic nanoparticles were successfully synthesized on polyethyleneimine- (PEI- functionalized multiwalled carbon nanotubes (MWCNTs via an effective and facile polyol reduction approach. Noncovalent surface modification of MWCNTs with PEI was confirmed by FTIR and zeta potential measurements. The morphology, crystalline structure, and composition of the hybrid material were characterized by transmission electron microscopy (TEM, scanning electron microscopy (SEM, X-ray powder diffraction (XRD, and energy dispersive X-ray spectroscopy (EDX, respectively. According to SEM and TEM observations, PtRu nanoparticles with narrow size distribution were homogeneously deposited on PEI-MWCNTs. Cyclic voltammetry tests demonstrated that the as-prepared PtRu/PEI-MWCNTs nanocomposite had a large electrochemical surface area and exhibited enhanced electrocatalytic activity towards methanol oxidation in comparison with oxidized MWCNTs as catalyst support. PEI-functionalized CNTs, as useful building blocks for the assembly of Pt-based electrocatalyst, may have great potential for applications such as direct methanol fuel cell (DMFC.

TEM of nanostructured metals and alloys

International Nuclear Information System (INIS)

Karnthaler, H.P.; Waitz, T.; Rentenberger, C.; Mingler, B.

2004-01-01

Nanostructuring has been used to improve the mechanical properties of bulk metals and alloys. Transmission electron microscopy (TEM) including atomic resolution is therefore appropriate to study these nanostructures; four examples are given as follows. (1) The early stages of precipitation at RT were investigated in an Al-Mg-Si alloy. By high resolution TEM it is shown that the precipitates lie on (0 0 1) planes having an ordered structure. (2) In Co alloys the fronts of martensitic phase transformations were analysed showing that the transformation strains are very small thus causing no surface relief. (3) Re-ordering and recrystallization were studied by in situ TEM of an Ni 3 Al alloy being nanocrystalline after severe plastic deformation. (4) In NiTi severe plastic deformation is leading to the formation of amorphous shear bands. From the TEM analysis it is concluded that the amorphization is caused by plastic shear instability starting in the shear bands

TEM Nanostructural Study of Al-6Si-3Cu-Mg Melt-Spun Ribbons

Directory of Open Access Journals (Sweden)

Ismeli Alfonso López

2008-01-01

Full Text Available Three quaternary Al-6Si-3Cu-xMg (x = 0.59, 3.80, and 6.78 wt.% alloys were produced by melt-spun and characterized using X-ray diffractometry (XRD, transmission electron microscopy (TEM, and microhardness techniques. Obtained second phases were Al2Cu( for the alloy with 0.59% Mg and Al5Cu2Mg8Si6 (Q for the alloys with 3.80 and 6.78% Mg. These phases are present as 30–50 nm or as 5–10 nm nanoparticles. Alloying elements content in solid solution increased, mainly for Si and Mg. The high alloying elements content in solid solution and the small -Al cell size for melt-spun alloys leads to microhardness values about 2 times higher than those of ingot counterparts. The microhardness increase for melt-spun alloys with 3.80 and 6.78% Mg depends on Mg content in solid solution.

Surfactant Assisted Stabilization of Carbon Nanotubes Synthesized by a Spray Pyrolysis Method

Directory of Open Access Journals (Sweden)

D. Mendoza-Cachú

2017-01-01

Full Text Available Surface modification of carbon nanotubes has been an interesting issue from a composites materials point of view. A nanotubes agglomeration has to be avoided to achieve a homogeneous dispersion in a composite matrix. In this research, we report on the synthesis of carbon nanotubes using a variant of the chemical vapor deposition technique known as spray pyrolysis method. X-ray diffraction (XRD, transmission electron microscopy (TEM, and scanning electron microscopy (SEM studies showed that the synthesized products had an aligned structure with low purity degree, high content of catalyst particles, and a smaller amount of amorphous carbon. A secondary method was applied, which involves an acidic treatment that dissolves contaminant particles to enhance the purity of the nanotubes. Microstructural analysis, which includes XRD and SEM, indicates an effective reduction of impurities. Dispersion of the nanotubes was assessed using different surfactants, such as sodium dodecyl-sulfate (SDS and ethylenediaminetetraacetic acid (EDTA. Finally, Raman spectroscopy, UV-Vis, and SEM techniques confirm that better results were obtained with EDTA. For EDTA and SDS surfactants, low concentrations of 0.3 mg/mL and 0.2 mg/mL were most efficient, respectively.

Evolution of interface and surface structures of ZnO/Al2 O3 multilayers upon rapid thermal annealing

Science.gov (United States)

Liu, H. H.; Chen, Q. Y.; Chang, C. F.; Hsieh, W. C.; Wadekar, P. V.; Huang, H. C.; Liao, H. H.; Seo, H. W.; Chu, W. K.

2015-03-01

ZnO ∖Al2O3 multilayers were deposited on sapphires by atomic layer deposition at 85°C. This low substrate temperature ensures good interface smoothness useful for study of interfacial reaction or interdiffusion. Our study aimed at the effects of rapid thermal annealing at different annealing temperatures, times and PAr:PO2. XRR and XRD techniques were used to investigate the kinetics from which various terms of the activation energies could be determined. HR-TEM and electron diffraction were carried out to correlate the microstructures and interfacial alignments as a result of the reactions. AFM were used to assist SEM profiling of the surface morphological evolution in association with the TEM observations.

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

Energy Technology Data Exchange (ETDEWEB)

Kale, R.B. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China)]. E-mail: rb_kale@yahoo.co.in; Sartale, S.D. [Hahn Meitner Institute, Glienicker Strasse-100, D-14109 Berlin (Germany); Ganesan, V. [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore 452017 (India); Lokhande, C.D. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (India); Lin, Y.-F. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China); Lu, S.-Y. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China)]. E-mail: sylu@mx.nthu.edu.tw

2006-11-15

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH{sub 3}COO){sub 2} as Pb{sup 2+} and Na{sub 2}SeSO{sub 3} as Se{sup 2-} ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

A novel nanostructure of cadmium oxide synthesized by mechanochemical method

Energy Technology Data Exchange (ETDEWEB)

Tadjarodi, A., E-mail: tajarodi@iust.ac.ir [Research Laboratory of Inorganic Materials Synthesis, Department of Chemistry, Iran University of Science and Technology, 16846-13114 Tehran (Iran, Islamic Republic of); Imani, M. [Research Laboratory of Inorganic Materials Synthesis, Department of Chemistry, Iran University of Science and Technology, 16846-13114 Tehran (Iran, Islamic Republic of)

2011-11-15

Highlights: {yields} A novel nanostructure of CdO was synthesized by mechanochemical reaction followed by calcination. {yields} Mechanochemical method is a simple and low-cost to synthesize nanomaterials. {yields} The obtained precursor was characterized by FT-IR, NMR techniques and elemental analysis. {yields} SEM images showed cauliflower-like shape of sample with components average diameter of 68 nm. {yields} The rods and tubes bundles with single crystalline nature were revealed by ED pattern and TEM images. -- Abstract: Cauliflower-like cadmium oxide (CdO) nanostructure was synthesized by mechanochemical reaction followed calcination procedure. Cadmium acetate dihydrate and acetamide were used as reagents and the resulting precursor was calcinated at 450 {sup o}C for 2 h in air. The structures of the precursor and resultant product of the heating treatment were characterized using Fourier transform infrared (FT-IR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy and elemental analysis, X-ray powder diffraction (XRD), energy-dispersive X-ray spectroscopy analysis (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction pattern (ED). SEM and TEM images revealed the cauliflower-like morphology of the sample. This structure includes the bundles of rods and tubes in nanoscale, which combine with each other and form the resulting morphology with the average diameter, 68 nm of the components. ED pattern indicated the single crystal nature of the formed bundles.

A novel nanostructure of cadmium oxide synthesized by mechanochemical method

International Nuclear Information System (INIS)

Tadjarodi, A.; Imani, M.

2011-01-01

Highlights: → A novel nanostructure of CdO was synthesized by mechanochemical reaction followed by calcination. → Mechanochemical method is a simple and low-cost to synthesize nanomaterials. → The obtained precursor was characterized by FT-IR, NMR techniques and elemental analysis. → SEM images showed cauliflower-like shape of sample with components average diameter of 68 nm. → The rods and tubes bundles with single crystalline nature were revealed by ED pattern and TEM images. -- Abstract: Cauliflower-like cadmium oxide (CdO) nanostructure was synthesized by mechanochemical reaction followed calcination procedure. Cadmium acetate dihydrate and acetamide were used as reagents and the resulting precursor was calcinated at 450 o C for 2 h in air. The structures of the precursor and resultant product of the heating treatment were characterized using Fourier transform infrared (FT-IR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy and elemental analysis, X-ray powder diffraction (XRD), energy-dispersive X-ray spectroscopy analysis (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction pattern (ED). SEM and TEM images revealed the cauliflower-like morphology of the sample. This structure includes the bundles of rods and tubes in nanoscale, which combine with each other and form the resulting morphology with the average diameter, 68 nm of the components. ED pattern indicated the single crystal nature of the formed bundles.

Fabrication of nano structural biphasic materials from phosphogypsum waste and their in vitro applications

Energy Technology Data Exchange (ETDEWEB)

Mohamed, Khaled R., E-mail: Kh_rezk966@yahoo.com [Biomaterials Department, National Research Centre, Dokki, Cairo (Egypt); Mousa, Sahar M. [Chemistry Department, Science and Art College, King Abdulaziz University, Rabigh Campus, P.O. Box 344, 21911 Rabigh (Saudi Arabia); Inorganic Chemistry Department, National Research Centre, Dokki, P.O. Box 12622, 11787 Cairo (Egypt); El Bassyouni, Gehan T. [Biomaterials Department, National Research Centre, Dokki, Cairo (Egypt); Medical Physics Department, College of Medicine, Taif University (Saudi Arabia)

2014-02-01

Graphical abstract: (a) Schema of the process, (b) TEM of nano particles of biphasic materials and (c) SEM of post-immersion. - Highlights: • Ratio of HA and β-TCP phases were controlled by thermal treatment. • HA partially decomposed into β-TCP with other bioactive phases. • Calcined HA at 900 °C is the best for the bioactivity behavior. - Abstract: In this study, a novel process of preparing biphasic calcium phosphate (BCP) is proposed. Also its bioactivity for the utilization of the prepared BCP as a biomaterial is studied. A mixture of calcium hydroxyapatite (HAP) and tricalcium phosphate (β-TCP) could be obtained by thermal treatment of HAP which was previously prepared from phosphogypsum (PG) waste. The chemical and phase composition, morphology and particle size of prepared samples was characterized by X-ray diffraction (XRD), Infrared spectroscopy (IR), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). The bioactivity was investigated by soaking of the calcined samples in simulated body fluid (SBF). Results confirmed that the calcination temperatures played an important role in the formation of calcium phosphate (CP) materials. XRD results indicated that HAP was partially decomposed into β-TCP. The in vitro data confirmed that the calcined HAP forming BCP besides other phases such as pyrophosphate and silica are bioactive materials. Therefore, BCP will be used as good biomaterials for medical applications.

Understanding the formation and growth of Ag nanoparticles on silver chromate induced by electron irradiation in electron microscope: A combined experimental and theoretical study

International Nuclear Information System (INIS)

Fabbro, Maria T.; Gracia, Lourdes; Silva, Gabriela S.; Santos, Luís P.S.; Andrés, Juan; Cordoncillo, Eloisa; Longo, E.

2016-01-01

Ag 2 CrO 4 microcrystals were synthesized using the co-precipitation method. These microcrystals were characterized through X-ray diffraction (XRD) with Rietveld analysis, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) with energy-dispersive spectroscopy (EDS), micro-Raman (MR). XRD patterns and Rietveld refinement data showed that the material exhibits an orthorhombic structure without any deleterious phases. FE-SEM and TEM micrographs revealed the morphology and the growth of Ag nanoparticles on Ag 2 CrO 4 microcrystals during electron beam irradiation. These events were directly monitored in real-time. Their optical properties were investigated using ultraviolet-visible (UV–vis) diffuse reflectance spectroscopy that allowed the calculation of the optical band gap energy. Theoretical analyses based on the density functional theory level indicate that the incorporation of electrons is responsible for structural modifications and formation of defects on the [AgO 6 ] and [AgO 4 ] clusters, generating ideal conditions for the growth of Ag nanoparticles. - Graphical abstract: Theoretical representation of the Ag 2 CrO 4 orthorhombic structure. Display Omitted - Highlights: • The Ag 2 CrO 4 microcrystals indicate an orthorhombic structure. • The formation of Ag 0 promotes Ag-nanoparticle growth on the surface of the Ag 2 CrO 4 . • Electron irradiation of the material induces the formation of Ag vacancies.

Precipitated nickel doped ZnO nanoparticles with enhanced low temperature ethanol sensing properties

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Umadevi Godavarti

2017-12-01

Full Text Available The Zn1-xNixO nanoparticles have been synthesized by novel co-precipitation method and systematically characterized by XRD, SEM, TEM and photo luminescence. The XRD patterns confirm the hexagonal wurzite structure without secondary phases in Ni substituted ZnO samples. SEM and TEM are used for the estimation of particle shape and size. In PL study there is a peak in the range of 380–390 nm in all samples that is attributed to the oxygen vacancies. Gas sensing tests reveal that Ni doped ZnO sensor has remarkably enhanced performance compared to pure ZnO detected at an optimum temperature 100 °C. It could detect ethanol gas in a wide concentration range with very high response, fast response–recovery time, good selectivity and stable repeatability. The possible sensing mechanism is discussed. The high response of ZnO Nanoparticles was attributed to large contacting surface area for electrons, oxygen, target gas molecule, and abundant channels for gas diffusion. The superior sensing features indicate the present Ni doped ZnO as a promising nanomaterial for gas sensors. The response time and recovery time of undoped is 75 s and 60 s and 0.25 at% Ni are found to be 60 s and 45 s at 100 °C respectively.

Fabrication and Assessment of ZnO Modified Polyethersulfone Membranes for Fouling Reduction of Bovine Serum Albumin

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Tshepo Duncan Dipheko

2017-01-01

Full Text Available ZnO/PES composite membranes were fabricated by phase inversion method using DMAc as a solvent. The structure of ZnO was investigated using TEM, SEM, XRD, and TGA. TEM images of ZnO nanoparticles were well-defined, small, and spherically shaped with agglomerated nanoparticles particles of 50 nm. The SEM and XRD results were an indication that ZnO nanoparticles were present in the prepared ZnO/PES composites membranes. Contact angle measurements were used to investigate surface structures of the composite membranes. The amount of ZnO nanoparticles on PES membranes was varied to obtain the optimal performance of the composite membranes in terms of pure water flux, flux recovery, and fouling resistance using the protein bovine serum albumin (BSA as a model organic foulant. The results showed that addition of ZnO to PES membranes improved the hydrophilicity, permeation, and fouling resistance properties of the membranes. Pure water flux increased from a low of 250 L/m2h for the neat membrane to a high of 410 L/m2h for the composite membranes. A high flux recovery of 80–94% was obtained for the composite membranes. The optimal performance of the composite membranes was obtained at 1.5 wt% of ZnO.

Green synthesis of silver nanoparticles using Cordia dichotoma fruit extract and its enhanced antibacterial, anti-biofilm and photo catalytic activity

Science.gov (United States)

Bharathi, Devaraj; Vasantharaj, Seerangaraj; Bhuvaneshwari, V.

2018-05-01

The present study describes the antibacterial, anti-biofilm and photo catalytic activity of silver nanoparticles synthesized using Cordia dichotoma fruits (Cd-AgNPs) for the first time. The phyto-synthesized Cd-AgNPs were characterized by UV-Visible spectroscopy, Field emission-scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), Energy dispersive x-ray spectrometer (EDX), Fourier transform infrared spectroscopy (FT-IR), and x-ray diffraction (XRD). FE-SEM and TEM observation showed that the average size of 2–60 nm with spherical shape of Cd-AgNPs and the presence of phyto-compounds which are responsible for capping and reduction were studied by FT-IR. XRD studies revealed the face-centered cubic structure of Cd-AgNPs. The synthesized Cd-AgNPs showed significant antibacterial activity against Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli, assayed using agar well diffusion method. Phyto-synthesized Cd-AgNPs exhibited more than 90% inhibition of biofilm activity formed by S. aureus and E. coli. Furthermore, photocatalytic degradation of crystal violet (CV) under UV light irradiation using Cd-AgNPs was performed. Synthesized Cd-AgNPs exhibited ∼85% degradation activity for CV. Collectively, our findings suggest that C.dichotoma is a green source for the eco-friendly synthesis of Cd-AgNPs, which further can be used as a novel biocidal agent against bacterial pathogens and a potent photo catalytic agent.

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

Science.gov (United States)

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.

Effect of high shear mixing parameters and degassing temperature on the morphology of epoxy-clay nanocomposites

KAUST Repository

Al-Qadhi, Muneer; Merah, N.; Mezghani, Khaled S.; Khan, Zafarullah; Gasem, Zuhair Mattoug Asad; Sougrat, Rachid

2013-01-01

Epoxy-clay nanocomposites were prepared by high shear mixing method using Nanomer I.30E nanoclay as nano-reinforcement in diglycidyl ether of bisphenol A (DGEBA). The effect of mixing speed and time on the nature and degree of clay dispersion were investigated by varying the mixing speed in the range of 500-8000 RPM and mixing time in the range of 15-90 minutes. The effect of degassing temperature on the morphology of the resultant nanocomposites was also studied. Scanning and transmission microscopy (SEM and TEM) along with x-ray diffraction (XRD) have been used to characterize the effect of shear mixing speed, mixing time and degassing temperature on the structure of the resultant nanocomposites. The SEM, TEM and XRD examinations demonstrated that the degree of clay dispersion was improved with increasing the high shear mixing speed and mixing time. The results showed that the optimum high shear mixing speed and mixing time were 6000 rpm and 60 min, respectively. It was observed that the structure of the nanocomposites that have been degassed at 65°C was dominated by ordered intercalated morphology while disordered intercalated with some exfoliated morphology was found for the sample degassed at 100°C for the first 2 hours of the degassing process. © (2013) Trans Tech Publications, Switzerland.

Non-vacuum mechanochemical route to the synthesis of Cu2SnS3 nano-ink for solar cell applications

International Nuclear Information System (INIS)

Vanalakar, S.A.; Agawane, G.L.; Shin, S.W.; Yang, H.S.; Patil, P.S.; Kim, J.Y.; Kim, J.H.

2015-01-01

Cu-based ternary chalcogenides such as Cu 2 SnS 3 (CTS) are attracting increasing interest due to their outstanding opto-electronic properties. Herein, a simple, cost-effective non-vacuum mechanochemical synthetic route for preparing CTS nanocrystals with controlled size and composition is presented. CTS nanocrystalline powders were synthesized by ball milling and subsequent annealing in an H 2 S atmosphere. These nanocrystal samples were characterized using powder X-ray diffraction (P-XRD), Raman spectroscopy, ultraviolet–visible optical spectroscopy, energy-dispersive X-ray spectroscopy (EDS), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) techniques. Texture structures with cubic crystallinity were observed from the P-XRD of (1 1 2), (2 0 0) planes of CTS nanopowders. The EDS results confirmed that the synthesized powders had an appropriate chemical purity. According to TEM/FE-SEM observations, a nanostructure CTS was obtained after 36 h of mechanochemical processing followed by annealing. The average particle size of single phase CTS after 48 h of milling was ∼45 nm. Based on obtained data using characterization methods, reaction mechanism steps were proposed to clarify the reactions that occurred during the mechanochemical process. In order to prepare nanocrystal ink, ethanol was used as a solvent, and polyvinylpyrrolidone, which acts as an organic stabilizing agent, was added to the CTS powder to prepare a printable paste

Synthesis and characterization of samarium-doped ZnS nanoparticles: A novel visible light responsive photocatalyst

Energy Technology Data Exchange (ETDEWEB)

Hanifehpour, Younes, E-mail: y_hanifehpour@yu.ac.kr [School of Mechanical Engineering, Yeungnam University, Gyeongsan 712-749 (Korea, Republic of); Soltani, Behzad; Amani-Ghadim, Ali Reza; Hedayati, Behnam [Department of Chemistry, Faculty of Basic Sciences, Azarbaijan Shahid Madani University, Tabriz (Iran, Islamic Republic of); Khomami, Bamin [Department of Chemical and Biomolecular Engineering, University of Tennessee, Knoxville, TN 37996 (United States); Joo, Sang Woo, E-mail: swjoo1@gmail.com [School of Mechanical Engineering, Yeungnam University, Gyeongsan 712-749 (Korea, Republic of)

2016-04-15

Highlights: • Sm-doped ZnS Nanomaterials were synthesized by hydrothermal method. • The as-prepared compounds were characterized by XRD, TEM, XPS, SEM and UV techniques. • The photocatalytic effect of compounds was determined by Reactive Red 43 degradation. • The degradation of RRed 43 followed the Langmuir–Hinshelwood kinetic model. - Abstract: We prepared pure and samarium-doped ZnS (Sm{sub x}Zn{sub 1−x}S{sub 1+0.5x}) nanoparticles via hydrothermal process at 160 °C for 24 h. XRD analysis shows that the particles were well crystallized and corresponds to a cubic sphalerite phase. SEM and TEM images indicate that the sizes of the particles were in the range of 20–60 nm. The photocatalytic activity of Sm-doped ZnS nanoparticles was evaluated by monitoring the decolorization of Reactive Red 43 in aqueous solution under visible light irradiation. The color removal efficiency of Sm{sub 0.04}Zn{sub 0.96}S and pure ZnS was 95.1% and 28.7% after 120 min of treatment, respectively. Among the different amounts of dopant agent used, 4% Sm-doped ZnS nanoparticles indicated the highest decolorization. We found that the presence of inorganic ions such as Cl{sup −}, CO{sub 3}{sup 2−} and other radical scavengers such as buthanol and isopropyl alcohol reduced the decolorization efficiency.

SAXS and TEM Investigation of Bentonite Structure

International Nuclear Information System (INIS)

Matusewicz, Michal; Liljestroem, Ville; Muurinen, Arto; Serimaa, Ritva

2013-01-01

A preliminary investigation of bentonite structure using Small-Angle X-ray Scattering (SAXS) and Transmission Electron Microscopy (TEM) is presented. Three types of clay were used: unchanged MX-80 bentonite and purified clays with sodium or calcium ions. Quantitative information in nano-scale - basal spacing, mean crystallite size - was obtained from SAXS, which was complemented by TEM to give qualitative information from micron to nanometre scale. SAXS seems to be a more reliable source of quantitative data than TEM. SAXS gives the averaged information about basal spacing. TEM in this study gives more qualitative information, but in a greater resolution range. The presented work is a starting point to combine more methods to obtain a better idea of bentonite structure. (authors)

Ao leitor sem medo

Directory of Open Access Journals (Sweden)

José Eisenberg

2000-05-01

Full Text Available O texto resenha Ao leitor sem medo, de Renato Janine Ribeiro (Belo Horizonte, UFMG, 1999.This text is a review of Ao leitor sem medo by Renato Janine Ribeiro (Belo Horizonte, UFMG, 1999

Application of TEM to highly reactive metals

International Nuclear Information System (INIS)

Sherry, W.M.; Prinz, F.

1982-01-01

In the following a method for the preparation and observation of sodium TEM specimens and the first TEM micrograph ever to be published on the dislocation microstructure of sodium are reported. (orig./IHOE) [de

Microstructure of thin film platinum electrodes on yttrium stabilized zirconia prepared by sputter deposition

Energy Technology Data Exchange (ETDEWEB)

Toghan, Arafat, E-mail: arafat.toghan@pci.uni-hannover.de [Institute of Physical Chemistry and Electrochemistry, Leibniz University of Hannover, Callinstrasse 3-3a, D-30167 Hannover (Germany); Khodari, M. [Chemistry Department, Faculty of Science, South Valley University, Qena, 83523 (Egypt); Steinbach, F.; Imbihl, R. [Institute of Physical Chemistry and Electrochemistry, Leibniz University of Hannover, Callinstrasse 3-3a, D-30167 Hannover (Germany)

2011-09-01

(111) oriented thin film Pt electrodes were prepared on single crystals of yttrium-stabilized zirconia (YSZ) by sputter deposition of platinum. The electrodes were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), X-ray diffraction (XRD), energy-dispersive X-ray analysis (EDX), atomic force microscopy (AFM) and by profilometry. SEM images of the as-sputtered platinum film show a compact amorphous Pt film covering uniformly the substrate. Upon annealing at 1123 K, gaps and pores at the interface develop leading to a partial dewetting of the Pt film. Increasing the annealing temperature to 1373 K transforms the polycrystalline Pt film into single crystalline grains exhibiting a (111) orientation towards the substrate.

Mechanical Conversion for High-Throughput TEM Sample Preparation

International Nuclear Information System (INIS)

Kendrick, Anthony B; Moore, Thomas M; Zaykova-Feldman, Lyudmila

2006-01-01

This paper presents a novel method of direct mechanical conversion from lift-out sample to TEM sample holder. The lift-out sample is prepared in the FIB using the in-situ liftout Total Release TM method. The mechanical conversion is conducted using a mechanical press and one of a variety of TEM coupons, including coupons for both top-side and back-side thinning. The press joins a probe tip point with attached TEM sample to the sample coupon and separates the complete assembly as a 3mm diameter TEM grid, compatible with commercially available TEM sample holder rods. This mechanical conversion process lends itself well to the high through-put requirements of in-line process control and to materials characterization labs where instrument utilization and sample security are critically important

Short review on chemical bath deposition of thin film and characterization

Energy Technology Data Exchange (ETDEWEB)

Mugle, Dhananjay, E-mail: dhananjayforu@gmail.com; Jadhav, Ghanshyam, E-mail: ghjadhav@rediffmail.com [Depertment of Physics, Shri Chhatrapati Shivaji College, Omerga-413606 (India)

2016-05-06

This reviews the theory of early growth of the thin film using chemical deposition methods. In particular, it critically reviews the chemical bath deposition (CBD) method for preparation of thin films. The different techniques used for characterizations of the chemically films such as X-ray diffractometer (XRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Electrical conductivity and Energy Dispersive Spectroscopy (EDS) are discussed. Survey shows the physical and chemical properties solely depend upon the time of deposition, temperature of deposition.

Facile Synthesis of Rambutan-Like ZnO Hierarchical Hollow Microspheres with Highly Photocatalytic Activity

Directory of Open Access Journals (Sweden)

Ke-Jian Ju

2015-01-01

Full Text Available Rambutan-like ZnO hierarchical hollow microspheres (ZnO HHMs were constructed under hydrothermal conditions, using carboxyl methyl starch (CMS as a soft template. The resulting products were characterized by using X-ray diffraction (XRD, scanning electron microscopy (SEM, and transmission electron microscopy (TEM. The experimental parameters and growth mechanism of rambutan-like ZnO HHMs were discussed in some detail. The as-prepared samples displayed improved photocatalytic activity for the degradation of rhodamine B under ultraviolet (UV irradiation.

Synthesis and characterization of Al2O3 obtained from the polymeric precursor method using glycerin as a poly alcohol

International Nuclear Information System (INIS)

Elicker, C.; Gaier, M.; Almeida, S.R.; Vieiraaa, B.M.; Ratmann, C.W.R.; Pereira, C.M.P. de; Cava, S.S.; Egea, J.J.

2014-01-01

In this study, calcium aluminate was synthesized using glycerin to replace ethylene glycol in the polymeric precursor method. The resulting resin was pre-calcined in a muffle at 300 °C for 2 h and the resulting material was calcined at 900 °C for 2 h. The powders were analyzed by XRD, SEM and EDX, TEM, Micro-Raman and IR. The results demonstrated the possibility of using glycerin as an alternative to ethylene glycol in the polymeric precursor method. (author)

Photoluminescence of Hexagonal ZnO Nanorods Hydrothermally Grown on Zn Foils in KOH Solutions with Different Values of Basicity

Directory of Open Access Journals (Sweden)

Nuengruethai Ekthammathat

2013-01-01

Full Text Available Aligned hexagonal ZnO nanorods on pure Zn foils were hydrothermally synthesized in 30 mL solutions containing 0.05–0.50 g KOH. The products were characterized by X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, and photoluminescence (PL spectroscopy. In this research, wurtzite hexagonal ZnO nanorods grown along the [002] direction with green light emission at 541 nm caused by singly ionized oxygen vacancies inside were detected.

Morphology and dispersion of FeCo alloy nanoparticles dispersed in a matrix of IR pyrolized polyvinyl alcohol

Science.gov (United States)

Vasilev, A. A.; Dzidziguri, E. L.; Muratov, D. G.; Zhilyaeva, N. A.; Efimov, M. N.; Karpacheva, G. P.

2018-04-01

Metal-carbon nanocomposites consisting of FeCo alloy nanoparticles dispersed in a carbon matrix were synthesized by the thermal decomposition method of a precursor based on polyvinyl alcohol and metals salts. The synthesized powders were investigated by X-ray diffraction (XRD), X-ray fluorescent spectrometry (XRFS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Surface characteristics of materials were measured by BET-method. The morphology and dispersity of metal nanoparticles were studied depending on the metals ratio in the composite.

Room-temperature synthesis and photoluminescence of hexagonal CePO4 nanorods

Science.gov (United States)

Zhu, J.; Zhang, K.; Zhao, H. Y.

2018-01-01

Hexagonal CePO4 nanorods were synthesized via a simple chemical precipitation route at room-temperature without the presence of surfactants and then characterized by powder X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectrometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption and photoluminescence (PL) spectroscopy. Hexagonal CePO4 nanorods exhibit strong ultraviolet absorption and ultraviolet luminescence, which correspond to the electronic transitions between 4f and 5d state of Ce3+ ions.

Microwave-assisted hydrothermal synthesis of coralloid nanostructured nickel hydroxide hydrate and thermal conversion to nickel oxide

International Nuclear Information System (INIS)

Lai, Teh-Long; Lai, Yuan-Lung; Yu, Jen-Wei; Shu, Youn-Yuen; Wang, Chen-Bin

2009-01-01

Coralloid nanostructured nickel hydroxide hydrate has been successfully synthesized by a simple microwave-assisted hydrothermal process using nickel sulfate hexahydrate as precursor and urea as hydrolysis-controlling agent. A pure coralloid nanostructured nickel oxide can be obtained from the nickel hydroxide hydrate after calcination at 400 deg. C. The thermal property, structure and morphology of samples were characterized by thermogravimetry (TG), temperature-programmed reduction (TPR), X-ray (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM).

Microwave-assisted hydrothermal synthesis of coralloid nanostructured nickel hydroxide hydrate and thermal conversion to nickel oxide

Energy Technology Data Exchange (ETDEWEB)

Lai, Teh-Long [Environmental Analysis Laboratory, Department of Chemistry, National Kaohsiung Normal University, Kaohsiung 802, Taiwan (China); Lai, Yuan-Lung [Department of Mechanical and Automation Engineering, Da-Yeh University, Changhua 515, Taiwan (China); Yu, Jen-Wei [Environmental Analysis Laboratory, Department of Chemistry, National Kaohsiung Normal University, Kaohsiung 802, Taiwan (China); Shu, Youn-Yuen, E-mail: shuyy@nknucc.nknu.edu.tw [Environmental Analysis Laboratory, Department of Chemistry, National Kaohsiung Normal University, Kaohsiung 802, Taiwan (China); Wang, Chen-Bin, E-mail: chenbin@ccit.edu.tw [Department of Applied Chemistry and Materials Science, Chung Cheng Institute of Technology, National Defense University, Tahsi, Taoyuan 335, Taiwan (China)

2009-10-15

Coralloid nanostructured nickel hydroxide hydrate has been successfully synthesized by a simple microwave-assisted hydrothermal process using nickel sulfate hexahydrate as precursor and urea as hydrolysis-controlling agent. A pure coralloid nanostructured nickel oxide can be obtained from the nickel hydroxide hydrate after calcination at 400 deg. C. The thermal property, structure and morphology of samples were characterized by thermogravimetry (TG), temperature-programmed reduction (TPR), X-ray (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM).

Synthesis and characterization of Al{sub 2}O{sub 3} obtained from the polymeric precursor method using glycerin as a poly alcohol; Sintese e caracterizacao de Al{sub 2}O{sub 3} obtida por meio do metodo dos precursores polimericos utilizando glicerina como polialcool

Energy Technology Data Exchange (ETDEWEB)

Elicker, C.; Gaier, M.; Almeida, S.R.; Vieiraaa, B.M.; Ratmann, C.W.R.; Pereira, C.M.P. de; Cava, S.S. [Universidade Federal de Pelotas (UFPel), Pelotas, RS (Brazil); Egea, J.J. [Consejo Superior de Investigaciones Cientificas, Madrid (Spain)

2014-07-01

In this study, calcium aluminate was synthesized using glycerin to replace ethylene glycol in the polymeric precursor method. The resulting resin was pre-calcined in a muffle at 300 °C for 2 h and the resulting material was calcined at 900 °C for 2 h. The powders were analyzed by XRD, SEM and EDX, TEM, Micro-Raman and IR. The results demonstrated the possibility of using glycerin as an alternative to ethylene glycol in the polymeric precursor method. (author)

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

Science.gov (United States)

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.

Modified solvothermal synthesis and characterization of CdS/ZnS core/shell nanorods

International Nuclear Information System (INIS)

Baby Suganthi, A.R.; Sagayaraj, P.

2013-01-01

Core/shell CdS/ZnS nanorods were synthesized using a two-step solvothermal approach. The first step is the formation of CdS nanoparticles initiated using nucleation followed by growth through coalescence-exchange and particle coagulation. The second step leads to the formation of ZnS and further coalescence-exchange leading to deposition and growth of a ZnS shell around CdS nanoparticles. The structural, morphological and chemical studies were performed using X-ray diffraction, Energy Dispersive X-ray spectroscopy (EDX) Scanning electron Microscopy (SEM), UV–vis absorption spectra and Transmission Electron Microscopy (TEM), provide direct evidence for shell growth. The present synthesis provides a rational approach to the design of novel core/shell nanomaterials with appealing applications in optoelectronic devices. - Graphical abstract: From the resulting TEM images, the formation of core/shell could be observed. The apparent microscopy contrast between the CdS core and the ZnS shell offers evidence for the formation of CdS/ZnS core/shell nanostructures. It is clearly evident that the surfaces of the nanorods became rough after coating and also the diameter of the nanorod is seen increased up to 40–50 nm. Highlights: ► CdS/ZnS core/shell nanorods were synthesized using two-step solvothermal approach. ► The nanoparticles were characterized by XRD, EDX, SEM, UV–vis and TEM. ► SEM images revealed the surface roughness after ZnS shell growth. ► TEM microscopy offers evidence for the formation of core/shell nanostructures

TEM-145 and TEM-146 β-lactamases produced by Escherichia coli ...

African Journals Online (AJOL)

GREGO

2007-03-05

Mar 5, 2007 ... Key words: Escherichia coli, plasmid-mediated, TEM β-lactamase. ... Enterobacteriaceae, the most prevalent mechanism of resistance to ... the production of a relatively inhibitor-resistant OXA-type β-lactamase .... and 8.6 as transcripts of the E. coli chromosomal AmpC .... Mode of action and mechanisms of.

A short note on how to convert a conventional analytical TEM into an analytical Low Voltage TEM

International Nuclear Information System (INIS)

Stöger-Pollach, M.

2014-01-01

The present work is a short note on the performance of a conventional transmission electron microscope (TEM) being operated at very low beam energies (below 20 keV). We discuss the high tension stability and resolving power of this uncorrected TEM. We find out that the theoretical lens performance can nearly be achieved in practice. We also demonstrate that electron energy loss spectra can be recorded at these low beam energies with standard equipment. The signal-to-noise ratio is sufficiently good for further data treatment like multiple scattering deconvolution and Kramers–Kronig analysis. - Highlights: • TEM operation at very low beam energies (below 20 keV). • Testing of hardware performance at low beam energies. • EELS spectra recorded with 10 keV electrons

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

Science.gov (United States)

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.

40 keV atomic resolution TEM

International Nuclear Information System (INIS)

Bell, David C.; Russo, Christopher J.; Kolmykov, Dmitry V.

2012-01-01

Here we present the first atomic resolution TEM imaging at 40 keV using an aberration-corrected, monochromated source TEM. Low-voltage High-Resolution Electron Microscopy (LVHREM) has several advantages, including increased cross-sections for inelastic and elastic scattering, increased contrast per electron and improved spectroscopy efficiency, decreased delocalization effects and reduced knock-on damage. Together, these often improve the contrast to damage ratio obtained on a large class of samples. Third-order aberration correction now allows us to operate the TEM at low energies while retaining atomic resolution, which was previously impossible. At low voltage the major limitation to resolution becomes the chromatic aberration limit. We show that using a source monochromator we are able to reduce the effect of chromatic aberration and achieve a usable high-resolution limit at 40 keV to less than 1 Å. We show various materials' examples of the application of the technique to image graphene and silicon, and compare atomic resolution images with electron multislice simulations. -- Highlights: ► We present the first atomic resolution images recorded at 40 keV using an aberration-corrected, monochromated TEM. ► We show information transfer measured to better than 1 Å. ► At 40 keV an aberration-corrected monochromated TEM is limited by fifth-order spherical aberration. ► We show that using a monochromator the effect of chromatic aberration is reduced to enable high resolution imaging. ► Low voltage high resolution electron microscopy will be beneficial for imaging the organic/inorganic materials interface.

Search Engine Marketing (SEM): Financial & Competitive Advantages of an Effective Hotel SEM Strategy

OpenAIRE

Leora Halpern Lanz

2015-01-01

Search Engine Marketing and Optimization (SEO, SEM) are keystones of a hotels marketing strategy, in fact research shows that 90% of travelers start their vacation planning with a Google search. Learn five strategies that can enhance a hotels SEO and SEM strategies to boost bookings.

Moessbauer effect and TEM in mineralogy

International Nuclear Information System (INIS)

Ferrow, E.A.

1994-01-01

Moessbauer effect (ME) provides useful information on oxidation state, co-ordination number, co-ordination state, site occupancies, and magnetic properties of Fe-bearing phases. The information gained by ME together with the information provided by other conventional techniques is used to extract temperature, pressure, and kinetics of rock-forming processes. Nevertheless, ME requires that the phases studied are homogeneous over an extremely large volume and that Fe is a major component of the system. Transmission electron microscopy (TEM), on the other hand, provides similar information over a very small volume for a system of any component. However, present TEM spectrometers do not provide sufficient resolution to detect the mixed oxidation state. A complete characterisation of phases in rocks requires, therefore, that conventional techniques be combined with TEM. (orig.)

Zinc vanadate nanorods and their visible light photocatalytic activity

International Nuclear Information System (INIS)

Pei, L.Z.; Lin, N.; Wei, T.; Liu, H.D.; Yu, H.Y.

2015-01-01

Highlights: • Zinc vanadate nanorods have been synthesized by a facile hydrothermal process. • The size of zinc vanadate nanorods can be controlled by growth conditions. • Zinc vanadate nanorods show good photocatalytic activities of methylene blue under solar light. - Abstract: Zinc vanadate nanorods have been synthesized by a simple hydrothermal process using zinc acetate and sodium vanadate as the raw materials. The zinc vanadate nanorods have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM) and solid UV–vis diffuse reflectance spectrum. XRD pattern and HRTEM image show that the zinc vanadate nanorods are composed of single crystalline monoclinic Zn 2 V 2 O 7 phase. SEM and TEM observations show that the diameter and length of the zinc vanadate nanorods are 50–100 nm and about 5 μm, respectively. Sodium dodecyl sulfonate (SDS) has an essential role in the formation of zinc vanadate nanorods. The SDS-assisted nucleation and growth process have been proposed to explain the formation and growth of the zinc vanadate nanorods. Solid UV–vis diffuse reflectance spectrum shows that the zinc vanadate nanorods have a band gap of 2.76 eV. The photocatalytic activities of the zinc vanadate nanorods have been evaluated by the photocatalytic degradation of methylene blue (MB) under solar light irradiation. The MB with the concentration of 10 mg L −1 can be degraded totally under the solar light irradiation for 4 h. It is suggested that the zinc vanadate nanorods exhibit promising application potential for the degradation of organic pollutants under solar light irradiation

Biosorption and biotransformation of chromium by Serratia sp. isolated from tannery effluent.

Science.gov (United States)

Srivastava, Shaili; Thakur, Indu Shekhar

2012-01-01

A bacterium isolated from soil and sediment ofa leather tanning mill's effluent was identified as Serratia sp. by the analysis of 16S rDNA. Scanning electron microscopy-energy dispersive X-ray analysis (SEM-EDX) and transmission electron microscopy (TEM) were used to assess morphological changes and confirm chromium biosorption in Serratia sp. both in a shake-flask culture containing chromium and in a tannery wastewater. The SEMEDX and the elemental analysis of the chromate-containing samples confirmed the binding of chromium with the bacterial biomass. The TEM exhibited chromium accumulation throughout the bacterial cell, with some granular deposits in the cell periphery and in the cytoplasm. X-ray diffraction analysis (XRD) was used to quantify the chromium and to determine the chemical nature of the metal-microbe interaction. The XRD data showed the crystalline character of the precipitates, which consisted of mainly calcium chromium oxide, chromium fluoride phosphate and related organo-Cr(III) complex crystals. The XRD data also revealed a strong involvement of cellular carboxyl and phosphate groups in chromium binding by the bacterial biomass. The results of the study indicated that a combined mechanism of ion-exchange, complexation, croprecipitation and immobilization was involved in the biosorption of chromium by bacterial cells in contaminated environments.

Novel sample preparation for operando TEM of catalysts

International Nuclear Information System (INIS)

Miller, Benjamin K.; Barker, Trevor M.; Crozier, Peter A.

2015-01-01

A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. - Highlights: • High in-situ conversion of CO to CO 2 achieved by a novel TEM sample preparation method. • A 3 mm fiber pellet increases the TEM sample surface area by 50×. • Operando atomic resolution is maintained by also including a 3 mm grid in the sample. • Evidence for a well-mixed gas composition inside the ETEM cell is given

Structural characterization and impedance studies of PbO nanofibers synthesized by electrospinning technique

Energy Technology Data Exchange (ETDEWEB)

Hari Prasad, Kamatam [Department of Physics, Pondicherry University, Puducherry, 605 014 (India); Vinoth, S. [Department of Physics, Pondicherry University, Puducherry, 605 014 (India); Centre for Nanoscience, Pondicherry University, Puducherry, 605014 (India); Jena, Paramananda [Department of Physics, Pondicherry University, Puducherry, 605 014 (India); School of Materials Science and Technology, Indian Institute of Technology(BHU), Varanasi, 221 005 (India); Venkateswarlu, M. [R & D, Amara Raja Batteries Ltd, Karakambadi, 517 520, A.P (India); Satyanarayana, N., E-mail: nallanis2011@gmail.com [Department of Physics, Pondicherry University, Puducherry, 605 014 (India)

2017-06-15

One-dimensional electrospun lead oxide nanofibers synthesized by a simple electrospinning technique. The prepared lead oxide nanofibers investigated by using TG/DTA, FTIR, Raman, X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) surface area analyzer, scanning electron microscopy–energy dispersive X-ray spectroscopy (SEM-EDX), atomic force microscopy (AFM), Transmission electron microscopy (TEM), and impedance spectroscopy techniques. TG/DTA results confirmed the thermal behavior of the as-spun nanofibers. XRD, FTIR, and Raman spectra results, respectively, confirm the formation of pure orthorhombic crystalline phase and structural coordination of the lead oxide (β-PbO) nanofibers. The BET specific surface area of β-PbO nanofibers sample is found to be 51.23 m{sup 2} g{sup -1}. SEM and AFM micrographs showed the formation of β-PbO nanofibers with a diameter of 85–300 nm. The impedance measurements of lead oxide nanofibers as a function of temperature, 25–150 °C, was evaluated by analyzing the measured impedance data using the winfit software. The electrical conductivity of the lead oxide (β-PbO) nanofibers evaluated by analyzing the measured impedance data using the winfit software is found to be 5.68 × 10{sup -6} S cm{sup -1} at 150 °C. Also, an activation energy (E{sub a}) for the migration of the charge carrier evaluated from the temperature dependence of conductivity plot is found to be 0.27 eV. The temperature dependence AC conductivity of β-PbO nanofibers was evaluated using the measured impedance data and sample dimension. The observed variation of high-frequency AC conductivity attributed to the hopping electrons between the adjacent sites. - Highlights: • First time, β-PbO nanofibers were successfully prepared by electrospinning technique. • Structural, morphological, roughness and electrical properties are studied. • TG/DTA, XRD, FTIR, Raman, SEM/AFM, TEM-EDX, and impedance measurements were made.

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

Science.gov (United States)

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.

Study of High Quality Indium Nitride Films Grown on Si(100 Substrate by RF-MOMBE with GZO and AlN Buffer Layers

Directory of Open Access Journals (Sweden)

Wei-Chun Chen

2012-01-01

Full Text Available Wurtzite structure InN films were prepared on Si(100 substrates using radio-frequency metal-organic molecular beam epitaxy (RF-MOMBE system. Ga-doped ZnO (GZO and Amorphous AlN (a-AlN film were used as buffer layers for InN films growth. Structural, surface morphology and optical properties of InN films were investigated by X-ray diffraction (XRD, field emission scanning electron microscopy (FE-SEM, transmission electron microscopy (TEM, and photoluminescence (PL. XRD results indicated that all InN films exhibited preferred growth orientation along the c-axis with different intermediate buffers. TEM images exhibit the InN/GZO growth by two-dimensional mode and thickness about 900 nm. Also, the InN films can be obtained by growth rate about ~1.8 μm/h. Optical properties indicated that the band gap of InN/GZO is about 0.79 eV. These results indicate that the control of buffer layer is essential for engineering the growth of InN on silicon wafer.

Synthesis and characterization of Ce, Cu co-doped ZnS nanoparticles

International Nuclear Information System (INIS)

Harish, G.S.; Sreedhara Reddy, P.

2015-01-01

Ce, Cu co-doped ZnS nanoparticles were prepared at room temperature using a chemical co-precipitation method. The prepared nanoparticles were characterized by X- ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive analysis of X-rays (EDAX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) and high resolution Raman spectroscopic techniques. Transmission electron microscopy (TEM) and X-ray diffraction studies showed that the diameter of the particles was around 2–3 nm. Broadened XRD peaks revealed the formation of nanoparticles with a face centered cubic (fcc) structure. DRS studies confirmed that the band gap increased with an increase in the dopant concentration. The Raman spectra of undoped and Ce, Cu ions co-doped ZnS nanoparticles showed longitudinal optical mode and transverse optical mode. Compared with the Raman modes (276 and 351 cm −1 ) of undoped ZnS nanoparticles, the Raman modes of Ce, Cu co- doped ZnS nanoparticles were slightly shifted towards lower frequency. PL spectra of the samples showed remarkable enhancement in the intensity upon doping

HRTEM characterization of melt-spun Al-Si-Cu-Mg alloys solidified at different rates

International Nuclear Information System (INIS)

Alfonso, Ismeli; Maldonado, Cuauhtemoc; Medina, Ariosto; Gonzalez, Gonzalo; Bejar, Luis

2006-01-01

Six quaternary alloys Al-6Si-3Cu-xMg (x = 0.59, 3.80 and 6.78 wt.%) were produced by melt spinning using two different tangential speeds of the copper wheel (30 and 45 ms -1 ), and characterized using optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and microhardness. At 30 ms -1 , XRD and TEM investigations revealed the presence of Al 2 Cu (θ) for the alloy with 0.59%Mg and Al 5 Cu 2 Mg 8 Si 6 (Q) for the alloys with 3.80 and 6.78%Mg. The increase in microhardness of the alloys with higher Mg content is attributed to the presence of nanosized a-Al particles and a higher content of Q nanoparticles. At 45 ms -1 the alloying element content in solid solution is increased due to the fact that the quantity of free second phases (θ and Q nanoparticles) has decreased. For this rotation speed, amorphous regions of α -Al were observed, increasing microhardness compared to the 30 ms -1 ribbons

Search Engine Marketing (SEM: Financial & Competitive Advantages of an Effective Hotel SEM Strategy

Directory of Open Access Journals (Sweden)

Leora Halpern Lanz

2015-05-01

Full Text Available Search Engine Marketing and Optimization (SEO, SEM are keystones of a hotels marketing strategy, in fact research shows that 90% of travelers start their vacation planning with a Google search. Learn five strategies that can enhance a hotels SEO and SEM strategies to boost bookings.

Synthesis, characterization and antibacterial study on the chitosan-functionalized Ag nanoparticles.

Science.gov (United States)

Biao, Linhai; Tan, Shengnan; Wang, Yuanlin; Guo, Ximin; Fu, Yujie; Xu, Fengjie; Zu, Yuangang; Liu, Zhiguo

2017-07-01

This study provided a facile, one-step hydrothermal method to synthesize stable Ag colloid in aqueous solution by utilizing chitosan as both reductant and stabilizer. The formation of chitosan-functionalized Ag nanoparticles was verified by UV-Vis, FTIR, TEM, AFM and XRD measurements. FTIR results revealed that the primary amine groups and amide groups of chitosan have specific interactions with the surface of Ag nanoparticles. The average diameter of the Ag nanoparticles is 10.0±5.4nm as determined by TEM. Ag nanoparticles are highly crystalline as revealed by HR-TEM and XRD measurements. The size and shape of Ag nanoparticles are also found to depend on the pH condition in the synthesis. Ag nanoparticles were the main products at pH5.0 whereas large Ag nanotriangle and truncated triangular nanoplate were dominant at pH4.0 in the synthesis. Due to its monodispersity and good stability, the chitosan-functionalized Ag colloid synthesized at pH5.0 was further tested for its antibacterial activities against gram-positive bacteria, gram-negative bacteria and fungus. The results of zone of inhibition, inhibition ratio and SEM characterization revealed that chitosan-functionalized Ag nanoparticles have great bactericidal efficiency against both bacteria and fungus. Copyright © 2017 Elsevier B.V. All rights reserved.

Effective reduction in the nanoparticle sizes of NiO obtained via the pyrolysis of nickel malonate precursor modified using oleylamine surfactant

Energy Technology Data Exchange (ETDEWEB)

Lontio Fomekong, Roussin, E-mail: lonforou@yahoo.fr [Chemistry Department, Higher Teacher Training College, University of Yaoundé I, B.P. 47, Yaoundé (Cameroon); Institut de la Matière Condensée et des Nanosciences, Université Catholique de Louvain, Croix du Sud 1, 1348 Louvain-La-Neuve (Belgium); Ngolui Lambi, John; Ebede, Guy Roland [Chemistry Department, Higher Teacher Training College, University of Yaoundé I, B.P. 47, Yaoundé (Cameroon); Kenfack Tsobnang, Patrice [Chemistry Department, University of Dschang, PO Box 96, Dschang (Cameroon); Tedjieukeng Kamta, Hypolite Mathias; Ngnintedem Yonti, Cedrik [Chemistry Department, Higher Teacher Training College, University of Yaoundé I, B.P. 47, Yaoundé (Cameroon); Delcorte, Arnaud [Institut de la Matière Condensée et des Nanosciences, Université Catholique de Louvain, Croix du Sud 1, 1348 Louvain-La-Neuve (Belgium)

2016-09-15

Nickel oxide nanoparticles were synthesized via thermal decomposition of two precursors, the first, a simple nickel malonate and the second, a nickel malonate modified by oleylamine, a surfactant, both having been synthesized by precipitation. While FTIR, TGA and ToF-SIMS were used to characterize the two precursors and to show the presence of oleylamine in the modified precursor, XRD, SEM, TEM and BET were employed to investigate the structure, the morphology and the specific surface area of the decomposition products obtained after pyrolysis. The results showed that the modification of nickel malonate by oleylamine was effective. The XRD results, which showed a cubic structure for the NiO obtained, suggest with SEM an important particle size reduction (at least 54%) when oleylamine was used to modify the nickel malonate precursor. The SEM images also showed a well-defined spherical nanoparticle morphology in both cases, not affected by the presence of oleylamine. The TEM also confirmed the reduction of particle size and their spherical nature but at the same time showed that, in the presence of oleylamine, there was no agglomeration resulting in a more uniform particle size distribution. The specific surface area of the NiO obtained by the oleylamine-modified precursor was 4.7 times larger than that obtained with the regular precursor. This again confirms the particle size reduction. - Highlights: • Nickel malonate precursor has been synthesized by precipitation method. • This precursor was successfully modified by a surfactant (oleylamine). • NiO was identified as the decomposition products of the previous precursors. • Oleylamine has provoked around 54% of particle size reduction of the NiO.

Accelerated carbonation of steelmaking slags in a high-gravity rotating packed bed

International Nuclear Information System (INIS)

Chang, E-E; Pan, Shu-Yuan; Chen, Yi-Hung; Tan, Chung-Sung; Chiang, Pen-Chi

2012-01-01

Highlights: ► The carbonation conversion in a RPB was higher than that in traditional reactors. ► The optimum conditions were operated at 750 rpm and 65 °C for 30 min. ► The product on BOF slag was identified as crystallized calcite based on SEM and XRD. ► The diffusivity ranged from 10 −7 to 10 −6 cm 2 s −1 based on the shrinking core model. - Abstract: Carbon dioxide (CO 2 ) sequestration using the accelerated carbonation of basic oxygen furnace (BOF) slag in a high-gravity rotating packed bed (RPB) under various operational conditions was investigated. The effects of reaction time, reaction temperature, rotation speed and slurry flow rate on the CO 2 sequestration process were evaluated. The samples of reacted slurry were analyzed quantitatively using thermogravimetric analysis (TGA) and atomic absorption spectrometry (AAS) and qualitatively using X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX), and transmission electron microscopy (TEM). The sequestration experiments were performed at a liquid-to-solid ratio of 20:1 with a flow rate of 2.5 L min −1 of a pure CO 2 stream under atmospheric temperature and pressure. The results show that a maximum conversion of BOF slag was 93.5% at a reaction time of 30 min and a rotation speed of 750 rpm at 65 °C. The experimental data were utilized to determine the rate-limiting mechanism based on the shrinking core model (SCM), which was validated by the observations of SEM and TEM. Accelerated carbonation in a RPB was confirmed to be a viable method due to its higher mass-transfer rate.

TEM sample preparation by FIB for carbon nanotube interconnects

International Nuclear Information System (INIS)

Ke, Xiaoxing; Bals, Sara; Romo Negreira, Ainhoa; Hantschel, Thomas; Bender, Hugo; Van Tendeloo, Gustaaf

2009-01-01

A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

TEM sample preparation by FIB for carbon nanotube interconnects

Energy Technology Data Exchange (ETDEWEB)

Ke, Xiaoxing, E-mail: xiaoxing.ke@ua.ac.be [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Bals, Sara [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Romo Negreira, Ainhoa [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Metallurgy and Materials Engineering Department, KU Leuven, Kasteelpark Arenberg 44, Leuven B-3001 (Belgium); Hantschel, Thomas; Bender, Hugo [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Van Tendeloo, Gustaaf [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium)

2009-10-15

A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

Application of some microorganisms for synthesis of gold and silver nanoparticles

International Nuclear Information System (INIS)

Frontas'eva, M.V.; Pavlov, S.S.; Zinicovscaia, I.I.; Kirkesali, E.I.; Kalabegishvili, T.; Murusidze, I.; Faanhof, A.

2012-01-01

In recent years, much attention has been paid to microbial technologies of nanoparticle production. Novel strains of actinomycetes Streptomyces glaucus 71 MD, Streptomyces spp. 211A, arthrobacter genera - Arthrobacter globiformis 151B and Arthrobacter oxydans 61B and blue-green microalga Spirulina platensis were used for synthesis of silver and gold nanoparticles. The studies were carried out using scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), transmission electron microscopy (TEM), X-ray diffraction (XRD), atomic absorption spectrometry (AAS), and neutron activation analysis (NAA)

Magnetism of FF6.2/SiO2 nanocomposites as observed by static and dynamic probes

International Nuclear Information System (INIS)

Vejpravova, J.; Kornak, R.; Niznansky, D.; Haimann, K.; Maruszewski, K.

2007-01-01

We report on magnetic behavior of the electromagnetic compatibility (EMC) compound FF6.2 and composites prepared by the modified Stoeber method using FF6.2 as the magnetic ion-containing (Fe 2+ /Fe 3+ ) precursor. The composites were characterized by the X-ray diffraction analysis (XRD) and morphology of the magnetic powders was investigated by a scanning electron microscope (SEM) and a high resolution transmision electron microscope (HR TEM). Magnetic properties of the materials were studied by measurements of the magnetization, AC susceptibility and Moessbauer spectra

Synthesis and characterization of ZnO nanoparticles: Application to one-pot synthesis of benzo[b][1,5]diazepines

Directory of Open Access Journals (Sweden)

Mohammad Ali Ghasemzadeh

2015-12-01

Full Text Available The pharmaceutical and biologically active heterocyclic compounds including benzo[b][1,5]diazepines were efficiently synthesized via three-(in situ five- component reactions of aromatic diamines, Meldrum’s acid, and isocyanide derivatives in the presence of zinc oxide nanoparticles at room temperature. ZnO nanoparticles, as an effective, mild, and reusable catalyst, significantly improved the reaction times and also the products were obtained in excellent yields. The prepared zinc oxide nanoparticles were fully characterized by EDX, XRD, BET, SEM, IR, and TEM analyses.

Investigation on VOX/CNTS Nanocomposites Act as Electrode of Supercapacitors

Science.gov (United States)

Zhu, Quanyao; Li, Zhaolong; Zhang, Xiaoyan; Huang, Shengnan; Yu, Yue; Chen, Wen; Zakharova, Galina S.

2013-07-01

The VOx/CNTs nanocomposites were synthesized by the hydrothermal method. The structure and morphologies of the nanocomposites were characteristic by XRD, SEM and TEM. The electrochemical properties of the nanocomposites were explored by cyclic voltammetry, constant current charge/discharge testing and electrochemical impedance spectroscopy in 1M KNO3 aqueous solution. The results showed that the nanocomposites perform characteristics of electrical both double-layer capacitance and pseudocapacitance. The specific capacitances were 136.5F/g, when the current density was 0.15A/g.

Photocatalytic degradation of dairy effluent using AgTiO2 nanostructures/polyurethane nanofiber membrane

DEFF Research Database (Denmark)

Kanjwal, Muzafar Ahmad; Barakat, Nasser A.M.; Chronakis, Ioannis S.

2015-01-01

Dairy effluent (DE) is environmentally toxic and needs special attention. Photocatalytic degradation of DE was studied using novel polyurethane (PU)-based membranes. Typically, silver-titanium dioxide nanofibers (AgTiO2 NFs) and silver-titanium dioxide nanoparticles (AgTiO2 NPs) were individually...... incorporated in PU electrospun nanofibers to overcome the mandatory sophisticated separation of the nanocatalysts, which can create a secondary pollution, after the treatment process. These nanomembranes were characterized in SEM, TEM, XRD and UV studies. The polymeric electrospun nanofibers were smooth...

Nanostructures obtained from a mechanically alloyed and heat treated molybdenum carbide

International Nuclear Information System (INIS)

Diaz Barriga Arceo, L.; Orozco, E.; Mendoza-Leon, H.; Palacios Gonzalez, E.; Leyte Guerrero, F.; Garibay Febles, V.

2007-01-01

Mechanical alloying was used to prepare molybdenum carbide. Microstructural characterization of samples was performed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) methods. Molybdenum carbide was heated at 800 o C for 15 min in order to produce carbon nanotubes. Nanoparticles of about 50-140 nm in diameter and nanotubes with diameters of about 70-260 nm and 0.18-0.3 μm in length were obtained after heating at 800 o C, by means of this process

Electron beam synthesis of silica/nano silver composite and its application in controlling microorganisms in drinking water

International Nuclear Information System (INIS)

Ramnani, S.P.; Biswal, Jayashree; Sabharwal, S.; Rama Rao, K.C.; Sai Prasad, P.

2008-01-01

Silica/nano silver composites were prepared by electron beam (EB) irradiation technique. The solution containing silica nanoparticles and AgNO 3 in various proportion were subjected to EB irradiation. The EB dose delivered was such that all the Ag + is converted into metallic silver. The samples were characterized by XRD, SEM and TEM analysis. The composites were tested for their anti microbial activity in water samples. The results indicated that there is an optimum size of Ag nanoparticles that shows better antimicrobial activity. (author)

Phytofabrication and characterization of monodisperse copper oxide nanoparticles using Albizia lebbeck leaf extract

Science.gov (United States)

Jayakumarai, G.; Gokulpriya, C.; Sudhapriya, R.; Sharmila, G.; Muthukumaran, C.

2015-12-01

Simple effective and rapid approach for the green synthesis of copper oxide nanoparticles (CONPs) using of Albizia lebbeck leaf extract was investigated in this study. Various instrumental techniques were adopted to characterize the synthesized CONPs, viz. UV-Vis spectroscopy, SEM, TEM, EDS and XRD. The synthesized CONPs were found to be spherical in shape and size less than 100 nm. It could be concluded that A. lebbeck leaf extract can be used as a cheap and effective reducing agent for CONPs production in large scale.

Electroreduction of CO2 into Ethanol over an Active Catalyst: Copper Supported on Titania

OpenAIRE

Jing Yuan; Li Liu; Rong-Rong Guo; Sheng Zeng; Huan Wang; Jia-Xing Lu

2017-01-01

A simple, inexpensive, and novel method was used to prepare electrocatalysts from Cu supported on titanium dioxide (Cu/TiO2). XRD, SEM, and TEM characterizations confirmed different loadings of Cu nanoparticles (NPs) on TiO2. Cyclic voltammetry tests indicated that Cu/TiO2 exhibited lower overpotential for CO2 reduction than that of Cu NPs. Moreover, 40 wt % Cu/TiO2 exhibited the highest faradaic efficiency for ethanol (FEethanol) of 27.4%, which is approximately 10-fold higher than that for ...

Facile Hydrogen Evolution Reaction on WO3Nanorods

Directory of Open Access Journals (Sweden)

Rajeswari Janarthanan

2007-01-01

Full Text Available AbstractTungsten trioxide nanorods have been generated by the thermal decomposition (450 °C of tetrabutylammonium decatungstate. The synthesized tungsten trioxide (WO3 nanorods have been characterized by XRD, Raman, SEM, TEM, HRTEM and cyclic voltammetry. High resolution transmission electron microscopy and X-ray diffraction analysis showed that the synthesized WO3nanorods are crystalline in nature with monoclinic structure. The electrochemical experiments showed that they constitute a better electrocatalytic system for hydrogen evolution reaction in acid medium compared to their bulk counterpart.

Synthesis and characterization of CuO flower-nanostructure processing by a domestic hydrothermal microwave

International Nuclear Information System (INIS)

Volanti, D.P.; Keyson, D.; Cavalcante, L.S.; Simoes, A.Z.; Joya, M.R.; Longo, E.; Varela, J.A.; Pizani, P.S.; Souza, A.G.

2008-01-01

The synthesis and characterization of CuO flower-nanostructure processed in domestic hydrothermal microwave oven was presented. Phase analysis was carried out using X-ray diffraction (XRD) and micro-Raman scattering (MRS) and the results confirmed the CuO flower-nanostructure as a single-phase. The field-emission scanning electron microscopy (FEG-SEM) was used to estimate the average spheres diameter while transmission electron microscope (TEM) to observe the thorn of the flower-nanostructures. The mechanism of CuO flower-nanostructures formation is proposed and explained

Synthesis and characterization of CuO flower-nanostructure processing by a domestic hydrothermal microwave

Energy Technology Data Exchange (ETDEWEB)

Volanti, D.P. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Keyson, D. [Laboratorio de Ensino de Ciencias e Laboratorio de Combustiveis e Materiais, Departamento de Quimica, Universidade Federal da Paraiba, 58051-900 Joao Pessoa, PB (Brazil); Cavalcante, L.S. [Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Departamento de Quimica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil)], E-mail: laeciosc@bol.com.br; Simoes, A.Z. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Joya, M.R. [Departamento de Fisica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil); Longo, E.; Varela, J.A. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Pizani, P.S. [Departamento de Fisica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil); Souza, A.G. [Laboratorio de Ensino de Ciencias e Laboratorio de Combustiveis e Materiais, Departamento de Quimica, Universidade Federal da Paraiba, 58051-900 Joao Pessoa, PB (Brazil)

2008-07-14

The synthesis and characterization of CuO flower-nanostructure processed in domestic hydrothermal microwave oven was presented. Phase analysis was carried out using X-ray diffraction (XRD) and micro-Raman scattering (MRS) and the results confirmed the CuO flower-nanostructure as a single-phase. The field-emission scanning electron microscopy (FEG-SEM) was used to estimate the average spheres diameter while transmission electron microscope (TEM) to observe the thorn of the flower-nanostructures. The mechanism of CuO flower-nanostructures formation is proposed and explained.

Nanostructures obtained from a mechanically alloyed and heat treated molybdenum carbide

Energy Technology Data Exchange (ETDEWEB)

Diaz Barriga Arceo, L. [Programa de Ingenieria Molecular, I.M.P. Lazaro Cardenas 152, C.P. 07730 D.F. Mexico (Mexico) and ESIQIE-UPALM, IPN Apdo Postal 118-395, C.P. 07051 D.F. Mexico (Mexico)]. E-mail: luchell@yahoo.com; Orozco, E. [Instituto de Fisica UNAM, Apdo Postal 20-364, C.P. 01000 D.F. Mexico (Mexico)]. E-mail: eorozco@fisica.unam.mx; Mendoza-Leon, H. [ESIQIE-UPALM, IPN Apdo Postal 118-395, C.P. 07051 D.F. Mexico (Mexico)]. E-mail: luchell@yahoo.com; Palacios Gonzalez, E. [Programa de Ingenieria Molecular, I.M.P. Lazaro Cardenas 152, C.P. 07730 D.F. Mexico (Mexico)]. E-mail: epalacio@imp.mx; Leyte Guerrero, F. [Programa de Ingenieria Molecular, I.M.P. Lazaro Cardenas 152, C.P. 07730 D.F. Mexico (Mexico)]. E-mail: fleyte@imp.mx; Garibay Febles, V. [Programa de Ingenieria Molecular, I.M.P. Lazaro Cardenas 152, C.P. 07730 D.F. Mexico (Mexico)]. E-mail: vgaribay@imp.mx

2007-05-31

Mechanical alloying was used to prepare molybdenum carbide. Microstructural characterization of samples was performed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) methods. Molybdenum carbide was heated at 800 {sup o}C for 15 min in order to produce carbon nanotubes. Nanoparticles of about 50-140 nm in diameter and nanotubes with diameters of about 70-260 nm and 0.18-0.3 {mu}m in length were obtained after heating at 800 {sup o}C, by means of this process.

Fe3O4@polyaniline yolk–shell micro/nanospheres as bifunctional materials for lithium storage and electromagnetic wave absorption

DEFF Research Database (Denmark)

Wang, Xiaoliang; Zhang, Minwei; Zhao, Jianming

2017-01-01

Unique Fe3O4/polyaniline (PANI) composite with yolk-shell micro/nanostructure (FPys) has been successfully synthesized by a facile silica-assisted in-situ polymerization and subsequent etching strategy. The structural and compositional studies of the FPys composites are performed by employing X......-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). The yolk-shell morphology of the products is confirmed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations. When evaluated as anode material for lithium-ion batteries, the as-prepared FPys electrodes...

A accountability nas organizações sem fins lucrativos: o caso particular de algumas fundações em Portugal

OpenAIRE

Costa, Ana Lúcia de Jesus

2011-01-01

Mestrado em Contabilidade A crescente importância das Organizações Sem Fins Lucrativos (OSFL) na actividade económica das sociedades modernas tem levado a um aumento da procura de informação financeira e não financeira sobre estas entidades. Cada vez mais as OSFL devem dar ênfase à accountability, atendendo às especificidades da sua actividade, de modo a que os seus documentos de prestação de contas garantam uma imagem fidedigna e apropriada do seu desempenho, devendo, portanto, afastar...

Mel de abelhas sem ferrão: proposta de regulamentação

Directory of Open Access Journals (Sweden)

Ricardo Costa Rodrigues de Camargo

Full Text Available Resumo Os méis das abelhas sem ferrão são produtos únicos da biodiversidade brasileira, presentes e valorizados pela cultura popular desde os povos originais das Américas. Por ser mais ácido e apresentar maior teor de umidade, seu sabor é peculiar e sua viscosidade é menor quando comparada ao mel proveniente da espécie exótica Apis mellifera. Devido a essas diferenças, esse produto necessita do estabelecimento de parâmetros físico-químicos específicos que sejam referência tanto para controle de qualidade como para sua comercialização. Com base em pesquisas realizadas pela Embrapa, pelo Instituto de Tecnologia de Alimentos de Campinas e pelo levantamento bibliográfico de diversos estudos científicos realizados por outros institutos de ensino e pesquisa, esta comunicação tem como objetivo esclarecer as peculiaridades deste produto e apresentar uma proposta de Regulamento Técnico de Identidade e Padrão para o Mel das Abelhas Sem Ferrão, visando sua comercialização no Estado de São Paulo, contribuindo assim para a disponibilidade de um produto seguro e de qualidade para o consumidor final.

XRD is the main key to the mechanochemical processing

International Nuclear Information System (INIS)

Mozaffari, M.; Amighian, J.

2000-01-01

Mechanochemical processing is a process that makes use of chemical reactions mechanically activated by high-energy ball milling (HEBM). This technique has been the subject of great interest in recent years due to its promise for producing improved novel materials. Ultra fine powders in the range 10-100 nm can be obtained by mixing the right ratio of the components, appropriate for a desired phase. These raw materials together with several hardened-steel vial and milled for an optimum time using Spex or Planetary mills. In this process 2 factors, milling time and the ball to powder mass ratio, should carefully be optimized. These will be checked by successive XRD patterns. To see the ability of XRD in this technique, some single phase Ni-Al and Mn ferrites were prepared. The main key to the formation of different phases at any stage of processing was XRD patterns. Also by using Scherrer formula it was possible to measure the particle size of the milled powders. (Author)

Spin-polarized SEM

International Nuclear Information System (INIS)

Konoto, Makoto

2007-01-01

Development of highly effective evaluation technology of magnetic structures on a nanometric scale is a key to understanding spintronics and related phenomena. A high-resolution spin-polarized scanning electron microscope (spin SEM) developed recently is quite suitable for probing such nanostructures because of the capability of analyzing local magnetization vectors in three dimensions. Utilizing the spin SEM, a layered antiferromagnetic structure with the 1nm-alternation of bilayer-sheet magnetization has been successfully resolved. The real-space imaging with full analysis of the temperature-dependent magnetization vectors will be demonstrated. (author)

Single crystalline Co{sub 3}O{sub 4}: Synthesis and optical properties

Energy Technology Data Exchange (ETDEWEB)

Hosny, Nasser Mohammed, E-mail: Nasserh56@yahoo.com

2014-04-01

Crystals of Co{sub 3}O{sub 4} have been prepared from thermal decomposition of molecular precursors derived from salicylic acid and cobalt (II) acetate or chloride at 500 °C. A cubic phase Co{sub 3}O{sub 4} micro- and nanocrystals have been obtained. The as-synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). The images of electron microscopes showed octahedral crystals of Co{sub 3}O{sub 4}. The volume and polarizability of the optimized structures of molecular precursors have been calculated and related to the particle size. The optical band gap of the obtained crystals has been measured. The results indicated two optical band gaps with values 2.65 and 2.95 eV for (E{sub g1}) (E{sub g2}), respectively. - Highlights: • Synthesis of Co{sub 3}O{sub 4} nanocrystals by decomposition of cobalt salicylic acid precursor. • Characterization of the isolated nanocrystals by using XRD, SEM and HRTEM. • The optical band gap has been measured.

Single crystalline Co3O4: Synthesis and optical properties

International Nuclear Information System (INIS)

Hosny, Nasser Mohammed

2014-01-01

Crystals of Co 3 O 4 have been prepared from thermal decomposition of molecular precursors derived from salicylic acid and cobalt (II) acetate or chloride at 500 °C. A cubic phase Co 3 O 4 micro- and nanocrystals have been obtained. The as-synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). The images of electron microscopes showed octahedral crystals of Co 3 O 4 . The volume and polarizability of the optimized structures of molecular precursors have been calculated and related to the particle size. The optical band gap of the obtained crystals has been measured. The results indicated two optical band gaps with values 2.65 and 2.95 eV for (E g1 ) (E g2 ), respectively. - Highlights: • Synthesis of Co 3 O 4 nanocrystals by decomposition of cobalt salicylic acid precursor. • Characterization of the isolated nanocrystals by using XRD, SEM and HRTEM. • The optical band gap has been measured

Characterization of TEM1/endosialin in human and murine brain tumors

International Nuclear Information System (INIS)

Carson-Walter, Eleanor B; Walter, Kevin A; Winans, Bethany N; Whiteman, Melissa C; Liu, Yang; Jarvela, Sally; Haapasalo, Hannu; Tyler, Betty M; Huso, David L; Johnson, Mahlon D

2009-01-01

TEM1/endosialin is an emerging microvascular marker of tumor angiogenesis. We characterized the expression pattern of TEM1/endosialin in astrocytic and metastatic brain tumors and investigated its role as a therapeutic target in human endothelial cells and mouse xenograft models. In situ hybridization (ISH), immunohistochemistry (IH) and immunofluorescence (IF) were used to localize TEM1/endosialin expression in grade II-IV astrocytomas and metastatic brain tumors on tissue microarrays. Changes in TEM1/endosialin expression in response to pro-angiogenic conditions were assessed in human endothelial cells grown in vitro. Intracranial U87MG glioblastoma (GBM) xenografts were analyzed in nude TEM1/endosialin knockout (KO) and wildtype (WT) mice. TEM1/endosialin was upregulated in primary and metastatic human brain tumors, where it localized primarily to the tumor vasculature and a subset of tumor stromal cells. Analysis of 275 arrayed grade II-IV astrocytomas demonstrated TEM1/endosialin expression in 79% of tumors. Robust TEM1/endosialin expression occurred in 31% of glioblastomas (grade IV astroctyomas). TEM1/endosialin expression was inversely correlated with patient age. TEM1/endosialin showed limited co-localization with CD31, αSMA and fibronectin in clinical specimens. In vitro, TEM1/endosialin was upregulated in human endothelial cells cultured in matrigel. Vascular Tem1/endosialin was induced in intracranial U87MG GBM xenografts grown in mice. Tem1/endosialin KO vs WT mice demonstrated equivalent survival and tumor growth when implanted with intracranial GBM xenografts, although Tem1/endosialin KO tumors were significantly more vascular than the WT counterparts. TEM1/endosialin was induced in the vasculature of high-grade brain tumors where its expression was inversely correlated with patient age. Although lack of TEM1/endosialin did not suppress growth of intracranial GBM xenografts, it did increase tumor vascularity. The cellular localization of TEM1

Analysis list: sem-4 [Chip-atlas[Archive

Lifescience Database Archive (English)

Full Text Available sem-4 Larvae + ce10 http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/target/sem-4.1....tsv http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/target/sem-4.5.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/target/sem...-4.10.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/colo/sem-4.Larvae.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/colo/Larvae.gml ...

Qualitative soil mineral analysis by EDXRF, XRD and AAS probes

International Nuclear Information System (INIS)

Singh, Virendra; Agrawal, H.M.

2012-01-01

Soil minerals study is vital in terms of investigating the major soil forming compounds and to find out the fate of minor and trace elements, essential for the soil–plant interaction purpose. X-ray diffraction (XRD) has been a popular technique to search out the phases for different types of samples. For the soil samples, however, employing XRD is not so straightforward due to many practical problems. In the current approach, principal component analysis (PCA) has been used to have an idea of the minerals present, in qualitative manner, in the soil under study. PCA was used on the elemental concentrations data of 17 elements, determined by the energy dispersive X-ray fluorescence (EDXRF) technique. XRD analysis of soil samples has been done also to identify the minerals of major elements. Some prior treatments, like removal of silica by polytetrafluoroethylene (PTFE) slurry and grinding with alcohol, were given to samples to overcome the peak overlapping problems and to attain fine particle size which is important to minimize micro-absorption corrections, to give reproducible peak intensities and to minimize preferred orientation. A 2θ step of 0.05°/min and a longer dwell time than normal were used to reduce interferences from background noise and to increase the counting statistics. Finally, the sequential extraction procedure for metal speciation study has been applied on soil samples. Atomic absorption spectroscopy (AAS) was used to find the concentrations of metal fractions bound to various forms. Applying all the three probes, the minerals in the soils can be studied and identified, successfully. - Highlights: ► Qualitative soil minerals analysis by EDXRF, AAS and XRD methods. ► There is a requirement of other means and methods due to inadequacy of XRD. ► Principal component analysis (PCA) provides an idea of minerals present in soil. ► Trace elements complexes can be determined by AAS probe. ► EDXRF, AAS and XRD, in combination, enable

A Defensoria Pública Como Instrumento Garantidor do Acesso à Justiça, Inclusive às Pessoas sem Moradia

OpenAIRE

Lima, Marcos Feitosa; Sant Anna, Marília Mendonça Morais

2015-01-01

O estudo presente tem por escopo demonstrar que a Defensoria Pública é instituição devidamente capitaneada na Constituição Federal incumbida de conferir acesso à justiça aos necessitados, que assim se declararem, e que não tenham condições de constituir advogado privado sem o comprometimento de sua própria subsistência, alcançando, por óbvio, as pessoas que vivem em situação de rua, que na maioria das vezes são ignoradas pela sociedade como um todo, passando-se por despercebidas ou chegando a...

Análisis de ítems y evidencias de fiabilidad de la Escala sobre Representación Cognitiva de la Enfermedad (ERCE

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Macarena De los Santos-Roig

2014-05-01

Full Text Available La Escala sobre Representación Cognitiva de la Enfermedad, ERCE (De los Santos-Roig, 2009 ha sido elaborada para evaluar las creencias de los pacientes sobre su enfermedad. El modelo de Sentido Común, donde se inserta el constructo, ha sido puesto a prueba en numerosas ocasiones, encontrándose evidencia sobre la importancia de la Representación Cognitiva en los procesos de adaptación a la enfermedad (Hagger y Orbell, 2003; Leventhal et al., 1997. Su medida en nuestro ámbito cultural es necesaria, tanto desde un punto de vista teórico, como desde una perspectiva aplicada. Lo que aquí se muestra es la continuación a un trabajo previo (De los Santos-Roig, 2009; De los Santos-Roig y Pérez-Meléndez, 2013 donde se concretó la definición semántica del constructo RCE y las Tablas de Especificaciones del Test y de los Ítems, que finalmente culminó con la presentación de los primeros ítems construidos. Siguiendo con lo establecido en los estándares (AERA, APA y NCME, 1999, se muestran ahora los resultados del análisis estadístico de los ítems correspondientes a las cinco escalas que componen la ERCE, así como los obtenidos sobre sus evidencias de fiabilidad. Al final, se concluye sobre la idoneidad de los ítems que conforman la escala.

Nickel Oxide (NiO nanoparticles prepared by solid-state thermal decomposition of Nickel (II schiff base precursor

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Aliakbar Dehno Khalaji

2015-06-01

Full Text Available In this paper, plate-like NiO nanoparticles were prepared by one-pot solid-state thermal decomposition of nickel (II Schiff base complex as new precursor. First, the nickel (II Schiff base precursor was prepared by solid-state grinding using nickel (II nitrate hexahydrate, Ni(NO32∙6H2O, and the Schiff base ligand N,N′-bis-(salicylidene benzene-1,4-diamine for 30 min without using any solvent, catalyst, template or surfactant. It was characterized by Fourier Transform Infrared spectroscopy (FT-IR and elemental analysis (CHN. The resultant solid was subsequently annealed in the electrical furnace at 450 °C for 3 h in air atmosphere. Nanoparticles of NiO were produced and characterized by X-ray powder diffraction (XRD at 2θ degree 0-140°, FT-IR spectroscopy, scanning electron microscopy (SEM and transmission electron microscopy (TEM. The XRD and FT-IR results showed that the product is pure and has good crystallinity with cubic structure because no characteristic peaks of impurity were observed, while the SEM and TEM results showed that the obtained product is tiny, aggregated with plate-like shape, narrow size distribution with an average size between 10-40 nm. Results show that the solid state thermal decomposition method is simple, environmentally friendly, safe and suitable for preparation of NiO nanoparticles. This method can also be used to synthesize nanoparticles of other metal oxides.

Synthesis and electrochemical characterization of nano-CeO2-coated nanostructure LiMn2O4 cathode materials for rechargeable lithium batteries

International Nuclear Information System (INIS)

Arumugam, D.; Kalaignan, G. Paruthimal

2010-01-01

LiMn 2 O 4 spinel cathode materials were coated with 0.5, 1.0, and 1.5 wt.% CeO 2 by a polymeric process, followed by calcination at 850 o C for 6 h in air. The surface-coated LiMn 2 O 4 cathode materials were physically characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron microscopy (XPS). XRD patterns of CeO 2 -coated LiMn 2 O 4 revealed that the coating did not affect the crystal structure or the Fd3m space group of the cathode materials compared to uncoated LiMn 2 O 4 . The surface morphology and particle agglomeration were investigated using SEM, TEM image showed a compact coating layer on the surface of the core materials that had average thickness of about 20 nm. The XPS data illustrated that the CeO 2 completely coated the surface of the LiMn 2 O 4 core cathode materials. The galvanostatic charge and discharge of the uncoated and CeO 2 -coated LiMn 2 O 4 cathode materials were measured in the potential range of 3.0-4.5 V (0.5 C rate) at 30 o C and 60 o C. Among them, the 1.0 wt.% of CeO 2 -coated spinel LiMn 2 O 4 cathode satisfies the structural stability, high reversible capacity and excellent electrochemical performances of rechargeable lithium batteries.

Electron microscopy study of microbial mat in the North Fiji basin hydrothermal vent

Science.gov (United States)

Park, H.; Kim, J. W.; Lee, J. W.

2017-12-01

Hydrothermal vent systems consisting of hydrothermal vent, hydrothermal sediment and microbial mat are widely spread around the ocean, particularly spreading axis, continental margin and back-arc basin. Scientists have perceived that the hydrothermal systems, which reflect the primeval earth environment, are one of the best places to reveal the origin of life and extensive biogeochemical process of microbe-mineral interaction. In the present study multiline of analytical methods (X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM)) were utilized to investigate the mineralogy/chemistry of microbe-mineral interaction in hydrothermal microbial mat. Microbial mat samples were recovered by Canadian scientific submersible ROPOS on South Pacific North Fiji basin KIOST hydrothermal vent expedition 1602. XRD analysis showed that red-colored microbial mat contains Fe-oxides and Fe-oxyhydroxides. Various morphologies of minerals in the red-colored microbial mat observed by SEM are mainly showed sheath shaped, resembled with Leptothrix microbial structure, stalks shaped, similar with Marioprofundus microbial structure and globule shaped microbial structures. They are also detected with DNA analysis. The cross sectional observation of microbial structures encrusted with Fe-oxide and Fe-oxyhydroxide at a nano scale by Transmission Electron Microscopy (TEM) and Focused Ion Beam (FIB) technique was developed to verify the structural/biogeochemical properties in the microbe-mineral interaction. Systematic nano-scale measurements on the biomineralization in the microbial mat leads the understandings of biogeochemical environments around the hydrothermal vent.

Luminescence properties of calcium doped zinc oxide nanoparticles

Energy Technology Data Exchange (ETDEWEB)

El Mir, L., E-mail: Lassaad.ElMir@fsg.rnu.tn [Al Imam Mohammad Ibn Saud Islamic University (IMSIU), College of Sciences, Department of Physics, Riyadh 11623 (Saudi Arabia); Laboratory of Physics of Materials and Nanomaterials Applied at Environment (LaPhyMNE), Gabes University, Faculty of Sciences in Gabes, Gabes (Tunisia)

2017-06-15

Aerogel nanopowder of calcium-doped zinc oxide (ZnO:Ca) was synthesized by modified sol-gel method. In this process, hydrolyses was slowly released and followed by a thermal drying in supercritical conditions or ethyl alcohol. The obtained nanopowder was characterized by various techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Cathodoluminescence (CL) and photoluminescence (PL). XRD data showed that Ca-doped ZnO sample has a hexagonal wurtzite structure with a slight distortion of ZnO lattice and no extra secondary phases, suggesting the substitution of Ca ions in the ZnO structure. SEM micrograph shows spherical microparticles having a rough porous fine-grained. From TEM micrograph, the samples are composed by single particles having an inhomogeneous size distribution, with most of them having a dimension in the range between 20 and 50 nm. This powder presents a strong photoluminescence band in the visible range. From photoluminescence excitation (PLE) the energy position of the obtained PL band depends on the wavelength of excitation. The luminescence results are also confirmed by cathodoluminescence technique and suggests the presence of photo-active centers in ZnO:Ca as deduced from new published works for visible photo-activated gas sensors and photo-catalysis of dyes degradation. We hope that this work provides some answers to the scientific community concerning the effect of doping in the creation of optical active centers in ZnO, promising for many technological applications.

Fabrication of MCM-41 fibers with well-ordered hexagonal mesostructure controlled in acidic and alkaline media

International Nuclear Information System (INIS)

Jafarzadeh, A.; Sohrabnezhad, Sh.; Zanjanchi, M.A.; Arvand, M.

2016-01-01

In this paper, synthesis and characterization of two type morphologies of the MCM-41mesoporous material, nano and microfibers, were investigated by electrospinning technique. The synthesis was performed in acidic and alkaline media, separately. The MCM-41 morphologies were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray powder diffraction (XRD), and nitrogen adsorption–desorption measurement. Tetraethylorthosilicate (TEOS) and cetyltrimethylammonium bromide (CTAB) were used as silica and template sources for the synthesis of MCM-41 morphologies, respectively. The SEM results showed that MCM-41 nanofibers were spun in acidic media and microfibers of MCM-41 were produced in alkaline media. The XRD study revealed a long range structural ordering of mesoporous materials. The TEM results indicated rough surfaces with uniform average diameter 200 nm for nanofibers and 2 µm for microfibers. The pore diameter and surface area of calcined MCM-41 nanofibers were 2.2 nm and 970 m 2 /g, respectively. For the MCM-41 microfibers, pore sizes of 2.7 nm and surface areas 420 m 2 /g was measured. - Graphical abstract: Electrospinning method was used for fabricating of MCM-41 microfibers from TEOS in alkaline media (top) and MCM-41 nanofibers in acidic media (bottom). - Highlights: • Synthesis of MCM-41 nanofibers and microfibers by electrospinning technique. • MCM-41 nanofibers were synthesized in acidic media. • MCM-41 manofibers spun in alkaline media. • Electrospinning was a simple method for preparing of fibers with respect to chemical method.

Microbial Precipitation of Cr(III)-Hydroxide and Se(0) Nanoparticles During Anoxic Bioreduction of Cr(VI)- and Se(VI)-Contaminated Water.

Science.gov (United States)

Kim, Yumi; Oh, Jong-Min; Roh, Yul

2017-04-01

This study examined the microbial precipitations of Cr(III)-hydroxide and Se(0) nanoparticles during anoxic bioreductions of Cr(VI) and Se(VI) using metal-reducing bacteria enriched from groundwater. Metal-reducing bacteria enriched from groundwater at the Korea Atomic Energy Research Institute (KAERI) Underground Research Tunnel (KURT), Daejeon, S. Korea were used. Metal reduction and precipitation experiments with the metal-reducing bacteria were conducted using Cr(VI)- and Se(VI)-contaminated water and glucose as a carbon source under an anaerobic environment at room temperature. XRD, SEM-EDX, and TEM-EDX analyses were used to characterize the mineralogy, crystal structure, chemistry, shape, and size distribution of the precipitates. The metal-reducing bacteria reduced Cr(VI) of potassium chromate (K₂CrO₄) to Cr(III) of chromium hydroxide [Cr(OH)3], and Se(VI) of sodium selenate (Na₂SeO₄) to selenium Se(0), with changes of color and turbidity. XRD, SEM-EDX, and TEM-EDX analyses revealed that the chromium hydroxide [Cr(OH)₃] was formed extracellularly with nanoparticles of 20–30 nm in size, and elemental selenium Se(0) nanoparticles had a sphere shape of 50–250 nm in size. These results show that metal-reducing bacteria in groundwater can aid or accelerate precipitation of heavy metals such as Cr(VI) and Se(VI) via bioreduction processes under anoxic environments. These results may also be useful for the recovery of Cr and Se nanoparticles in natural environments.

Extraction of Alumina from Red Mud for Synthesis of Mesoporous Alumina by Adding CTABr as Mesoporous Directing Agent

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Eka Putra Ramdhani

2018-05-01

Full Text Available Mines in Bintan were producing bauxite for many years. The production process of bauxite to alumina produced much red mud. From X-ray Fluorescence (XRF, alumina content on Bintan’s red mud was 28.87 wt.%. This research was studying on the extraction alumina from red mud with reduction of hematite (Fe2O3 and desilication processes. After extraction process alumina was collected about 52.89 wt.%. Synthesis of mesoporous alumina from red mud using sol-gel method at the room temperature for 72 h with cetyltrimethylammonium bromide (CTABr as mesoporous directing agent. The CTABr/Al-salt ratio, i.e. 1.57; 4.71 and 7.85 with the sample code of AMC-1, AMC-3, AMC-5, respectively. The product was calcined at 550 °C for 6 h. The synthesized materials were characterized by X-ray Diffraction (XRD, scanning electron microscopy-energy dispersive X-ray (SEM-EDX, transmission electron microscopy (TEM, and N2 adsorption-desorption techniques. XRD pattern of AMC-1, AMC-3, and AMC-5 showed that all synthesized materials have amorphous phase. The morphology were wormhole aggregate that were showed by SEM and TEM characterization. N2 adsorption-desorption characterization showed the distribution of pore size of about 3.2 nm. The highest surface area and pore volume were obtained in solid-solid ratio CTABr/GM-AL by 1.57 (AMC-1 i.e. 241 m2/g and 0.107 cm3/g, respectively.

Decorating Mg/Fe oxide nanotubes with nitrogen-doped carbon nanotubes

Energy Technology Data Exchange (ETDEWEB)

Cao Yong, E-mail: caoyangel@126.com [Institute of Environment and Municipal Engineering, North China Institute of Water Conservancy and Hydroelectric Power, Zhengzhou 450011 (China); Jiao Qingze, E-mail: jiaoqz@bit.edu.cn [School of Chemical Engineering and the Environment, Beijing Institute of Technology, Beijing 100081 (China); Zhao Yun [School of Chemical Engineering and the Environment, Beijing Institute of Technology, Beijing 100081 (China); Dong Yingchao [Materials and Surface Science Institute (MSSI), University of Limerick, Limerick (Ireland)

2011-09-22

Graphical abstract: Highlights: > Mg/Fe oxide nanotubes arrayed parallel to each other were prepared by an AAO template method. > The Mg/Fe oxide nanotubes decorated with CN{sub x} were realized by CVD of ethylenediamine on the outer surface of oxide nanotubes. > The magnetic properties of Mg/Fe oxide nanotubes were highly improved after being decorated. - Abstract: Mg/Fe oxide nanotubes decorated with nitrogen-doped carbon nanotubes (CN{sub x}) were fabricated by catalytic chemical vapor deposition of ethylenediamine on the outer surface of oxide nanotubes. Mg/Fe oxide nanotubes were prepared using a 3:1 molar precursor solution of Mg(NO{sub 3}){sub 2} and Fe(NO{sub 3}){sub 3} and anodic aluminum oxide as the substrate. The obtained samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and vibrating sample magnetometer (VSM). The XRD pattern shows that the oxide nanotubes are made up of MgO and Fe{sub 2}O{sub 3}. TEM and SEM observations indicate the oxide nanotubes are arrayed roughly parallel to each other, and the outer surface of oxide nanotubes are decorated with CN{sub x}. XPS results show the nitrogen-doped level in CN{sub x} is about 7.3 at.%. Magnetic measurements with VSM demonstrate the saturated magnetization, remanence and coercivity of oxide nanotubes are obvious improved after being decorated with CN{sub x}.

Synthesis of SiC nanoparticles by SHG 532 nm Nd:YAG laser ablation of silicon in ethanol

Science.gov (United States)

Khashan, Khawla S.; Ismail, Raid A.; Mahdi, Rana O.

2018-06-01

In this work, colloidal spherical nanoparticles NPs of silicon carbide SiC have been synthesized using second harmonic generation 532 nm Nd:YAG laser ablation of silicon target dipped in ethanol solution at various laser fluences (1.5-5) J/cm2. X-Ray diffraction XRD, scanning electron microscopy SEM, transmission electron microscope TEM, Fourier transformed infrared spectroscopy FT-IR, Raman spectroscopy, photoluminescence PL spectroscopy, and UV-Vis absorption were employed to examine the structural, chemical and optical properties of SiC NPs. XRD results showed that all synthesised SiC nanoparticles are crystalline in nature and have hexagonal structure with preferred orientation along (103) plane. Raman investigation showed three characteristic peaks 764,786 and 954 cm-1, which are indexing to transverse optic TO phonon mode and longitudinal optic LO phonon mode of 4H-SiC structure. The optical absorption data showed that the values of optical energy gap of SiC nanoparticles prepared at 1.5 J/cm2 was 3.6 eV and was 3.85 eV for SiC synthesised at 5 J/cm2. SEM investigations confirmed that the nanoparticles synthesised at 5 J/cm2 are agglomerated to form larger particles. TEM measurements showed that SiC particles prepared at 1.5 J/cm2 have spherical shape with average size of 25 nm, while the particles prepared at 5 J/cm2 have an average size of 55 nm.

Micelle-template synthesis of hollow silica spheres for improving water vapor permeability of waterborne polyurethane membrane

Science.gov (United States)

Bao, Yan; Wang, Tong; Kang, Qiaoling; Shi, Chunhua; Ma, Jianzhong

2017-04-01

Hollow silica spheres (HSS) with special interior spaces, high specific surface area and excellent adsorption and permeability performance were synthesized via micelle-template method using cetyl trimethyl ammonium bromide (CTAB) micelles as soft template and tetraethoxysilane (TEOS) as silica precursor. SEM, TEM, FT-IR, XRD, DLS and BET-BJH were carried out to characterize the morphology and structure of as-obtained samples. The results demonstrated that the samples were amorphous with a hollow structure and huge specific surface area. The growth of HSS was an inward-growth mechanism along template. Notably, we have provided a new and interesting fundamental principle for HSS materials by precisely controlling the ethanol-to-water volume ratio. In addition, the as-obtained HSS were mixed with waterborne polyurethane (WPU) to prepare WPU/HSS composite membrane. Various characterizations (SEM, TEM, FT-IR and TGA) revealed the morphology, polydispersity and adherence between HSS and WPU. Performance tests showed that the introduction of HSS can improve the water vapor permeability of composite membrane, promoting its water resistance and mechanical performance at the same time.

Low-Temperature Synthesis and Gas Sensitivity of Perovskite-Type LaCoO3 Nanoparticles

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Lorenzo Gildo Ortiz

2014-01-01

Full Text Available LaCoO3 nanoparticles with perovskite-type structure were prepared by a microwave-assisted colloidal method. Lanthanum nitrate, cobalt nitrate, and ethylenediamine were used as precursors and ethyl alcohol as solvent. The thermal decomposition of the precursors leads to the formation of LaCoO3 from a temperature of 500°C. The structural, morphological, and compositional properties of LaCoO3 nanoparticles were studied in this work by X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, and atomic force microscopy (AFM. Pellets were manufactured in order to test the gas sensing properties of LaCoO3 powders in carbon monoxide (CO and propane (C3H8 atmospheres. Agglomerates of nanoparticles with high connectivity, forming a porous structure, were observed from SEM and TEM analysis. LaCoO3 pellets presented a high sensitivity in both CO and C3H8 at different concentrations and operating temperatures. As was expected, sensitivity increased with the gas concentration and operation temperature increase.

Urea and sucrose assisted combustion synthesis of LiFePO4/C nano-powder for lithium-ion battery cathode application

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Erabhoina Hari Mohan

2014-11-01

Full Text Available In this paper, we are reporting a combustion method to prepare carbon coated LiFePO4 nanoparticles using urea as fuel and sucrose as carbon source. The process involves exothermic decomposition of a viscous liquid, containing fuel to oxidizer molar ratio of 1:1 at 300 ℃, followed by heat treatment at 600 ℃ for 6 h, under Ar (95% and H2 (5% mixed gas atmosphere. The resultant products are characterized by Thermogravimetric analysis (TG-DSC, Field emission-scanning Electron microscopy (SEM, Transmission electron microscopy (TEM, X-Ray diffraction (XRD, Raman Spectroscopy, Fourier transformation infrared spectroscopy (FTIR, and Moss-Bauer spectroscopy. The investigation reveals that the prepared sample has ordered olivine structure|with average crystallite size in the range of 30-40 nm. The SEM and TEM images show porous network type morphology with the size of the individual particles in range of 30-40 nm with spherical and oval shape morphology. The cathode obtained by combustion method exhibits a high discharge capacity (~156 mAhg-1 with a good cyclic performance and rate capability.

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

Science.gov (United States)

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.

Synchrotron-based XRD from rat bone of different age groups

Energy Technology Data Exchange (ETDEWEB)

Rao, D.V., E-mail: dvrao_9@yahoo.com [Science Based Applications to Engineering (SBAI), Physics Division, University of Rome “La Sapienza”, Via Scarpa 10, 00161 Roma (Italy); Gigante, G.E. [Science Based Applications to Engineering (SBAI), Physics Division, University of Rome “La Sapienza”, Via Scarpa 10, 00161 Roma (Italy); Cesareo, R.; Brunetti, A. [Istituto di Matematica e Fisica, Università di Sassari, Via Vienna 2, 07100 Sassari (Italy); Schiavon, N. [Hercules Laboratory, University of Evora (Portugal); Akatsuka, T.; Yuasa, T. [Department of Bio-System Engineering, Faculty of Engineering, Yamagata University, Yonezawa-shi, Yamagata 992-8510 (Japan); Takeda, T. [Allied Health Science, Kitasato University, 1-15-1 Kitasato, Sagamihara, Kanagawa 228-8555 (Japan)

2017-05-01

Synchrotron-based XRD spectra from rat bone of different age groups (w, 56 w and 78w), lumber vertebra at early stages of bone formation, Calcium hydroxyapatite (HAp) [Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}] bone fill with varying composition (60% and 70%) and bone cream (35–48%), has been acquired with 15 keV synchrotron X-rays. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15 keV X-rays (λ = 0.82666 A{sup 0}). Diffraction data were quantitatively analyzed using the Rietveld refinement approach, which allowed us to characterize the structure of these samples in their early stages. Hydroxyapatite, received considerable attention in medical and materials sciences, since these materials are the hard tissues, such as bone and teeth. Higher bioactivity of these samples gained reasonable interest for biological application and for bone tissue repair in oral surgery and orthopedics. The results obtained from these samples, such as phase data, crystalline size of the phases, as well as the degree of crystallinity, confirm the apatite family crystallizing in a hexagonal system, space group P6{sub 3}/m with the lattice parameters of a = 9.4328 Å and c = 6.8842 Å (JCPDS card #09-0432). Synchrotron-based XRD patterns are relatively sharp and well resolved and can be attributed to the hexagonal crystal form of hydroxyapatite. All the samples were examined with scanning electron microscope at an accelerating voltage of 15 kV. The presence of large globules of different sizes is observed, in small age groups of the rat bone (8w) and lumber vertebra (LV), as distinguished from, large age groups (56 and 78w) in all samples with different magnification, reflects an amorphous phase without significant traces of crystalline phases. Scanning electron microscopy (SEM) was used to characterize the morphology and crystalline properties of Hap, for all the samples, from 2 to 100 μm resolution. - Highlights: • For

FIB/SEM and SEM/EDS microstructural analysis of metal-ceramic and zirconia-ceramic interfaces.

Science.gov (United States)

Massimi, F; Merlati, G; Sebastiani, M; Battaini, P; Menghini, P; Bemporad, E

2012-01-10

Recently introduced FIB/SEM analysis in microscopy seems to provide a high-resolution characterization of the samples by 3D (FIB) cross-sectioning and (SEM) high resolution imaging. The aim of this study was to apply the FIB/SEM and SEM/EDS analysis to the interfaces of a metal-ceramic vs. two zirconia-ceramic systems. Plate samples of three different prosthetic systems were prepared in the dental lab following the manufacturers' instructions, where metal-ceramic was the result of a ceramic veneering (porcelain-fused-to-metal) and the two zirconia-ceramic systems were produced by the dedicated CAD-CAM procedures of the zirconia cores (both with final sintering) and then veneered by layered or heat pressed ceramics. In a FIB/SEM equipment (also called DualBeam), a thin layer of platinum (1 μm) was deposited on samples surface crossing the interfaces, in order to protect them during milling. Then, increasingly deeper trenches were milled by a focused ion beam, first using a relatively higher and later using a lower ion current (from 9 nA to 0.28 nA, 30KV). Finally, FEG-SEM (5KV) micrographs (1000-50,000X) were acquired. In a SEM the analysis of the morphology and internal microstructure was performed by 13KV secondary and backscattered electrons signals (in all the samples). The compositional maps were then performed by EDS probe only in the metal-ceramic system (20kV). Despite the presence of many voids in all the ceramic layers, it was possible to identify: (1) the grain structures of the metallic and zirconia substrates, (2) the thin oxide layer at the metal-ceramic interface and its interactions with the first ceramic layer (wash technique), (3) the roughness of the two different zirconia cores and their interactions with the ceramic interface, where the presence of zirconia grains in the ceramic layer was reported in two system possibly due to sandblasting before ceramic firing.

XRD and HREM studies of nanocrystalline Cu and Pd

International Nuclear Information System (INIS)

Nieman, G.W.; Weertmen, J.R.; Siegel, R.W.

1991-01-01

Consolidated powders of nanocrystalline Cu and Pd have been studied by x-ray diffraction (XRD) and high resolution electron microscopy (HREM) as part of an investigation of the mechanical behavior of nanocrystalline pure metals. XRD line broadening measurements were made to estimate rain size, qualitative grain size distribution and average long range strains in a number of samples. Mean grain sized range from 4-60 nm and have qualitatively narrow grain size distributions. Long range lattice strains are of the order of 0.2-3% in consolidated samples. These strains apparently persist and even increase in Cu samples after annealing at 0.35 Tm (498K) for 2h, accompanied by an apparent increase in grain size of ≥2x. Grain size, grain size distribution width and internal strains vary somewhat among samples produced under apparently identical processing conditions. HREM studies show that twins, stacking faults and low-index facets are abundant in as-consolidated nanocrystalline Cu samples. In this paper methodology, results and analysis of XRD and HREM experiments are presented

Novel sample preparation for operando TEM of catalysts.

Science.gov (United States)

Miller, Benjamin K; Barker, Trevor M; Crozier, Peter A

2015-09-01

A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. Copyright © 2015 Elsevier B.V. All rights reserved.

The thermal behaviour of cuprite: An XRD-EXAFS combined approach

International Nuclear Information System (INIS)

Dapiaggi, M.; Tiano, W.; Artioli, G.; Sanson, A.; Fornasini, P.

2003-01-01

Cuprite (Cu 2 O) is a low thermal expansion material with a negative thermal expansion coefficient below room temperature. Its peculiar thermal behaviour encompasses the increase of the shear modulus with increasing temperature, and the presence of rather intense symmetry-forbidden eeo reflections below room temperature. The thermal expansion of cuprite was studied at low temperature (between 5 and 298 K) by means of high-resolution (10 -5 A) X-ray powder diffraction at European Synchrotron Radiation Facility (Grenoble, BM16) and extended X-ray absorption fine structure (EXAFS) (BM29). Negative thermal expansion is confirmed up to 200 K, by EXAFS as well as by XRD measurements, and no sign of transition was found in XRD data. The comparison between EXAFS and XRD results provides a valuable insight into vibrational behaviour of cuprite at low temperature

A-10/TF34 Turbine Engine Monitoring System (TEMS)

Science.gov (United States)

Christopher, R. G.

1981-01-01

The hardware and software development of the A-10/TF34 turbine engine monitoring system (TEMS) is described. The operation and interfaces of the A-10/TF34 TEMS hardware are discussed with particular emphasis on function, capabilities, and limitations. The TEMS data types are defined and the various data acquisition modes are explained. Potential data products are also discussed.

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

Science.gov (United States)

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

2011-03-01

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

Facile electrochemical synthesis of tellurium nanorods and their photoconductive properties

Energy Technology Data Exchange (ETDEWEB)

Li, H.H. [Center for Photon Manufacturing Science and Technology, School of Materials Science and Engineering, Jiangsu University, Zhenjiang - 212013 (China); Zhang, P. [Dongguan University of Technology, Dongguan-523808 (China); School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou - 510275 (China); Liang, C.L. [Instrumental Analysis and Research Center, SunYat-sen University, Guangzhou - 510275 (China); Yang, J. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang - 212013 (China); Zhou, M. [Center for Photon Manufacturing Science and Technology, School of Materials Science and Engineering, Jiangsu University, Zhenjiang - 212013 (China); The State Key Laboratory of Tribology, Tsinghua University, Beijing - 10084 (China); Lu, X.H. [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou - 510275 (China); Hope, G.A. [School of Biomolecular and Physical Sciences, Griffith University, Nathan - Qld 4111 (Australia)

2012-10-15

Tellurium nanorods have been successfully fabricated by template and surfactant-free electrochemical technique from an aqueous solution at room temperature. The as-prepared tellurium nanorods were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectrometry, UV-vis spectroscopy and photoluminescence spectroscopy. Films based on tellurium nanorods were constructed to study the photoresponse and I-V curves. These photoresponse measurements demonstrate that tellurium nanorods exhibited enhanced conductivity under illumination compared to in the dark measurement. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

CuI nanoparticles as a remarkable catalyst in the synthesis of benzo[b][1,5]diazepines: an eco-friendly approach.

Science.gov (United States)

Ghasemzadeh, Mohammad Ali; Safaei-Ghomi, Javad

2015-01-01

Highly efficient CuI nanoparticles catalyzed one-pot synthesis of some benzo[b][1,5]diazepine derivatives via multi-component condensation of aromatic diamines, Meldrum's acid and isocyanides. The present approach creates a variety of benzo[b][1,5]diazepines as pharmaceutical and biologically active heterocyclic compounds in excellent yields and short reaction times. The salient features of the copper iodide nanoparticles are: easy preparation, cost-effective, high stability, low loading and reusability of the catalyst. The prepared copper iodide nanoparticles were fully characterized by XRD, EDX, FT-IR, SEM and TEM analysis.

Effect of deep cryogenic treatment on the formation of nano-sized carbides and the wear behavior of D2 tool steel

Science.gov (United States)

Amini, Kamran; Akhbarizadeh, Amin; Javadpour, Sirus

2012-09-01

The effect of deep cryogenic treatment on the microstructure, hardness, and wear behavior of D2 tool steel was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), hardness test, pin-on-disk wear test, and the reciprocating pin-on-flat wear test. The results show that deep cryogenic treatment eliminates retained austenite, makes a better carbide distribution, and increases the carbide content. Furthermore, some new nano-sized carbides form during the deep cryogenic treatment, thereby increasing the hardness and improving the wear behavior of the samples.

TiO2 supported over porous silica photocatalysts for pesticide degradation using solar light: Part 2. Silica prepared using acrylic acid emulsion

International Nuclear Information System (INIS)

Phanikrishna Sharma, Mangalampalli V.; Durga Kumari, Valluri; Subrahmanyam, Machiraju

2010-01-01

An acrylic acid emulsion mixture is used for synthesis of novel porous silica (E-Si) material. The photocatalytic activity of TiO 2 under solar light irradiation for isoproturon (herbicide) degradation is drastically increased when dispersed over E-Si support using solid state dispersion (SSD) technique. The composite material is characterized by XRD, nitrogen adsorption-desorption isotherms, UV-vis DRS, SEM and TEM measurements. The photocatalytic activities of the composite catalysts are evaluated for different parameters. The 5 wt% TiO 2 /E-Si is found to be highly active for isoproturon degradation.

Rapid Synthesis of Lead Oxide Nanorods by One-step Solid-state Chemical Reaction at Room Temperature

Institute of Scientific and Technical Information of China (English)

CAO, Ya-Li(曹亚丽); JIA, Dian-Zeng(贾殿赠); LIU, Lang(刘浪); LUO, Jian-Min(骆建敏)

2004-01-01

A simple and facile method was reported to synthesize lead oxide nanorods. Nanorods of lead oxide were obtained directly from grinding solid metal salt and sodium hydroxide in agate mortar with the assistance of a suitable nonionic surfactant in only one step, which is different from the result of hydroxide in solution. The product has been characterized by XRD, TEM and SEM. The formation mechanism of rod-like morphology is discussed and the surfactant plays an important soft-template role in modifying the interface of solid-state reaction and according process of rod-formation.

Microwave-assisted aqueous synthesis of ultralong ZnO nanowires: photoluminescence and photovoltaic performance for dye-sensitized solar cell

Energy Technology Data Exchange (ETDEWEB)

Min, C.; Shen, X.; Sheng, W. [Jiangsu University, School of Materials Science and Engineering, Zhenjiang (China)

2009-09-15

Ultralong ZnO nanowires were successfully prepared on a large scale by a microwave-assisted aqueous route without using any surfactant or template at relatively low temperature of 120 C. The obtained nanowires were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), and energy-dispersive X-ray spectrum (EDX). The growth mechanism and photoluminescence of the one-dimensional nanostructure, and photovoltaic performances for dye-sensitized solar cell (DSSC) of the nanowires were discussed in detail. (orig.)

Solution-combustion synthesis of Tb3+-doped Y3Al5O12 nanoparticles

International Nuclear Information System (INIS)

Fadlalla, H.M.H.; Tang, C.C.; Elsanousi, A.; Ding, X.X.; Qi, S.R.

2009-01-01

Nano-sized YAG:Tb powder phosphors were prepared by a solution-combustion method, using the general inorganic salts as starting materials. The X-ray diffraction (XRD) measurements showed that the precursor can be well-crystallized at 900 deg. C. As-prepared particles have sizes mostly in the range between 30 and 100 nm as obtained by scanning electron microscope (SEM) and transition electron microscope (TEM). Selected area electron diffraction (SAED) patterns proved that the larger particles are monocrystalline. The effects of annealing temperature and Tb-doping concentration on the luminescence intensity were studied

Hydroxyapatite-Functionalized Graphene: A New Hybrid Nanomaterial

Directory of Open Access Journals (Sweden)

C. Rodríguez-González

2014-01-01

Full Text Available Graphene oxide sheets (GO were functionalized with hydroxyapatite nanoparticles (nHAp through a simple and effective hydrothermal treatment and a novel physicochemical process. Microstructure and crystallinity were investigated by Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy, X-ray diffraction (XRD, ultraviolet-visible (UV-Vis absorption spectroscopy, and thermogravimetric analysis (TGA. Transmission electron microscopy (TEM and scanning electron microscopy (SEM were performed to characterize the morphology of the functionalized material. The resulting novel materials combine the biocompatibility of the nHAp with the strength and physical properties of the graphene.

Plasma-chemical production of metal-polypyrrole-catalysts for the reduction of oxygen in fuel cells. Precious-metal-free catalysts for fuel cells.; Plasmachemische Erzeugung von Metall-Polypyrrol-Katalysatoren fuer die Sauerstoffreduktion in Brennstoffzellen. Edelmetallfreie Katalysatoren fuer Brennstoffzellen

Energy Technology Data Exchange (ETDEWEB)

Walter, Christian

2013-07-01

This thesis is about the production of non noble metal catalysts for the oxygen reduction reaction in fuel cells. Therefore, a novel dual plasma process is developed, constructed and the so-produced films are analysed by various electrochemical (CV, RDE and RRDE) and structural methods (SEM, EDX, IR, XPS, conductivity, XRD, NEXAFS, EXAFS and TEM). It is shown, that by doing this, non noble metal catalysts could be produced without the need of a high temperature treatment. Furthermore, the catalytic activity obtained is superior to that of chemically produced metal-polypyrrole films.

Facile aqueous synthesis and growth mechanism of CdTe nanorods

International Nuclear Information System (INIS)

Gong Haibo; Hao Xiaopeng; Gao Chang; Wu Yongzhong; Du Jie; Xu Xiangang; Jiang Minhua

2008-01-01

Single-crystal CdTe nanorods with diameters of 50-100 nm were synthesized under a surfactant-assisted hydrothermal condition. The experimental results indicated that with a temporal dependence the morphologies of CdTe nanocrystallites changed from nanoparticles to smooth surface nanorods. The crystal structure, morphology and optical properties of the products were investigated by x-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM) and fluorescence spectrophotometer. Furthermore, the formation mechanisms of the nanorods were investigated and discussed on the basis of the experimental results.

FE3O4@SIO2-OSO3H NANOCOMPOSITE AS AN EFFICIENT CATALYST FOR THE PREPARATION OF TRICARBOXAMIDES

Directory of Open Access Journals (Sweden)

Mohammad Ali Ghasemzadeh

Full Text Available In this research a highly efficient one-pot preparation of tricarboxamide derivatives via five-component reactions of isocyanides, aldehydes Meldrum's acid and 2equiv. of amines have been developed in the presence of Fe3O4@SiO2-OSO3H nanocomposite. Nano-Fe3O4 encapsulated-silica particles bearing sulfonic acid was readily recovered using an external magnet and could be reused several times without significant loss of reactivity. The catalyst was fully characterized by VSM, FT-IR, SEM, XRD, EDX and TEM analysis.

Reducción catalítica selectiva de NOx usando nanopartículas de ferritas Cu1-XCoXFe2O4 como catalizador

Directory of Open Access Journals (Sweden)

Sarah Briceño1*

2009-12-01

Full Text Available Nanostructured catalysts AB2O4 spinel type oxides (A = Co and B = Cu were prepared by the sol-gel self-combustion method using citric acid as precursor. They were characterized by X-ray diffraction (XRD, Scanning Electron Microscopy (SEM, Transmission Electron Microscopy (TEM and Catalytic activity tests, which have proven to be effective for selective catalytic reduction of NOx using hydrocarbon as a reducing agent (SCR-HC in a temperature range 250 - 450 ° C, reaching up to 40% conversion of NO and 100% selectivity towards the formation of N2

Characteristics of nano Ti-doped SnO2 powders prepared by sol-gel method

International Nuclear Information System (INIS)

Liu, X.M.; Wu, S.L.; Chu, Paul K.; Zheng, J.; Li, S.L.

2006-01-01

Ti 4+ -doped SnO 2 nano-powders were prepared by the sol-gel process using tin tetrachloride and titanium tetrachloride as the starting materials. The crystallinity and purity of the powders were analyzed by X-ray diffraction (XRD) and the size and distribution of Ti 4+ -doped SnO 2 grains were studied using transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The results show that Ti 4+ has been successfully incorporated into the SnO 2 crystal lattice and the electrical conductivity of the doped materials improves significantly

Silica functionalized Cu(II) acetylacetonate Schiff base complex: An efficient catalyst for the oxidative condensation reaction of benzyl alcohol with amines

Science.gov (United States)

Anbarasu, G.; Malathy, M.; Karthikeyan, P.; Rajavel, R.

2017-09-01

Silica functionalized Cu(II) acetylacetonate Schiff base complex via the one pot reaction of silica functionalized 3-aminopropyltriethoxysilane with acetyl acetone and copper acetate has been reported. The synthesized material was well characterized by analytical techniques such as FT-IR, UV-DRS, XRD, SEM-EDX, HR-TEM, EPR, ICP-AES and BET analysis. The characterization results confirmed the grafting of Cu(II) Schiff base complex on the silica surface. The catalytic activity of synthesized silica functionalized Cu(II) acetylacetonate Schiff base complex was evaluated through the oxidative condensation reaction of benzyl alcohol to imine.

Composition, speciation and distribution of iron minerals in Imperata cylindrica.

Science.gov (United States)

Amils, Ricardo; de la Fuente, Vicenta; Rodríguez, Nuria; Zuluaga, Javier; Menéndez, Nieves; Tornero, Jesús

2007-05-01

A comparative study of the roots, rhizomes and leaves of an iron hyperaccumulator plant, Imperata cylindrica, isolated from the banks of an extreme acidic environment, using complementary techniques: Mösbauer spectroscopy (MS), X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled to energy-dispersive X-ray microanalysis (EDAX) and transmission electron microscopy (TEM), has shown that two main biominerals, jarosite and ferrihydrate-ferritin, accumulate in the different tissues. Jarosite accumulates mainly in roots and rhizomes, while ferritin has been detected in all the structures. A model of iron management in I. cylindrica is presented.

TiO{sub 2} supported over porous silica photocatalysts for pesticide degradation using solar light: Part 2. Silica prepared using acrylic acid emulsion

Energy Technology Data Exchange (ETDEWEB)

Phanikrishna Sharma, Mangalampalli V.; Durga Kumari, Valluri [Inorganic and Physical Chemistry Division, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500607, Andhra Pradesh (India); Subrahmanyam, Machiraju, E-mail: subrahmanyam@iict.res.in [Inorganic and Physical Chemistry Division, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500607, Andhra Pradesh (India)

2010-03-15

An acrylic acid emulsion mixture is used for synthesis of novel porous silica (E-Si) material. The photocatalytic activity of TiO{sub 2} under solar light irradiation for isoproturon (herbicide) degradation is drastically increased when dispersed over E-Si support using solid state dispersion (SSD) technique. The composite material is characterized by XRD, nitrogen adsorption-desorption isotherms, UV-vis DRS, SEM and TEM measurements. The photocatalytic activities of the composite catalysts are evaluated for different parameters. The 5 wt% TiO{sub 2}/E-Si is found to be highly active for isoproturon degradation.

Tuning the architectures of lead deposits on metal substrates by electrodeposition

International Nuclear Information System (INIS)

Yao Chenzhong; Liu Meng; Zhang Peng; He Xiaohui; Li Gaoren; Zhao Wenxia; Liu Peng; Tong Yexiang

2008-01-01

Different morphologies of lead (Pb) deposited on different metal substrates have been prepared via electrochemical deposition in aqueous solution. The morphologies of as-deposited lead were determined by scanning electron microscope (SEM). It is found that the various morphologies of the products are dependent on the electrodeposition conditions, including the deposition current densities, concentration of additives, substrates and deposition time. X-ray diffraction (XRD) and transmission electron microscope (TEM) results reveal that all these lead deposits with different morphologies can be assigned to the space group Fm-3m (2 2 5)

Investigation of morphology and bioactive properties of composite coating of HA/vinyl acetate on pure titanium

International Nuclear Information System (INIS)

Afshar, Abdollahe; Yousefpour, Mardali; Xiudong, Yang; Li Xudong; Yang Bangcheng; Wu Yao; Chen Jiyong; Zhang Xingdong

2006-01-01

Electrochemical co-deposition approach was expanded to prepare composite bio-ceramic coating of hydroxyapatite (HA)/polyvinyl acetate on the surface of titanium. The role is to improve the bioactive and crystallization properties. The results of XRD, XPS, SEM and TEM characterization showed that by increasing amount of vinyl acetate in the composite bio-ceramic coating before and after immersing in the simulated body fluid (SBF), an oriented growth of HA planes on the (0 0 2) direction had been observed on titanium substrate. Also significant surface morphology changes were obtained

SiC Conversion Coating Prepared from Silica-Graphite Reaction

Directory of Open Access Journals (Sweden)

Back-Sub Sung

2017-01-01

Full Text Available The β-SiC conversion coatings were successfully synthesized by the SiO(v-graphite(s reaction between silica powder and graphite specimen. This paper is to describe the effects on the characteristics of the SiC conversion coatings, fabricated according to two different reaction conditions. FE-SEM, FE-TEM microstructural morphologies, XRD patterns, pore size distribution, and oxidation behavior of the SiC-coated graphite were investigated. In the XRD pattern and SAD pattern, the coating layers showed cubic SiC peak as well as hexagonal SiC peak. The SiC coatings showed somewhat different characteristics with the reaction conditions according to the position arrangement of the graphite samples. The SiC coating on graphite, prepared in reaction zone (2, shows higher intensity of beta-SiC main peak (111 in XRD pattern as well as rather lower porosity and smaller main pore size peak under 1 μm.

Destructive interference of TEM and ITG turbulence

International Nuclear Information System (INIS)

Merz, F.; Jenko, F.

2009-01-01

Full text: Turbulence driven by ion temperature gradient (ITG) modes and trapped electron modes (TEMs) is generally considered the key mechanism for anomalous transport in fusion devices on ion scales. But while pure ITG and, to a lesser extent, also pure TEM turbulence have been studied in detail over the last years, not much is presently known about nonlinear interactions between ITG modes and TEMs, which are often present simultaneously in experimentally relevant situations. This important issue is addressed by means of linear and nonlinear gyrokinetic simulations with the GENE code. To examine the properties of the (linear) TEM and ITG instabilities in the (realistic) transitional regime, the GENE code is run as eigenvalue solver, which allows for a systematic study of dominant and subdominant modes. Corresponding nonlinear initial value computations show that the particle transport of the turbulent system can be completely suppressed if the two driving instabilities are active simultaneously. The direct comparison of the linear modes and the corresponding turbulent system reveals a coexistence of the two microinstabilities in a transitional regime even at the same wave number. The consequences of this dual turbulence drive for transport modeling is discussed. (author)

TEM-turbulence in stellarators and its optimization

Science.gov (United States)

Proll, Josefine H. E.; Helander, Per; Lazerson, Samuel; Mynick, Harry; Xanthopoulos, Pavlos

2014-10-01

Quasi-isodynamic stellarators, which are especially optimized for neoclassical transport, have been shown to be resilient towards trapped-electrons modes (TEMs) in large regions of parameter space. In these configurations, all particles have average ``good curvature.'' It was shown analytically that, thanks to this property, particles that bounce faster than the mode in question draw energy from it near marginal stability, so that the ordinary density-gradient-driven TEM has to be stable in the electrostatic and collisionless limit.This has been confirmed in linear flux-tube simulations that were performed with the GENE code. Several magnetic field configurations were compared and it was found that the growth rates of the TEMs drop with increasing degree of quasi-isodynamicity. These findings can be used to optimize stellarators with respect to TEM turbulence by reducing the fraction of trapped particles with bounce averaged ``bad curvature.'' An appropriate proxy function has therefore been designed to be implemented in STELLOPT, a stellarator optimization tool that can now be used to further explore the configuration space of neoclassically optimized stellarators with the aim to extract designs with improved turbulent transport. This work was facilitated by the Max-Planck/Princeton Center for Plasma Physics.

In-situ TEM Studies : Heat-treatment and Corrosion

NARCIS (Netherlands)

Malladi, S.R.K.

2014-01-01

Transmission electron microscopy (TEM) has been well known as a powerful characterisation tool to understand the structure and composition of various materials down to the atomic level. Over the years, several TEM studies have been carried out to understand the compositional, structural and

Indications and techniques of transanal endoscopic microsurgery (TEMS).

Science.gov (United States)

Qi, Yanjie; Stoddard, David; Monson, John R T

2011-08-01

Transanal endoscopic microsurgery (TEMS) has recently reemerged as a valuable technique for the management of rectal neoplasms - both benign and malignant. Since the original description of this technique in the early 1980s, TEMS has emerged as the approach of choice for most benign rectal tumors because of the excellent views provided and superior dissection techniques possible when compared to traditional transanal excision. Many published reports demonstrate that the lowest rates of recurrence are associated with TEMS probably because of full-thickness excision with negative margins. Increasingly, TEMS is being applied to primary rectal cancer when used alone as a full-thickness excision alone or in combination with additional therapies, depending on tumor stage. There is now a significant evidence base to suggest that this approach should be considered as part of a multidisciplinary approach to rectal cancer. This paper describes indications and techniques for this technology.

Magnetostatic Interaction in Fe-Co Nanowires

Directory of Open Access Journals (Sweden)

Laura Elbaile

2012-01-01

Full Text Available Arrays of Fe-Co alloy nanowires with diameter around 35 nm and several micrometers in length have been synthesized by codepositing Fe and Co into porous anodic alumina. The morphology, structure, and magnetic properties of the nanowires (hysteresis loops and remanence curves were characterized by SEM, TEM, X-ray diffraction (XRD, and VSM, respectively. The XRD patterns indicate that the Fe-Co nanowires present a body-centered cubic (bcc structure and a preferred (110 orientation perpendicular to the template surface. From the hysteresis loops obtained with the magnetic field applied in the axis direction of the nanowires, we can observe that the coercive field slightly decreases when the nanowire length increases. This magnetic behaviour is analyzed considering the shape anisotropy and the dipolar interactions among nanowires.

MnMoO4 nanolayers : Synthesis characterizations and electrochemical detection of QA

Science.gov (United States)

Muthamizh, S.; Kumar, S. Praveen; Munusamy, S.; Narayanan, V.

2018-04-01

MnMoO4 nanolayers were prepared by precipitation method. The MnMoO4 nanolayers were synthesized by using commercially available (CH3COO)2Mn.4H2O and Na2WO4.2H2O. The XRD pattern reveals that the synthesized MnMoO4 has monoclinic structure. In addition, lattice parameter values were also calculated using XRD data. The Raman analysis confirm the presence of Mo-O in MnMoO4 nanolayers. DRS-UV analysis shows that MnMoO4 has a band gap of 2.59 eV. FE-SEM and HR-TEM analysis along with EDAX confirms the material morphology in stacked layers like structure in nano scale. Synthesized nanolayers were utilized for the detection of biomolecule quercetin (QA).

Synthesis of α-Alumina (Corundum) and its Application

International Nuclear Information System (INIS)

Nay Thwe Kyi; Kyaw Myo Naing; Tin Tin Aye; Nyunt Wynn

2005-09-01

This paper described the preparation of aluminium isopropoxide from aluminium sheet at different heating times.Aluminium sheet is found to have a reaction with absolute isopropyl alcohol and mercury (II) chloride as a catalyst under nitrogen atmosphere. Aluminium isopropoxide was characterized by NMR, XRD and IR. Aluminium isopropoxide serves as a molecular precursor to derive pure alumina gel by hydrolysis under both homogeneous and heterogeneous conditions. Pyrolysis to this alumina gel transforms it into -aluminia (corundum) at 1200'C. The phase transformation during pyrolysis was characterized by XRD, SEM and TEM. The alumina (corundum) has porous crystalline nature with high surface aera, which may be used as efficient adsorbent packing material in coloumn chromatography for the seperation of vitamin A from the leaves. -alumina can be also used in catalysis

Structural and functional characterization of barium zirconium titanate / epoxy composites

Directory of Open Access Journals (Sweden)

Filiberto González Garcia

2011-12-01

Full Text Available The dielectric behavior of composite materials (barium zirconium titanate / epoxy system was analyzed as a function of ceramic concentration. Structure and morphologic behavior of the composites was investigated by X-ray Diffraction (XRD, Fourier transformed infrared spectroscopy (FT-IR, Raman spectroscopy, field emission scanning electron microscopy (FE-SEM and transmission electron microscopy (TEM analyses. Composites were prepared by mixing the components and pouring them into suitable moulds. It was demonstrated that the amount of inorganic phase affects the morphology of the presented composites. XRD revealed the presence of a single phase while Raman scattering confirmed structural transitions as a function of ceramic concentration. Changes in the ceramic concentration affected Raman modes and the distribution of particles along into in epoxy matrix. Dielectric permittivity and dielectric losses were influenced by filler concentration.

Comparing the detection of iron-based pottery pigment on a carbon-coated sherd by SEM-EDS and by Micro-XRF-SEM.

Science.gov (United States)

Pendleton, Michael W; Washburn, Dorothy K; Ellis, E Ann; Pendleton, Bonnie B

2014-03-01

The same sherd was analyzed using a scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) and a micro X-ray fluorescence tube attached to a scanning electron microscope (Micro-XRF-SEM) to compare the effectiveness of elemental detection of iron-based pigment. To enhance SEM-EDS mapping, the sherd was carbon coated. The carbon coating was not required to produce Micro-XRF-SEM maps but was applied to maintain an unbiased comparison between the systems. The Micro-XRF-SEM analysis was capable of lower limits of detection than that of the SEM-EDS system, and therefore the Micro-XRF-SEM system could produce elemental maps of elements not easily detected by SEM-EDS mapping systems. Because SEM-EDS and Micro-XRF-SEM have been used for imaging and chemical analysis of biological samples, this comparison of the detection systems should be useful to biologists, especially those involved in bone or tooth (hard tissue) analysis.

Using the in situ lift-out technique to prepare TEM specimens on a single-beam FIB instrument

International Nuclear Information System (INIS)

Lekstrom, M; McLachlan, M A; Husain, S; McComb, D W; Shollock, B A

2008-01-01

Transmission electron microscope (TEM) specimens are today routinely prepared using focussed ion beam (FIB) instruments. Specifically, the lift-out method has become an increasingly popular technique and involves removing thin cross-sections from site-specific locations and transferring them to a TEM grid. This lift-out process can either be performed ex situ or in situ. The latter is mainly carried out on combined dual-beam FIB and scanning electron microscope (SEM) systems whereas conventional single-beam instruments often are limited to the traditional ex situ method. It is nevertheless desirable to enhance the capabilities of existing single-beam instruments to allow for in situ lift-out preparation to be performed since this technique offers a number of advantages over the older ex situ method. A single-beam FIB instrument was therefore modified to incorporate an in situ micromanipulator fitted with a tungsten needle, which can be attached to a cut-out FIB section using ion beam induced platinum deposition. This article addresses the issues of using an ion beam to monitor the in situ manipulation process as well as approaches that can be used to create stronger platinum welds between two objects, and finally, views on how to limit the extent of ion beam damage to the specimen surface.

Preparation of carbon-free TEM microgrids by metal sputtering

International Nuclear Information System (INIS)

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

2009-01-01

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 775 K under vacuum conditions.

Preparation of carbon-free TEM microgrids by metal sputtering.

Science.gov (United States)

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.

Focus-variation image reconstruction in field-emission TEM

NARCIS (Netherlands)

Coene, W.M.J.; Janssen, A.J.E.M.; Op de Beeck, M.; Van Dyck, D.; Van Zwet, E.J.; Zandbergen, H.W.; Bailey, G.W.; Rieder, C.L.

1993-01-01

The use of a field emission gun (FEG) in high resolution TEM (HRTEM) improves the information limit much below the point resolution. In the area between point and information resolution of the FEG-TEM, image interpretation is complicated by the lens aberrations and focus effects. Different

ToTem: a tool for variant calling pipeline optimization.

Science.gov (United States)

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 .

Radiation induced deposition of copper nanoparticles inside the nanochannels of poly(acrylic acid)-grafted poly(ethylene terephthalate) track-etched membranes

Science.gov (United States)

Korolkov, Ilya V.; Güven, Olgun; Mashentseva, Anastassiya A.; Atıcı, Ayse Bakar; Gorin, Yevgeniy G.; Zdorovets, Maxim V.; Taltenov, Abzal A.

2017-01-01

Poly(ethylene terephthalate) PET, track-etched membranes (TeMs) with 400 nm average pore size were UV-grafted with poly(acrylic acid) (PAA) after oxidation of inner surfaces by H2O2/UV system. Carboxylate groups of grafted PAA chains were easily complexed with Cu2+ ions in aqueous solutions. These ions were converted into metallic copper nanoparticles (NPs) by radiation-induced reduction of copper ions in aqueous-alcohol solution by gamma rays in the dose range of 46-250 kGy. Copper ions chelating with -COOH groups of PAA chains grafted on PET TeMs form polymer-metal ion complex that prevent the formation of agglomerates during reduction of copper ions to metallic nanoparticles. The detailed analysis by X-Ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed the deposition of copper nanoparticles with the average size of 70 nm on the inner surface of nanochannels of PET TeMs. Samples were also investigated by FTIR, ESR spectroscopies to follow copper ion reduction.

The fabrication of nanocomposites via calcium phosphate formation on gelatin–chitosan network and the gelatin influence on the properties of biphasic composites

International Nuclear Information System (INIS)

Babaei, Zahra; Jahanshahi, Mohsen; Rabiee, Sayed Mahmood

2013-01-01

A novel biodegradable polymer–ceramic nanocomposite which consisted of gelatin (Gel), chitosan (CS), and calcium phosphate (CaP) nanoparticles was prepared based on in situ preparation method. The fabricated biocomposites were characterized by FTIR, X-ray diffraction (XRD), transmission electron microscopy (TEM) as well as scanning electron microscope with X-ray elemental analysis (SEM-EDX). The characterization results confirmed that the crystalline calcium phosphate nanoparticles were mineralized in polymeric matrix and the interaction between Ca2+ in calcium phosphate and functional groups in polymers molecular chains was formed. XRD result showed that in addition to hydroxyapatite (HA), Brushite (BR) and tricalcium phosphate (β-TCP) particles also were formed due to lack of complete penetration of the basic solution into the polymeric matrix. However, SEM image indicated that the polymeric matrix has the controlling role in the particle size of calcium phosphate. The size of particles in three component composites was about 100 nm while in two component composites proved to be more in μm size. TEM observation supported SEM results and showed that the three component composites have calcium phosphate nanoparticles. The elastic modulus and compressive strength of the composites were also improved by the employment of gelatin and chitosan together, which can make them more beneficial for surgical applications. - Highlights: ► A new type of calcium phosphate nanocomposites consisted chitosan and gelatin as polymeric matrix was obtained via in situ precipitation method. ► The formed particles into the polymeric matrix are hydroxyapatite, Brushite and β-tricalcium phosphate. ► The polymer concentration is a predominant factor for inhibiting nucleation and growth of calcium phosphate particles as the particles size was also decreased by increasing the amount of polymeric phase. ► The nano particles formed in three component composites and micro particles

Effect of MnCuFe{sub 2}O{sub 4} content on magnetic and dielectric properties of poly (O-Phenylenediamine)/MnCuFe{sub 2}O{sub 4} nanocomposites

Energy Technology Data Exchange (ETDEWEB)

Kannapiran, Nagarajan [PG and Research Department of Chemistry, Sri Ramakrishna Mission Vidyalaya College of Arts and Science, Coimbatore 641020, Tamil Nadu (India); Muthusamy, Athianna, E-mail: muthusrkv@gmail.com [PG and Research Department of Chemistry, Sri Ramakrishna Mission Vidyalaya College of Arts and Science, Coimbatore 641020, Tamil Nadu (India); Chitra, Palanisamy [PG and Research Department of Chemistry, Sri Ramakrishna Mission Vidyalaya College of Arts and Science, Coimbatore 641020, Tamil Nadu (India)

2016-03-01

Poly o-phenylenediamine (PoPD)/MnCuFe{sub 2}O{sub 4} nanocomposites with three different ratios of MnCuFe{sub 2}O{sub 4} (10%, 20%, 30% w/w) were synthesized by in-situ oxidative chemical polymerization method ammonium persulphate used as oxidant, while MnCuFe{sub 2}O{sub 4} nanoparticles was prepared by auto-combustion method. The structure, morphology and magnetic properties of synthesized PoPD/MnCuFe{sub 2}O{sub 4} nanocomposites were characterized by FT-IR, UV–visible absorption spectra, X-ray diffraction (XRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Thermogravimetric analysis (TGA) and Vibrating sample magnetometer (VSM). FTIR spectra and XRD were confirmed the formation of the PoPD/MnCuFe{sub 2}O{sub 4} nanocomposites. The morphology of PoPD/MnCuFe{sub 2}O{sub 4} nanocomposites is visualized through SEM and TEM. The spherical morphology of the PoPD was confirmed using SEM analysis. Dielectric properties of PoPD/MnCuFe{sub 2}O{sub 4} nanocomposites at different temperatures have been performed in the frequency range of 50 Hz–5 MHz. The optical absorption experiments of PoPD/MnCuFe{sub 2}O{sub 4} nanocomposites reveal that the direct transition with an energy band gap is around 2 eV. - Highlights: • Green synthesis of PoPD (the polymerization carried out only in aqueous medium) by in-situ chemical polymerization method. • For the first time, PoPD incorporated with MnCuFe{sub 2}O{sub 4} with lesser particle size. • The auto combustion reaction, support to achieve less particle size. • Ferrite content affects the magnetic properties of the nanocomposites.

Ag@polypyrrole: A highly efficient nanocatalyst for the N-alkylation of amines using alcohols.

Science.gov (United States)

Mandi, Usha; Kundu, Sudipta K; Salam, Noor; Bhaumik, Asim; Islam, Sk Manirul

2016-04-01

We have synthesized Ag@polypyrrole nanomaterial by dispersing ultrafine silver nanoparticles (Ag NPs) over the organic polymer polypyrrole. The Ag@polypyrrole material has been characterized by powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), electron paramagnetic resonance (EPR), Fourier transform infrared (FT-IR), ultraviolet-visible absorption (UV-vis) and atomic adsorption spectroscopy (AAS), and thermogravimetric analysis (TGA). The XRD pattern suggested the cubic crystalline phase of Ag NPs in Ag@polypyrrole. TEM image analysis revealed that silver nanoparticles are highly dispersed in the polymer matrix. The Ag@polypyrrole acts as an efficient and versatile heterogeneous nanocatalyst in the N-alkylation of amines using alcohols. The catalyst can be easily prepared, highly robust and reused several times without decrease in its catalytic activity. Copyright © 2016 Elsevier Inc. All rights reserved.

Effect of Fe on the phases and microstructure of TiC-Fe cermets by combustion synthesis/quasi-isostatic pressing

International Nuclear Information System (INIS)

Zhang Weifang; Zhang Xinghong; Wang Jianli; Hong Changqing

2004-01-01

Fully dense TiC-Fe cermets (x = 10, 20, 30, and 40 wt.%) were produced from Ti-C-Fe powder mixtures by combustion synthesis with quasi-isostatic pressing. The effect of Fe content on combustion temperature, combustion wave velocity, and final product density was investigated. The final product was characterized by XRD, SEM, and TEM. The combustion temperature and wave velocity decreased with increasing Fe content. Product density increased with increasing Fe content (96% at 30 wt.%). X-ray diffraction and transmission electron microscopy (TEM) revealed the final product to contain TiC, Fe phases, lath martensite, and Fe 2 Ti. The TiC particle size decreased with increasing Fe content. In addition, a low density of dislocations was observed in both the TiC particles and Fe binder, indicative of annealing and recrystallization, respectively

Custo de produção de goiabas para mesa produzidas com e sem ensacamento: estudo de caso

OpenAIRE

Tatiane de Oliveira Tokairin; Fernando Perez Cappello; Marcel Bellato Spósito

2014-01-01

O ensacamento de goiabas para mesa tem por finalidade proteger os frutos contra o ataque de pragas, reduzir a aplicações e os níveis de resíduo de agroquímicos. O objetivo deste trabalho foi avaliar a sustentabilidade econômica da produção de goiabas, por meio da comparação do custo de produção entre os sistemas de cultivo com e sem ensacamento dos frutos. Foi realizado um estudo de caso com dados obtidos de uma propriedade comercial de goiabas para mesa no município de Valinhos - SP. O custo...

Preparation of carbon-free TEM microgrids by metal sputtering

Energy Technology Data Exchange (ETDEWEB)

Janbroers, S., E-mail: stephan.janbroers@albemarle.com [Albemarle Catalysts B.V., Nieuwendammerkade 1-3, 1030 BE, Amsterdam (Netherlands); Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Kruijff, T.R. de; Xu, Q. [Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Kooyman, P.J. [DelftChemTech, Delft University of Technology, Julianalaan 136, 2628 BL, Delft (Netherlands); Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Zandbergen, H.W. [Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands)

2009-08-15

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 775 K under vacuum conditions.

Regulation of ETG turbulence by TEM driven zonal flows

Science.gov (United States)

Asahi, Yuuichi; Ishizawa, Akihiro; Watanabe, Tomohiko; Tsutsui, Hiroaki; Tsuji-Iio, Shunji

2013-10-01

Anomalous heat transport driven by electron temperature gradient (ETG) turbulence is investigated by means of gyrokinetic simulations. It is found that the ETG turbulence can be suppressed by zonal flows driven by trapped electron modes (TEMs). The TEMs appear in a statistically steady state of ETG turbulence and generate zonal flows, while its growth rate is much smaller than those of ETGs. The TEM-driven zonal flows with lower radial wave numbers are more strongly generated than those driven by ETG modes, because of the higher zonal flow response to a density source term. An ExB shearing rate of the TEM-driven zonal flows is strong enough to suppress the long-wavelength ETG modes which make the main contribution to the turbulent transport.

Performance of a field emission gun TEM/STEM

International Nuclear Information System (INIS)

Carpenter, R.W.; Bentley, J.

1979-01-01

First experimental results on a Phillips EM 400 TEM/STEM fitted with a field-emission electron gun and objective twin lens are given here. Operation of the FEG is reliable up to maximum design voltage (120 kV). Highest resolution achieved in TEM was 1.9 A fringe. A wide variety of diffraction modes were demonstrated, ranging from CBDP from a small area (approx. 10 A dia) in STEM mode to SAD with angular resolution of 8 μrad in TEM mode. The EDS sensitivity is very high. STEM imaging performance to the highest magnifications examined (200 kx) is good. Work is in progress to evaluate the limits of STEM performance

Hydrogen absorption in Mg1.95Ti0.05Ni0.95Cu0.05 alloy prepared with mechanical alloying and thermal treatment; Absorcion de hidrogeno en la aleacion Mg1.95Ti0.05Ni0.95Cu0.05 preparada por aleado mecanico y tratamiento termico

Energy Technology Data Exchange (ETDEWEB)

Martinez, Juan Bonifacio; Urena Nunez, Fernando [Instituto Nacional de Investigaciones Nucleares, Ocoyoacac, Estado de Mexico (Mexico)]. E-mail: juan.bonifacio@inin.gob.mx

2009-09-15

This work presents hydrogen absorption in quaternary alloy Mg1.95Ti0.05Ni0.95Cu0.05 obtained by the mechanical alloying method, followed by thermal treatment in ultra-high pure argon atmosphere. The composition of the phases, microstructure and morphology of ground powders and with thermal treatment were characterized by DRX, SEM/EDS and TEM. After 20 hours of mechanical grinding and recooked at 300 degrees Celsius/1h in argon atmosphere, the quaternary alloy has a Mg{sub 2}Ni crystalline hexagonal structure with a crystallite size under 10 nm. The absorption measurements were performed under a pressure of 0.2 to 1.2 MPa at a temperature of 200 degrees Celsius in a micro-reactor. The quantification of absorption-desorption of hydrogen in the intermetallic was conducted in a TGA-DSC simultaneous calorimeter. Metallic hydride-dehydride powder was characterized with SEM and XRD. [Spanish] En este trabajo se presenta la absorcion de hidrogeno en la aleacion cuaternaria Mg1.95Ti0.05Ni0.95Cu0.05 obtenida por el metodo de aleado mecanico, seguida de tratamiento termico en atmosfera de argon de ultra alta pureza. La composicion de las fases, microestructura y morfologia de los polvos molidos y con tratamiento termico fue caracterizada por DRX, SEM/EDS y TEM. Despues de 20 h de molienda mecanica con recocido a 300 grados Celsios/1h en atmosfera de argon, la aleacion cuaternaria tiene una estructura cristalina hexagonal Mg{sub 2}Ni con tamano de cristalito menor a 10 nm. Las mediciones de absorcion fueron realizadas bajo una presion de 0.2 a 1.2 MPa a una temperatura de 200 grados Celsios en un micro-reactor. La cuantificacion de absorcion-desorcion de hidrogeno en el intermetalico se realizo en un calorimetro simultaneo TGA-DSC. Se determino que la cantidad maxima absorbida de hidrogeno en la aleacion cuaternaria fue de 3.24% en peso cuando la presion fue de 0.8 MPa a dicha temperatura. Polvos metalicos hidrurados-deshidrurados se caracterizaron por SEM y XRD.

Retrofit implementation of Zernike phase plate imaging for cryo-TEM.

Science.gov (United States)

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.

Experimental study on propagation properties of large size TEM antennas

International Nuclear Information System (INIS)

Zhang Guowei; Wang Haiyang; Chen Weiqing; Wang Wei; Zhu Xiangqin; Xie Linshen

2014-01-01

The propagation properties of large size TEM antennas were studied by experiment. The size of the TEM antennas is 60 m × 20 m × 10 m and the character Impedance is 120 Ω. A kind of dielectric foil switch is designed compactly with TEM antennas which can generate double exponential waveform with altitude of 10 kV and rise time of l.2 ns. The radiated field distribution was measured. The relationship between rise time/altitude and distance were provided, and the propagation properties of large size TEM antennas were summarized. (authors)

FIB-SEM tomography in biology.

Science.gov (United States)

Kizilyaprak, Caroline; Bittermann, Anne Greet; Daraspe, Jean; Humbel, Bruno M

2014-01-01

Three-dimensional information is much easier to understand than a set of two-dimensional images. Therefore a layman is thrilled by the pseudo-3D image taken in a scanning electron microscope (SEM) while, when seeing a transmission electron micrograph, his imagination is challenged. First approaches to gain insight in the third dimension were to make serial microtome sections of a region of interest (ROI) and then building a model of the object. Serial microtome sectioning is a tedious and skill-demanding work and therefore seldom done. In the last two decades with the increase of computer power, sophisticated display options, and the development of new instruments, an SEM with a built-in microtome as well as a focused ion beam scanning electron microscope (FIB-SEM), serial sectioning, and 3D analysis has become far easier and faster.Due to the relief like topology of the microtome trimmed block face of resin-embedded tissue, the ROI can be searched in the secondary electron mode, and at the selected spot, the ROI is prepared with the ion beam for 3D analysis. For FIB-SEM tomography, a thin slice is removed with the ion beam and the newly exposed face is imaged with the electron beam, usually by recording the backscattered electrons. The process, also called "slice and view," is repeated until the desired volume is imaged.As FIB-SEM allows 3D imaging of biological fine structure at high resolution of only small volumes, it is crucial to perform slice and view at carefully selected spots. Finding the region of interest is therefore a prerequisite for meaningful imaging. Thin layer plastification of biofilms offers direct access to the original sample surface and allows the selection of an ROI for site-specific FIB-SEM tomography just by its pronounced topographic features.

Overview - XRF and XRD

International Nuclear Information System (INIS)

Jenkins, R.

1999-01-01

Full text: While the roots of both X-ray Fluorescence Spectrometry (XRF) and X-ray Powder Diffractometry (XRD) go back 80 years or so, it is only in the last 30 years or so that both techniques have become widely used in the industrial and research environments. It is the experience of the author that all instrumental techniques go through four basic stages: 1. Innovation - someone has a bright idea 2. Application - people start to apply the bright idea 3. Frustration - the bright idea is found to have complications 4. Consolidation - the complications are understood and resolved. XRF went through these four stages by the mid 1980s. This means that, today, if one understands what one is doing, applies the correct (and generally well known) analytical strategy, there is a high probability that one will obtain the correct result. XRD, on the other hand, is still hovering between 3 and 4 on the list. Problems such as the effect of preferred orientation on intensities, difficulties in obtaining accurate data for larger d-spacings, etc., although better understood today, still pose significant challenges to those involved in both routine and research analysis. The development of low-cost computers has made a dramatic impact in both techniques and it is estimated that today, about 90% of all new spectrometer and diffractometer systems sold, are fully automated. There are about 30,000 X-ray spectrometers and about 25,000 diffractometers in use in the world today. Of these about one half are automated. The process of automation has brought its rewards as well as its consequences. In general, the automation of the two techniques has resulted in a poorer understanding of the instrumentation and methodology, on the part of the typical user. Many laboratories employ both techniques, since they are largely complimentary. This workshop will cover the basics of the two methods, highlighting the advantages and shortcomings of both. Copyright (1999) Australian X-ray Analytical

Synthesis, structure and electrochemical properties of polyaniline/MoO3 nanobelt composite for lithium battery

International Nuclear Information System (INIS)

Mohan, Varishetty Madhu; Chen, Wen; Murakami, Kenji

2013-01-01

Graphical abstract: Hydrothermal method was introduced for the synthesis of MoO 3 nanobelts and polyaniline (PANI)/MoO 3 nanobelt composites. The structure and morphology of the samples were studied by X-ray diffraction (XRD), Fourier transform infrared radiation (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis. We can see the presence of polyaniline on the MoO 3 nanobelts surface in the TEM pictures as shown in Fig. (a). The pure MoO 3 nanobelts exhibit the initial specific capacity 276 mAhg −1 , whereas PANI/MoO 3 nanobelt composite shows little low initially 228 mAhg −1 after that it has more stabilized specific capacity with increasing cycle numbers as shown in Fig. (b). The cyclic voltammograms of the PANI/MoO 3 nanobelt composite show better cyclic performance compared to pure MoO 3 nanobelts. The electrochemical impedance spectres were studied for both the pure and PANI/MoO 3 samples at 2.0 and 3.5 potentials. The role of the PANI polymeric component of the composite material seems to be the stabilization of the specific capacity due to probable homogeneous distribution of the induced stress during cycling. Display Omitted Highlights: ► Hydrothermal synthesis of MoO 3 , PANI/MoO 3 nanobelts. ► Samples were characterised by XRD, FTIR, DSC, SEM, TEM, CV and impedance. ► MoO 3 nanobelts cathode battery shows initial specific capacity 276 mAhg −1 . ► PANI/MoO 3 nanobelts show initial specific capacity 228 mAhg −1 but high stability. ► PANI/MoO 3 sample studies by impedance at the potentials of 2.0 and 3.5 V. -- Abstract: The MoO 3 nanobelts and polyaniline (PANI)/MoO 3 nanobelt composite were synthesized using hydrothermal method. The crystal structure and morphology of the samples were studied by X-ray diffraction (XRD), Fourier transform infrared radiation (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Differential scanning calorimetric (DSC) and thermo

Green Biosynthesis of Silver Nanoparticles Using Callicarpa maingayi Stem Bark Extraction

Directory of Open Access Journals (Sweden)

Mohammed Zidan

2012-07-01

Full Text Available Different biological methods are gaining recognition for the production of silver nanoparticles (Ag-NPs due to their multiple applications. The use of plants in the green synthesis of nanoparticles emerges as a cost effective and eco-friendly approach. In this study the green biosynthesis of silver nanoparticles using Callicarpa maingayi stem bark extract has been reported. Characterizations of nanoparticles were done using different methods, which include; ultraviolet-visible spectroscopy (UV-Vis, powder X-ray diffraction (XRD, transmission electron microscopy (TEM, scanning electron microscopy (SEM, energy dispersive X-ray fluorescence (EDXF spectrometry, zeta potential measurements and Fourier transform infrared (FT-IR spectroscopy. UV-visible spectrum of the aqueous medium containing silver nanoparticles showed absorption peak at around 456 nm. The TEM study showed that mean diameter and standard deviation for the formation of silver nanoparticles were 12.40 ± 3.27 nm. The XRD study showed that the particles are crystalline in nature, with a face centered cubic (fcc structure. The most needed outcome of this work will be the development of value added products from Callicarpa maingayi for biomedical and nanotechnology based industries.

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

Science.gov (United States)

LSammons, R.; Thackray, A. C.; Medina Ledo, H.; Marquis, P. M.; Jones, I. P.; Yong, P.; Macaskie, L. E.

2007-12-01

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of β-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600° C showed resolvable ring (unsintered) or dot (600° C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200° C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 Å and c = 6.875 Å, consistent with HA.

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

International Nuclear Information System (INIS)

LSammons, R; Thackray, A C; Ledo, H Medina; Marquis, P M; Jones, I P; Yong, P; Macaskie, L E

2007-01-01

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of β-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600 0 C showed resolvable ring (unsintered) or dot (600 0 C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200 0 C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 A and c = 6.875 A, consistent with HA

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

Energy Technology Data Exchange (ETDEWEB)

LSammons, R [University of Birmingham School of Dentistry, St Chad' s Queensway, Birmingham, B4 6NN (United Kingdom); Thackray, A C [University of Birmingham School of Dentistry, St Chad' s Queensway, Birmingham, B4 6NN (United Kingdom); Ledo, H Medina [University of Birmingham School of Engineering, Metallurgy and Materials, Birmingham B15 2TT (United Kingdom); Marquis, P M [University of Birmingham School of Dentistry, St Chad' s Queensway, Birmingham, B4 6NN (United Kingdom); Jones, I P [University of Birmingham School of Engineering, Metallurgy and Materials, Birmingham B15 2TT (United Kingdom); Yong, P [University of Birmingham, School of Biosciences, Birmingham B15 2TT (United Kingdom); Macaskie, L E [University of Birmingham, School of Biosciences, Birmingham B15 2TT (United Kingdom)

2007-12-15

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of {beta}-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600{sup 0} C showed resolvable ring (unsintered) or dot (600{sup 0} C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200{sup 0} C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 A and c = 6.875 A, consistent with HA.

Crystallization kinetics and growth mechanism of 8 mol% yttria-stabilized zirconia (8YSZ) nano-powders prepared by a sol-gel process

International Nuclear Information System (INIS)

Kuo, C.-W.; Lee, Y.-H.; Hung, I-M.; Wang, M.-C.; Wen, S.-B.; Fung, K.-Z.; Shih, C.-J.

2008-01-01

Eight mol% yttria-stabilized zirconia (8YSZ) gel powders were synthesized at 348 K for 2 h using ZrOCl 2 .8H 2 O and Y(NO 3 ) 3 .6H 2 O as starting materials in an ethanol-water solution by a sol-gel process. The crystallization kinetics and growth mechanism of the 8YSZ gel powders have been investigated using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The XRD results and SAED pattern show that the 8YSZ gel powders calcined at 773 K for 2 h is a cubic ZrO 2 . The activation energy for the crystallization of the cubic ZrO 2 formation in the 8YSZ gel powders is determined as 231.76 kJ/mol by a non-isothermal DTA method. Both growth morphology parameter (n) and crystallization mechanism index (m) are close to 3.0, indicating that the bulk nucleation is dominant in the cubic ZrO 2 formation. The TEM examination shows that the cubic ZrO 2 has a spherical-like morphology with a size ranging from 10 to 20 nm

Mesoporous CdS via Network of Self-Assembled Nanocrystals: Synthesis, Characterization and Enhanced Photoconducting Property.

Science.gov (United States)

Patra, Astam K; Banerjee, Biplab; Bhaumik, Asim

2018-01-01

Semiconduction nanoparticles are intensively studied due to their huge potential in optoelctronic applications. Here we report an efficient chemical route for hydrothermal synthesis of aggregated mesoporous cadmium sulfide (CdS) nanoparticles using supramolecular-assembly of ionic and water soluble sodium salicylate as the capping agent. The nanostructure, mesophase, optical property and photoconductivity of these mesoporous CdS materials have been characterized by using small and wide angle powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N2-sorption, Raman analysis, Fourier transformed infrared (FT-IR), UV-Visible DSR spectroscopy, and photoconductivity measurement. Wide angle XRD pattern and high resolution TEM image analysis suggested that the particle size of the materials is within 10 nm and the nanoparticles are in well-crystallized cubic phase. Mesoporous CdS nanoparticles showed drastically enhanced photoelectrochemical response under visible light irradiation on entrapping a photosensitizer (dye) molecule in the interparticle spaces. Efficient synthesis strategy and the enhanced photo response in the mesoporous CdS material could facilitate the designing of other porous semiconductor oxide/sulfide and their applications in photon-to-electron conversion processes.

Synthesis and characterization of nickel substituted cobalt ferrite nanoparticles by sol–gel auto-combustion method

Energy Technology Data Exchange (ETDEWEB)

Hankare, P.P., E-mail: p_hankarep@rediffmail.com [Solid State Research Laboratory, Department of Chemistry, Shivaji University, Kolhapur, Maharashtra 416 004 (India); Sanadi, K.R., E-mail: sanadikishor@gmail.com [Solid State Research Laboratory, Department of Chemistry, Shivaji University, Kolhapur, Maharashtra 416 004 (India); Garadkar, K.M. [Solid State Research Laboratory, Department of Chemistry, Shivaji University, Kolhapur, Maharashtra 416 004 (India); Patil, D.R. [Material Research Laboratory, Department of Physics, R.L. College, Parola, Jalgaon, Maharashtra 425 111 (India); Mulla, I.S. [Emeritus Scientist-CSIR, Centre for Materials for Electronics and Technology (C-MET), Panchawati, Pune 411 008 (India)

2013-03-15

Highlights: ► Co{sub 1−x}Ni{sub x}Fe{sub 2}O{sub 4} Mixed Metal oxides. ► Sol–gel auto-combustion method. ► Cubic spinel symmetry. ► Nanocrystaline material. ► Semiconducting nature. -- Abstract: Nanocrystalline Co{sub 1−x}Ni{sub x}Fe{sub 2}O{sub 4} (where x = 0.0, 0.25, 0.50, 0.75, 1) were successfully synthesized by sol–gel method using citrate–nitrate precursors. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were effectively utilized to investigate the different structural parameters. XRD showed single cubic spinel phase for all the samples. The decrease in lattice parameter and increase in crystallite size of the ferrispinel was observed with increasing nickel content. The surface morphology and elemental composition were studied by Scanning electron microscope (SEM) and Energy Dispersive X-ray analysis (EDAX) respectively. The nanosize of the synthesized material had been identified by TEM investigation and which is lies in between 20–25 nm. The semiconducting nature of the samples was studied by variation of resistivity and thermal emf with temperature.

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

Science.gov (United States)

Jung, Chan-Ok; Park, Dong-Wha

2013-02-01

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

Sexual Arousal and Sexually Explicit Media (SEM)

DEFF Research Database (Denmark)

Hald, Gert Martin; Stulhofer, Aleksandar; Lange, Theis

2018-01-01

-mainstream and mainstream SEM groups, and (iii) to explore the validity and predictive accuracy of the Non-Mainstream Pornography Arousal Scale (NPAS). METHODS: Online cross-sectional survey of 2,035 regular SEM users in Croatia. MAIN OUTCOMES MEASURES: Patterns of sexual arousal to 27 different SEM themes, sexual...

Poly(o-phenylenediamine)/NiCoFe2O4 nanocomposites: Synthesis, characterization, magnetic and dielectric properties

Science.gov (United States)

Kannapiran, Nagarajan; Muthusamy, Athianna; Chitra, Palanisamy; Anand, Siddeswaran; Jayaprakash, Rajan

2017-02-01

In this study, poly(o-phenylenediamine) (PoPD)/NiCoFe2O4 nanocomposites were synthesized by in-situ oxidative chemical polymerization method with different amount of NiCoFe2O4 nanoparticles. The NiCoFe2O4 nanoparticles were prepared by auto-combustion method. The structural, morphological, thermal properties of the synthesized PoPD/NiCoFe2O4 nanocomposites were characterized by fourier transform infrared spectrum (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). Magnetic properties of NiCoFe2O4 nanoparticles and PoPD/NiCoFe2O4 nanocomposites were studied by vibrating sample magnetometer (VSM). The FTIR and XRD techniques were used to confirm the formation of PoPD/NiCoFe2O4 nanocomposites. The average crystalline size of NiCoFe2O4 nanoparticles and PoPD/NiCoFe2O4 nanocomposites were calculated from XRD. From the SEM analysis, spherical morphology of the PoPD was confirmed. The TGA results showed that the NiCoFe2O4 nanoparticles have improved the thermal stability of PoPD. Dielectric properties of PoPD/NiCoFe2O4 nanocomposites at different temperatures have been carried in the frequency range 50 Hz to 5 MHz.

Synthesis and controlled release properties of 2,4-dichlorophenoxy acetate–zinc layered hydroxide nanohybrid

International Nuclear Information System (INIS)

Bashi, Abbas M.; Hussein, Mohd Zobir; Zainal, Zulkarnain; Tichit, Didier

2013-01-01

Direct reaction of ZnO with 2,4-dichlorophenoxyacetic acid (24D) solutions of different concentrations allows obtaining new organic–inorganic nanohybrid materials formed by intercalation of 24D into interlayers of zinc layered hydroxide (ZLH). XRD patterns show a progressive evolution of the structure as 24D concentration increases. The nanohybrid obtained at higher 24D concentration (24D–ZLH(0.4)) reveals a well ordered layered structure with two different basal spacings at 25.2 Å and 24 Å. The FTIR spectrum showing the vibrations bands of the functional groups of 24D and of the ZLH confirms the intercalation. SEM images are in agreement with the structural evolution observed by XRD and reveal the ribbon morphology of the nanohybrids. The release studies of 24D showed a rapid release of 94% for the first 100 min governed by the pseudo-second order kinetic model. - Graphical abstract: The phenomenon indicates that the optical energy gap is enlarged with the increase of molar concentrations in 2,4-dichlorophenoxy acetate anion content into ZnO to create a ZLH–24D nanohybrid. - Highlights: • Nanohybrid was synthesized from 2,4-dichlorophenoxy acetate with-Zinc LHD, using wet chemistry. • Characterized using SEM, TEM, EDX, FTIR, XRD and TGA. • Ribbon-shaped 24D–Zn-layered hydroxide nanoparticles with (003) diffractions of 2.5 nm phase were synthesized

FIB/SEM study of AA2024 corrosion under a seawater drop, part II

International Nuclear Information System (INIS)

King, Peter C.; Cole, Ivan S.; Corrigan, Penny A.; Hughes, Anthony E.; Muster, Tim H.; Thomas, Sebastian

2012-01-01

Highlights: ► Dealloying has a directional nature, exhibits banding. ► Oxidation state of copper in sponge remnants found to be variable. ► Dissolution and breakdown of copper sponge structure observed. ► Crystalline defects imaged in dealloyed S-phase. - Abstract: The dissolution of S-phase clusters in aluminium alloy 2024 (AA2024) exposed to a 0.5 μl seawater droplet is presented. Foils for transmission electron microscopy (TEM) were made from local attack sites using a focussed ion beam/scanning electron microscope (FIB/SEM). The sections showed that clusters of S-phase particles underwent dealloying. The resulting copper sponge morphology, banding, preferred orientation and crystal defect structure as a result of plastic deformation have been characterised. With build-up of amorphous corrosion product, physical and electrical isolation of parts of the clusters developed, with the result of copper dissolution from the S-phase remnants.

Karakteristik Beberapa Jenis Antibiotik Berdasarkan Pola Difraksi Sinar-X (XRD Dan Spektrum FTIR

Directory of Open Access Journals (Sweden)

Mirzan T Razzak

2017-03-01

Full Text Available Telah dilakukan pengukuran karakteristik difraksi sinar-x (XRD terhadap beberapa jenisantibiotik. Penelitian ini bertujuan untuk memahami karakteristik difraksi sinar-x suatuantibiotik sebagai upaya untuk identifikasi antibiotik secara cepat. Dalam penelitian ini diamatikarakteristik difraksi sinar-x dari 15 (lima belas antibiotik yang tersedia di pasaran. SpektrumXRD diukur pada sudut 2 antara 5 – 75 untuk dibandingkan dan dievaluasi mengenai bentukkristalnya. Selanjutnya diukur pula spektrum XRD dari pencampuran antibiotik dengan tepungtapioka. Pengukuran spektrum infrared dengan FTIR juga dilakukan untuk menguji konsistensihasil evaluasi spektrum XRD. Hasil penelitian menunjukkan bahwa amoxicillin dan ampicillinmempunyai struktur kristal yang sama, yaitu orthorombic primitif. Sayangnya baik XRDmaupun FTIR, tidak memberikan nilai kuantitatif pada antibiotik. Oleh sebab itu, perbedaankonsentrasi dengan pencampuran tepung tapioka tidak dapat dideteksi. Walaupun demikian,metode ini terbukti dapat digunakan untuk membedakan komposisi zat penyusun antibiotiksecara cepat dan akurat.

Corrosion mechanisms of spent fuel under oxidizing conditions

International Nuclear Information System (INIS)

Finn, P.A.; Finch, R.; Buck, E.; Bates, J.

1997-01-01

The release of 99 Tc can be used as a reliable marker for the extent of spent oxide fuel reaction under unsaturated high-drip-rate conditions at 90 degrees C. Evidence from leachate data and from scanning and transmission electron microscopy (SEM and TEM) examination of reacted fuel samples is presented for radionuclide release, potential reaction pathways, and the formation of alteration products. In the ATM-103 fuel, 0.03 of the total inventory of 99 Tc is released in 3.7 years under unsaturated and oxidizing conditions. Two reaction pathways that have been identified from SEM are (1) through-grain dissolution with subsequent formation of uranyl alteration products, and (2) grain-boundary dissolution. The major alteration product identified by x-ray diffraction (XRD) and SEM, is Na-boltwoodite, Na[(UO 2 )(SiO 3 OH)]lg-bullet H 2 O, which is formed from sodium and silicon in the water leachant

Efficiency of Advanced H2O2/ZnO Oxidation Process in Ceftriaxone Antibiotic Removal from Aqueous Solutions

Directory of Open Access Journals (Sweden)

Maryam Noroozi cholcheh

2017-11-01

Full Text Available A major concern about pharmaceutical pollution is the presence of antibiotics in water resources through their release into sewers where they cause bacterial resistance and enhanced drug-resistance in human-borne pathogens and growing microbial populations in the environment. The objective of this study was to investigate the efficiency of  the advanced H2O2/ZnO oxidation process in removing ceftriaxone from aqueous solutions. For this purpose, an experimental study was conducted in which the SEM, XRD, and TEM techniques were employed to determine the size of Zinc oxide nano-particles. Additionally, the oxidation process parameters of pH (3-11, molar ratio of H2O2/ZnO (1.5-3, initial concentration of ceftriaxone (5–15 mg/L, and contact time (30-90 min were investigated. Teh data thus obntained were subjected top statistical analysis using the SPSS (ANOVA test. XRD results revealeda hexagonal crystal structure for the nano-ZnO. TEM images confirmed the spherical shape of the nanoparticles. Finally, SEM images revealed that the Zn nanoparticles used in this study were less than 30 nanometers in diameter. Based on the results, an optimum pH of 11, a contact time of 90 minutes, and a H2O2/ZnO molar ratio equal to 1.5 were the optimum conditions to achieve a ceftriaxone removal efficiency of 92%. The advance H2O2/ZnO oxidation process may thus be claimed to be highly capable of removing ceftriaxone from aqueous solutions.

Synthesis and melting behaviour of Bi, Sn and Sn–Bi nanostructured alloy

Energy Technology Data Exchange (ETDEWEB)

Frongia, F.; Pilloni, M.; Scano, A.; Ardu, A.; Cannas, C.; Musinu, A. [Università di Cagliari, Dipartimento di Scienze Chimiche e Geologiche and Cagliari Research Unit of the National Consortium of Materials Science and Technology (INSTM), Cittadella Universitaria di Monserrato, 09042 Monserrato, CA (Italy); Borzone, G.; Delsante, S. [Department of Chemistry and Industrial Chemistry, Genoa University and Genoa Research Unit of the National Consortium of Materials Science and Technology (INSTM), Via Dodecaneso 31, I-16146 Genoa (Italy); Novakovic, R. [National Research Council (CNR), Institute for Energetics and Interphases (IENI), Via De Marini 6, 16149 Genoa (Italy); Ennas, G., E-mail: ennas@unica.it [Università di Cagliari, Dipartimento di Scienze Chimiche e Geologiche and Cagliari Research Unit of the National Consortium of Materials Science and Technology (INSTM), Cittadella Universitaria di Monserrato, 09042 Monserrato, CA (Italy)

2015-02-25

Highlights: • Aqueous solution route is used to produce Bi, Sn and Bi–Sn nanoparticles. • HRTEM revealed core–shell and Janus type structures of Bi–Sn nanoparticles. • Melting temperature depression of Bi and Bi–Sn nanoparticles were measured by DSC. • DSC data on Bi melting temperature depression agrees with theoretical values. - Abstract: Lead-free solders based on Bi–Sn bimetallic nanoclusters with eutectic composition (Bi{sub 43}Sn{sub 57}) were synthesized at low temperature by simultaneous reduction reaction from aqueous solution containing bismuth and tin chlorides, using potassium borohydride as a reducing agent. By the same processing route, pure bismuth and tin nanoparticles have also been prepared. Microstructure, morphology and composition of the samples were characterized by X-ray powder diffraction (XRD), transmission (TEM) and scanning electron microscopy (SEM). TEM images of Bi–Sn nanoparticles show average size ranging from 30 to 100 nm. Thermal behaviour of Bi–Sn nanopowders was studied by DSC (differential scanning calorimetry) and a melting temperature (135 °C) lower than that of the corresponding microcrystalline sample (139 °C) was observed. SEM micrographs of the thermally treated sample up to 400 °C show fine spherical grains in the micrometer range with finer powder particles on the surface. XRD powder diffraction analysis indicates the formation of bismuth and tin nanophases with an average particle size of 85 and 126 nm, respectively. The oxidation behaviour of the samples was also investigated. The results obtained have been analyzed in view of theoretical models describing the melting temperature depression of nanoparticles.

Surfactant and template free synthesis of porous ZnS nanoparticles

International Nuclear Information System (INIS)

Akhtar, Muhammad Saeed; Riaz, Saira; Mehmood, Rana Farhat; Ahmad, Khuram Shahzad; Alghamdi, Yousef; Malik, Mohammad Azad; Naseem, Shahzad

2017-01-01

ZnS thin films composed of porous nanoparticles have been deposited on to glass substrates by combining three simple synthesis methodologies i.e. chemical bath deposition, co-precipitation and spin coating. The XRD results reveal the cubic phase of ZnS thin films crystallized at nano scale. The crystallite size estimated by Scherrer formula was 3.4 nm. The morphology of the samples was analyzed through scanning electron microscopy (SEM) and is evident that thin films are composed of porous nanoparticles with an average size of 150 nm and pores of 40 nm on almost every grain. Crystallinity, phase and morphology were further confirmed via transmission electron microscopy (TEM). The stoichiometry and phase purity of thin films were determined by energy dispersive X-ray (EDX) spectrum and X-ray photoelectron spectroscopy (XPS) analysis, respectively. The surface topography and homogeneity of thin films were analyzed by atomic force microscopy (AFM) and obtained root mean square roughness (4.0326 nm) reveals the morphologically homogeneous growth of ZnS on glass substrates. The UV–Vis spectroscopy and photoluminescence (PL) were carried out to estimate the band gap and observe the emission spectra in order to speculate the viability of ZnS porous nanoparticles in optoelectronic devices and sensors. - Highlights: • ZnS thin films composed of porous nanoparticles have been deposited. • Methodology is based on a combination of three techniques. • Cubic phase ZnS nanoparticles deposited onto glass substrates. • Films characterized by UV/Vis, PL, XRD, SEM, TEM, AFM and XPS.

Role of Cu in engineering the optical properties of SnO2 nanostructures: Structural, morphological and spectroscopic studies

Science.gov (United States)

Kumar, Virender; Singh, Kulwinder; Jain, Megha; Manju; Kumar, Akshay; Sharma, Jeewan; Vij, Ankush; Thakur, Anup

2018-06-01

We have carried out a systematic study to investigate the effect of Cu doping on the optical properties of SnO2 nanostructures synthesized by chemical route. Synthesized nanostructures were characterized using X-ray diffraction (XRD), Field emission scanning electron microscopy (FE-SEM), High resolution transmission electron microscopy (HR-TEM), Energy dispersive X-ray spectroscopy, Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, UV-visible and Photoluminescence (PL) spectroscopy. The Rietveld refinement analysis of XRD patterns of Cu-doped SnO2 samples confirmed the formation of single phase tetragonal rutile structure, however some localized distortion was observed for 5 mol% Cu-doped SnO2. Crystallite size was found to decrease with increase in dopant concentration. FE-SEM images indicated change in morphology of samples with doping. HR-TEM images revealed that synthesized nanostructures were nearly spherical and average crystallite size was in the range 12-21 nm. Structural defects, crystallinity and size effects on doping were investigated by Raman spectroscopy and results were complemented by FTIR spectroscopy. Optical band gap of samples was estimated from reflectance spectra. We have shown that band gap of SnO2 can be engineered from 3.62 to 3.82 eV by Cu doping. PL emission intensity increased as the doping concentration increased, which can be attributed to the development of defect states in the forbidden transition region of band gap of SnO2 with doping. We have also proposed a band model owing to defect states in SnO2 to explain the observed PL in Cu doped SnO2 nanostructures.