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

NASA Astrophysics Data System (ADS)

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.

Barite aerosol particles from volcanic plumes and fumaroles - FESEM/EDS analysis

NASA Astrophysics Data System (ADS)

Obenholzner, J. H.; Schroettner, H.; Delgado, H.

2003-04-01

Studies of aerosol particles (AP) contained in volcanic plumes has been enormously benefited by the use of field emission scanning electron microscope (FESEM/EDS; responsability by H. Schroettner) permitting morphological, mineralogical and chemical detailed observations and opening new scientific questions. This work shows the ubiquitous presence of Ba in volcanic emissions. We sampled e.g. a volcanic plume (Popocatepetl v.; 1997, 2002) revealing Ba-S-O particles, interpreteted as barite (BaSO4) and Sr-bearing barite with Fe-rich rim (w=1µm). The ca. 500 nm - 4 µm long crystals are +/- euhedral, anhedral and/or partially etched. The µm-sized crystals had been collected on a Teflon fiber filter (1997), the nm-sized on borosilicate fiber filter (BFF, 2002); one set of crystals (ca. l=500-800 nm) is scattered on Fe-hydr/oxide(?). APs collected from the degassing lava flow of Etna (2001) revealed barite (l= ca. 100 nm) on a rounded NaCl (d= 500 nm) and on Fe-hydr/oxides (?). BFF exposed to the F0 fumarole at Vulcano (2001) showed incrustations of barite (l=ca.200 nm) on fibers indicating barite formation during 5 min sampling. At Solfatra we observed almost euhedral barite particles (l=ca.300 nm) of unusual pseudo-trigonal shape. APs from Alpine air masses (A) did not reveal barite. Sources for barite could be vesicle fillings of lavas (known from continental-crust settings), vapor-phase crystallization of ignimbrites (Bandelier Tuff, USA), Ba-rich fumarolic incrustations, rock coatings in the vicinity of fumaroles (Vulcano, I.), sinter of hot springs (Akita-Yaka-Yama v., J.), barite veins (Milos, Gr.), contact-metamorphosed sedimentary xenoliths (Kloech, A.) or lithics associated with hydrovolcanic eruptions (Alban Hills v., I.). Barite has been observed in many Si-tube experiments. Stratospheric APs (1985) of the El Chichon eruption (1982) revealed barite. Ba is known as a trace element in fumarole gases of Vulcano (F11) and TOF mass spectrometry studies detected

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

NASA Technical Reports Server (NTRS)

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.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

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.

Nanorods, nanospheres, nanocubes: Synthesis, characterization and catalytic activity of nanoferrites of Mn, Co, Ni, Part-89

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

Singh, Supriya; Srivastava, Pratibha; Singh, Gurdip, E-mail: gsingh4us@yahoo.com

2013-02-15

Graphical abstract: Prepared nanoferrites were characterized by FE-SEM and bright field TEM micrographs. The catalytic effect of these nanoferrites was evaluated on the thermal decomposition of ammonium perchlorate using TG and TG–DSC techniques. The kinetics of thermal decomposition of AP was evaluated using isothermal TG data by model fitting as well as isoconversional method. Display Omitted Highlights: ► Synthesis of ferrite nanostructures (∼20.0 nm) by wet-chemical method under different synthetic conditions. ► Characterization using XRD, FE-SEM, EDS, TEM, HRTEM and SAED pattern. ► Catalytic activity of ferrite nanostructures on AP thermal decomposition by thermal techniques. ► Burning rate measurements ofmore » CSPs with ferrite nanostructures. ► Kinetics of thermal decomposition of AP + nanoferrites. -- Abstract: In this paper, the nanoferrites of Mn, Co and Ni were synthesized by wet chemical method and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive, X-ray spectra (EDS), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HR-TEM). It is catalytic activity were investigated on the thermal decomposition of ammonium perchlorate (AP) and composite solid propellants (CSPs) using thermogravimetry (TG), TG coupled with differential scanning calorimetry (TG–DSC) and ignition delay measurements. Kinetics of thermal decomposition of AP + nanoferrites have also been investigated using isoconversional and model fitting approaches which have been applied to data for isothermal TG decomposition. The burning rate of CSPs was considerably enhanced by these nanoferrites. Addition of nanoferrites to AP led to shifting of the high temperature decomposition peak toward lower temperature. All these studies reveal that ferrite nanorods show the best catalytic activity superior to that of nanospheres and nanocubes.« less

Ultrasonically assisted solvothermal synthesis of novel Ni/Al layered double hydroxide for capturing of Cd(II) from contaminated water

NASA Astrophysics Data System (ADS)

Rahmanian, Omid; Maleki, Mohammad Hassan; Dinari, Mohammad

2017-11-01

A novel adsorbent of nickel aluminum layered double hydroxide (Ni/Al-LDH) was prepared through the precipitation of metal nitrates by ultrasonically assisted solvothermal method. The surface morphology, chemical structure and thermal properties of this compound were examined by X-ray diffraction (XRD), Fourier Transform Infrared (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) techniques. The XRD, TEM and FE-SEM results established that the synthesized LDH have a well-ordered layer structure with good crystalline nature. Then it was applied to remove excessive Cd(II) ions from water and the effects of contact time, pH and adsorbent dose were examined at initial Cd(II) concentration of 10 mg/L. Results show that the time required to reach equilibrium was fast (40 min) and working pH solution was neutral (pH 7). Langmuir and Freundlich model of adsorption isotherms were explored; the results show that the Freundlich model was better fitted than that Langmuir model. This results predicting a multilayer adsorption of Cd(II) on LDH. The equilibrium kinetic adsorption data were fixed to the pseudo-second order kinetic equation.

Influence of Mg doping on ZnO nanoparticles decorated on graphene oxide (GO) crumpled paper like sheet and its high photo catalytic performance under sunlight

NASA Astrophysics Data System (ADS)

Labhane, P. K.; Sonawane, S. H.; Sonawane, G. H.; Patil, S. P.; Huse, V. R.

2018-03-01

Mg doped ZnO nanoparticles decorated on graphene oxide (GO) sheets were synthesized by a wet impregnation method. The effect of Mg doping on ZnO and ZnO-GO composite has been evaluated by using x-ray diffraction (XRD), Williamson-Hall Plot (Wsbnd H Plot), field emission scanning electron microscope (FESEM), transmission electron microscopy (TEM) and energy dispersive x-ray spectroscopy (EDX). The physical parameters of as-prepared samples were estimated by XRD data. FESEM and HR-TEM images showed the uniform distribution of nanoparticles on GO crumpled paper like sheet. Solar light photocatalytic activities of samples were evaluated spectrophotometrically by the degradation of p-nitrophenol (PNP) and indigo carmine (IC) solution. Mgsbnd ZnO decorated on GO sheets exhibit excellent catalytic efficiency compared to all other prepared samples under identical conditions, degrading PNP and IC nearly 99% within 60 min under sunlight. The effective degradation by Mgsbnd ZnO decorated on GO sheet would be due to extended solar light absorption, enhanced adsorptivity on the composite catalyst surface and efficient charge separation of photo-induced electrons. Finally, plausible mechanism was suggested with the help of scavengers study.

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

PubMed

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

2017-08-29

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

Synthesis and luminescence behavior of SrGd1.76Eu0.24O4 host for display and dosimetric applications

NASA Astrophysics Data System (ADS)

Singh, Jyoti; Manam, J.; Singh, Fouran

2018-05-01

Novel SrGd1.76Eu0.24O4 materials were synthesized by conventional high-temperature solid-state reaction method in air ambiance. The structural and luminescence properties of as-prepared phosphors were explored by XRD, FESEM, TEM, PL and TL techniques. The confirmation of orthorhombic phase formation was obtained by XRD studies. The agglomerated ginger-like morphology of as-synthesized SrGd1.76Eu0.24O4 samples was unfolded by FESEM and TEM studies. Upon 276 and 395 nm UV excitation, SrGd1.76Eu0.24O4 phosphors showed intense red emission. The TL glow curve of SrGd1.76Eu0.24O4 irradiated with γ-rays exhibits two well-resolved peaks at 393 K and 598 K having a shoulder at 537 K. Linearity in a wide dose range 500 Gy-3 kGy are observed in the as-formed SrGd1.76Eu0.24O4 samples. Intense red emission, linear dose response and high reproducibility of SrGd1.76Eu0.24O4 samples broadly indicated its suitability for display and TL dosimetry applications.

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

NASA Astrophysics Data System (ADS)

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.

Synthesis and characterization of protocatechuic acid-loaded gadolinium-layered double hydroxide and gold nanocomposite for theranostic application

NASA Astrophysics Data System (ADS)

Usman, Muhammad Sani; Hussein, Mohd Zobir; Kura, Aminu Umar; Fakurazi, Sharida; Masarudin, Mas Jaffri; Saad, Fathinul Fikri Ahmad

2018-03-01

A theranostic nanocomposite was developed using anticancer agent, protocatechuic acid (PA) and magnetic resonance imaging (MRI) contrast agent gadolinium nitrate (Gd) for simultaneous delivery using layered double hydroxide (LDH) as the delivery agent. Gold nanoparticles (AuNPs) were adsorbed on the surface of the LDH, which served as a complementary contrast agent. Based on the concept of supramolecular chemistry (SPC) and multimodal delivery system (MDS), the PA and Gd guests were first intercalated into the LDH host and subsequently AuNPs were surface adsorbed as the third guest. The nanohybrid developed was named MAPGAu. The MAPGAu was exposed to various characterizations at different stages of synthesis, starting with XRD analysis, which was used to confirm the intercalation episode and surface adsorption of the guest molecules. Consequently, FESEM, Hi-TEM, XRD, ICP-OES, CHNS, FTIR and UV-Vis analyses were done on the nanohybrids. The result of XRD analysis indicated successful intercalation of the Gd and PA as well the adsorption of AuNPs. The UV-Vis release study showed 90% of the intercalated drug was released at pH 4.8, which is the pH of the cancer cells. The FESEM and TEM micrographs obtained equally confirmed the formation of MAGPAu nanocomposite, with AuNPs conspicuously deposited on the LDH surface. The cytotoxicity study of the nanohybrid also showed insignificant toxicity to normal cell lines and significant toxicity to cancer cell lines. The developed MAGPAu nanocomposite has shown prospects for future theranostic cancer treatment.

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

PubMed

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.

Isolation and characterization of nanocrystalline cellulose from roselle-derived microcrystalline cellulose.

PubMed

Kian, Lau Kia; Jawaid, Mohammad; Ariffin, Hidayah; Karim, Zoheb

2018-07-15

Roselle fiber is a renewable and sustainable agricultural waste enriched with cellulose polysaccharides. The isolation of Nanocrystalline cellulose (NCC) from roselle-derived microcrystalline cellulose (MCC) is an alternative approach to recover the agricultural roselle plant residue. In the present study, acid hydrolysis with different reaction time was carried out to degrade the roselle-derived MCC to form NCC. The characterizations of isolated NCC were conducted through Fourier Transform Infrared Ray (FTIR), Transmission Electron Microscopy (TEM), Field Emission Scanning Electron Microscopy (FESEM), Atomic Force Microscopy (AFM), Dynamic Light Scattering (DLS), Energy Dispersive Spectroscopy (EDS), X-ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). As evaluated from the performed morphological investigations, the needle-like shape NCC nanostructures were observed under TEM and AFM microscopy studies, while irregular rod-like shape of NCC was observed under FESEM analysis. With 60min hydrolysis time, XRD analysis demonstrated the highest NCC crystallinity degree with 79.5%. In thermal analysis by TGA and DSC, the shorter hydrolysis time tended to produce NCC with higher thermal stability. Thus, the isolated NCC from roselle-derived MCC has high potential to be used in application of pharmaceutical and biomedical fields for nanocomposite fabrication. Copyright © 2018 Elsevier B.V. All rights reserved.

Tuning effect of polysaccharide Chitosan on structural, morphological, optical and photoluminescence properties of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Magesh, G.; Bhoopathi, G.; Nithya, N.; Arun, A. P.; Ranjith Kumar, E.

2018-05-01

Chitosan/ZnO nanocomposites was synthesized by in-situ chemical precipitation method. The effect of polysaccharide Chitosan concentration (0.1 g, 0.5 g, 1 g and 3 g) was investigated by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) with Energy dispersive spectroscopy (EDX), High Resolution Transmission Electron Microscopy (HRTEM), UV-visible (UV), Fourier Transform Infrared (FTIR) and Photoluminescence Spectroscopy (PL). XRD pattern confirms the hexagonal wurtzite structure of the Chitosan/ZnO nanocomposites. The structural morphology and the elemental composition of the samples were analysed by FESEM and EDX respectively. From TEM analysis, it is observed that the particles in spindle shape morphology with average particle size ranges 10-20 nm. UV-Vis analysis reveals that the Chitosan concentration affect the absorption band edge and shift towards lower wavelength. The oxygen vacancy induced photoluminescence of ZnO nanoparticles was observed and its intensity decreases by tuning the Chitosan concentration.

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

NASA Technical Reports Server (NTRS)

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

2012-01-01

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

The use of novel biodegradable, optically active and nanostructured poly(amide-ester-imide) as a polymer matrix for preparation of modified ZnO based bionanocomposites

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

Abdolmaleki, Amir, E-mail: abdolmaleki@cc.iut.ac.ir; Nanotechnology and Advanced Materials Institute, Isfahan University of Technology, Isfahan 84156-83111, Islamic Republic of Iran; Mallakpour, Shadpour, E-mail: mallak@cc.iut.ac.ir

Highlights: Black-Right-Pointing-Pointer A novel biodegradable and nanostructured PAEI based on two amino acids, was synthesized. Black-Right-Pointing-Pointer ZnO nanoparticles were modified via two different silane coupling agents. Black-Right-Pointing-Pointer PAEI/modified ZnO BNCs were synthesized through ultrasound irradiation. Black-Right-Pointing-Pointer ZnO particles were dispersed homogeneously in PAEI matrix on nanoscale. Black-Right-Pointing-Pointer The effect of ZnO nanoparticles on the properties of synthesized polymer was examined. -- Abstract: A novel biodegradable and nanostructured poly(amide-ester-imide) (PAEI) based on two different amino acids, was synthesized via direct polycondensation of biodegradable N,N Prime -bis[2-(methyl-3-(4-hydroxyphenyl)propanoate)]isophthaldiamide and N,N Prime -(pyromellitoyl)-bis-L-phenylalanine diacid. The resulting polymer was characterized by FT-IR, {sup 1}H NMR,more » specific rotation, elemental analysis, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM) analysis. The synthesized polymer showed good thermal stability with nano and sphere structure. Then PAEI/ZnO bionanocomposites (BNCs) were fabricated via interaction of pure PAEI and ZnO nanoparticles. The surface of ZnO was modified with two different silane coupling agents. PAEI/ZnO BNCs were studied and characterized by FT-IR, XRD, UV/vis, FE-SEM and TEM. The TEM and FE-SEM results indicated that the nanoparticles were dispersed homogeneously in PAEI matrix on nanoscale. Furthermore the effect of ZnO nanoparticle on the thermal stability of the polymer was investigated with TGA and DSC technique.« less

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

NASA Astrophysics Data System (ADS)

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.

Graphene/Ruthenium Active Species Aerogel as Electrode for Supercapacitor Applications

PubMed Central

Gigot, Arnaud; Fontana, Marco; Pirri, Candido Fabrizio; Rivolo, Paola

2017-01-01

Ruthenium active species containing Ruthenium Sulphide (RuS2) is synthesized together with a self-assembled reduced graphene oxide (RGO) aerogel by a one-pot hydrothermal synthesis. Ruthenium Chloride and L-Cysteine are used as reactants. The hydrothermal synthesis of the innovative hybrid material occurs at 180 °C for 12 h, by using water as solvent. The structure and morphology of the hybrid material are fully characterized by Raman, XRD, XPS, FESEM and TEM. The XRD and diffraction pattern obtained by TEM display an amorphous nanostructure of RuS2 on RGO crystallized flakes. The specific capacitance measured in planar configuration in 1 M NaCl electrolyte at 5 mV s−1 is 238 F g−1. This supercapacitor electrode also exhibits perfect cyclic stability without loss of the specific capacitance after 15,000 cycles. In summary, the RGO/Ruthenium active species hybrid material demonstrates remarkable properties for use as active material for supercapacitor applications. PMID:29301192

Graphene/Ruthenium Active Species Aerogel as Electrode for Supercapacitor Applications.

PubMed

Gigot, Arnaud; Fontana, Marco; Pirri, Candido Fabrizio; Rivolo, Paola

2017-12-30

Ruthenium active species containing Ruthenium Sulphide (RuS₂) is synthesized together with a self-assembled reduced graphene oxide (RGO) aerogel by a one-pot hydrothermal synthesis. Ruthenium Chloride and L-Cysteine are used as reactants. The hydrothermal synthesis of the innovative hybrid material occurs at 180 °C for 12 h, by using water as solvent. The structure and morphology of the hybrid material are fully characterized by Raman, XRD, XPS, FESEM and TEM. The XRD and diffraction pattern obtained by TEM display an amorphous nanostructure of RuS₂ on RGO crystallized flakes. The specific capacitance measured in planar configuration in 1 M NaCl electrolyte at 5 mV s -1 is 238 F g -1 . This supercapacitor electrode also exhibits perfect cyclic stability without loss of the specific capacitance after 15,000 cycles. In summary, the RGO/Ruthenium active species hybrid material demonstrates remarkable properties for use as active material for supercapacitor applications.

Improvement in the Characterization of the 2099 Al-Li Alloy by FE-SEM

NASA Astrophysics Data System (ADS)

Brodusch, Nicolas; Trudeau, Michel L.; Michaud, Pierre; Brochu, Mathieu; Rodrigue, Lisa; Boselli, Julien; Gauvin, Raynald

This paper describes how state-of-the-art Field-Emission Scanning Electron Microscopy (FE-SEM) can contribute to the characterization of the 2099 aluminum-lithium alloy, and metallic alloys in general. Investigations were carried out on bulk and thinned samples. BSE imaging at 3kV and STEM imaging at 30kV along with highly efficient microanalysis permitted to correlate experimental and expected structures. Although our results confirm previous studies, this work points out possible substitutions of Mg and Zn with Li, Al and Cu in the T1 precipitates. Zinc and magnesium are also present in "rice grain" shaped precipitates at the grain boundaries. The versatility of the FE-SEM is highlighted in that it can provide information at the macro and micro scales with relevant details. Its ability to probe the distribution of precipitates from nano-to micro-sizes throughout the matrix makes Field-Emission Scanning Electron Microscopy a suitable technique for the characterization of metallic alloys.

The dual role of sulfur-containing amino acids in the synthesis of IV-VI semiconductor nanocrystals: a mechanochemical approach.

PubMed

Baláž, Peter; Baláž, Matej; Caplovičová, Mária; Zorkovská, Anna; Caplovič, Lubomír; Psotka, Miroslav

2014-01-01

PbS@cystine nanocrystals were synthesized mechanochemically, with lead acetate and L-cystine being used as the lead and sulfur precursors, respectively. The resulting nanocrystals are 22-34 nm in size, well-faceted and octahedral in shape. Characterization by XRD, FT-IR, NMR, FE-SEM, EDS, TEM (HRTEM) and surface area measurement methods showed that the particles are single, defect-free crystals with a high crystallinity. Furthermore, the crystals were prepared using a solvent-free procedure that was performed under ambient temperature and atmospheric pressure.

Magnetically recyclable Ni0.5Zn0.5Fe2O4/Zn0.95Ni0.05O nano-photocatalyst: structural, optical, magnetic and photocatalytic properties.

PubMed

Qasim, Mohd; Asghar, Khushnuma; Singh, Braj Raj; Prathapani, Sateesh; Khan, Wasi; Naqvi, A H; Das, Dibakar

2015-02-25

A novel visible light active and magnetically separable nanophotocatalyst, Ni0.5Zn0.5Fe2O4/Zn0.95Ni0.05O (denoted as NZF@Z), with varying amount of Ni0.5Zn0.5Fe2O4, has been synthesized by egg albumen assisted sol gel technique. The structural, optical, magnetic, and photocatalytic properties have been studied by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), fourier transform infrared spectroscopy (FTIR), UV-visible (UV-Vis) spectroscopy, and vibrating sample magnetometry (VSM) techniques. Powder XRD, TEM, FTIR and energy dispersive spectroscopic (EDS) analyses confirm coexistence of Ni0.5Zn0.5Fe2O4 and Zn0.95Ni0.05O phases in the catalyst. Crystallite sizes of Ni0.5Zn0.5Fe2O4 and Zn0.95Ni0.05O in pure phases and nanocomposites, estimated from Debye-Scherrer equation, are found to be around 15-25 nm. The estimated particle sizes from TEM and FESEM data are ∼(22±6) nm. The calculated energy band gaps, obtained by Tauc relation from UV-Vis absorption spectra, of Zn0.95Ni0.05O, 15%NZF@Z, 40%NZF@Z and 60%NZF@Z are 2.95, 2.72, 2.64, and 2.54 eV respectively. Magnetic measurements (field (H) dependent magnetization (M)) show all samples to be super-paramagnetic in nature and saturation magnetizations (Ms) decrease with decreasing ferrite content in the nanocomposites. These novel nanocomposites show excellent photocatalytic activities on Rhodamin Dye. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2007-04-01

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

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

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

Fabbro, Maria T.; Department of Inorganic and Organic Chemistry, Universitat Jaume I, Campus del Riu Sec, E-12071 Castellón; Gracia, Lourdes

Ag{sub 2}CrO{sub 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{sub 2}CrO{sub 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 themore » 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{sub 6}] and [AgO{sub 4}] clusters, generating ideal conditions for the growth of Ag nanoparticles. - Graphical abstract: Theoretical representation of the Ag{sub 2}CrO{sub 4} orthorhombic structure. Display Omitted - Highlights: • The Ag{sub 2}CrO{sub 4} microcrystals indicate an orthorhombic structure. • The formation of Ag{sup 0} promotes Ag-nanoparticle growth on the surface of the Ag{sub 2}CrO{sub 4}. • Electron irradiation of the material induces the formation of Ag vacancies.« less

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

USGS Publications Warehouse

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

1997-01-01

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

Dendritic Ag-Fe nanocrystalline alloy synthesized by pulsed electrodeposition and its characterization

NASA Astrophysics Data System (ADS)

Santhi, Kalavathy; Revathy, T. A.; Narayanan, V.; Stephen, A.

2014-10-01

Synthesis of dendrite shaped Ag-Fe alloy nanomaterial by pulsed electrodeposition route was investigated. The alloy samples were deposited at different current densities from electrolytes of different compositions to study the influence of current density and bath composition on metal contents in the alloy, which was determined by ICP-OES analysis. The XRD studies were carried out to determine the structure of these samples. Magnetic characterization at room temperature and during heating was carried out to understand their magnetic behaviour and to confirm the inferences drawn from the XRD results. The XPS spectra proved the presence of Fe and Ag in the metallic form in the alloy samples. The FESEM and TEM micrographs were taken to view the surface morphology of the nanosized particles.

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

Pan Qingtao; Huang Kai; Ni Shibing

Well-crystalline flower- and rod-like NiS nanostructures have been synthesized by an organic-free hydrothermal process at a low temperature of 200 deg. C. X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) were employed to characterize the as-synthesized NiS nanostructures. The effects of temperature and reaction time on the morphology have been also investigated. The two-step flake-cracking mechanism for the formation of flower- and rod-like NiS nanostructures was discussed. The products were also investigated by photoluminescence (PL) spectroscopy.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

PubMed

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

2013-12-01

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

Optimizing use of the structural chemical analyser (variable pressure FESEM-EDX Raman spectroscopy) on micro-size complex historical paintings characterization.

PubMed

Guerra, I; Cardell, C

2015-10-01

The novel Structural Chemical Analyser (hyphenated Raman spectroscopy and scanning electron microscopy equipped with an X-ray detector) is gaining popularity since it allows 3-D morphological studies and elemental, molecular, structural and electronic analyses of a single complex micro-sized sample without transfer between instruments. However, its full potential remains unexploited in painting heritage where simultaneous identification of inorganic and organic materials in paintings is critically yet unresolved. Despite benefits and drawbacks shown in literature, new challenges have to be faced analysing multifaceted paint specimens. SEM-Structural Chemical Analyser systems differ since they are fabricated ad hoc by request. As configuration influences the procedure to optimize analyses, likewise analytical protocols have to be designed ad hoc. This paper deals with the optimization of the analytical procedure of a Variable Pressure Field Emission scanning electron microscopy equipped with an X-ray detector Raman spectroscopy system to analyse historical paint samples. We address essential parameters, technical challenges and limitations raised from analysing paint stratigraphies, archaeological samples and loose pigments. We show that accurate data interpretation requires comprehensive knowledge of factors affecting Raman spectra. We tackled: (i) the in-FESEM-Raman spectroscopy analytical sequence, (ii) correlations between FESEM and Structural Chemical Analyser/laser analytical position, (iii) Raman signal intensity under different VP-FESEM vacuum modes, (iv) carbon deposition on samples under FESEM low-vacuum mode, (v) crystal nature and morphology, (vi) depth of focus and (vii) surface-enhanced Raman scattering effect. We recommend careful planning of analysis strategies prior to research which, although time consuming, guarantees reliable results. The ultimate goal of this paper is to help to guide future users of a FESEM-Structural Chemical Analyser system

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

Raul, Prasanta Kumar, E-mail: prasanta.drdo@gmail.com; Devi, Rashmi Rekha; Umlong, Iohborlang M.

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

Effect of zinc oxide amounts on the properties and antibacterial activities of zeolite/zinc oxide nanocomposite.

PubMed

Alswat, Abdullah A; Ahmad, Mansor Bin; Saleh, Tawfik A; Hussein, Mohd Zobir Bin; Ibrahim, Nor Azowa

2016-11-01

Nanocomposites of zinc oxide loaded on a zeolite (Zeolite/ZnO NCs) were prepared using co-precipitation method. The ratio effect of ZnO wt.% to the Zeolite on the antibacterial activities was investigated. Various techniques were used for the nanocomposite characterization, including UV-vis, FTIR, XRD, EDX, FESEM and TEM. XRD patterns showed that ZnO peak intensity increased while the intensities of Zeolite peaks decreased. TEM images indicated a good distribution of ZnO-NPs onto the Zeolite framework and the cubic structure of the zeolite was maintained. The average particle size of ZnO-nanoparticles loaded on the surface of the Zeolite was in the range of 1-10nm. Moreover, Zeolite/ZnO NCs showed noticeable antibacterial activities against the tested bacteria; Gram- positive and Gram- negative bacteria, under normal light. The efficiency of the antibacterial increased with increasing the wt.% from 3 to 8 of ZnO NPs, and it reached 87% against Escherichia coli E266. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2010-11-01

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

MnMoO4 nanolayers : Synthesis characterizations and electrochemical detection of QA

NASA Astrophysics Data System (ADS)

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).

Role of Cu in engineering the optical properties of SnO2 nanostructures: Structural, morphological and spectroscopic studies

NASA Astrophysics Data System (ADS)

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.

Transparent Al+3 doped MgO thin films for functional applications

NASA Astrophysics Data System (ADS)

Maiti, Payel; Sekhar Das, Pradip; Bhattacharya, Manjima; Mukherjee, Smita; Saha, Biswajit; Mullick, Awadesh Kumar; Mukhopadhyay, Anoop Kumar

2017-08-01

The present work reports the utilization of a relatively simple, cost effective sol-gel technique based route to synthesize highly transparent, spin coated 4.1 at% Al+3 doped MgO thin films on quartz substrates. The films were characterized by XRD, XPS, Raman spectroscopy, and SIMS techniques. The microstructures were characterized by FESEM and TEM while the nanomechanical properties were assessed by the nanoindentation technique. Finally the optical transmittance was measured by UV-vis technique. The x-ray diffraction (XRD) study suggests the crystal facet (2 0 0) of MgO lattice to be distorted after incorporation of Al+3 into MgO lattice. From FESEM the doped films were found to have a dense microstructure with a crystallite size of about 20 nm as revealed by the TEM studies. Nanoindentation measurements indicated drastic increase of elastic modulus for the Al+3 doped MgO thin films by ~73% compared to that of the pristine MgO thin films along with retaining the nanohardness at ~8 GPa. The transmittance of Al+3 doped MgO thin films in the visible range was significantly higher (~99%) than that of pristine MgO (~90%) thin films. The films also had a relatively higher refractive index of about 1.45 as evaluated from the optical properties. The enhanced transmittance as well as the improved elastic modulus of Al+3 doped MgO thin films suggest its promising candidature in magnetic memory devices and as buffer layers of solar cells.

Temperature dependent selective detection of hydrogen and acetone using Pd doped WO3/reduced graphene oxide nanocomposite

NASA Astrophysics Data System (ADS)

Kaur, Jasmeet; Anand, Kanica; Kohli, Nipin; Kaur, Amanpreet; Singh, Ravi Chand

2018-06-01

Reduced graphene oxide (RGO) and Pd doped WO3 nanocomposites were fabricated by employing electrostatic interactions between poly (diallyldimethylammonium chloride) (PDDA) modified Pd doped WO3 nanostructures and graphite oxide (GO) and studied for their gas sensing application. XRD, Raman, FTIR, FESEM-EDX, TEM, TGA, XPS and Photoluminescence techniques were used for characterization of as-synthesized samples. Gas sensing studies revealed that the sensor with optimized doping of 1.5 mol% Pd and 1 wt% GO shows temperature dependent selectivity towards hydrogen and acetone. The role of WO3, Pd and RGO has been discussed in detail for enhanced sensing performance.

CdS loaded on coal based activated carbon nanofibers with enhanced photocatalytic property

NASA Astrophysics Data System (ADS)

Guo, Jixi; Guo, Mingxi; Jia, Dianzeng; Song, Xianli; Tong, Fenglian

2016-08-01

The coal based activated carbon nanofibers (CBACFs) were prepared by electrospinning a mixture of polyacrylonitrile (PAN) and acid treated coal. Cadmium sulfide (CdS) nanoparticles loaded on CBACFs were fabricated by solvothermal method. The obtained samples were characterized by FESEM, TEM, and XRD. The results reveal that the CdS nanoparticles are homogeneously dispersed on the surfaces of CBACFs. The CdS/CBACFs nanocomposites exhibited higher photoactivity for photodegradation of methyl blue (MB) under visible light irradiation than pure CdS nanoparticles. CBACFs can be used as low cost support materials for the preparation of nanocomposites with high photocatalytic activity.

Preparation of Pd/Fe3O4 nanoparticles by use of Euphorbia stracheyi Boiss root extract: A magnetically recoverable catalyst for one-pot reductive amination of aldehydes at room temperature.

PubMed

Nasrollahzadeh, Mahmoud; Sajadi, S Mohammad

2016-02-15

We describe a method for supporting palladium nanoparticles on magnetic nanoparticles using Euphorbia stracheyi Boiss root extract as the natural source of reducing and stabilizing agent. The progress of the reaction was monitored using UV-visible spectroscopy. The nanocatalyst was characterized by FE-SEM, TEM, XRD, EDS, FT-IR spectroscopy and ICP. The nanocatalyst was applied as an efficient, magnetically recoverable, highly reusable and heterogeneous catalyst for one-pot reductive amination of aldehydes at room temperature. The nanocatalyst was easily recovered by applying an external magnet and reused several times without considerable loss of activity. Copyright © 2015 Elsevier Inc. All rights reserved.

Green synthesis of stabilized spherical shaped gold nanoparticles using novel aqueous Elaeis guineensis (oil palm) leaves extract

NASA Astrophysics Data System (ADS)

Ahmad, Tausif; Bustam, Mohamad Azmi; Irfan, Muhammad; Moniruzzaman, Muhammad; Anwaar Asghar, Hafiz Muhammad; Bhattacharjee, Sekhar

2018-05-01

In the last decade, development of bioinspired protocols to synthesize gold nanoparticles (AuNPs) using plants and their extracts have been dealt by researchers due to their low cost, renewability and non-toxic features. A simple, cheap and ecofriendly method is reported to synthesize stabilized AuNPs of size 35-75 nm at room temperature using aqueous Elaeis guineensis (oil palm) leaves extract without addition of any external agent. Oil palm leaves mediated AuNPs were characterized using FTIR, UV-vis spectrophotometer, EDAX, XPS, FESEM, TEM, DLS and TGA. FTIR spectra results revealed contribution of phenolic, carboxylic, amines and amides in reduction of trivalent gold ions and stabilization of formed gold atoms. Reaction solution color change and UV-vis spectra confirmed reduction of gold ions to generate gold atoms. Reaction mechanism explained the role of phenolic compounds in reduction reaction using FTIR and UV-vis spectra results. EDAX and XPS results further validated the formation of metallic gold particles through bioreduction of gold ions. Crystal structure of metallic gold particles was confirmed through XRD peaks indexing to (111), (200), (220) and (311) planes. TEM and FESEM particles size measurements exhibited the formation of nanostructured AuNPs. Synthesis of well scattered and spherical shaped AuNPs was revealed through FESEM and TEM images. The excellent stability of AuNPs was shown through high negative zeta potential value (-14.7 ± 4.68 mV) and uniform dispersion in aqueous media. Our results disclosed the excellent potential of Elaeis guineensis (oil palm) leaves as reducing and stabilizing agents in green synthesis of well scattered spherical shaped AuNPs, which can be employed as strong candidates in medical drug delivery and industrial applications.

A High Sensitivity Isopropanol Vapor Sensor Based on Cr₂O₃-SnO₂ Heterojunction Nanocomposites via Chemical Precipitation Route.

PubMed

Jawaher, K Rackesh; Indirajith, R; Krishnan, S; Robert, R; Pasha, S K Khadheer; Deshmukh, Kalim; Sastikumar, D; Das, S Jerome

2018-08-01

Cr2O3-SnO2 heterojunction nanocomposites were prepared via chemical precipitation method. The prepared samples were characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectra and Field Emission Electron Microscopy (FESEM). The XRD spectrum confirms the presence of both tetragonal rutile SnO2 and rhombohedral corundum Cr2O3 structure. Further investigation into the gas sensing performances of the prepared Cr2O3-SnO2 nanocomposites exhibited an enhanced sensitivity towards VOPs such as isopropanol, acetone, ethanol and formaldehyde. Especially, isopropanol vapor sensor shows excellent sensitivity at an operating temperature of 100 °C. The highest sensitivity for Cr2O3-SnO2 heterojunction nanocomposites indicate that these materials can be a good candidate for the production of high-performance isopropanol sensors.

A novel ultrasound assisted method in synthesis of NZVI particles.

PubMed

Jamei, Mir Roozbeh; Khosravi, Mohamad Reza; Anvaripour, Bagher

2014-01-01

This research is about a novel ultrasound assisted method for synthesis of nano zero valent iron particles (NZVI). The materials were characterized using TEM, FESEM, XRD, BET and acoustic PSA. The effect of ultrasonic power, precursor/reductant concentration (NaBH4, FeSO4·7H2O) and delivery rate of NaBH4 on NZVI characteristics were investigated. Under high ultrasonic power the morphology of nano particles changed from spherical type to plate and needle type. Also, when high precursor/reductant and high ultrasonic power was used the particle size of NZVI decreased. The surface area of NZVI particles synthesized by ultrasonic method was increased when compared by the other method. From the XRD patterns it was found also the crystallinity of particles was poor. Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis and characterization of titanate nanotube/single-walled carbon nanotube (TNT/SWCNT) porous nanocomposite and its photocatalytic activity on 4-chlorophenol degradation under UV and solar irradiation

NASA Astrophysics Data System (ADS)

Payan, A.; Fattahi, M.; Jorfi, S.; Roozbehani, B.; Payan, S.

2018-03-01

The titanate nanotube/single-wall carbon nanotube (TNT/SWCNT) nanocomposites from different titania precursors were prepared by a two-step hydrothermal process. These nanocomposites were characterized by XRD, BET, Raman, FESEM, TEM, EDX, EDS, EIS, UV-vis DRS and FTIR techniques. The FESEM and TEM images showed the high porous nanocomposites with two types of tubular structure relating to TNTs and SWCNTs which were interwoven together uniformly. The XRD and Raman analysis further corroborated the chemical interaction between the SWCNT and the TNT in the nanocomposites. The photocatalytic performance of the as-synthesized composites were examined by the photodegradation of 4-CP under solar and UV illumination. The results revealed an impressive enhancement in photocatalytic activity of the nanocomposites under both irradiation conditions comparison to bare TNPs and TNTs. Amongst the TNT/SWCNT nanocomposites, 10% loading of SWCNT under UV irradiation and 5% loading of SWCNT under solar irradiation exhibited the maximum photocatalytic performance while the photocatalytic degradation efficiency of nanocomposites were not affected considerably by the type of precursor. Moreover, the mechanism and role of SWCNT were investigated and the plausible degradation pathways of 4-CP was suggested. TOC analyses was performed for determination of 4-CP mineralization rate and results showed complete mineralization after 240 and 390 min under UV and solar irradiation, respectively. The trapping experiments corroborated the O2- and OH radicals as the main reactive species in 4-CP degradation process. Langmuir-Hinshelwood kinetic model was fittingly matched with the experimental data (R2: 0.9218 and 0.9703 for UV and solar irradiation). Additionally, the stability of the nanocomposites were investigated and revealed 8% decrease in degradation efficiency after four cycles.

Synthesis and characterization of novel fluoroalkyl-terminated hyperbranched polyurethane latex

NASA Astrophysics Data System (ADS)

Xu, Wei; Zhao, Weijia; Hao, Lifen; Wang, Sha; Pei, Mengmeng; Wang, Xuechuan

2018-04-01

Waterborne polyurethane (PU) emulsions are widely used in various fields and the demand for them is ever-increasing over the years. However, the hydrophilic chain extender inevitably bonded into the PU backbone can affect the water tolerance of PU. Thus, it is of great importance to improve PU water resistance effectively. Herein, novel fluoroalkyl-terminated hyperbranched polyurethane (HBPUF) latex was accordingly synthesized by graft reaction of perfluorohexyl ethyl alcohol and hyperbranched polyurethane (HBPU), which was previously obtained from interaction between hydroxyl-terminated hyperbranched polymer and PU prepolymer manufactured via the acetone process, as well as using neutralization, adding water, and high-speed stirring operations. We characterized the resultants and investigated its surface properties by IR, NMR, TEM, XRD, TGA, DSC, FE-SEM, AFM, XPS, and contact angle measurements, etc. IR and NMR tests confirmed that the fluorinated fragments had been grafted onto the tail end of HBPU. TEM, XRD, DSC, and FE-SEM results all accounted for the fact that there were multi-crystals in PU, HBPU and HBPUF. TGA results showed that thermal stabilities of the PU, HBPU, and HBPUF latex films were enhanced in turn. XPS and AFM analyses demonstrated that the fluorine-containing segments from the HBPUF terminals were prone to migrate and enrich on the film-air surface of the HBPUF latex film, which made water contact angle and water absorption of the HBPUF film be as 113.9° and 11.1%, respectively, compared to those of the PU film (77.8° and 136.2%). This research indicates that water resistance of the PU film can be efficiently enhanced by fluorinated polyurethane with novel fluoroalkyl-terminated hyperbranched structure.

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

PubMed

Jung, Chan-Ok; Park, Dong-Wha

2013-02-01

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

Paper-based transparent flexible thin film supercapacitors

NASA Astrophysics Data System (ADS)

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

2013-05-01

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

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

NASA Astrophysics Data System (ADS)

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.

Biosynthesis of silver nanoparticles using citrus sinensis peel extract and its antibacterial activity.

PubMed

Kaviya, S; Santhanalakshmi, J; Viswanathan, B; Muthumary, J; Srinivasan, K

2011-08-01

Biosynthesis of silver nanoparticles (AgNPs) was achieved by a novel, simple green chemistry procedure using citrus sinensis peel extract as a reducing and a capping agent. The effect of temperature on the synthesis of silver nanoparticles was carried out at room temperature (25°C) and 60°C. The successful formation of silver nanoparticles has been confirmed by UV-vis, FTIR, XRD, EDAX, FESEM and TEM analysis and their antibacterial activity against Escherichia coli, Pseudomonas aeruginosa (gram-negative), and Staphylococcus aureus (gram-positive) has been studied. The results suggest that the synthesized AgNPs act as an effective antibacterial agent. Copyright © 2011 Elsevier B.V. All rights reserved.

Micro-emulsion-assisted synthesis of ZnS nanospheres and their photocatalytic activity

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

Li Yao; He Xiaoyan; Cao Minhua

2008-11-03

ZnS nanospheres with rough surface were synthesized by using a micro-emulsion-assisted solvothemal process. The molar ratio of [water]/[surfactant] played an important role in controlling the size of the ZnS nanospheres. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), field emission-scanning electron microscope (FE-SEM), and selected area electron diffraction (SAED) were used for the characterization of the resulting ZnS nanospheres. A possible formation mechanism was proposed. These ZnS nanospheres exhibited a good photocatalytic activity for degradation of an aqueous p-nitrophenol solution and the total organic carbon (TOC) of the degradation product has also been investigated.

Realistic representation of Bacillus subtilis biofilms architecture using combined microscopy (CLSM, ESEM and FESEM).

PubMed

Bridier, A; Meylheuc, T; Briandet, R

2013-05-01

In this contribution, we used a set of microscopic techniques including confocal laser scanning microscopy (CLSM), environmental scanning electron microscopy (ESEM) and field emission scanning electron microscopy (FESEM) to analyze the three-dimensional spatial arrangement of cells and their surrounding matrix in Bacillus subtilis biofilm. The combination of the different techniques enabled a deeper and realistic deciphering of biofilm architecture by providing the opportunity to overcome the limits of each single technique. Copyright © 2013 Elsevier Ltd. All rights reserved.

Strength and Stiffness Development in Soft Soils: A FESEM aided Soil Microstructure Viewpoint

NASA Astrophysics Data System (ADS)

Wijeyesekera, D. C.; Ho, M. H.; Bai, X.; Bakar, I.

2016-07-01

This paper opens with an overview of the debatable definition of soft soil that goes beyond a (CH) organic / inorganic clay and OH peat to include weakly cemented periglacial deposits of loess and alike. It then outlines the findings obtained from stiffness test on cement-stabilised soft clay. The findings are complemented with a microstructure viewpoint obtained using field emission scanning electron microscope (FESEM). Research also comprised of making cylindrical stabilised clay samples, prepared in the laboratory with various rubber chips contents and cement, and then aged for 28 days. The samples were then subjected to unconfined compressive strength (UCS) test and observations were also made of its microstructure using the FESEM. The impact of the soil microstructure on the stiffness result was studied both with the stabilized soil and also of some of the natural undisturbed loess soils. Sustainability aspect and the potential of the use of rubber chips and sand as additives to cement stabilisation are also discussed. The overall test results indicated that rubber chips and sand contributed to the improvement in unconfined compressive strength (qu). The derogatory influence of moisture on the stiffness of the stabilised clay was studied simultaneously. SEM micrographs are presented that show bonding of cement, rubber chips/ sand and soft clay, granular units and aggregated / agglomerated units in loess. The paper concludes with observations on the dependence of soil microstructure on the soil strength and deformability and even collapsibility of the loess. Current practices adopted as engineering solutions to these challenging soils are outlined.

A study on structure, morphology, optical properties, and photocatalytic ability of SrTiO3/TiO2 granular composites

NASA Astrophysics Data System (ADS)

Thi Mai Oanh, Le; Xuan Huy, Nguyen; Thi Thuy Phuong, Doan; Danh Bich, Do; Van Minh, Nguyen

2018-03-01

(1-x)SrTiO3-xTiO2 granular composites with x=0.3, 0.4, 0.5, 0.6, 0.7, and 0.8 were synthesized by sol-gel process. Structure, morphology, optical properties, and photocatalytic activity were investigated in detail using x-ray diffraction (XRD) analysis, Raman scattering, field-emission scanning electron microscopy (FE-SEM), Transmission Electron Microscopy (TEM), ultraviolet-visible (UV-vis) absorption spectra, and photoluminescence (PL). XRD analysis showed the formation of single phase for parent phases and the present of two component phases in all composites without any impurity. A tight cohesion between TiO2 and SrTiO3 (STO) at grain boundary region was inferred from lattice parameter change of STO. Moreover, FE-SEM images revealed a granular structure of composite in which SrTiO3 particles were surrounded by smaller TiO2 nanoparticles. As TiO2 concentration increased, absorption edge firstly shifted to the left for composite with x=0.3 and then shifted gradually to the right with further increasing of TiO2 content from 30 mol% to 80 mol%. Composites exhibited a stronger photocatalytic activity than parent phases, with the highest efficiency at 50 mol% of TiO2. PL analysis result showed that the recombination rate of photogenerated electron-hole pairs decreased in composite sample, which partly explained the enhanced photocatalytic property.

Production of polyimide ceria nanocomposites by development of molecular hook technology in nano-sonochemistry.

PubMed

Hatami, Mehdi

2018-06-01

Poly(amic acid), the precursor of polyimide (PI), was used for the preparation of PI/CeO 2 nanocomposites (NC)s by ultrasonic assisted technique via insertion of the surface modified CeO 2 nanoparticles (NP)s into PI matrix. In the preparation stages, in the first, the modifications of CeO 2 NPs by using hexadecyltrimethoxysilane (HDTMS) as a binder were targeted using ultrasonic waves. In the second step, newly designed PI structure was formed from the sonochemical imidization process as a molecular hook. In this step two different reactions were occurred. The acetic acid elimination reaction in the main chain of macromolecule, and the acetylation reaction in the side chains of poly(amic acid) were accomplished. By acetylation process the hook structure was created for trapping of the modified nanoparticles. In the final step the preparation of PI NCs were achieved by sonochemical process. The structural and thermal properties of pure PI and PI/CeO 2 NCs were studied by several techniques such as fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (NMR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD), and thermal analyses. FT-IR and 1 H NMR spectra confirmed the success in preparation of PI matrix. The FE-SEM, TEM, and AFM analyses showed the uniform distribution of CeO 2 NPs in PI matrix. The XRD patterns of NCs show the presence of crystalline CeO 2 NPs in amorphous PI matrix. The thermal analysis results reveal that, with increases in the content of CeO 2 NPs in PI matrix, the thermally stability factors of samples were improved. Copyright © 2018 Elsevier B.V. All rights reserved.

Nanowires of silver-polyaniline nanocomposite synthesized via in situ polymerization and its novel functionality as an antibacterial agent.

PubMed

Tamboli, Mohaseen S; Kulkarni, Milind V; Patil, Rajendra H; Gade, Wasudev N; Navale, Shalaka C; Kale, Bharat B

2012-04-01

Silver-polyaniline (Ag-PANI) nanocomposite was synthesized by in situ polymerization method using ammonium persulfate (APS) as an oxidizing agent in the presence of dodecylbenzene sulfonic acid (DBSA) and silver nitrate (AgNO(3)). The as synthesized Ag-PANI nanocomposite was characterized by using different analytical techniques such as UV-visible (UV-vis) and Fourier transform Infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), thermo gravimetric analysis (TGA), X-ray diffraction (XRD), and transmission electron microscopy (TEM). UV-visible spectra of the synthesized nanocomposite showed a sharp peak at ~420 nm corresponding to the surface plasmon resonance (SPR) of the silver nanoparticles (AgNPs) embedded in the polymer matrix which is overlapped by the polaronic peak of polyaniline appearing at that wavelength. Nanowires of Ag-PANI nanocomposite with diameter 50-70 nm were observed in FE-SEM and TEM. TGA has indicated an enhanced thermal stability of nanocomposite as compared to that of pure polymer. The Ag-PANI nanocomposite has shown an antibacterial activity against model organisms, a gram positive Bacillus subtilis NCIM 6633 in Mueller-Hinton (MH) medium, which is hitherto unattempted. The Ag-PANI nanocomposite with monodispersed AgNPs is considered to have potential applications in sensors, catalysis, batteries and electronic devices. Copyright © 2011 Elsevier B.V. All rights reserved.

Self-assembled spongy-like MnO2 electrode materials for supercapacitors

NASA Astrophysics Data System (ADS)

Dong, Meng; Zhang, Yu Xin; Song, Hong Fang; Qiu, Xin; Hao, Xiao Dong; Liu, Chuan Pu; Yuan, Yuan; Li, Xin Lu; Huang, Jia Mu

2012-08-01

Mesoporous spongy-like MnO2 has been synthesized via a facile and biphasic wet method, accompanied with tetraoctylammonium bromide (TOAB) as a soft template under ambient condition. A well-defined spongy morphology of MnO2 with uniform filament diameters 10-20 nm have been observed by FESEM, TEM, HRTEM, XRD, FT-IR,TGA-DSC studies. Further physical characterizations revealed that MnO2 sponges owned a large surface area of 155 m2 g-1 with typical mesoporous appearance. A specific capacitance value as high as 336 F g-1 was obtained. This improved capacitive behavior was attributed to the large surface area, morphology nature of nano-MnO2, and its broad pore size distribution.

Formation of randomly distributed nano-tubes, -rods and -plates of n-type and p-type bismuth telluride via molecular legation

NASA Astrophysics Data System (ADS)

Ram, Jasa; Ghosal, Partha

2015-08-01

Randomly distributed nanotubes, nanorods and nanoplates of Bi0.5Sb1.5Te3 and Bi2Te2.7Se0.3 ternary compounds have been synthesized via a high yield solvo-thermal process. Prior to solvo-thermal heating at 230 °C for crystallization, we ensured molecular legation in room temperature reaction by complete reduction of precursor materials, dissolved in ethylene glycol and confirmed it by replicating Raman spectra of amorphous and crystalline materials. These nanomaterials have also been characterized using XRD, FE-SEM, EDS and TEM. Possible formation mechanism is also discussed. This single process will enable development of thermoelectric modules and random distribution of diverse morphology will be beneficial in retaining nano-crystallite sizes.

Preparation, characterization and gas sensing performance of BaTiO3 nanostructured thin films

NASA Astrophysics Data System (ADS)

Suryawanshi, Dinesh N.; Pathan, Idris G.; Bari, Anil. R.; Patil, Lalchand A.

2018-05-01

Spray pyrolysis techniques was employed to prepare BaTiO3 thin films. AR grade solutions of Barium chloride (0.05 M) and Titanium chloride (0.05 M) were mixed in the proportion of 30:70, 50:50 and 70:30. The solutions were sprayed on quartz substrate heated at 350°C temperature to obtain the films. These thin films were annealed for a two hours at 600°C in air medium respectively. The prepared thin films were characterized using XRD, FESEM, EDAX, TEM. The electrical and gas sensing properties of these films were investigated. 50:50 film showed better response to Liquid Petroleum Gas (LPG) as compare 30:70 and 70:30 films.

Preparation of silver nanoparticles loaded graphene oxide nanosheets for antibacterial activity

NASA Astrophysics Data System (ADS)

T, T. T., Vi; Lue, S. J.

2016-11-01

A simple, facile method to fabricate successfully silver nanoparticle (AgNPs) decorated on graphene oxide (GO) layers via grafted thiol groups. Samples were prepared with different concentrations of AgNO3. Resulting AgNPs were quasi-spherical in shape and attached on the layers of GO. Physical properties were confirmed by X-ray diffraction (XRD), zeta potential, dynamic light scattering (DLS), Fourier transform infrared (FTIR) spectra, thermogravimetric analyzer (TGA), transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE-SEM). Antimicrobial test was effectively showed using MRSA (Staphylococcus areus). The GO-Ag NPs with appropriate Ag NPs content of 0.2 M AgNO3 exhibited the strongest antibacterial activity at 48.77% inhibition after 4 hours incubation.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

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

NASA Astrophysics Data System (ADS)

Kazemizadeh, Fatemeh; Malekfar, Rasoul

2018-02-01

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

Thermal stability enhancement of modified carboxymethyl cellulose films using SnO2 nanoparticles.

PubMed

Baniasad, Arezou; Ghorbani, Mohsen

2016-05-01

In this study, in-situ and ex-situ hydrothermal synthesis procedures were applied to synthesize novel CMC/porous SnO2 nanocomposites from rice husk extracted carboxymethyl cellulose (CMC) biopolymer. In addition, the effects of SnO2 nanoparticles on thermal stability of the prepared nanocomposite were specifically studied. Products were investigated in terms of morphology, particle size, chemical structure, crystallinity and thermal stability by using field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermogravimetric analysis (TGA), respectively. Presence of characteristic bands in the FTIR spectra of samples confirmed the successful formation of CMC and CMC/SnO2 nanocomposites. In addition, FESEM images revealed four different morphologies of porous SnO2 nanoparticles including nanospheres, microcubes, nanoflowers and olive-like nanoparticles with hollow cores which were formed on CMC. These nanoparticles possessed d-spacing values of 3.35Å. Thermal stability measurements revealed that introduction of SnO2 nanoparticles in the structure of CMC enhanced stability of CMC to 85%. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis of hollow ZnO microspheres by an integrated autoclave and pyrolysis process.

PubMed

Duan, Jinxia; Huang, Xintang; Wang, Enke; Ai, Hanhua

2006-03-28

Hollow zinc oxide microspheres have been synthesized from a micro ZnBr2·2H2O precursor obtained by an autoclave process in bromoform steam at 220 °C /2.5 MPa. Field-emission scanning electron microscropy (FE-SEM) and transmission electron microscopy (TEM) show that the products are about 1.0 µm single crystal spherical particles with hollow interiors, partly open surfaces and walls self-assembled by ZnO nanoparticles. X-ray diffraction (XRD) analysis shows that the as-prepared ZnO hollow spheres are of a hexagonal phase structure. A possible formation mechanism is suggested on the basis of the shape evolution of ZnO nanostructures observed by SEM and TEM. The room-temperature photoluminescence (PL) spectrum shows UV emission around 386 nm and weak green emission peaks indicating that there are few defects in the single crystal grains of the ZnO microspheres.

Production of new cellulose nanomaterial from red algae marine biomass Gelidium elegans.

PubMed

Chen, You Wei; Lee, Hwei Voon; Juan, Joon Ching; Phang, Siew-Moi

2016-10-20

Nanocellulose was successfully isolated from Gelidium elegans red algae marine biomass. The red algae fiber was treated in three stages namely alkalization, bleaching treatment and acid hydrolysis treatment. Morphological analysis was performed by field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). TEM results revealed that the isolated nanocellulose had the average diameter and length of 21.8±11.1nm and of 547.3±23.7nm, respectively. Fourier transform infrared (FTIR) spectroscopy proved that the non-cellulosic polysaccharides components were progressively removed during the chemically treatment, and the final derived materials composed of cellulose parent molecular structure. X-ray diffraction (XRD) study showed that the crystallinity of yielded product had been improved after each successive treatments subjected to the treated fiber. The prepared nano-dimensional cellulose demonstrated a network-like structure with higher crystallinity (73%) than that of untreated fiber (33%), and possessed of good thermal stability which is suitable for nanocomposite material. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2011-05-01

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.

Controlling the Optical and Magnetic Properties of Nanostructured Cuprous Oxide Synthesized from Waste Electric Cables

NASA Astrophysics Data System (ADS)

Abdelbasir, S. M.; El-Sheikh, S. M.; Rashad, M. M.; Rayan, D. A.

2018-03-01

Cuprous oxide Cu2O nanopowders were purposefully synthesised from waste electric cables (WECs) via a simple precipitation route at room temperature using lactose as a reducing agent. In this regard, dimethyl sulfoxide (DMSO) was first applied as an organic solvent for the dissolution of the cable insulating materials. Several parameters were investigated during dissolution of WECs such as dissolution temperature, time and solid/liquid ratio to determine the dissolution percentage of the insulating materials in DMSO. The morphology and the optical properties of the formed Cu2O particles were investigated using X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), Fourier-transform infrared spectroscopy and UV-visible-near IR spectrophotometer. XRD data confirmed the presence of single crystalline phase of Cu2O nanoparticles. FE-SEM and TEM images revealed spherical, cubic and octahedral shapes with the various particle sizes ranged from 16 to 57 nm depending on the synthesis conditions. A possible mechanism explaining the Cu2O nanostructures formation was proposed. The band gap energies of the Cu2O nanostructures were estimated and the values were located between 1.5 and 2.08 eV. Photoluminescence spectroscopy analysis clearly showed a noticeably blue-shifted emission for the synthesized samples compared to spectrum of the bulk. Eventually, magnetic properties of the synthesized nanoparticles have been measured by vibrating sample magnetometer and the attained results implied that the synthesized particles are weakly ferromagnetic in nature at normal temperature.

Characterization and morphology of prepared titanium dioxide nanofibers by electrospinning.

PubMed

Park, Ju-Young; Lee, In-Hwa

2010-05-01

Dispersed titanium dioxide in polymer nanofibers were prepared by sol-gel processing and electrospinning techniques using titanium isopropoxide (TiP)/polyvinylpyrrolidone (PVP) solution. The prepared titanium dioxide nanofibers were characterized by FE-SEM, TEM, XRD, and FT-IR. Pure titanium dioxide nanofibers were obtained from calcination of inorganic-organic composite fiber. The diameter of titanium oxide nanofibers were in the range of 70 nm to 150 nm. Prepared titanium dioxide nanofibers show rough surface and rather small diameter compare with TiP/PVP composite nanofibers. After calcined at 500 degrees C, TiO2 nanofibers convert into anatase and rutile mixed phased from amorphous structure. Calcination of these composite fibers above 600 degrees C resulted in pure rutile TiO2 nanofibers.

Synthesis, characterization, in vitro anti-proliferative and hemolytic activity of hydroxyapatite

NASA Astrophysics Data System (ADS)

Palanivelu, R.; Ruban Kumar, A.

2014-06-01

Hydroxyapatite (Ca10(PO4)6(OH)2, HAP) nanoparticles are widely used in several biomedical applications due to its compositional similarities to bone mineral, excellent biocompatibility and bioactivity, osteoconductivity. In this present investigation, HAP nanoparticles synthesized by precipitation technique using calcium nitrate and di-ammonium phosphate. The crystalline nature and the functional group analysis are confirmed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Fourier transform Raman spectroscopy (FT-Raman) respectively. The morphological observations are ascertained from field emission electron scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). In vitro anti-proliferative and hemolytic activities are carried out on the synthesized HAP samples and the studies reveals that HAP have mild activity against erythrocytes.

Simple route to (NH4)xWO3 nanorods for near infrared absorption

NASA Astrophysics Data System (ADS)

Guo, Chongshen; Yin, Shu; Dong, Qiang; Sato, Tsugio

2012-05-01

Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows.Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film

Liposomes self-assembled from electrosprayed composite microparticles

NASA Astrophysics Data System (ADS)

Yu, Deng-Guang; Yang, Jun-He; Wang, Xia; Tian, Feng

2012-03-01

Composite microparticles, consisting of polyvinylpyrrolidone (PVP), naproxen (NAP) and lecithin (PC), have been successfully prepared using an electrospraying process and exploited as templates to manipulate molecular self-assembly for the synthesis of liposomes in situ. Field emission scanning electron microscope (FESEM) and transmission electron microscope (TEM) observations demonstrate that the microparticles have an average diameter of 960 ± 140 nm and a homogeneous structure. X-ray diffraction (XRD) patterns, differential scanning calorimetry (DSC) and attenuated total reflectance-Fourier transform infrared (ATR-FTIR) results verify that the building blocks NAP and PC are scattered in the polymer matrix in a molecular way owing to the very fast drying of the electrospraying process and the favorable secondary interactions among the components. FESEM, scanning probe microscope (SPM) and TEM observations demonstrate that the liposomes can be achieved through molecular self-assembly in situ when the microparticles contact water thanks to ‘like prefers like’ and by means of the confinement effect of the microparticles. The liposomes have an encapsulation rate of 91.3%, and 80.7% of the drug in the liposomes can be freed into the dissolution medium in a sustained way and by a diffusion mechanism over a period of 24 h. The developed strategy not only provides a new, facile, and effective method to assemble and organize molecules of multiple components into liposomes with electrosprayed microparticles as templates, but also opens a new avenue for nanofabrication in a step-by-step and controllable way.

Y3Fe5O12 nanoparticulate garnet ferrites: Comprehensive study on the synthesis and characterization fabricated by various routes

NASA Astrophysics Data System (ADS)

Niaz Akhtar, Majid; Azhar Khan, Muhammad; Ahmad, Mukhtar; Murtaza, G.; Raza, Rizwan; Shaukat, S. F.; Asif, M. H.; Nasir, Nadeem; Abbas, Ghazanfar; Nazir, M. S.; Raza, M. R.

2014-11-01

The effects of synthesis methods such as sol-gel (SG), self combustion (SC) and modified conventional mixed oxide (MCMO) on the structure, morphology and magnetic properties of the (Y3Fe5O12) garnet ferrites have been studied in the present work. The samples of Y3Fe5O12 were sintered at 950 °C and 1150 °C (by SG and SC methods). For MCMO route the sintering was done at 1350 °C for 6 h. Synthesized samples prepared by various routes were investigated using X-ray diffraction (XRD) analysis, Field emission scanning electron microscopy (FESEM), Impedance network analyzer and transmission electron microscopy (TEM). The structural analysis reveals that the samples are of single phase structure and shows variations in the particle sizes and cells volumes, prepared by various routes. FESEM and TEM images depict that grain size increases with the increase of sintering temperature from 40 nm to 100 nm.Magnetic measurements reveal that garnet ferrite synthesized by sol gel method has high initial permeability (60.22) and low magnetic loss (0.0004) as compared to other garnet ferrite samples, which were synthesized by self combustion and MCMO methods. The M-H loops exhibit very low coercivity which enables the use of these materials in relays and switching devices fabrications. Thus, the garnet nanoferrites with low magnetic loss prepared by different methods may open new horizon for electronic industry for their use in high frequency applications.

TEM Study of SAFARI-2000 Aerosols

NASA Technical Reports Server (NTRS)

Buseck, Peter R.

2004-01-01

The aim of our research was to obtain data on the chemical and physical properties of individual aerosol particles from biomass smoke plume s in southern Africa and from air masses in the region that are affec ted by the smoke. We used analytical transmission electron microscopy (ATEM), including energy-dispersive X-ray spectrometry (EDS) and ele ctron energy-loss spectroscopy (EELS), and field-emission electron microscopy (FESEM) to study aerosol particles from several smoke and haz e samples and from a set of cloud samples.

Structural, Morphological, and Electron Transport Studies of Annealing Dependent In2O3 Dye-Sensitized Solar Cell

PubMed Central

Mahalingam, S.; Abdullah, H.; Shaari, S.; Muchtar, A.; Asshari, I.

2015-01-01

Indium oxide (In2O3) thin films annealed at various annealing temperatures were prepared by using spin-coating method for dye-sensitized solar cells (DSSCs). The objective of this research is to enhance the photovoltaic conversion efficiency in In2O3 thin films by finding the optimum annealing temperature and also to study the reason for high and low performance in the annealed In2O3 thin films. The structural and morphological characteristics of In2O3 thin films were studied via XRD patterns, atomic force microscopy (AFM), field-emission scanning electron microscopy (FESEM), EDX sampling, and transmission electron microscopy (TEM). The annealing treatment modified the nanostructures of the In2O3 thin films viewed through FESEM images. The In2O3-450°C-based DSSC exhibited better photovoltaic performance than the other annealed thin films of 1.54%. The electron properties were studied by electrochemical impedance spectroscopy (EIS) unit. The In2O3-450°C thin films provide larger diffusion rate, low recombination effect, and longer electron lifetime, thus enhancing the performance of DSSC. PMID:26146652

Technical Evaluation Motor No. 7 (TEM-7)

NASA Technical Reports Server (NTRS)

Hughes, Phil

1991-01-01

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

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

PubMed

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

2012-10-01

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

Facile one-pot synthesis of hexagons of NaSrB5O9:Tb3+ phosphor for solid-state lighting

NASA Astrophysics Data System (ADS)

Ramesh, B.; Dillip, G. R.; Deva Prasad Raju, B.; Somasundaram, K.; Prasad Peddi, Siva; de Carvalho dos Anjos, Virgilio; Joo, S. W.

2017-04-01

NaSrB5O9:Tb3+ hexagons were synthesized by a facile solid-state reaction method. The synthesized powders were structurally examined by x-ray diffraction analysis (XRD), and Rietveld refinement was performed using the XRD data and Fullprof software. Hexagon-like morphology was observed using field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The elemental composition of the phosphors was investigated qualitatively by energy dispersive x-ray analysis (EDS) and quantitatively by x-ray photoelectron spectroscopy (XPS). The phosphor has a strong green emission at 545 nm under excitation of 379 nm, which is due to the 5{{\\text{D}}4}{{\\to}7}{{\\text{F}}5} transition of the Tb3+ ion. A lifetime of 3.48 ms was obtained for the phosphor. The important parameters of the light source were determined, such as the thermal quenching, critical distance, the nature of the dopant ion interaction, color coordinates, and quantum yield values. Other reported properties include the site occupancy of the dopant, surface properties, morphological properties, and optical properties.

Highly Sensitive NiO Nanoparticle based Chlorine Gas Sensor

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Optical and structural properties of Mo-doped NiTiO3 materials synthesized via modified Pechini methods

NASA Astrophysics Data System (ADS)

Pham, Thanh-Truc; Kang, Sung Gu; Shin, Eun Woo

2017-07-01

In this study, molybdenum (Mo)-doped nickel titanate (NiTiO3) materials were successfully synthesized as a function of Mo content through a modified Pechini method followed by a solvothermal treatment process. Various characterization methods were employed to investigate the optical and structural properties of the materials. XRD patterns clearly showed that the NiTiO3 structure maintained a single phase with no observed crystalline structure transformations, even after the addition of 10 wt.% Mo. In the Raman spectra and XRD patterns, peak positions shifted with a change in Mo content, confirming that the NiTiO3 lattice was doped with Mo. On the other hand, Mo doping of NiTiO3 materials changed their optical properties. DRS-UV demonstrated that the addition of Mo increased photon absorption within the UV region. Relaxation processes were inhibited by Mo doping, which was evident in the PL spectra. Structural properties of the prepared materials were studied via FE-SEM and HR-TEM. The measured surface area increased proportionally with Mo content due to a reduction in grain size of the materials.

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

NASA Astrophysics Data System (ADS)

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

2012-11-01

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

Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

NASA Technical Reports Server (NTRS)

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

2001-01-01

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

A ‘NanoSuit’ surface shield successfully protects organisms in high vacuum: observations on living organisms in an FE-SEM

PubMed Central

Takaku, Yasuharu; Suzuki, Hiroshi; Ohta, Isao; Tsutsui, Takami; Matsumoto, Haruko; Shimomura, Masatsugu; Hariyama, Takahiko

2015-01-01

Although extremely useful for a wide range of investigations, the field emission scanning electron microscope (FE-SEM) has not allowed researchers to observe living organisms. However, we have recently reported that a simple surface modification consisting of a thin extra layer, termed ‘NanoSuit’, can keep organisms alive in the high vacuum (10−5 to 10−7 Pa) of the SEM. This paper further explores the protective properties of the NanoSuit surface-shield. We found that a NanoSuit formed with the optimum concentration of Tween 20 faithfully preserves the integrity of an organism's surface without interfering with SEM imaging. We also found that electrostatic charging was absent as long as the organisms were alive, even if they had not been coated with electrically conducting materials. This result suggests that living organisms possess their own electrical conductors and/or rely on certain properties of the surface to inhibit charging. The NanoSuit seems to prolong the charge-free condition and increase survival time under vacuum. These findings should encourage the development of more sophisticated observation methods for studying living organisms in an FE-SEM. PMID:25631998

Technical Evaluation Motor No. 10 (TEM-10)

NASA Technical Reports Server (NTRS)

1993-01-01

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

Synthesis of SiO2-coated ZnMnFe2O4 nanospheres with improved magnetic properties.

PubMed

Wang, Jun; Zhang, Kai; Zhu, Yuejin

2005-05-01

A core-shell structured composite, SiO2 coated ZnMnFe2O4 spinel ferrite nanoparticles (average diameter of approximately 80 nm), was prepared by hydrolysis of tetraethyl orthosilicate (TEOS) in the presence of ZnMnFe2O4 nanoparticles (average diameter of approximately 10 nm) synthesized by a hydrothermal method. The obtained samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FESEM). The magnetic measurements were carried out on a vibrating sample magnetometer (VSM), and the measurement results indicate that the core-shell samples possess better magnetic properties at room temperature, compared with paramagnetic colloids with a magnetic core by a coprecipitation method. These core-shell nanospherical particles with self-assembly under additional magnetic fields could have potential application in biomedical systems.

An efficient copper-based magnetic nanocatalyst for the fixation of carbon dioxide at atmospheric pressure.

PubMed

Sharma, Rakesh Kumar; Gaur, Rashmi; Yadav, Manavi; Goswami, Anandarup; Zbořil, Radek; Gawande, Manoj B

2018-01-30

In the last few decades, the emission of carbon dioxide (CO 2 ) in the environment has caused havoc across the globe. One of the most promising strategies for fixation of CO 2 is the cycloaddition reaction between epoxides and CO 2 to produce cyclic carbonates. For the first time, we have fabricated copper-based magnetic nanocatalyst and have applied for the CO 2 fixation. The prepared catalyst was thoroughly characterized using various techniques including XRD, FT-IR, TEM, FE-SEM, XPS, VSM, ICP-OES and elemental mapping. The reactions proceeded at atmospheric pressure, relatively lower temperature, short reaction time, solvent- less and organic halide free reaction conditions. Additionally, the ease of recovery through an external magnet, reusability of the catalyst and excellent yields of the obtained cyclic carbonates make the present protocol practical and sustainable.

Synthesis, characterization, in vitro anti-proliferative and hemolytic activity of hydroxyapatite.

PubMed

Palanivelu, R; Ruban Kumar, A

2014-06-05

Hydroxyapatite (Ca10(PO4)6(OH)2, HAP) nanoparticles are widely used in several biomedical applications due to its compositional similarities to bone mineral, excellent biocompatibility and bioactivity, osteoconductivity. In this present investigation, HAP nanoparticles synthesized by precipitation technique using calcium nitrate and di-ammonium phosphate. The crystalline nature and the functional group analysis are confirmed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Fourier transform Raman spectroscopy (FT-Raman) respectively. The morphological observations are ascertained from field emission electron scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). In vitro anti-proliferative and hemolytic activities are carried out on the synthesized HAP samples and the studies reveals that HAP have mild activity against erythrocytes. Copyright © 2014 Elsevier B.V. All rights reserved.

Studies on the chemical synthesis and characterization of lead oxide nanoparticles with different organic capping agents

NASA Astrophysics Data System (ADS)

Arulmozhi, K. T.; Mythili, N.

2013-12-01

Lead oxide (PbO) nanoparticles were chemically synthesized using Lead (II) acetate as precursor. The effects of organic capping agents such as Oleic acid, Ethylene Diamine Tetra Acetic acid (EDTA) and Cetryl Tri Methyl Butoxide (CTAB) on the size and morphology of the nanoparticles were studied. Characterization techniques such as X-ray diffraction (XRD), Fourier Transform-Infrared spectroscopy (FT-IR), Photoluminescence (PL) Field Emission Scanning Electron Microscopy (FE-SEM), Energy Dispersive Spectroscopy (EDS) and Transmission Electron Microscopy (TEM) were used to analyse the prepared nanoparticles for their physical, structural and optical properties. The characterization studies reveal that the synthesized PbO nanoparticles had well defined crystalline structure and sizes in the range of 25 nm to 36 nm for capping agents used and 40 nm for pure PbO nanoparticles.

Significant enhancement in volumetric and gravimetric capacitance of Cu-TiO2/PPY composite for supercapacitor application

NASA Astrophysics Data System (ADS)

Purty, B.; Choudhary, R. B.

2018-04-01

Copper doped titanium dioxide-polypyrrole (Cu-TiO2/PPY) composite was successfully synthesized via chemical oxidative in-situ polymerization process. The structural and morphological properties of Cu-TiO2/PPY composite were investigated using X-ray diffractometer (XRD), field emission electron microscopy (FESEM) and transmission electron microscopy(TEM) techniques. The electrochemical properties of as-synthesized composite were studied using cyclic voltammetry (CV), galvanostatic charge discharge (GCD) and electrochemical impedance spectroscopic (EIS) techniques. The novel Cu-TiO2/PPY composite showed enhanced volumetric capacitance ˜714 F cm-1 and gravimetric capacitance ˜674 F g-1 at 1 A g-1. In addition an excellent coulombic efficiency and comparabley low charge transfer resistance than pure PPY suggests improved supercapacitive performance of Cu-TiO2/PPY composite as an electrode material.

Synthesis and structural studies of Mg doped LiNi0.5Mn0.5O2 cathode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Murali, N.; Margarette, S. J.; Madhuri Sailaja, J.; Kondala Rao, V.; Himakar, P.; Kishore Babu, B.; Veeraiah, V.

2018-02-01

Layered Mg doped LiNi0.5Mn0.5O2 materials have been synthesized by sol-gel method. The physical properties of these materials were examined by XRD, FESEM and FT-IR studies. From XRD patterns, the phase formation of α-NaFeO2 layered structure with R\\bar 3m space group is confirmed. The surface morphology of the synthesized materials has been examined by FESEM analysis in which the average particle size is found to be about 2 - 2.5 µm. These materials show some changes in the local ion environment, as examined by FT-IR studies.

Multiscale deformation behavior for multilayered steel by in-situ FE-SEM

NASA Astrophysics Data System (ADS)

Tanaka, Y.; Kishimoto, S.; Yin, F.; Kobayashi, M.; Tomimatsu, T.; Kagawa, K.

2010-03-01

The multi-scale deformation behavior of multi-layered steel during tensile loading was investigated by in-situ FE-SEM observation coupled with multi-scale pattern. The material used was multi-layered steel sheet consisting of martensitic and austenitic stainless steel layers. Prior to in-situ tensile testing, the multi-scale pattern combined with a grid and random dots were fabricated by electron beam lithography on the polished surface in the area of 1 mm2 to facilitate direct observation of multi-scale deformation. Both of the grids with pitches of 10 μm and a random speckle pattern ranging from 200 nm to a few μm sizes were drawn onto the specimen surface at same location. The electron moiré method was applied to measure the strain distribution in the deformed specimens at a millimeter scale and digital images correlation method was applied to measure the in-plane deformation and strain distribution at a micron meter scale acquired before and after at various increments of straining. The results showed that the plastic deformation in the austenitic stainless steel layer was larger than the martensitic steel layer at millimeter scale. However, heterogeneous intrinsic grain-scale plastic deformation was clearly observed and it increased with increasing the plastic deformation.

A Facile Synthesis of a Palladium-Doped Polyaniline-Modified Carbon Nanotube Composites for Supercapacitors

NASA Astrophysics Data System (ADS)

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

2013-08-01

Supercapacitors have evolved as the premier choice of the era for storing huge amounts of charge in the field of energy storage devices, but it is still necessary to enhance their performance to meet the increasing requirements of future systems. This could be achieved either through advancing the interfaces of the material at the nanoscale or by using novel material compositions. We report a high-performance material composition prepared by combining a transition metal (palladium)-doped conductive polymer with multiwalled carbon nanotubes (MWCNTs). MWCNTs/palladium-doped polyaniline (MWCNTs/Pd/PANI) composites and multiwalled carbon nanotube/polyaniline (MWCNTs/PANI) composites (for comparison) were prepared via in situ oxidative polymerization of aniline monomer. The reported composites were characterized by Fourier-transform infrared (FTIR), x-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM) studies. FESEM and TEM studies indicated the narrow size distribution of the π-conjugated polymer-protected palladium nanoparticles on the surface of the carbon nanotubes. All the electrochemical characterizations were executed using a three-electrode system in 1 M H2SO4 electrolyte. Cyclic voltammetry (CV) analysis was performed to observe the capacitive performance and redox behavior of the composites. The ion transfer behavior and cyclic stability of the composites were investigated by electrochemical impedance spectroscopy (EIS) analysis and cyclic charge-discharge (CCD) testing, respectively. The MWCNTs/Pd/PANI composite was found to exhibit an especially high specific capacitance value of 920 F/g at scan rate of 2 mV/s.

Compressive Classification for TEM-EELS

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

Hao, Weituo; Stevens, Andrew; Yang, Hao

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

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

PubMed

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

2012-04-01

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

Structural characterizations of pure SnS and In-doped SnS thin films using isotropic and anisotropic models

NASA Astrophysics Data System (ADS)

Kafashan, Hosein

2018-04-01

An electrochemical route has been employed to prepare pure SnS and indium-doped SnS thin films. Six samples including undoped SnS and In-doped SnS thin films deposited on the fluorine-doped tin oxide (FTO) glass substrates. An aqueous solution having SnCl2 and Na2S2O3 used as the primary electrolyte. Different In-doped SnS samples were prepared by adding a different amount of 1 mM InCl3 solution into the first electrolyte. The applied potential (E), time of deposition (t), pH and bath temperature (T) were kept at ‑1 V, 30 min, 2.1 and 60 °C, respectively. For all samples, except the In-dopant concentration, all the deposition parameters are the same. After preparation, X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) with an energy dispersive X-ray analyzer (EDX) attachment, atomic force microscopy (AFM), and transmission electron microscopy (TEM) were used to determine structural properties of as-deposited films. XRD patterns revealed that the synthesized undoped- and In-doped SnS thin films were crystallized in the orthorhombic structure. The shape of SnS crystals was spherical in the TEM image. X-ray peak broadening studies was done by applying Scherrer’s method, Williamson-Hall (W–H) models (including uniform deformation model (UDM), uniform strain deformation model (UDSM), and uniform deformation energy density model (UDEDM)), and size-strain plot (SSP) method. Using these techniques, the crystallite size and the lattice strains have been predicted. There was a good agreement in the particle size achieved by W–H- and SSP methods with TEM image.

Recognition and Resistance in TEM [superscript beta]-Lactamase

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

Wang, Xiaojun; Minasov, George; Blazquez, Jesus

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

Technical Evaluation Motor no. 5 (TEM-5)

NASA Technical Reports Server (NTRS)

Cook, M.

1990-01-01

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

Structural morphology of zinc oxide structures with antibacterial application of calamine lotion

NASA Astrophysics Data System (ADS)

Ann, Ling Chuo; Mahmud, Shahrom; Bakhori, Siti Khadijah Mohd; Sirelkhatim, Amna; Mohamad, Dasmawati; Hasan, Habsah; Seeni, Azman; Rahman, Rosliza Abdul

2015-04-01

In this study, we report the structural morphology of a zinc oxide (ZnO) sample and antibacterial application of the ZnO structures in calamine lotion. Antibacterial activities of the calamine lotion towards Staphylococcus aureus and Pseudomonas aeruginosa were investigated. The structural morphology of ZnO sample was studied using a transmission electron microscope (TEM) and a field-emission scanning electron microscope (FESEM). The morphologies of the ZnO structure consisted of many rod and spherical structures. The particle sizes of the sample ranged from 40 nm to 150 nm. A calamine lotion was prepared through mixing the ZnO structures with other constituents in suitable proportion. The energy-dispersive x-ray spectroscopy (EDS) revealed the presence of large amount of ZnO structures whiles the X-ray diffraction (XRD) results showed a good crystalline property of ZnO in the calamine lotion mixture. The morphological structures of ZnO were found to remain unchanged in the calamine lotion mixture through FESEM imaging. In the antibacterial test, prepared calamine lotion exhibited a remarkable bacterial inhibition on Staphylococcus aureus and Pseudomonas aeruginosa after 24 h of treatment. The bactericidal capability of calamine lotion was largely due to the presence of ZnO structures which induce high toxicity and killing effect on the bacteria.

Preparation and characterization of potato starch nanocrystal reinforced natural rubber nanocomposites.

PubMed

Rajisha, K R; Maria, H J; Pothan, L A; Ahmad, Zakiah; Thomas, S

2014-06-01

Potato starch nanocrystals were found to serve as an effective reinforcing agent for natural rubber (NR). Starch nanocrystals were obtained by the sulfuric acid hydrolysis of potato starch granules. After mixing the latex and the starch nanocrystals, the resulting aqueous suspension was cast into film by solvent evaporation method. The composite samples were successfully prepared by varying filler loadings, using a colloidal suspension of starch nanocrystals and NR latex. The morphology of the nanocomposite prepared was analyzed by field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). FESEM analysis revealed the size and shape of the crystal and their homogeneous dispersion in the composites. The crystallinity of the nanocomposites was studied using XRD analysis which indicated an overall increase in crystallinity with filler content. The mechanical properties of the nanocomposites such as stress-strain behavior, tensile strength, tensile modulus and elongation at break were measured according to ASTM standards. The tensile strength and modulus of the composites were found to improve tremendously with increasing nanocrystal content. This dramatic increase observed can be attributed to the formation of starch nanocrystal network. This network immobilizes the polymer chains leading to an increase in the modulus and other mechanical properties. Copyright © 2014 Elsevier B.V. All rights reserved.

Low Temperature Synthesis of Cobalt-Chromium Carbide Nanoparticles-Doped Carbon Nanofibers.

PubMed

Yousef, Ayman; Brooks, Robert M; Abutaleb, Ahmed; Al-Deyab, Salem S; El-Newehy, Mohamed H

2018-04-01

Electrospinning has been used to synthesize cobalt-chromium carbide nanoparticles (NPs)-doped carbon nanofibers (CNFs) (Composite). Electrospun mat comprising of cobalt acetate, chromium acetate and poly(vinyl alcohol) (PVA) has been carbonized at low temperature (850 °C) for 3 h under argon atmosphere to produce the introduced composite. The process was achieved at low temperature due to the presence of cobalt as an activator. Field emission scanning electron microscope (FE-SEM), X-ray diffractometry (XRD), and transmission electron microscopy (TEM) equipped with EDX techniques were used to determine the products characteristics. The results indicated the formation of pure cobalt (Co), Cr7C3 NPs and crystalline CNFs. The Co and Cr7C3 NPs were covered with CNFs. Overall, the proposed NFs open new avenue to prepare different metals-metal carbides-carbon NFs at low temperature and short reaction time.

Significantly enhanced photocatalytic activity of visible light responsive AgBr/Bi2Sn2O7 heterostructured composites

NASA Astrophysics Data System (ADS)

Hu, Chaohao; Zhuang, Jing; Zhong, Liansheng; Zhong, Yan; Wang, Dianhui; Zhou, Huaiying

2017-12-01

Heterostructured AgBr/Bi2Sn2O7 photocatalysts were synthesized successfully via the ultrasonic-assisted chemical precipitation method. XRD, FT-IR, FE-SEM, TEM, XPS, UV-vis-DRS and PL spectroscopy were used to characterize the phase structure, morphology, chemical composition, oxidation state, and optical properties of AgBr/Bi2Sn2O7 heterojunction. The photocatalytic activity of as-prepared catalysts was evaluated by the degradation of RhB under visible light irradiation. The obtained AgBr/Bi2Sn2O7 composite with the 1:1 molar ratio exhibited significantly enhanced photocatalytic performance. Further first-principles calculations indicated that the hybridization interaction between Ag and O atoms at AgBr/Bi2Sn2O7 interface is expected to be beneficial for enhancing the charge transfer and improving the photocatalytic activity of heterostructured composites.

Superhydrophilic poly (styrene co acrylonitrile)-ZnO nanocomposite surfaces for UV shielding and self-cleaning applications

NASA Astrophysics Data System (ADS)

Singh, Rajender; Sharma, Ramesh; Barman, P. B.; Sharma, Dheeraj

2017-11-01

UV shielding based super hydrophilic material is developed in the present formulation by in situ emulsion polymerization of poly (styrene-acrylonitrile) with ZnO nanoparticles. The ESI-MS technique confirms the structure of polymer nanocomposite by their mass fragments. The XRD study confirms the presence of ZnO phase in polymer matrix. PSAN/ZnO nanocomposite leads to give effective UV shielding (upto 375 nm) and visible luminescence with ZnO content in polymer matrix. The FESEM and TEM studies confirm the symmetrical, controlled growth of PNs. The incorporation of ZnO nanofillers into PSAN matrix lead to restructuring the PNs surfaces into superhydrophilic surfaces in water contact angle (WCA) from 70° to 10°. We believe our synthesized PSAN/ZnO nanocomposite could be potential as UV shielding, luminescent and super hydrophilic nature based materials in related commercial applications.

Synthesis and high catalytic properties of mesoporous Pt nanowire array by novel conjunct template method

NASA Astrophysics Data System (ADS)

Zhong, Yi; Xu, Cai-Ling; Kong, Ling-Bin; Li, Hu-Lin

2008-12-01

A novel conjunct template method for fabricating mesoporous Pt nanowire array through direct current (DC) electrodeposition of Pt into the pores of anodic aluminum oxide (AAO) template on Ti/Si substrate from hexagonal structured lyotropic liquid crystalline phase is demonstrated in this paper. The morphology and structure of as-prepared Pt nanowire array are characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The electrocatalytic properties of Pt nanowire array for methanol are also investigated in detail. The results indicate that Pt nanowire array has the unique mesoporous structure of approximate 40-50 nm in diameter, which resulted in the high surface area and greatly improved electrocatalytic activity for methanol. The mesoporous Pt nanowire array synthesized by the new conjunct template method has a very promising application in portable fuel cell power sources.

Visible-light-assisted SLCs template synthesis of sea anemone-like Pd/PANI nanocomposites with high electrocatalytic activity for methane oxidation in acidic medium

NASA Astrophysics Data System (ADS)

Tan, De-Xin; Wang, Yan-Li

2018-03-01

Sea anemone-like palladium (Pd)/polyaniline (PANI) nanocomposites were synthesized via visible-light-assisted swollen liquid crystals (SLCs) template method. The resulting samples were characterized by transmission electron microscopy (TEM), selected area electron diffraction (SAED), energy dispersive spectrometer (EDS), x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), ultraviolet-visible (UV–vis) absorption spectroscopy and Fourier transform infrared (FT-IR) spectroscopy, respectively. The electrocatalytic properties of Pd/PANI nanocomposites modified glass carbon electrode (GCE) for methane oxidation were investigated by cycle voltammetry (CV) and chronoamperometry. Those dispersed sea anemone-like Pd/PANI nanocomposites had an average diameter of 320 nm. The obtained Pd nanoparticles with an average diameter of about 45 nm were uniformly distributed in PANI matrix. Sea anemone-like Pd/PANI nanocomposites exhibited excellent electrocatalytic activity and stability for oxidation of methane (CH4).

Strong Flux Pinning of Nano-Sized Ysz Particles in Ybco Films Prepared by Mod Method

NASA Astrophysics Data System (ADS)

Ye, S.; Suo, H. L.; Liu, M.; Tang, X.; Wu, Z. P.; Zhao, Y.; Zhou, M. L.

The YBCO films with doped YSZ nanoparticles have been prepared successfully by metal organic doepositon method using trifluoroacetates (TFA-MOD) through dissolving Zr organic salt into the YBCO precursor solution. The doped films have well in-plane and out-plane textures detected by both XRD Φ-scan and ω-scan. The YSZ nanoparticles with the size of about 5 ~ 15 nm were observed on the surface of the YBCO films using both FE-SEM and TEM. By comparing the superconducting properties, it was found that the doped YBCO films had lower Tc than that of undoped YBCO films. However, as increasing the applied magnetic field, Jc of the doped YBCO films were much better than that of undoped one. The Jc was as higher as 2.5 times than that of undoped YBCO film at 77 K and 1 T applied field.

Manganese porphyrin immobilized on magnetic MCM-41 nanoparticles as an efficient and reusable catalyst for alkene oxidations with sodium periodate

NASA Astrophysics Data System (ADS)

Hajian, Robabeh; Ehsanikhah, Amin

2018-01-01

This study describes the immobilization of tetraphenylporphyrinatomanganese(III) chloride, (MnPor), onto imidazole functionalized MCM-41 with magnetite nanoparticle core (Fe3O4@MCM-41-Im). The resultant material (Fe3O4@MCM-41-Im@MnPor) was characterized by X-ray diffractometry (XRD), Fourier transform infra-red (FT-IR), diffuse reflectance UV-Vis spectrophotometry (DR UV-Vis), field emission scanning electron microscopy (FESEM), Inductively coupled plasma (ICP), analyzer transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) surface area. This new heterogenized catalyst was applied as an efficient catalyst for the epoxidation of a variety of cyclic and linear olefins with NaIO4 under mild conditions. The prepared catalyst can be easily recovered through the application of an external magnet, and reused several times without any significant decrease in activity and magnetic properties.

Synthesis, characterization, and photocatalytic properties of Ni12P5 hollow microspheres

NASA Astrophysics Data System (ADS)

Liu, Shuling; Han, Xiaoli; Zhang, Hongzhe; Liu, Hui

2017-05-01

Ni12P5 hollow microspheres were prepared by a simple mixed cetyltrimethyl ammonium bromide/sodium dodecyl sulfate surfactant-assisted hydrothermal route. The as-prepared Ni12P5 microstructures were characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). It was interesting to find that cetyltrimethyl ammonium bromide/sodium dodecyl sulfate could form a micro-reactor by the mixed micelles in the aqueous solution, which served as a soft template for Ni12P5 hollow microspheres with a diameter of 2 6 μm. Moreover, the as-prepared Ni12P5 hollow microspheres exhibited a good photocatalytic degradation activity for some organic dyes (such as Rhodamine B, Methylene Blue, Pyronine B, and Safranine T), and the degradation ratio could achieve more than 80%.

Green synthesis of the Pd nanoparticles supported on reduced graphene oxide using barberry fruit extract and its application as a recyclable and heterogeneous catalyst for the reduction of nitroarenes.

PubMed

Nasrollahzadeh, Mahmoud; Sajadi, S Mohammad; Rostami-Vartooni, Akbar; Alizadeh, Mohammad; Bagherzadeh, Mojtaba

2016-03-15

Through this manuscript the green synthesis of palladium nanoparticles supported on reduced graphene oxide (Pd NPs/RGO) under the mild conditions through reduction of the graphene oxide and Pd(2+) ions using barberry fruit extract as reducing and stabilizing agent is reported. The as-prepared Pd NPs/RGO was characterized by UV-vis spectroscopy, X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS). The Pd NPs/RGO could be used as an efficient and heterogeneous catalyst for reduction of nitroarenes using sodium borohydride in an environmental friendly medium. Excellent yields of products were obtained with a wide range of substrates and the catalyst was recycled multiple times without any significant loss of its catalytic activity. Copyright © 2015 Elsevier Inc. All rights reserved.

Amorphous V-O-C composite nanofibers electrospun from solution precursors as binder- and conductive additive-free electrodes for supercapacitors with outstanding performance

NASA Astrophysics Data System (ADS)

Chen, Xia; Zhao, Bote; Cai, Yong; Tadé, Moses O.; Shao, Zongping

2013-11-01

Flexible V-O-C composite nanofibers were fabricated from solution precursors via electrospinning and were investigated as free-standing and additive-free film electrodes for supercapacitors. Specifically, composite nanofibers (V0, V5, V10 and V20) with different vanadyl acetylacetonate (VO(acac)2) contents of 0, 5, 10 and 20 wt% with respect to polyacrylonitrile (PAN) were prepared. The composite nanofibers were comparatively studied using XRD, Raman spectroscopy, XPS, N2 adsorption-desorption, FE-SEM, TEM and S-TEM. The vanadium element was found to be well-dispersed in the carbon nanofibers, free from the formation of an aggregated crystalline phase, even in the case of V20. A specific surface area of 587.9 m2 g-1 was reached for V10 after calcination, which is approximately twice that of the vanadium-free carbon nanofibers (V0, 300.9 m2 g-1). To perform as an electrode for supercapacitors in an aqueous electrolyte, the V10 film delivered a specific capacitance of 463 F g-1 at 1 A g-1. V10 was also able to retain a specific capacitance of 380 F g-1, even at a current density of 10 A g-1. Additionally, very stable cycling stability was achieved, maintaining an outstanding specific capacitance of 400 F g-1 at 5 A g-1 after charge-discharge cycling 5000 times. Thus, V-O-C composite nanofibers are highly attractive electrode materials for flexible, high-power, thin film energy storage devices and applications.Flexible V-O-C composite nanofibers were fabricated from solution precursors via electrospinning and were investigated as free-standing and additive-free film electrodes for supercapacitors. Specifically, composite nanofibers (V0, V5, V10 and V20) with different vanadyl acetylacetonate (VO(acac)2) contents of 0, 5, 10 and 20 wt% with respect to polyacrylonitrile (PAN) were prepared. The composite nanofibers were comparatively studied using XRD, Raman spectroscopy, XPS, N2 adsorption-desorption, FE-SEM, TEM and S-TEM. The vanadium element was found to be well

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

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

TEM Derivative-Producing Enterobacter aerogenes Strains: Dissemination of a Prevalent Clone

PubMed Central

Dumarche, P.; De Champs, C.; Sirot, D.; Chanal, C.; Bonnet, R.; Sirot, J.

2002-01-01

TEM-24 (CAZ-6) extended-spectrum β-lactamase (ESBL) was detected in 1988 in Clermont-Ferrand, France, in Klebsiella pneumoniae (blaTEM-24) and Enterobacter aerogenes (blaTEM-24b), and since 1994, a TEM-24-producing E. aerogenes clonal strain has been observed elsewhere in the country. To determine if the spread of this clonal strain was restricted to TEM-24-producing E. aerogenes strains, 84 E. aerogenes strains (non-TEM/SHV-producing strains, TEM-1- or -2-producing strains, and different ESBL-producing strains), isolated from 1988 to 1999 in Clermont-Ferrand (n = 59) and in 11 other French hospitals in 1998 (n = 25), were studied. A clonal strain was found for TEM-24- but also for TEM-3- and TEM-1- or 2-producing isolates. This study shows that there is a clonal strain dependent on acquisition of the TEM-type enzyme (TEM-24 and other TEM types). PMID:11897606

TEM PSHA2015 Reliability Assessment

NASA Astrophysics Data System (ADS)

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

2016-12-01

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

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

PubMed

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

2011-01-01

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

Comparative electrochemical analysis of crystalline and amorphous anodized iron oxide nanotube layers as negative electrode for LIB.

PubMed

Pervez, Syed Atif; Kim, Doohun; Farooq, Umer; Yaqub, Adnan; Choi, Jung-Hee; Lee, You-Jin; Doh, Chil-Hoon

2014-07-23

This work is a comparative study of the electrochemical performance of crystalline and amorphous anodic iron oxide nanotube layers. These nanotube layers were grown directly on top of an iron current collector with a vertical orientation via a simple one-step synthesis. The crystalline structures were obtained by heat treating the as-prepared (amorphous) iron oxide nanotube layers in ambient air environment. A detailed morphological and compositional characterization of the resultant materials was performed via transmission electron microscopy (TEM), field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), and Raman spectroscopy. The XRD patterns were further analyzed using Rietveld refinements to gain in-depth information on their quantitative phase and crystal structures after heat treatment. The results demonstrated that the crystalline iron oxide nanotube layers exhibit better electrochemical properties than the amorphous iron oxide nanotube layers when evaluated in terms of the areal capacity, rate capability, and cycling performance. Such an improved electrochemical response was attributed to the morphology and three-dimensional framework of the crystalline nanotube layers offering short, multidirectional transport lengths, which favor rapid Li(+) ions diffusivity and electron transport.

Influence of the synthesis parameters on the properties of amidoxime grafted sepiolite nanocomposites

NASA Astrophysics Data System (ADS)

Taimur, Shaista; Yasin, Tariq

2017-11-01

Novel polyacrylonitrile (PAN) grafted sepiolite nanocomposites were synthesized via emulsion polymerization. The influence of synthesis parameters on the degree of grafting was studied by varying the concentrations of monomer, initiator and surfactant. The nitrile groups of PAN were chemically modified into amidoxime. Both the grafting and amidoxime percentages were determined gravimetrically and maximum grafting of 373% was achieved at 5% acrylonitrile, 1% surfactant and 0.1% initiator concentrations. The presence of vibration at 2242 cm-1 in Fourier transform infrared (FT-IR) spectrum and x-ray diffraction (XRD) reflection at 2θ = 16.9° (010) confirmed the grafting of PAN chains onto modified sepiolite. XRD patterns also indicated a decrease in crystallinity of sepiolite and appearance of new amorphous region in grafted nanocomposites. The morphological changes of sepiolite during silanization and grafting of PAN is also confirmed by field emission scanning electron microscope (FESEM). Transmission electron microscope (TEM) images clearly showed the shortening of fibers after silanization of sepiolite and the same were involved in heterogeneous nucleation in micelles. These developed amidoxime grafted sepiolite nanocomposites can be used as adsorbent for the metal recovery.

In situ TEM of radiation effects in complex ceramics.

PubMed

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

2009-03-01

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

Synthesis of Gd2O3:Eu nanoplatelets for MRI and fluorescence imaging

NASA Astrophysics Data System (ADS)

Maalej, Nabil M.; Qurashi, Ahsanulhaq; Assadi, Achraf Amir; Maalej, Ramzi; Shaikh, Mohammed Nasiruzzaman; Ilyas, Muhammad; Gondal, Mohammad A.

2015-05-01

We synthesized Gd2O3 and Gd2O3 doped by europium (Eu) (2% to 10%) nanoplatelets using the polyol chemical method. The synthesized nanoplatelets were characterized by X-ray diffraction (XRD), FESEM, TEM, and EDX techniques. The optical properties of the synthesized nanoplatelets were investigated by photoluminescence spectroscopy. We also studied the magnetic resonance imaging (MRI) contrast enhancement of T1 relaxivity using 3 T MRI. The XRD for Gd2O3 revealed a cubic crystalline structure. The XRD of Gd2O3:Eu3+ nanoplatelets were highly consistent with Gd2O3 indicating the total incorporation of the Eu3+ ions in the Gd2O3 matrix. The Eu doping of Gd2O3 produced red luminescence around 612 nm corresponding to the radiative transitions from the Eu-excited state 5D0 to the 7F2. The photoluminescence was maximal at 5% Eu doping concentration. The stimulated CIE chromaticity coordinates were also calculated. Judd-Ofelt analysis was used to obtain the radiative properties of the sample from the emission spectra. The MRI contrast enhancement due to Gd2O3 was compared to DOTAREM commercial contrast agent at similar concentration of gadolinium oxide and provided similar contrast enhancement. The incorporation of Eu, however, decreased the MRI contrast due to replacement of gadolinium by Eu.

Synthesis of Gd2O3:Eu nanoplatelets for MRI and fluorescence imaging.

PubMed

Maalej, Nabil M; Qurashi, Ahsanulhaq; Assadi, Achraf Amir; Maalej, Ramzi; Shaikh, Mohammed Nasiruzzaman; Ilyas, Muhammad; Gondal, Mohammad A

2015-01-01

We synthesized Gd2O3 and Gd2O3 doped by europium (Eu) (2% to 10%) nanoplatelets using the polyol chemical method. The synthesized nanoplatelets were characterized by X-ray diffraction (XRD), FESEM, TEM, and EDX techniques. The optical properties of the synthesized nanoplatelets were investigated by photoluminescence spectroscopy. We also studied the magnetic resonance imaging (MRI) contrast enhancement of T1 relaxivity using 3 T MRI. The XRD for Gd2O3 revealed a cubic crystalline structure. The XRD of Gd2O3:Eu(3+) nanoplatelets were highly consistent with Gd2O3 indicating the total incorporation of the Eu(3+) ions in the Gd2O3 matrix. The Eu doping of Gd2O3 produced red luminescence around 612 nm corresponding to the radiative transitions from the Eu-excited state (5)D0 to the (7)F2. The photoluminescence was maximal at 5% Eu doping concentration. The stimulated CIE chromaticity coordinates were also calculated. Judd-Ofelt analysis was used to obtain the radiative properties of the sample from the emission spectra. The MRI contrast enhancement due to Gd2O3 was compared to DOTAREM commercial contrast agent at similar concentration of gadolinium oxide and provided similar contrast enhancement. The incorporation of Eu, however, decreased the MRI contrast due to replacement of gadolinium by Eu.

TEM-nanoindentation studies of semiconducting structures.

PubMed

Le Bourhis, E; Patriarche, G

2007-01-01

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

Microwave-assisted hydrothermal synthesis of biocompatible silver sulfide nanoworms

NASA Astrophysics Data System (ADS)

Xing, Ruimin; Liu, Shanhu; Tian, Shufang

2011-10-01

In this study, silver sulfide nanoworms were prepared via a rapid microwave-assisted hydrothermal method by reacting silver nitrate and thioacetamide in the aqueous solution of the Bovine Serum Albumin (BSA) protein. The morphology, composition, and crystallinity of the nanoworms were characterized by field emission scanning electron microscopy (FESEM), X-ray powder diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), X-ray energy dispersive spectroscopy (EDS), and Fourier transform infrared (FTIR) spectroscopy. The results show that the nanoworms were assembled by multiple adjacent Ag2S nanoparticles and stabilized by a layer of BSA attached to their surface. The nanoworms have the sizes of about 50 nm in diameter and hundreds of nanometers in length. The analyses of high-resolution TEM and their correlative Fast Fourier Transform (FFT) indicate that the adjacent Ag2S nanoparticles grow by misoriented attachment at the connective interfaces to form the nanoworm structure. In vitro assays on the human cervical cancer cell line HeLa show that the nanoworms exhibit good biocompatibility due to the presence of BSA coating. This combination of features makes the nanoworms attractive and promising building blocks for advanced materials and devices.

Synthesis and characterization of nanocomposite GO@α-Fe2O3:Efficient material for dye removal

NASA Astrophysics Data System (ADS)

Mandal, B.; Panda, J.; Tudu, B.

2018-05-01

In this work a composite of Graphene Oxide (GO) supported α-Fe2O3 nanoparticles (GF) has been synthesized via a simple co-precipitation method. Structural, and morphological study of nanocomposite (GF) are examined by powder X-ray diffraction (PXRD), field emission scanning electron microscopy (FESEM) and Transmission electron microscopy (TEM). The XRD study indicates that Graphene oxide is implanted with well crystalline α-Fe2O3 which has pure rhombohedral phase. Surface morphological study of SEM depicts sphere-like shaped α-Fe2O3 particles with formation of clusters have been embedded on Graphene oxide nano sheet. TEM image reveals that GO sheet acts as a good supporting material for anchoring nano sized α -Fe2O3 particles. Efficiency of dye removal of the prepared GF composite has been measured by the degradation of methylene blue (MB) in an aqueous solution under visible light irradiation. The degradation of the dye has been evaluated by a UV-visible spectroscopy, by decrease in the intensity of absorbance and concentration. The degradation efficiency of GF is found to be 90% towards MB.

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

NASA Astrophysics Data System (ADS)

Jernsletten, J. A.

2005-05-01

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

Dynamic XRD, Shock and Static Compression of CaF2

NASA Astrophysics Data System (ADS)

Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew; Smith, Jesse; Sinogeikin, Stanislav

2017-06-01

The high-pressure behavior of CaF2 is probed with x-ray diffraction (XRD) combined with both dynamic compression, using a two-stage light gas gun, and static compression, using diamond anvil cells. We use XRD to follow the unfolding of a shock-driven, fluorite to cotunnite phase transition, on the timescale of nanoseconds. The dynamic behavior of CaF2 under shock loading is contrasted with that under static compression. This work leverages experimental capabilities at the Advanced Photon Source: dynamic XRD and shock experiments at the Dynamic Compression Sector, as well as XRD and static compression in diamond anvil cell at the High-Pressure Collaborative Access Team. These experiments and cross-platform comparisons, open the door to an unprecedented understanding of equations of state and phase transitions at the microstructural level and at different time scales and will ultimately improve our capability to simulate the behavior of materials at extreme conditions. Sandia National Laboratories is a multi-mission laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

Preparation, photoluminescent properties and luminescent dynamics of BaAlF{sub 5}:Eu{sup 2+} nanophosphors

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

Zhang, Wei; College of Life Science, Dalian Nationalities University, Dalian, Liaoning 116600; Hua, Ruinian, E-mail: rnhua@dlnu.edu.cn

2014-12-15

Graphical abstract: Rice-shaped BaAlF{sub 5}:Eu{sup 2+} nanophosphors were synthesized via one-pot hydrothermal process. The as-prepared BaAlF{sub 5}:Eu{sup 2+} are composed of many particles with an average diameter of 40 nm. When excited at 260 nm, the sharp line emission located at 361 nm of Eu{sup 2+} was observed. The optimum doping concentration of Eu{sup 2+} was confirmed to be 5 mol%. The strong ultraviolet emission of Eu{sup 2+} ions in BaAlF{sub 5}:Eu{sup 2+} nanoparticles suggests that these nanoparticles may have potential applications for sensing, solid-state lasers and spectrometer calibration. - Highlights: • BaAlF{sub 5}:Eu{sup 2+} nanophosphors were synthesized via amore » mild hydrothermal process. • The Van and Huang models were used to research the mechanism of concentration quenching. • The optimum doping concentration of Eu2+ was confirmed to be 5 mol%. - Abstract: Eu{sup 2+}-doped BaAlF{sub 5} nanophosphors were synthesized via a facile one-pot hydrothermal method. The final products were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and photoluminescence (PL) spectroscopy. XRD results showed that the prepared samples are single-phase. The FE-SEM and TEM images indicated that the prepared BaAlF{sub 5}:Eu{sup 2+} nanophosphors are composed of many rice-shaped particles with an average diameter of 40 nm. When excited at 260 nm, BaAlF{sub 5}:Eu{sup 2+} nanophosphors exhibit the sharp line emissions of Eu{sup 2+} at room temperature. The optimum doping concentration of Eu{sup 2+} was confirmed to be 5 mol%. The Van and Huang models were used to study the mechanism of concentration quenching and the electric dipole–dipole interaction between Eu{sup 2+} can be deduced to be a dominant for quenching fluorescence in BaAlF{sub 5}:Eu{sup 2+} nanophosphors. The strong ultraviolet emission of Eu{sup 2+} in BaAlF{sub 5}:Eu{sup 2+} nanophosphors suggests

High Rate Deposition of Thick CrN and Cr2N Coatings Using Modulated Pulse Power (MPP) Magnetron Sputtering

DTIC Science & Technology

2010-12-01

in the conventional Bragg-Bentano mode. The residual stress of the coatings was measured by glancing incident angle XRD (GIXRD) in the same X - ray ...micro-analysis (EPMA), x - ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), nanoindentation, scratch test, and ball-on...the coatings was determined by XRD using a SIEMENS X - ray diffractometer (Model KRISTALLOFLEX-810) operated with K-alpha Cu radiation (30 kV and 20 mA

Bio-derived hierarchically macro-meso-micro porous carbon anode for lithium/sodium ion batteries

NASA Astrophysics Data System (ADS)

Elizabeth, Indu; Singh, Bhanu Pratap; Trikha, Sunil; Gopukumar, Sukumaran

2016-10-01

Nitrogen doped hierarchically porous carbon derived from prawn shells have been efficiently synthesized through a simple, economically viable and environmentally benign approach. The prawn shell derived carbon (PSC) has high inherent nitrogen content (5.3%) and possesses a unique porous structure with the co-existence of macro, meso and micropores which can afford facile storage and transport channels for both Li and Na ions. PSC is well characterized using X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Transmission electron Microscopy (TEM), High resolution TEM (HR-TEM) and X-ray photoelectron spectroscopy (XPS). Electron Paramagnetic Resonance (EPR) and Solid state-Nuclear Magnetic Resonance (NMR) studies have been conducted on pristine PSC and Li/Na interacted PSC. PSC as anode for Lithium ion batteries (LIBs) delivers superior electrochemical reversible specific capacity (740 mAh g-1 at 0.1 Ag-1 current density for 150 cycles) and high rate capability. When used as anode material for Sodium ion batteries (SIBs), PSC exhibits excellent reversible specific capacity of 325 mAh g-1 at 0.1 Ag-1 for 200 cycles and rate capability of 107 mAh g-1 at 2 Ag-1. Furthermore, this study demonstrates the employment of natural waste material as a potential anode for both LIB and SIB, which will definitively make a strike in the energy storage field.

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

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

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

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

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

DOE PAGES

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

2016-07-25

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

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

Biosynthesis of ZnO nanoparticles using rambutan (Nephelium lappaceumL.) peel extract and their photocatalytic activity on methyl orange dye

NASA Astrophysics Data System (ADS)

Karnan, Thenmozhi; Selvakumar, Stanly Arul Samuel

2016-12-01

In the present study, describes the synthesis of ZnO nanoparticles from rambutan (Nephelium lappaceumL.) peel extract via bio synthesis method and developed a new low cost technology to prepare ZnO nanoparticles. During the synthesis, fruit peel extract act as a natural ligation agent. The successfully prepared product was analyzed with some standard characterization studies like X-Ray Diffraction (XRD), UV-VIS Diffuse reflectance spectra (UV-Vis DRS), Field Emission Scanning Electron Microscope (FESEM), High resolution transmittance electron microscope (HR-TEM), N2 adsorption-desorption isotherm and UV-Vis absorption Spectroscopy. The photocatalytic activity of ZnO nanoparticles was evaluated by photodegradation of methyl orange (MO) dye under UV light and the result depicts around 83.99% decolorisation efficiency at 120 min of illumination. In addition with photodecolorisation, mineralization was also achieved. The mineralization has been confirmed by measuring Chemical Oxygen Demand (COD) values.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Enhanced visible-light-driven photocatalytic H2-production activity of CdS-loaded TiO2 microspheres with exposed (001) facets

NASA Astrophysics Data System (ADS)

Gao, Bifen; Yuan, Xia; Lu, Penghui; Lin, Bizhou; Chen, Yilin

2015-12-01

CdS-loaded TiO2 microspheres with highly exposed (001) facets were prepared by hydrothermal treatment of a TiF4-HCl-H2O mixed solution followed by a chemical bath deposition of CdS onto TiO2 microspheres. The crystal structure, surficial micro-structure and photo-absorption property of the samples were characterized by XRD, FE-SEM, TEM and UV-vis diffuse reflectance spectroscopy, etc. The as-prepared samples exhibited superior visible-light-driven photocatalytic H2-production activity from lactic acid aqueous solution in comparison with CdS-sensitized TiO2 nanoparticles, whose surface was dominated by (101) facets. Photoelectrochemical measurement confirmed that (001) facet is beneficial for the transfer of photo-generated electron from CdS to TiO2 microsphere, which led to the unexpected high photocatalytic activity of CdS-loaded TiO2 microspheres.

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

NASA Astrophysics Data System (ADS)

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

2010-10-01

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

Investigation of optical properties and the photocatalytic activity of synthesized YbYO4 nanoparticles and YbVO4/NiWO4 nanocomposites by polymeric capping agents

NASA Astrophysics Data System (ADS)

Pourmasoud, Saeid; Sobhani-Nasab, Ali; Behpour, Mohsen; Rahimi-Nasrabadi, Mehdi; Ahmadi, Farhad

2018-04-01

YbVO4 nanoparticles YbVO4/NiWO4 nanocomposites were synthesized by simple and new method. The effect of various polymeric capping agents such as Tween 80, Tween 20 and PEG on the shape and size of YbVO4/NiWO4 nanocomposites were investigated. YbVO4/NiWO4 nanocomposites were analyzed through some techniques including, X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectroscopy, vibrating sample magnetometer (VSM), thermogravimetry differential thermal analysis (TG-DTA), transmission electron microscopy (TEM), field emission electron microscopy (FESEM), ultraviolet-visible spectroscopy (UV-Vis), and energy-dispersive X-ray spectroscopy (EDX). This attempt is the first study on the photocatalytic performance of the YbVO4/NiWO4 nanocomposites in various conditions such as size of particles and kind of dyes (rhodamine B (Rh B), methylene blue (MB), methyl orange (MO), and phenol red (Ph R)), under visible light.

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

NASA Astrophysics Data System (ADS)

Saberi, Maliheh; Ashkarran, Ali Akbar

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

Facile synthesis of Ni/NiO@GO nanocomposites and its enhanced dielectric constant

NASA Astrophysics Data System (ADS)

Sarkar, S.; Giri, N.; Mondal, A.; Ray, R.

2018-05-01

Ni/NiO embedded Graphene Oxide (GO): Ni/NiO@GO is synthesized by citric acid assisted Pechini-type method. Structural and morphological characterizations are performed by X-ray powdered diffraction (XRD), field emission scanning electron microscopy (FESEM) and tunneling electron microscopy (TEM). Defects in GO sheets are probed by RAMAN spectroscopy. The temperature variation of dielectric constant (ɛR) and dielectric loss (tan δ) are investigated in the temperature range 300 - 400 K. Decoration of GO with Ni/NiO nanoparticles enhances its ɛR by˜55 times. Moreover, its dielectric constant measured at 5 MHz is found to be˜430 times to that of Ni/NiO along with the reduction of dielectric loss by a factor˜0.5. The enhanced dielectric constant makes the composite Ni/NiO@GO a potential candidate for using in ecologically friendly energy storage devices.

Achillea millefolium L. extract mediated green synthesis of waste peach kernel shell supported silver nanoparticles: Application of the nanoparticles for catalytic reduction of a variety of dyes in water.

PubMed

Khodadadi, Bahar; Bordbar, Maryam; Nasrollahzadeh, Mahmoud

2017-05-01

In this paper, silver nanoparticles (Ag NPs) are synthesized using Achillea millefolium L. extract as reducing and stabilizing agents and peach kernel shell as an environmentally benign support. FT-IR spectroscopy, UV-Vis spectroscopy, X-ray Diffraction (XRD), Field emission scanning electron microscopy (FESEM), Energy Dispersive X-ray Spectroscopy (EDS), Thermo gravimetric-differential thermal analysis (TG-DTA) and Transmission Electron Microscopy (TEM) were used to characterize peach kernel shell, Ag NPs, and Ag NPs/peach kernel shell. The catalytic activity of the Ag NPs/peach kernel shell was investigated for the reduction of 4-nitrophenol (4-NP), Methyl Orange (MO), and Methylene Blue (MB) at room temperature. Ag NPs/peach kernel shell was found to be a highly active catalyst. In addition, Ag NPs/peach kernel shell can be recovered and reused several times with no significant loss of its catalytic activity. Copyright © 2017 Elsevier Inc. All rights reserved.

Facile synthesis of ZnFe2O4 photocatalysts for decolourization of organic dyes under solar irradiation

PubMed Central

Behera, Arjun; Kandi, Debasmita; Majhi, Sanjit Manohar

2018-01-01

ZnFe2O4 was fabricated by a simple solution-combustion method. The structural, optical and electronic properties are investigated by XRD, TEM, FESEM, UV–vis DRS, PL, FTIR and photocurrent measurements. The photocatalytic activity of the prepared material is studied with regard to the degradation of rhodamine B (Rh B) and Congo red under solar irradiation. The kinetic study showed that the material exhibits zeroth and first order reaction kinetics for the degradation of Rh B and Congo red, respectively. The photocatalytic behaviour of ZnFe2O4 was systematically studied as a function of the activation temperature. ZnFe2O4 prepared at 500 °C showed the highest activity in degrading Rh B and Congo red. The highest activity of ZnFe2O4-500 °C correlates well with the lowest PL intensity, highest photocurrent and lowest particle size. PMID:29515956

High Coke-Resistance Pt/Mg1-xNixO Catalyst for Dry Reforming of Methane

PubMed Central

Al-Doghachi, Faris A. J.; Islam, Aminul; Zainal, Zulkarnain; Saiman, Mohd Izham; Embong, Zaidi; Taufiq-Yap, Yun Hin

2016-01-01

A highly active and stable nano structured Pt/Mg1-xNixO catalysts was developed by a simple co-precipitation method. The obtained Pt/Mg1-xNixO catalyst exhibited cubic structure nanocatalyst with a size of 50–80 nm and realized CH4 and CO2 conversions as high as 98% at 900°C with excellent stability in the dry reforming of methane. The characterization of catalyst was performed using various kinds of analytical techniques including XRD, BET, XRF, TPR-H2, TGA, TEM, FESEM, FT-IR, and XPS analyses. Characterization of spent catalyst further confirms that Pt/Mg1-xNixO catalyst has high coke-resistance for dry reforming. Thus, the catalyst demonstrated in this study, offers a promising catalyst for resolving the dilemma between dispersion and reducibility of supported metal, as well as activity and stability during high temperature reactions. PMID:26745623

Technical Evaluation Motor No. 7 (TEM-07)

NASA Technical Reports Server (NTRS)

Hugh, Phil

1991-01-01

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

Preparation of carbon-free TEM microgrids by metal sputtering.

PubMed

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

2009-08-01

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

ToTem: a tool for variant calling pipeline optimization.

PubMed

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

2018-06-26

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

Synthesis, characterization and antibacterial activity of hybrid chitosan-cerium oxide nanoparticles: As a bionanomaterials.

PubMed

Senthilkumar, R P; Bhuvaneshwari, V; Ranjithkumar, R; Sathiyavimal, S; Malayaman, V; Chandarshekar, B

2017-11-01

The hybrid chitosan cerium oxide nanoparticles were prepared for the first time by green chemistry approach using plant leaf extract. The intense peak observed around 292nm in the UV-vis spectrum indicate the formation of cerium oxide nanoparticles. The XRD pattern revealed that the hybrid chitosan-cerium oxide nanoparticles have a polycrystalline structure with cubic fluorite phase. The FTIR spectrum of prepared samples showed the formation of Ce-O bonds and chitosan main chains COC and CO. The FESEM image of hybrid chitosan cerium oxide nanoparticles revealed that the particles are spherical in shape with grains size varying from 23.12nm to 89.91nm. EDAX analysis confirmed the presence of Ce, O, C and N elements in the prepared sample. TEM images showed that the prepared hybrid chitosan-cerium oxide nanoparticles are predominantly uniform in size and most of the particles are spherical in shape with less agglomeration and the particles size varies from 3.61nm to 24.40nm. The prepared chitosan cerium oxide nanoparticles of 50μL concentration showed good antibacterial properties against test pathogens, which was confirmed by the FESEM analysis. The prepared small particle size facilitate that these hybrid ChiCO 2 NPs could effectively be used in biomedical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Structural morphology of zinc oxide structures with antibacterial application of calamine lotion

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

Ann, Ling Chuo; Mahmud, Shahrom; Bakhori, Siti Khadijah Mohd

In this study, we report the structural morphology of a zinc oxide (ZnO) sample and antibacterial application of the ZnO structures in calamine lotion. Antibacterial activities of the calamine lotion towards Staphylococcus aureus and Pseudomonas aeruginosa were investigated. The structural morphology of ZnO sample was studied using a transmission electron microscope (TEM) and a field-emission scanning electron microscope (FESEM). The morphologies of the ZnO structure consisted of many rod and spherical structures. The particle sizes of the sample ranged from 40 nm to 150 nm. A calamine lotion was prepared through mixing the ZnO structures with other constituents in suitable proportion. Themore » energy-dispersive x-ray spectroscopy (EDS) revealed the presence of large amount of ZnO structures whiles the X-ray diffraction (XRD) results showed a good crystalline property of ZnO in the calamine lotion mixture. The morphological structures of ZnO were found to remain unchanged in the calamine lotion mixture through FESEM imaging. In the antibacterial test, prepared calamine lotion exhibited a remarkable bacterial inhibition on Staphylococcus aureus and Pseudomonas aeruginosa after 24 h of treatment. The bactericidal capability of calamine lotion was largely due to the presence of ZnO structures which induce high toxicity and killing effect on the bacteria.« less

Physicochemical characterization of cellulose nanocrystal and nanoporous self-assembled CNC membrane derived from Ceiba pentandra.

PubMed

Mohamed, Mohamad Azuwa; W Salleh, W N; Jaafar, Juhana; Ismail, A F; Abd Mutalib, Muhazri; Mohamad, Abu Bakar; M Zain, M F; Awang, Nor Asikin; Mohd Hir, Zul Adlan

2017-02-10

This research involves the rare utilisation of the kapok fibre (Ceiba pentandra) as a raw material for the fabrication of cellulose nanocrystal (CNC) and self-assembled CNC membranes. The isolation of CNC from Ceiba pentandra began with the extraction of cellulose via the chemical alkali extraction by using 5wt% NaOH, followed by the typical acidified bleaching method and, finally, the CNC production through acid hydrolysis with 60wt% H 2 SO 4 at the optimum time of 60min. The prepared CNC was then employed for the preparation of self-assembled membrane through the water suspension casting evaporation technique. The obtained CNC membrane was characterised in terms of its composition, crystallinity, thermal stability, as well as, structural and morphological features with the use of several techniques including FTIR, XRD, AFM, TEM, FESEM, and TGA. The FESEM and AFM analyses had illustrated the achievement of a self-assembled CNC membrane with a smooth surface and a well-distributed nano-porous structure, with the porosity of 52.82±7.79%. In addition, the findings proved that the self-assembled CNC membrane displayed good adsorption capability indicated by the recorded efficiency of 79% and 85% for 10mg/L and 5mg/L of methylene blue in an aqueous solution, respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

Production of electrospun polyvinyl alcohol/microbial synthesized silver nanoparticles scaffold for the treatment of fungating wounds

NASA Astrophysics Data System (ADS)

Yahyaei, Behrooz; Manafi, Sahebali; Fahimi, Bijan; Arabzadeh, Sepideh; Pourali, Parastoo

2018-03-01

Fungating wounds usually develop in patients with advanced cancer, which responds poorly to treatments. Such wounds can be treated using suitable dressings. For this purpose, a recent research produced a new type of wound dressing with antibacterial and anticancer properties. The culture supernatant of Fusarium oxysporum was challenged with silver nitrate and heated for 5 min. Production of silver nanoparticles (SNPs) was confirmed using spectrophotometer, transmission electron microscopy (TEM), and X-ray diffraction (XRD) analysis. A solution of 10% (w/w) poly vinyl alcohol (PVA) and different volumes of SNP solutions were provided, where each solution was separately used for electrospinning. The obtained PVA/SNPs film evaluated under morphological characterization using field emission scanning electron microscope (FE-SEM) and its antibacterial and anticancer activities were measured. Results confirmed the presence of SNPs in the reaction mixture with sizes less than 50 nm, spherical and oval in shapes. FE-SEM results confirmed that SNPs were seen inside and entrapped between PVA in the PVA/SNPs membrane, composed of 50% of each material. This film had acceptable antibacterial properties against four different bacterial strains and a good anticancer activity against the human melanoma cell line (COLO 792) in contrast to the control one. A recent research introduced a new and fast biological method for the synthesis of SNPs, having acceptable antibacterial and anticancer activities. Further studies are needed to support the obtained results.

Retrofit implementation of Zernike phase plate imaging for cryo-TEM

PubMed Central

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

2011-01-01

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

Design of a TEM cell EMP simulator

NASA Astrophysics Data System (ADS)

Sevat, Pete

1991-06-01

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

Evaluation of structural, morphological and magnetic properties of CuZnNi (CuxZn0.5-xNi0.5Fe2O4) nanocrystalline ferrites for core, switching and MLCI's applications

NASA Astrophysics Data System (ADS)

Akhtar, Majid Niaz; Khan, Muhammad Azhar; Ahmad, Mukhtar; Nazir, M. S.; Imran, M.; Ali, A.; Sattar, A.; Murtaza, G.

2017-01-01

The influence of Cu substitution on the structural and morphological characteristics of Ni-Zn nanocrystalline ferrites have been discussed in this work. The detailed and systematic magnetic characterizations were also done for Cu substituted Ni-Zn nanoferrites. The nanocrystalline ferrites of Cu substituted CuxZn0.5-xNi0.5Fe2O4 ferrites (x=0, 0.1, 0.2, 0.3, 0.4 and 0.5) were synthesized using sol gel self-combustion hybrid method. X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Transmission electron microscope (TEM) and Vibrating sample magnetometer (VSM) were used to investigate the properties of Cu substituted nanocrystalline ferrites. Single phase structure of Cu substituted in Ni-Zn nanocrystalline ferrites were investigated for all the samples. Crystallite size, lattice constant and volume of the cell were found to increase by increasing Cu contents in spinel structure. The better morphology with well-organized nanocrystals of Cu-Zn-Ni ferrites at x=0 and 0.5 were observed from both FESEM and TEM analysis. The average grain size was 35-46 nm for all prepared nanocrystalline samples. Magnetic properties such as coercivity, saturation, remanence, magnetic squareness, magneto crystalline anisotropy constant (K) and Bohr magneton were measured from the recorded M-H loops. The magnetic saturation and remanence were increased by the incorporation of Cu contents. However, coercivity follow the Stoner-Wolforth model except for x=0.3 which may be due to the site occupancy and replacement of Cu contents from octahedral site. The squareness ratio confirmed the super paramgnetic behaviour of the Cu substituted in Ni-Zn nanocrystalline ferrites. Furthermore, Cu substituted Ni-Zn nanocrystalline ferrites may be suitable for many industrial and domestic applications such as components of transformers, core, switching, and MLCI's due to variety of the soft magnetic characteristics.

Preparation, characterization, physical properties, and photoconducting behaviour of anthracene derivative nanowires

NASA Astrophysics Data System (ADS)

Xiao, Jinchong; Yin, Zongyou; Yang, Bo; Liu, Yi; Ji, Li; Guo, Jun; Huang, Ling; Liu, Xuewei; Yan, Qingyu; Zhang, Hua; Zhang, Qichun

2011-11-01

Organic nanowires of 9,10-dibromoanthracene (DBA) and 9,10-dicyanoanthracene (DCNA) were obtained by adding the THF solution of DBA/DCNA into water containing P123 surfactants. The as-prepared nanowires were characterized by UV-vis, fluorescence spectra, Field Emission Scanning Electron Microscopy (FESEM), and Transmission Electron Microscopy (TEM). We found that DBA and DCNA nanowires emitted green light rather than blue light for molecules in THF solution. The red-shift UV and fluorescent spectra of DBA and DCNA nanowires implied that these nanowires were formed through J-aggregation. The photoconducting study of DBA/DCNA nanowire-based network on rGO/SiO2/Si shows different photocurrent behaviors upon irradiation, which displayed that electron transfer from DCNA nanowire to rGO was stronger than that of DBA nanowires to rGO.Organic nanowires of 9,10-dibromoanthracene (DBA) and 9,10-dicyanoanthracene (DCNA) were obtained by adding the THF solution of DBA/DCNA into water containing P123 surfactants. The as-prepared nanowires were characterized by UV-vis, fluorescence spectra, Field Emission Scanning Electron Microscopy (FESEM), and Transmission Electron Microscopy (TEM). We found that DBA and DCNA nanowires emitted green light rather than blue light for molecules in THF solution. The red-shift UV and fluorescent spectra of DBA and DCNA nanowires implied that these nanowires were formed through J-aggregation. The photoconducting study of DBA/DCNA nanowire-based network on rGO/SiO2/Si shows different photocurrent behaviors upon irradiation, which displayed that electron transfer from DCNA nanowire to rGO was stronger than that of DBA nanowires to rGO. Electronic supplementary information (ESI) available: XRD patterns and simulations, and FT-IR spectra. CCDC reference numbers 840471. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c1nr10655d

Retrofit implementation of Zernike phase plate imaging for cryo-TEM.

PubMed

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

2011-05-01

In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. Copyright © 2011 Elsevier Inc. All rights reserved.

Effects of nano-YAG (Y 3Al 5O 12) crystallization on the structure and photoluminescence properties of Nd 3+-doped K 2O-SiO 2-Y 2O 3-Al 2O 3 glasses

NASA Astrophysics Data System (ADS)

Tarafder, Anal; Molla, Atiar Rahaman; Karmakar, Basudeb

2010-10-01

Nd 3+-doped precursor glass in the K 2O-SiO 2-Y 2O 3-Al 2O 3 (KSYA) system was prepared by the melt-quench technique. The transparent Y 3Al 5O 12 (YAG) glass-ceramics were derived from this glass by a controlled crystallization process at 750 °C for 5-100 h. The formation of YAG crystal phase, size and morphology with progress of heat-treatment was examined by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and Fourier transformed infrared reflectance spectroscopy (FT-IRRS). The crystallite sizes obtained from XRD are found to increase with heat-treatment time and vary in the range 25-40 nm. The measured photoluminescence spectra have exhibited emission transitions of 4F 3/2 → 4I J ( J = 9/2, 11/2 and 13/2) from Nd 3+ ions upon excitation at 829 nm. It is observed that the photoluminescence intensity and excited state lifetime of Nd 3+ ions decrease with increase in heat-treatment time. The present study indicates that the incorporation of Nd 3+ ions into YAG crystal lattice enhance the fluorescence performance of the glass-ceramic nanocomposites.

Synthesis and Characterization of SiO2@Y2MoO6:Eu3+ Core-Shell Structured Spherical Phosphors by Sol-Gel Process.

PubMed

Li, G Z; Liu, F H; Chu, Z S; Wu, D M; Yang, L B; Li, J L; Wang, M N; Wang, Z L

2016-04-01

SiO2@Y2MoO6:Eu3+ core-shell phosphors were prepared by the sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL) spectra as well as kinetic decays were used to characterize the resulting SiO2@Y2MoO6:Eu3+ core-shell phosphors. The XRD results demonstrated that the Y2MoO6:Eu3+ layers on the SiO2 spheres crystallized after being annealed at 700 °C and the crystallinity increased with raising the annealing temperature. The obtained core-shell phosphors have spherical shape with narrow size distribution (average size ca. 640 nm), non-agglomeration, and smooth surface. The thickness of the Y2MoO6:Eu3+ shells on the SiO2 cores could be easily tailored by varying the number of deposition cycles (70 nm for four deposition cycles). The Eul+ shows a strong PL emission (dominated by 5D0-7F2 red emission at 614 nm) under the excitation of 347 nm UV light. The PL intensity of Eu3+ increases with increasing the annealing temperature and the number of coating cycles.

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

Influence of Zr doping on structure and morphology of TiO2 nanorods prepared using hydrothermal method

NASA Astrophysics Data System (ADS)

Muslimin, Masliana; Jumali, Mohammad Hafizuddin; Tee, Tan Sin; Beng, Lee Hock; Hui, Tan Chun; Chin, Yap Chi

2018-04-01

The aim of this work is to investigate the effect of Zr doping on TiO2 nanostructure. TiO2 nanorods thin films with different Zr-doping concentrations (6 × 10-3 M, 13 × 10-3 M and 25 × 10-3 M) were successfully prepared using a simple hydrothermal method. The structural and morphological properties of the samples were evaluated using XRD and FESEM respectively. The XRD results revealed that the TiO2 in all samples stabilized as rutile phase. The FESEM micrographs confirmed that TiO2 exist as square like nanorods with blunt tips. Although the crystallographic nature remains unchanged, the introduction of Zr has altered the surface density, structure and morphology of TiO2 which subsequently will have significant effect on its properties.

Synthesis of Mn-doped ZnS architectures in ternary solution and their optical properties

NASA Astrophysics Data System (ADS)

Wang, Xinjuan; Zhang, Qinglin; Zou, Bingsuo; Lei, Aihua; Ren, Pinyun

2011-10-01

Mn-doped ZnS sea urchin-like architectures were fabricated by a one-pot solvothermal route in a ternary solution made of ethylenediamine, ethanolamine and distilled water. The as-prepared products were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and photoluminescence spectra (PL). It was demonstrated that the as-prepared sea urchin-like architectures with diameter of 0.5-1.5 μm were composed of nanorods, possessing a wurtzite structures. The preferred growth orientation of nanorods was found to be the [0 0 2] direction. The PL spectra of the Mn-doped ZnS sea urchin-like architectures show a strong orange emission at 587 nm, indicating the successful doping of Mn 2+ ions into ZnS host. Ethanolamine played the role of oriented-assembly agent in the formation of sea urchin-like architectures. A possible growth mechanism was proposed to explain the formation of sea urchin-like architectures.

One-step solvothermal deposition of ZnO nanorod arrays on a wood surface for robust superamphiphobic performance and superior ultraviolet resistance

PubMed Central

Yao, Qiufang; Wang, Chao; Fan, Bitao; Wang, Hanwei; Sun, Qingfeng; Jin, Chunde; Zhang, Hong

2016-01-01

In the present paper, uniformly large-scale wurtzite-structured ZnO nanorod arrays (ZNAs) were deposited onto a wood surface through a one-step solvothermal method. The as-prepared samples were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG), and differential thermal analysis (DTA). ZNAs with a diameter of approximately 85 nm and a length of approximately 1.5 μm were chemically bonded onto the wood surface through hydrogen bonds. The superamphiphobic performance and ultraviolet resistance were measured and evaluated by water or oil contact angles (WCA or OCA) and roll-off angles, sand abrasion tests and an artificially accelerated ageing test. The results show that the ZNA-treated wood demonstrates a robust superamphiphobic performance under mechanical impact, corrosive liquids, intermittent and transpositional temperatures, and water spray. Additionally, the as-prepared wood sample shows superior ultraviolet resistance. PMID:27775091

Biosynthesis, characterization and cytotoxic effect of plant mediated silver nanoparticles using Morinda citrifolia root extract.

PubMed

Suman, T Y; Radhika Rajasree, S R; Kanchana, A; Elizabeth, S Beena

2013-06-01

Silver has been used since time to control bodily infection, prevent food spoilage and heal wounds by preventing infection. The present study aims at an environmental friendly method of synthesizing silver nanoparticles, from the root of Morinda citrifolia; without involving chemical agents associated with environmental toxicity. The obtained nanoparticles were characterized by UV-vis absorption spectroscopy with an intense surface plasmon resonance band at 413 nm clearly reveals the formation of silver nanoparticles. Fourier transmission infra red spectroscopy (FTIR) showed nanopartilces were capped with plant compounds. Field emission-scanning electron microscopy (FE-SEM) and Transmission electron microscopy (TEM) showed that the spherical nature of the silver nanoparticles with a size of 30-55 nm. The X-ray diffraction spectrum XRD pattern clearly indicates that the silver nanoparticles formed in the present synthesis were crystalline in nature. In addition these biologically synthesized nanoparticles were also proved to exhibit excellent cytotoxic effect on HeLa cell. Copyright © 2013 Elsevier B.V. All rights reserved.

Studies on hydrothermal synthesis of photolumniscent rare earth (Eu3+ & Tb3+) doped NG@FeMoO4 for enhanced visible light photodegradation of methylene blue dye

NASA Astrophysics Data System (ADS)

Singh, R.; Kumar, M.; Khajuria, H.; Sharma, S.; Sheikh, H. Nawaz

2018-02-01

FeMoO4 nanorods and their rare earth (Eu3+ and Tb3+) doped composites with nitrogen doped graphene (NG) were synthesized by facile hydrothermal method in aqueous medium. X-ray diffraction (XRD) analysis of the as-synthesized samples was done to study the phase purity and crystalline nature. FTIR and Raman Spectroscopy have been studied for investigating the bonding in nanostructures. The surface morphology of the samples was investigated with field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The photolumniscent nature of the samples was investigated by the using the fluorescence spectrophotometer. The photocatalytic degradation efficiency of the prepared pure FeMoO4 and its rare earth doped composites with nitrogen doped graphene was evaluated as function of visible light irradiation versus concentration of methylene blue (MB dye). The prepared nanocomposites show enhanced photocatalytic efficiency as compared to the bare FeMoO4 nanorods.

Novel one-step route for synthesizing CdS/polystyrene nanocomposite hollow spheres.

PubMed

Wu, Dazhen; Ge, Xuewu; Zhang, Zhicheng; Wang, Mozhen; Zhang, Songlin

2004-06-22

CdS/polystyrene nanocomposite hollow spheres with diameters between 240 and 500 nm were synthesized under ambient conditions by a novel microemulsion method in which the polymerization of styrene and the formation of CdS nanoparticles were initiated by gamma-irradiation. The product was characterized by transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), X-ray powder diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and thermogravimetric analysis (TGA), which show the walls of the hollow spheres are porous and composed of polystyrene containing homogeneously dispersed CdS nanoparticles. The quantum-confined effect of the CdS/polystyrene nanocomposite hollow spheres is confirmed by the ultraviolet-visible (UV-vis) and photoluminescent (PL) spectra. We propose that the walls of these nanocomposite hollow spheres originate from the simultaneous synthesis of polystyrene and CdS nanoparticles at the interface of microemulsion droplets. This novel method is expected to produce various inorganic/polymer nanocomposite hollow spheres with potential applications in the fields of materials science and biotechnology.

One-step solvothermal deposition of ZnO nanorod arrays on a wood surface for robust superamphiphobic performance and superior ultraviolet resistance

NASA Astrophysics Data System (ADS)

Yao, Qiufang; Wang, Chao; Fan, Bitao; Wang, Hanwei; Sun, Qingfeng; Jin, Chunde; Zhang, Hong

2016-10-01

In the present paper, uniformly large-scale wurtzite-structured ZnO nanorod arrays (ZNAs) were deposited onto a wood surface through a one-step solvothermal method. The as-prepared samples were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG), and differential thermal analysis (DTA). ZNAs with a diameter of approximately 85 nm and a length of approximately 1.5 μm were chemically bonded onto the wood surface through hydrogen bonds. The superamphiphobic performance and ultraviolet resistance were measured and evaluated by water or oil contact angles (WCA or OCA) and roll-off angles, sand abrasion tests and an artificially accelerated ageing test. The results show that the ZNA-treated wood demonstrates a robust superamphiphobic performance under mechanical impact, corrosive liquids, intermittent and transpositional temperatures, and water spray. Additionally, the as-prepared wood sample shows superior ultraviolet resistance.

Effect of Cu Salt Molarity on the Nanostructure of CuO Prolate Spheroid

NASA Astrophysics Data System (ADS)

Sabeeh, Sabah H.; Hussein, Hashim Abed; Judran, Hadia Kadhim

Copper sulfate pentahydrate was used as a source of Cu ion with five different molarities (0.02, 0.05, 0.1, 0.15, 2 and 0.25M). XRD, FE-SEM and TEM techniques all showed that CuO samples have polycrystalline monoclinic structure. CuO prolate spheroid is assembled from nanoparticles as building units. It was demonstrated that the purity, morphology, size range of prolate spheroid and density of nano building units are significantly influenced by Cu precursor’s molarity. The pure phase of CuO prolate spheroid was produced via molarity of 0.2M with crystallite size of 15.1565nm while the particle size of building units ranges from 16nm to 21nm. The stability of CuO nanosuspension or nanofluid was evaluated by zeta potential analysis. The obtained properties of specific structure with large surface area of CuO prolate spheroid make it a promising candidate for wide range of potential applications as in nanofluids for cooling purposes.

Low-temperature growth of aligned ZnO nanorods: effect of annealing gases on the structural and optical properties.

PubMed

Umar, Ahmad; Hahn, Yoon-Bong; Al-Hajry, A; Abaker, M

2014-06-01

Aligned ZnO nanorods were grown on ZnO/Si substrate via simple aqueous solution process at low-temperature of - 65 degrees C by using zinc nitrate and hexamethylenetetramine (HMTA). The detailed morphological and structural properties measured by FESEM, XRD, EDS and TEM confirmed that the as-grown nanorods are vertically aligned, well-crystalline possessing wurtzite hexagonal phase and grown along the [0001] direction. The room-temperature photoluminescence spectrum of the grown nanorods exhibited a strong and broad green emission and small ultraviolet emission. The as-prepared ZnO nanorods were post-annealed in nitrogen (N2) and oxygen (O2) environments and further characterized in terms of their morphological, structural and optical properties. After annealing the nanorods exhibit well-crystallinity and wurtzite hexagonal phase. Moreover, by annealing the PL spectra show the enhancement in the UV emission and suppression in the green emission. The presented results demonstrate that simply by post-annealing process, the optical properties of ZnO nanostructures can be controlled.

Synthesis and photocatalytic activity of anatase TiO2 nanoparticles for degradation of methyl orange

NASA Astrophysics Data System (ADS)

Singh, Manmeet; Duklan, Neha; Singh, Pritpal; Sharma, Jeewan

2018-05-01

In present study, TiO2 nanoparticles, in anatase form, were successfully synthesized using TiCl4 as precursor. These nanoparticles were synthesized by sol-gel method at room temperature (298 K). As prepared samples were characterized for phase structure, optical absorption and surface properties using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Raman spectroscopy and UV-Visible spectroscopy. The synthesized TiO2 nanoparticles sample was compared with one of the most efficient commercial photocatalyst Degussa TiO2 also known as P(25). The effect of phase composition of anatase TiO2 nanoparticles, as compared to P(25), on photocatalytic decomposition of organic dye, methyl orange (MO) was studies under UV light illumination. An enhanced degradation of hazardous dye was observed in the presence of anatase TiO2 nanoparticles as compared to P(25) due to slow recombination rate. Other possible reasons for this enhancement have also been discussed.

Facile synthesis and characterization of silver nanoparticle/bis(o-phenolpropyl)silicone composites using a gold catalyst.

PubMed

Roh, Sung-Hee; Cheong, Hyeonsook; Kim, Do-Heyoung; Woo, Hee-Gweon; Lee, Byeong-Gweon; Yang, Kap-Seung; Kim, Bo-Hye; Sohn, Honglae

2013-01-01

The generation of silver nanoparticle/bis(o-phenolpropyl)silicone composites have been facilitated by the addition of sodium tetrachloroaurate or gold(Ill) chloride (< 1 wt% of NaAuCl4 or AuCl3) to the reaction of silver nitrate (AgNO3) with bis(o-phenolpropyl)silicone [BPPS, (o-phenolpropyl)2(SiMe2O)n, n = 2,3,8,236]. TEM and FE-SEM data showed that the silver nanoparticles having the size of < 20 nm are well dispersed throughout the BPPS silicone matrix in the composites. XRD patterns are consistent with those for polycrystalline silver. The size of silver nanoparticles augmented with increasing the relative molar concentration of AgNO3 added with respect to BPPS. The addition of gold complexes (1-3 wt%) did not affect the size distribution of silver nanoparticles appreciably. In the absence of BPPS, the macroscopic precipitation of silver by agglomeration, indicating that BPPS is necessary to stabilize the silver nanoparticles surrounded by coordination.

Synthesis of CdS/BiOBr nanosheets composites with efficient visible-light photocatalytic activity

NASA Astrophysics Data System (ADS)

Cui, Haojie; Zhou, Yawen; Mei, Jinfeng; Li, Zhongyu; Xu, Song; Yao, Chao

2018-01-01

The efficient charge separation action and visible-light responding could enhance the photocatalytic property of photocatalysts. In the present study, novel CdS/BiOBr nanosheets composites were synthesized by a three-step process. The as-prepared samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (FE-SEM), diffuse reflection spectroscopy (DRS), Raman spectroscopy and photoluminescence (PL). Under visible-light irradiation, the as-prepared CdS nanoparticles decorated BiOBr nanosheets exhibited the excellent photocatalytic activity and high stability for malachite green (MG) degradation. The photodegradation achieved maximum degradation efficiency (99%) using CdS/BiOBr-3 composites as photocatalyst. Furthermore, the possible photocatalytic mechanism upon CdS/BiOBr composites was also discussed through radical and holes trapping experiments. The heterostructure between CdS and BiOBr improved photocatalytic activity dramatically, which greatly promoted migration rate of the photoinduced electrons besides limiting the recombination of photogenerated electron-hole pairs.

Large-scale synthesis and microwave absorption enhancement of actinomorphic tubular ZnO/CoFe2O4 nanocomposites.

PubMed

Cao, Jing; Fu, Wuyou; Yang, Haibin; Yu, Qingjiang; Zhang, Yanyan; Liu, Shikai; Sun, Peng; Zhou, Xiaoming; Leng, Yan; Wang, Shuangming; Liu, Bingbing; Zou, Guangtian

2009-04-09

Actinomorphic tubular ZnO/CoFe(2)O(4) nanocomposites were fabricated in large scale via a simple solution method at low temperature. The phase structures, morphologies, particle size, shell thickness, chemical compositions of the composites have been characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), energy dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). The as-synthesized nanocomposites were uniformly dispersed into the phenolic resin then the mixture was pasted on metal plate with the area of 200 mm x 200 mm as the microwave absorption test plate. The test of microwave absorption was carried out by the radar-absorbing materials (RAM) reflectivity far field radar cross-section (RCS) method. The range of microwave absorption is from 2 to 18 Hz and the best microwave absorption reach to 28.2 dB at 8.5 Hz. The results indicate that the composites are of excellence with respect to microwave absorption.

Ultrasound-assisted synthesis of CuO nanostructures templated by cotton fibers

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

Zou, Yunling, E-mail: zouyunling1999@126.com; Li, Yan; Guo, Ying

Highlights: ► Flower-like and corn-like CuO nanostructures were synthesized by a simple method. ► Cotton fibers purchased from commercially are used as template. ► The concentration of Cu(NO{sub 3}){sub 2} solution is an important parameter. -- Abstract: Flower-like and corn-like CuO nanostructures composed of CuO nanoparticles were successfully synthesized via ultrasound-assisted template method, respectively, by controlling the initial concentration of Cu(NO{sub 3}){sub 2} solution. Here, cotton fibers were used as template agent. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FE-SEM) and energy-dispersive spectroscopy (EDS), respectively. The results demonstrated that the initialmore » concentration of Cu(NO{sub 3}){sub 2} solution was an important parameter for determining whether CuO nanoparticles assembled into flower-like structures or corn-like structures. The mechanism of forming different nanostructures of CuO was discussed.« less

Process dependent thermoelectric properties of EDTA assisted bismuth telluride

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

Kulsi, Chiranjit; Banerjee, Dipali, E-mail: dipalibanerjeebesu@gmail.com; Kargupta, Kajari

2016-04-13

Comparison between the structure and thermoelectric properties of EDTA (Ethylene-diamine-tetra-acetic acid) assisted bismuth telluride prepared by electrochemical deposition and hydrothermal route is reported in the present work. The prepared samples have been structurally characterized by high resolution X-ray diffraction spectra (HRXRD), field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopic images (HRTEM). Crystallite size and strain have been determined from Williamson-Hall plot of XRD which is in conformity with TEM images. Measurement of transport properties show sample in the pellet form (S{sub 1}) prepared via hydrothermal route has higher value of thermoelectric power (S) than the electrodepositedmore » film (S{sub 2}). But due to a substantial increase in the electrical conductivity (σ) of the film (S{sub 2}) over the pellet (S{sub 1}), the power factor and the figure of merit is higher for sample S{sub 2} than the sample S{sub 1} at room temperature.« less

Synthesis, characterization and catalytic performance of ZnO-CeO2 nanoparticles in wet oxidation of wastewater containing chlorinated compounds

NASA Astrophysics Data System (ADS)

Anushree; Kumar, S.; Sharma, C.

2017-11-01

Here we report the catalytic property of ZnO-CeO2 nanoparticles towards oxidative degradation of organic pollutants present in industrial wastewater. The catalysts were prepared by co-precipitation method without using any surfactant. The physicochemical properties of catalysts were studied by XRD, Raman, XPS, N2-sorption, FE-SEM, TEM and EDX techniques. The characterization results confirmed the formation of porous ZnO-CeO2 nanocatalysts with high surface area, pore volume and oxygen vacancies. ZnO-CeO2 nanocatalysts exhibited appreciable efficiency in CWAO of industrial wastewater under mild conditions. The Ce40Zn60 catalyst was found to be most efficient with 72% color, 64% chemical oxygen demand (COD) and 63% total organic carbon (TOC) removal. Efficient removal of chlorophenolics (CHPs, 59%) and adsorbable organic halides (AOX, 54%) indicated the feasibility of using ZnO-CeO2 nanocatalysts in degradation of non-biodegradable and toxic chlorinated compounds.

Self-assembled synthesis of 3D Cu(In1 - xGax)Se2 nanoarrays by one-step electroless deposition into ordered AAO template

NASA Astrophysics Data System (ADS)

Zhang, Bin; Zhou, Tao; Zheng, Maojun; Xiong, Zuzhou; Zhu, Changqing; Li, Hong; Wang, Faze; Ma, Li; Shen, Wenzhong

2014-07-01

Quaternary nanostructured Cu(In1 - xGax)Se2 (CIGS) arrays were successfully fabricated via a novel and simple solution-based protocol on the electroless deposition method, using a flexible, highly ordered anodic aluminium oxide (AAO) substrate. This method does not require electric power, complicated sensitization processes, or complexing agents, but provides nearly 100% pore fill factor to AAO templates. The field emission scanning electron microscopy (FE-SEM) images show that we obtained uniformly three-dimensional nanostructured CIGS arrays, and we can tailor the diameter and wall thicknesses of the nanostructure by adjusting the pore diameter of the AAO and metal Mo layer. Their chemical composition was determined by energy-dispersive spectroscopy analysis, which is very close to the stoichiometric value. The Raman spectroscopy, x-ray diffraction (XRD) pattern, and transmission electron microscopy (TEM) further confirm the formation of nanostructured CIGS with prominent chalcopyrite structure. The nanostructured CIGS arrays can support the design of low-cost, highlight-trapping, and enhanced carrier collection nanostructured solar cells.

Preparation of nanostructured and nanosheets of MoS2 oxide using oxidation method.

PubMed

Amini, Majed; Ramazani S A, Ahmad; Faghihi, Morteza; Fattahpour, Seyyedfaridoddin

2017-11-01

Molybdenum disulfide (MoS 2 ), a two-dimensional transition metal has a 2D layered structure and has recently attracted attention due to its novel catalytic properties. In this study, MoS 2 has been successfully intercalated using chemical and physical intercalation techniques, while enhancing its surface properties. The final intercalated MoS 2 is of many interests because of its low-dimensional and potential properties in in-situ catalysis. In this research, we report different methods to intercalate the layers of MoS 2 successfully using acid-treatment, ultrasonication, oxidation and thermal shocking. The other goal of this study is to form SO bonds mainly because of expected enhanced in-situ catalytic operations. The intercalated MoS 2 is further characterized using analyses such as Fourier Transform Infrared Spectroscopy (FTIR), Raman, Contact Angle, X-ray diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), Energy Dispersive X-Ray Microanalysis (EDAX), Transmission electron microscopy (TEM), and BET. Copyright © 2017. Published by Elsevier B.V.

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

PubMed

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

2010-06-15

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

An electrochemical sensor for warfarin determination based on covalent immobilization of quantum dots onto carboxylated multiwalled carbon nanotubes and chitosan composite film modified electrode.

PubMed

Gholivand, Mohammad Bagher; Mohammadi-Behzad, Leila

2015-12-01

A method is described for the construction of a novel electrochemical warfarin sensor based on covalent immobilization of CdS-quantum dots (CdS-QDs) onto carboxylated multiwalled carbon nanotubes/chitosan (CS) composite film on the surface of a glassy carbon electrode. The CdS-QDs/CS/MWCNTs were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infra-red (FTIR) spectroscopy, XRD analysis and electrochemical impedance spectroscopy (EIS). The sensor showed optimum anodic stripping response within 90s at an accumulation potential of 0.75V. The modified electrode was used to detect the concentration of warfarin with a wide linear range of 0.05-80 μM and a detection limit (S/N=3) of 8.5 nM. The proposed sensor has good storage stability, repeatability and reproducibility and was successfully applied for the determination of warfarin in real samples such as urine, serum and milk. Copyright © 2015. Published by Elsevier B.V.

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

Wu Changle; Qiao Xueliang; Luo Langli

Flower-like ZnO nano/microstructures have been synthesized by thermal treatment of Zn(NH{sub 3}){sub 4}{sup 2+} precursor in aqueous solvent, using ammonia as the structure directing agent. A number of techniques, including X-ray diffraction (XRD), field emission scan electron microscopy (FESEM), transmission electron microscopy (TEM), thermal analysis, and photoluminescence (PL) were used to characterize the obtained ZnO structures. The photoluminescence (PL) measurements indicated that the as-synthesized ZnO structures showed UV ({approx}375 nm), blue ({approx}465 nm), and yellow ({approx}585 nm) emission bands when they were excited by a He-Gd laser using 320 nm as the excitation source. Furthermore, it has been interestingly foundmore » that the intensity of light emission at {approx}585 nm remarkably decreased when the obtained ZnO nanocrystals were annealed at 600 deg. C for 3 h in air. The reason might be the possible oxygen vacancies and interstitials in the sample decreased at high temperature.« less

FIB-NanoSIMS-TEM Coordinated Study of a Wark-Lovering Rim in a Vigarano Type A CAI

NASA Technical Reports Server (NTRS)

Cai, A.; Ito, M.; Keller, L. P.; Ross, D. K.; Nakamura-Messenger, K.

2010-01-01

Wark-Lovering (WL) rims are thin multi layered mineral sequences that surround most Ca, Al-rich inclusions (CAIs). Unaltered WL rims are composed of the same primary high temperature minerals as CAIs, such as melilite, spinel, pyroxene, hibonite, perovskite, anorthite and olivine. It is still unclear whether the rim minerals represent a different generation formed by a separate event from their associated CAIs or are a byproduct of CAI formation. Several models have been proposed for the origins of WL rims including condensation, flashheating, reaction of a CAI with a Mg-Si-rich reservoir (nebular gas or solid); on the basis of mineralogy, abundances of trace elements, O and Mg isotopic studies. Detailed mineralogical characterizations of WL rims at micrometer to nanometer scales have been obtained by TEM observations, but so far no coordinated isotopic - mineralogical studies have been performed. Thus, we have applied an O isotopic imaging technique by NanoSIMS 50L to investigate heterogeneous distributions of O isotopic ratios in minerals within a cross section of a WL rim prepared using a focused ion beam (FIB) instrument. After the isotopic measurements, we determine the detailed mineralogy and microstructure of the same WL FIB section to gain insight into its petrogenesis. Here we present preliminary results from O isotopic and elemental maps by NanoSIMS and mineralogical analysis by FE-SEM of a FIB section of a WL rim in the Vigarano reduced CV3 chondrite.

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

PubMed

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

2006-03-15

The removal of As(V), one of the most poisonous groundwater pollutants, by synthetic nanoscale zero-valent iron (NZVI) was studied. Batch experiments were performed to investigate the influence of pH, adsorption kinetics, sorption mechanism, and anionic effects. Field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Mossbauer spectroscopy were used to characterize the particle size, surface morphology, and corrosion layer formation on pristine NZVI and As(V)-treated NZVI. The HR-TEM study of pristine NZVI showed a core-shell-like structure, where more than 90% of the nanoparticles were under 30 nm in diameter. Mössbauer spectroscopy further confirmed its structure in which 19% were in zero-valent state with a coat of 81% iron oxides. The XRD results showed that As(V)-treated NZVI was gradually converted into magnetite/maghemite corrosion products over 90 days. The XPS study confirmed that 25% As(V) was reduced to As(III) by NZVI after 90 days. As(V) adsorption kinetics were rapid and occurred within minutes following a pseudo-first-order rate expression with observed reaction rate constants (Kobs) of 0.02-0.71 min(-1) at various NZVI concentrations. Laser light scattering analysis confirmed that NZVI-As(V) forms an inner-sphere surface complexation. The effects of competing anions revealed that HCO3-, H4SiO4(0), and H2PO4(2-) are potential interfering agents in the As(V) adsorption reaction. Our results suggest that NZVI is a suitable candidate for As(V) remediation.

RECENT DEVELOPMENT IN TEM CHARACTERIZATION OF IRRADIATED RERTR FUELS

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

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

2011-10-01

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

Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

Double-tilt in situ TEM holder with ultra-high stability.

PubMed

Xu, Mingjie; Dai, Sheng; Blum, Thomas; Li, Linze; Pan, Xiaoqing

2018-05-06

A double tilting holder with high stability is essential for acquiring atomic-scale information by transmission electron microscopy (TEM), but the availability of such holders for in situ TEM studies under various external stimuli is limited. Here, we report a unique design of seal-bearing components that provides ultra-high stability and multifunctionality (including double tilting) in an in situ TEM holder. The seal-bearing subsystem provides superior vibration damping and electrical insulation while maintaining excellent vacuum sealing and small form factor. A wide variety of in situ TEM applications including electrical measurement, STM mapping, photovoltaic studies, and CL spectroscopy can be performed on this platform with high spatial resolution imaging and electrical sensitivity at the pA scale. Copyright © 2018 Elsevier B.V. All rights reserved.

Complete Tem-Tomography: 3D Structure of Gems Cluster

NASA Technical Reports Server (NTRS)

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

2015-01-01

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

2D Inversion of Transient Electromagnetic Method (TEM)

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

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

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

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

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

Synthesis, characterization and study of arsenate adsorption from aqueous solution by {alpha}- and {delta}-phase manganese dioxide nanoadsorbents

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

Singh, Mandeep; Thanh, Dong Nguyen, E-mail: Dong.Nguyen.Thanh@vscht.c; Ulbrich, Pavel

2010-12-15

Single-phase {alpha}-MnO{sub 2} nanorods and {delta}-MnO{sub 2} nano-fiber clumps were synthesized using manganese pentahydrate in an aqueous solution. These nanomaterials were characterized using the Transmission Electron Microscope (TEM), Field Emission Scanning Electron Microscope (FE-SEM), Powder X-ray diffraction (XRD) and the Brunauer-Elmet-Teller nitrogen adsorption technique (BET-N{sub 2} adsorption). The structural analysis shows that {alpha}-MnO{sub 2} (2x2 tunnel structure) has the form of needle-shaped nanorods and {delta}-MnO{sub 2} (2D-layered structure) consists of fine needle-like fibers arranged in ball-like aggregates. Batch adsorption experiments were carried out to determine the effect of pH on adsorption kinetics and adsorption capacity for the removal of As(V)more » from aqueous solution onto these two types of nanoadsorbents. The adsorption capacity of As(V) was found to be highly pH dependent. The adsorption of As(V) onto {alpha}-MnO{sub 2} reached equilibrium more rapidly with higher adsorption capacity compared to {delta}-MnO{sub 2}. -- Graphical abstract: {alpha}-MnO{sub 2} (2x2 tunnel structure) nanorods and {delta}-MnO{sub 2} (2-D layered structure) nano-fiber clumps were synthesized in a facile way in an aqueous solution and characterized by TEM, FE-SEM, XRD and BET-N{sub 2} adsorption techniques. The structural analysis shows that {alpha}-MnO{sub 2} is needle shaped nanorods and {delta}-MnO{sub 2} consists of 2-D platelets of fine needle-like fibers arranged in ball-like aggregates. Further batch experiments confirmed that both nanoadsorbents are potential candidates for the adsorption of As(V) with a capacity of 19.41 and 15.33 mg g{sup -1} for {alpha}-MnO{sub 2} and {delta}-MnO{sub 2}, respectively. The presence of As3d peak in XPS study indicates that arsenic on the surface of nanoadsorbents is in the stable form of As(V) with a percentage of arsenate onto {alpha}-MnO{sub 2} is 0.099% as compared to 0.021% onto {delta}-MnO{sub 2

Study the oxidation kinetics of uranium using XRD and Rietveld method

NASA Astrophysics Data System (ADS)

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

2010-03-01

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

Development of 89Zr-Ontuxizumab for in vivo TEM-1/endosialin PET applications

PubMed Central

Lange, Sara E.S.; Zheleznyak, Alex; Studer, Matthew; O'Shannessy, Daniel J.; Lapi, Suzanne E.; Van Tine, Brian A.

2016-01-01

Purpose The complexity of sarcoma has led to the need for patient selection via in vivo biomarkers. Tumor endothelial marker-1 (TEM-1) is a cell surface marker expressed by the tumor microenvironment. Currently MORAb-004 (Ontuxizumab), an anti-TEM-1 humanized monoclonal antibody, is in sarcoma clinical trials. Development of positron emission tomography (PET) for in vivo TEM-1 expression may allow for stratification of patients, potentially enhancing clinical outcomes seen with Ontuxizumab. Results Characterization of cell lines revealed clear differences in TEM-1 expression. One high expressing (RD-ES) and one low expressing (LUPI) cell line were xenografted, and mice were injected with 89Zr-Ontuxizumab. PET imaging post-injection revealed that TEM-1 was highly expressed and readily detectable in vivo only in RD-ES. In vivo biodistribution studies confirmed high radiopharmaceutical uptake in tumor relative to normal organs. Experimental Design Sarcoma cell lines were characterized for TEM-1 expression. Ontuxizumab was labeled with 89Zr and evaluated for immunoreactivity preservation. 89Zr-Ontuxizumab was injected into mice with high or null expressing TEM-1 xenografts. In vivo PET imaging experiments were performed. Conclusion 89Zr-Ontuxizumab can be used in vivo to determine high versus low TEM-1 expression. Reliable PET imaging of TEM-1 in sarcoma patients may allow for identification of patients that will attain the greatest benefit from anti-TEM-1 therapy. PMID:26909615

Exploring the potential reservoirs of non specific TEM beta lactamase (bla(TEM)) gene in the Indo-Gangetic region: A risk assessment approach to predict health hazards.

PubMed

Singh, Gulshan; Vajpayee, Poornima; Rani, Neetika; Amoah, Isaac Dennis; Stenström, Thor Axel; Shanker, Rishi

2016-08-15

The emergence of antimicrobial resistant bacteria is an important public health and environmental contamination issue. Antimicrobials of β-lactam group accounts for approximately two thirds, by weight, of all antimicrobials administered to humans due to high clinical efficacy and low toxicity. This study explores β-lactam resistance determinant gene (blaTEM) as emerging contaminant in Indo-Gangetic region using qPCR in molecular beacon format. Quantitative Microbial Risk Assessment (QMRA) approach was adopted to predict risk to human health associated with consumption/exposure of surface water, potable water and street foods contaminated with bacteria having blaTEM gene. It was observed that surface water and sediments of the river Ganga and Gomti showed high numbers of blaTEM gene copies and varied significantly (p<0.05) among the sampling locations. The potable water collected from drinking water facility and clinical settings exhibit significant number of blaTEM gene copies (13±0.44-10200±316 gene copies/100mL). It was observed that E.crassipes among aquatic flora encountered in both the rivers had high load of blaTEM gene copies. The information on prevalence of environmental reservoirs of blaTEM gene containing bacteria in Indo-Gangetic region and risk associated will be useful for formulating strategies to protect public from menace of clinical risks linked with antimicrobial resistant bacteria. Copyright © 2016 Elsevier B.V. All rights reserved.

A Potential Waste to be Selected as Media for Metal and Nutrient Removal

NASA Astrophysics Data System (ADS)

Zayadi, N.; Othman, N.; Hamdan, R.

2016-07-01

This study describes the potential of application of cassava peel, banana peel, coconut shell, and coconut coir to be selected as metal removal while limestone and steel slag for nutrient removal. The media were characterized by X-Ray Fluorescence (XRF), Fourier Transform Infrared (FTIR), Field Emission Scanning Electron Microscopy-Energy Dispersive X-Ray (FESEM-EDX), and X-Ray Powder Diffraction (XRD). The results of XRF analysis medias show the present of calcium oxide, CaO which confirm the high efficiency in adsorbing metal ions and nutrient which is in agreement with the result of XRD. The characteristics of medias by FTIR analysis also confirmed the involvement of alcohol, carboxylic, alkanes, amines and ethers which play important role to reduce ions while FESEM-EDX indicates the porous structures of study medias. The characterization analysis highlight that cassava peel and steel slag were selected as a potential media in this study.

A green chemistry approach for the synthesis and characterization of bioactive gold nanoparticles using Azolla microphylla methanol extract

NASA Astrophysics Data System (ADS)

Kunjiappan, Selvaraj; Chowdhury, Ranjana; Bhattacharjee, Chiranjib

2014-06-01

This article reports the environmentally benign synthesis of gold nanoparticles (GNPs) using methanol extract of Azolla microphylla as the stabilizing and reducing agent. The GNPs were characterized by UV-vis spectrophotometry and FTIR, and the morphological characteristics were analyzed by XRD, FESEM-EDX and HRTEM. The GNPs could be formed in very short time, even in less than 30 min. The nanoparticles measured by UV-spectrophotometer demonstrated a peak at 540 nm corresponding to surface plasmon resonance spectra, and the peaks showed by FTIR suggested the presence of organic biomolecules on the surface of the GNPs. XRD results confirmed the crystalline nature of the GNPs, and FESEM-EDX and HRTEM analyses had been performed in the size ranges of 17-40 nm and 1.25-17.5 nm respectively. The synthesized GNPs showed excellent antioxidant activity. This study shows the feasibility of using plant sources for the biosynthesis of GNPs.

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

PubMed

Ma, Li-Jing; Guo, Lie-Jin

2011-04-01

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

In-vitro antibacterial study of zinc oxide nanostructures on Streptococcus sobrinus

NASA Astrophysics Data System (ADS)

Bakhori, Siti Khadijah Mohd; Mahmud, Shahrom; Ann, Ling Chuo; Sirelkhatim, Amna; Hasan, Habsah; Mohamad, Dasmawati; Masudi, Sam'an Malik; Seeni, Azman; Rahman, Rosliza Abd

2014-10-01

Zinc oxide nanostructures were prepared using a pilot plant of zinc oxide boiling furnace. Generally, it produced two types of nanostructures different in morphology; one is rod-like shaped (ZnO-1) and a plate-like shape (ZnO-2). The properties of ZnO were studied by structural, optical and morphological using XRD, PL and FESEM respectively. The XRD patterns confirmed the wurtzite structures of ZnO with the calculated crystallite size of 41 nm (ZnO-1) and 42 nm (ZnO-2) using Scherrer formula. The NBE peaks were determined by photoluminescence spectra which reveal peak at 3.25 eV and 3.23 eV for ZnO-1 and ZnO-2 respectively. Prior to that, the morphologies for both ZnO-1 and ZnO-2 were demonstrated from FESEM micrographs. Subsequently the antibacterial study was conducted using in-vitro broth dilution technique towards a gram positive bacterium Streptococcus sobrinus (ATCC 33478) to investigate the level of antibacterial effect of zinc oxide nanostructures as antibacterial agent. Gradual increment of ZnO concentrations from 10-20 mM affected the inhibition level after twenty four hours of incubation. In conjunction with concentration increment of ZnO, the percentage inhibition towards Streptococcus sobrinus was also increased accordingly. The highest inhibition occurred at 20 mM of ZnO-1 and ZnO-2 for 98% and 77% respectively. It showed that ZnO has good properties as antibacterial agent and relevancy with data presented by XRD, PL and FESEM were determined.

Effective aqueous arsenic removal using zero valent iron doped MWCNT synthesized by in situ CVD method using natural α-Fe2O3 as a precursor.

PubMed

Alijani, Hassan; Shariatinia, Zahra

2017-03-01

This research presents an efficient system for removing aqua's arsenic based on in situ zero valent iron doping onto multiwall carbon nanotube (MWCNT) through MWCNT growth onto the natural α-Fe 2 O 3 surface in chemical vapor deposition (CVD) reactor. The as-synthesized magnetic nanohybrid was characterized by XRD, VSM, FE-SEM and TEM techniques. The result of XRD analysis revealed that MWCNT has been successfully generated on the surface of zero valent iron. Moreover, the material showed good superparamagnetic characteristic to be employed as a magnetic adsorbent. The hematite, nanohybrid and its air oxidized form were used for removing aqueous arsenite and arsenate; however, non oxidized material exhibited greater efficiency for the analytes uptake. Equilibrium times were 60 and 90 min for arsenate and arsenite adsorption using nanohybrid and oxidized sorbent but the equilibrium time was 1320 min using hematite. The adsorption efficiencies of hematite and oxidized sorbent were 18, 74% and 26, 77% for arsenite and arsenate, respectively, at initial concentration of 10 mg L -1 . At this situation, the removal efficiencies were 96 and 98.5% for arsenite and arsenate adsorption using raw nanohybrid. Thermodynamic study was also performed and results indicated that arsenic adsorption onto nanohybrid and oxidized sorbent was spontaneous however hematite followed a nonspontaneous path for the arsenic removal. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis of SnO2 pillared carbon using long chain alkylamine grafted graphene oxide: an efficient anode material for lithium ion batteries

NASA Astrophysics Data System (ADS)

Reddy, M. Jeevan Kumar; Ryu, Sung Hun; Shanmugharaj, A. M.

2015-12-01

With the objective of developing new advanced composite materials that can be used as anodes for lithium ion batteries (LIBs), herein we describe the synthesis of SnO2 pillared carbon using various alkylamine (hexylamine; dodecylamine and octadecylamine) grafted graphene oxides and butyl trichlorotin precursors followed by its calcination at 500 °C for 2 h. While the grafted alkylamine induces crystalline growth of SnO2 pillars, thermal annealing of alkylamine grafted graphene oxide results in the formation of amorphous carbon coated graphene. Field emission scanning electron microscopy (FE-SEM) results reveal the successful formation of SnO2 pillared carbon on the graphene surface. X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy characterization corroborates the formation of rutile SnO2 crystals on the graphene surface. A significant rise in the BET surface area is observed for SnO2 pillared carbon, when compared to pristine GO. Electrochemical characterization studies of SnO2 pillared carbon based anode materials showed an enhanced lithium storage capacity and fine cyclic performance in comparison with pristine GO. The initial specific capacities of SnO2 pillared carbon are observed to be 1379 mA h g-1, 1255 mA h g-1 and 1360 mA h g-1 that decrease to 750 mA h g-1, 643 mA h g-1 and 560 mA h g-1 depending upon the chain length of grafted alkylamine on the graphene surface respectively. Electrochemical impedance spectral analysis reveals that the exchange current density of SnO2 pillared carbon based electrodes is higher, corroborating its enhanced electrochemical activity in comparison with GO based electrodes.With the objective of developing new advanced composite materials that can be used as anodes for lithium ion batteries (LIBs), herein we describe the synthesis of SnO2 pillared carbon using various alkylamine (hexylamine; dodecylamine and octadecylamine) grafted graphene oxides and butyl trichlorotin precursors

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

PubMed Central

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

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 μm loosely amorphous particles. XRD test shows that β-HgS, S8, 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. PMID:27738409

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

PubMed

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.

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

PubMed

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

2010-01-01

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

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

PubMed

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

2014-04-23

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

Structural and magnetic characterization of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} nanoparticles prepared via a facile microwave-assisted method

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

Moradi, J., E-mail: j_moradi@yahoo.com; Ghazi, M.E.; Ehsani, M.H., E-mail: mhe_ehsani@yahoo.com

2014-07-01

Nanoparticles of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LSMO) with different particle sizes are synthesized by a very fast, inexpensive, reproducible, and environmentally friendly method: the microwave irradiation of the corresponding mixture of nitrates. The structural and magnetic properties of the samples are investigated by the X-Ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and magnetic (DC magnetization and AC susceptibility) measurements. The XRD study coupled with the Rietveld refinement show that all samples crystallize in a rhombohedral structure with the space group of R−3C. The FT-IR spectroscopy and FE-SEM images indicate formationmore » of the perovskite structure of LSMO. The DC magnetization measurements confirm the decrease in the particle size effects on the magnetic properties, e.g. reduction in the ferromagnetic (FM) moment and increase in the surface spin disorder. Magnetic dynamics of the samples studied by AC magnetic susceptibility shows that the magnetic behavior of the nanometer-sized samples is well-described by the Vogel-Fulcher and critical slowing down laws. Strong interaction between magnetic nanoparticles of LSMO was detected by fitting the experimental data with the mentioned models. - Graphical abstract: Temperature dependence of the magnetization M(T) was measured in the zero-field-cooling (ZFC) and field-cooling (FC) modes at the applied magnetic field of 100 Oe for the La{sub 0.8}Sr{sub 0.2}MnO{sub 3} with different size prepared via a facile microwave-assisted method. - Highlights: • Nanoparticles of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} were synthesized by the microwave irradiation process. • The structural studies show that all samples crystallize in a rhombohedral structure with space group of R−3C. • The DC magnetic studies confirm tuning of the magnetic properties due to the particle size effects. �

Matching 4.7-Å XRD spacing in amelogenin nanoribbons and enamel matrix.

PubMed

Sanii, B; Martinez-Avila, O; Simpliciano, C; Zuckermann, R N; Habelitz, S

2014-09-01

The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. © International & American Associations for Dental Research.

Matching 4.7-Å XRD Spacing in Amelogenin Nanoribbons and Enamel Matrix

PubMed Central

Sanii, B.; Martinez-Avila, O.; Simpliciano, C.; Zuckermann, R.N.; Habelitz, S.

2014-01-01

The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. PMID:25048248

Fabrication of Mesoporous Silica/Alumina Hybrid Membrane Film Nanocomposites using Template Sol-Gel Synthesis of Amphiphilic Triphenylene

NASA Astrophysics Data System (ADS)

Lintang, H. O.; Jalani, M. A.; Yuliati, L.; Salleh, M. M.

2017-05-01

Herein we reported that by introducing a one-dimensional (1D) substrate with a porous structure such as anodic aluminum oxide (AAO) membrane, mesoporous silica/alumina hybrid nanocomposites were successfully fabricated by using amphiphilic triphenylene (TPC10TEG) as a template in sol-gel synthesis (TPC10TEG/silicahex). For the optical study of the nanocomposites, TPC10TEG/silicahex showed absorption peak at 264 nm due to the ordered and long-range π-π stacking of the disc-like aromatic triphenylene core. Moreover, the hexagonal arrangement of TPC10TEG/silicahex was proven based on their diffraction peaks of d 100 and d 200 at 2θ = 2.52° and 5.04° and images of transmission electron microscopy (TEM), respectively. For fabrication of mesoporous silica/alumina hybrid membrane, TPC10TEG/silicahex was drop-casted onto AAO membrane for penetration into the porous structure via gravity. X-ray diffraction (XRD) analysis on the resulted hybrid nanocomposites showed that the diffraction peaks of d 100 and d 200 of TPC10TEG/silicahex were still preserved, indicating that the hexagonal arrangements of mesoporous silica were maintained even on AAO substrate. The morphology study on the hybrid nanocomposites using TEM, scanning electron microscope (SEM) and field emission scanning electron microscope (FE-SEM) showed the successful filling of most AAO channels with the TPC10TEG/silicahex nanocomposites.

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

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

DTIC Science & Technology

2017-05-01

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

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Johnson, David K; Lee, Christopher; Dazen, Kevin

2015-07-04

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Lee, Christopher M; Dazen, Kevin; Kafle, Kabindra

2015-01-01

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

Allyl triphenyl phosphonium bromide based DES-functionalized carbon nanotubes for the removal of mercury from water.

PubMed

AlOmar, Mohamed Khalid; Alsaadi, Mohammed Abdulhakim; Hayyan, Maan; Akib, Shatirah; Ibrahim, Muhammad; Hashim, Mohd Ali

2017-01-01

Recently, deep eutectic solvents (DESs) have shown their new and interesting ability for chemistry through their involvement in variety of applications. This study introduces carbon nanotubes (CNTs) functionalized with DES as a novel adsorbent for Hg 2+ from water. Allyl triphenyl phosphonium bromide (ATPB) was combined with glycerol as the hydrogen bond donor (HBD) to form DES, which can act as a novel CNTs functionalization agent. The novel adsorbent was characterized using Raman, FTIR, XRD, FESEM, EDX, BET surface area, TGA, TEM and Zeta potential. Response surface methodology was used to optimize the removal conditions for Hg 2+ . The optimum removal conditions were found to be pH 5.5, contact time 28 min, and an adsorbent dosage of 5 mg. Freundlich isotherm model described the adsorption isotherm of the novel adsorbent, and the maximum adsorption capacity obtained from the experimental data was 186.97 mg g -1 . Pseudo-second order kinetics describes the adsorption rate order. Copyright © 2016 Elsevier Ltd. All rights reserved.

Optical, thermal and combustion properties of self-colored polyamide nanocomposites reinforced with azo dye surface modified ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Hajibeygi, Mohsen; Shabanian, Meisam; Omidi-Ghallemohamadi, Mehrdad; Khonakdar, Hossein Ali

2017-09-01

New self-colored aromatic-polyamide (PA) nanocomposites containing azo and naphthalene chromophores were prepared with azo-dye surface-modified ZnO nanoparticles (SMZnO) using solution method in dimethylformamide. The X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) results showed the uniform distribution for ZnO nanoparticles in the PA matrix. The UV-vis spectra of PA/ZnO nanocomposites (PANC) showed a blue shift as well as reduction in absorbance intensities and the photoluminescence studies revealed that the increasing intensities of the violet emission in SMZnO loading. From thermo gravimetric analysis (TGA), the temperature at 10% mass loss (T10) increased from 291.8 °C to 387.6 °C for PANC containing 8 mass% of SMZnO, as well as the char yield enhanced significantly, which was about 23.5% higher than the neat PA. The peak heat release rate resulted from microscale combustion calorimeter (MCC), by 8 mass% loading of SMZnO, decreased about 56.9% lower than the neat PA.

Galvanostatically deposited Fe: MnO2 electrodes for supercapacitor application

NASA Astrophysics Data System (ADS)

Dubal, D. P.; Kim, W. B.; Lokhande, C. D.

2012-01-01

The present investigation describes the addition of iron (Fe) in order to improve the supercapacitive properties of MnO2 electrodes using galvanostatic mode. These amorphous worm like Fe: MnO2 electrodes are characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDAX), Fourier transform infrared spectroscopy (FTIR) and wettability test. The supercapacitive properties of MnO2 and Fe: MnO2 electrodes are investigated using cyclic voltammetry, chronopotentiometry and impedance techniques. It is seen that the supercapacitance increases with increase in Fe doping concentration and achieved a maximum of 173 F g-1 at 2 at% Fe doping. The maximum supercapacitance obtained is 218 F g-1 for 2 at% Fe: MnO2 electrode. This hydrous binary oxide exhibited ideal capacitive behavior with high reversibility and high pulse charge-discharge property between -0.1 and +0.9 V/SCE in 1 M Na2SO4 electrolyte indicating a promising electrode material for electrochemical supercapacitors.

Nitrogen enriched mesoporous organic polymer anchored copper(II) material: an efficient and reusable catalyst for the synthesis of esters and amides from aromatic systems.

PubMed

Molla, Rostam Ali; Iqubal, Md Asif; Ghosh, Kajari; Kamaluddin; Islam, Sk Manirul

2015-04-14

A new copper-grafted mesoporous poly-melamine-formaldehyde (Cu-mPMF) has been synthesized from melamine and paraformaldehyde in DMSO medium, followed by grafting of Cu(ii) at its surface. Cu-mPMF has been characterized by elemental analysis, powder XRD, HR TEM, FE-SEM, N2 adsorption study, FT-IR, UV-vis DRS, TGA-DTA, EPR spectroscopy, Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The Cu-grafted mesoporous material showed very good catalytic activity in methyl esterification of benzylic alcohols and amidation of nitriles. Moreover, the catalyst is easily recoverable and can be reused seven times without appreciable loss of catalytic activity in the above reactions. The highly dispersed and strongly bound Cu(ii) sites in the Cu-grafted mesoporous polymer could be responsible for the observed high activities of the Cu-mPMF catalyst. Due to strong binding with the functional groups of the polymer, no evidence of leached copper from the catalyst during the course of reaction emerged, suggesting true heterogeneity in the catalytic process.

Photocatalytic studies of electrochemically synthesized polysaccharide-functionalized ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Kaur, Simranjeet; Kaur, Harpreet

2018-05-01

The present work reports the electrochemical synthesis of polysaccharide-functionalized ZnO nanoparticles using sodium hydroxide, starch, and zinc electrodes for the degradation of cationic dye (Rhodamine-B) under sunlight. Physiochemical properties of synthesized sample have been characterized by different techniques such as XRD, TEM, FESEM, EDS, IR, and UV-visible spectroscopic techniques. The influence of various factors such as effect of dye concentration, contact time, amount of photocatalyst, and pH has been studied. The results obtained from the photodegradation study showed that degradation rate of Rhodamine-B dye has been increased with increase of amount of photocatalyst and decreased with increase in initial dye concentration. Furthermore, the kinetics of the degradation has been investigated. It has been found that the photodegradation of Rhodamine-B dye follows pseudo-first-order kinetics and prepared photocatalyst can effectively degrade the cationic dye. Thus, this ecofriendly and efficient photocatalyst can be used for the treatment of dye-contaminated water. This catalyst also showed the antibacterial activity against Bacillus pumilus and Escherichia coli bacterial strains, so the synthesized nanoparticles also have the pharmaceutical properties.

SAPO-34/AlMCM-41, as a novel hierarchical nanocomposite: preparation, characterization and investigation of synthesis factors using response surface methodology

NASA Astrophysics Data System (ADS)

Roohollahi, Hossein; Halladj, Rouein; Askari, Sima; Yaripour, Fereydoon

2018-06-01

SAPO-34/AlMCM-41, as a new hierarchical nanocomposite was successfully synthesized via hydrothermal and dry-gel conversion. In an experimental and statistical study, effect of five input parameters including synthesis period, drying temperature, NaOH/Si, water/dried-gel and SAPO% were investigated on range-order degree of mesochannels and the relative crystallinity. X-ray diffraction (XRD) patterns were recorded to characterize the ordered AlMCM-41 and crystalline SAPO-34 structures. Nitrogen adsorption-desorption technique, scanning electron microscopy (SEM), field-emission SEM (FESEM) equipped with an energy-dispersive X-ray spectroscopy (EDS-Map) and transmission electron microscopy (TEM) were used to study the textural properties, morphology and surface elemental composition. Two reduced polynomials were fitted to the responses with good precision. Further, based on analysis of variances, SAPO% and time duration of dry-gel conversion were observed as the most effective parameters on the composite structure. The hierarchical porosity, narrow pore size distribution, high external surface area and large specific pore volume were of interesting characteristics for this novel nanocomposite.

AgBr/MgBi2O6 heterostructured composites with highly efficient visible-light-driven photocatalytic activity

NASA Astrophysics Data System (ADS)

Zhong, Liansheng; Hu, Chaohao; Zhuang, Jing; Zhong, Yan; Wang, Dianhui; Zhou, Huaiying

2018-06-01

AgBr/MgBi2O6 heterostructured photocatalysts were synthesized by the deposition-precipitation method. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), photoluminescence (PL), and UV-Visible diffuse reflectance spectroscopy (UV-Vis DRS) were employed to examine the phase structure, morphology and optical properties of the as-prepared samples. The photocatalytic activity was investigated by decomposing methylene blue (MB) solution under visible light irradiation (λ > 420 nm). AgBr/MgBi2O6 composites exhibited significantly enhanced visible-light-driven photocatalytic properties in comparison with pure MgBi2O6 and AgBr. When the molar ratio of AgBr to MgBi2O6 was 3:1, the composite catalyst showed the optimal photocatalytic activity and excellent stability. The enhanced photocatalytic activity of AgBr/MgBi2O6 composites was attributed to the formation of p-n heterojunction between AgBr and MgBi2O6, thereby resulting in the effective separation and transfer of photogenerated electrons-hole pairs.

Ultraviolet photosensor based on few layered reduced graphene oxide nanosheets

NASA Astrophysics Data System (ADS)

Shelke, Nitin T.; Karche, B. R.

2017-10-01

Reduced graphene oxide (RGO), a two-dimensional (2D) system, has attracted much interest in photonic applications owing to its ability to absorb light over a broad wavelength. This leads to several studies on RGO-based photosensors. In this paper, chemical oxidation of graphite was carried out at room temperature for the preparation of large area reduced graphene oxide using a modified Hummer's method. The as-prepared reduced graphene oxide was characterized by XRD, Raman spectroscopy, FESEM, and TEM to confirm the absence of impurities and to ascertain their morphology. In addition, the as-prepared reduced graphene oxide for its possible application as UV photosensor is reported. The electric and optoelectronic properties of RGO based UV photosensor shows a fast response and recovery time of 1 s and 3 s; high photoresponsitivity (3.74 AW-1) and quantum efficiency (1274%) indicating that the graphene oxide is an important material for high performance photosensor. This work demonstrates the ultrafast photoresponse with high photoresponsivity, proving its potential as a promising material for optoelectronic devices.

Fabrication and Characterization of New Composite Tio2 Carbon Nanofiber Anodic Catalyst Support for Direct Methanol Fuel Cell via Electrospinning Method.

PubMed

Abdullah, N; Kamarudin, S K; Shyuan, L K; Karim, N A

2017-12-06

Platinum (Pt) is the common catalyst used in a direct methanol fuel cell (DMFC). However, Pt can lead towards catalyst poisoning by carbonaceous species, thus reduces the performance of DMFC. Thus, this study focuses on the fabrication of a new composite TiO 2 carbon nanofiber anodic catalyst support for direct methanol fuel cells (DMFCs) via electrospinning technique. The distance between the tip and the collector (DTC) and the flow rate were examined as influencing parameters in the electrospinning technique. To ensure that the best catalytic material is fabricated, the nanofiber underwent several characterizations and electrochemical tests, including FTIR, XRD, FESEM, TEM, and cyclic voltammetry. The results show that D18, fabricated with a flow rate of 0.1 mLhr -1 and DTC of 18 cm, is an ultrafine nanofiber with the smallest average diameter, 136.73 ± 39.56 nm. It presented the highest catalyst activity and electrochemical active surface area value as 274.72 mAmg -1 and 226.75m 2  g -1 PtRu , respectively, compared with the other samples.

Synthesis and property of novel MnO2@polypyrrole coaxial nanotubes as electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Yao, Wei; Zhou, Hui; Lu, Yun

2013-11-01

Novel MnO2@polypyrrole (PPy) coaxial nanotubes have been prepared via a simple and green approach without any surfactant and additional oxidant. Under the acidic condition, MnO2 nanotubes act as both template and oxidant to initiate the polymerization of pyrrole monomers on its fresh-activated surface. Fourier transform infrared spectra (FT-IR), X-ray diffraction patterns (XRD), thermo-gravimetric analysis data (TG) and X-ray photoelectron spectra (XPS) suggest the formation of composite structure of MnO2@PPy. Also, FESEM and TEM images intuitively confirm that the PPy shell is coated uniformly on the surface of MnO2 nanotubes. Adjusting the concentrations of sulfuric acid or adding oxidant can modulate the morphology of the products accordingly. Due to the synergic effect between MnO2 core and PPy shell, the MnO2@PPy coaxial nanotubes possess better rate capability, larger specific capacitance of 380 F g-1, doubling the specific capacitance of MnO2 nanotubes, and good capacitance retention of 90% for its initial capacitance after 1000 cycles.

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

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

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

Facile synthesis and color-tunable properties of BaLuF5:Ce,Tb,Eu(Sm) submicrospheres via a facile ionic liquid/EG two-phase system.

PubMed

Song, Yanhua; Li, Yi; Zhao, Tianqi; Wang, Yuexin; Cui, Tingting; Sheng, Ye; Zheng, Keyan; Zhou, Xiuqing; You, Hongpeng; Zou, Haifeng

2017-02-01

BaLuF 5 :Ce,Tb,Eu(Sm) submicrospheres were synthesized via an ILs/ethylene glycol(EG) two-phase system. The crystalline phase, size, morphology, and luminescence properties were characterized using powder X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), photoluminescence (PL) spectra. The results show that 1-methyl-3-octylimidazolium hexafluorophosphate ([Omim]PF 6 ) was used as fluoride source and capping agent to tune morphology and size of the crystals. The formation mechanism has been supposed. Under the excitation of ultraviolet, the BaLuF 5 :5%Ce 3+ ,5%Tb 3+ , BaLuF 5 :Eu 3+ , and BaLuF 5 :5%Ce 3+ ,5%Sm 3+ exhibit green and red emission, which was derived from Tb 3+ , Eu 3+ , and Sm 3+ emission. When codoping Ce 3+ , Tb 3+ , Sm 3+ or Eu 3+ together, multi-color emission can be realized. Furthermore, this synthetic route may have potential applications for fabricating other lanthanide fluorides. Copyright © 2016 Elsevier Inc. All rights reserved.

Synthesis and electrochemical performance of polyaniline @MnO2/graphene ternary composites for electrochemical supercapacitors

NASA Astrophysics Data System (ADS)

Pan, Chao; Gu, Haiteng; Dong, Li

2016-01-01

We introduce a facile method to construct new ternary hierarchical nanocomposites by combining MnO2 coated one dimensional (1D) conducting polyaniline (PANI) nanowires with 2D graphene sheets (GNs). The hierarchical nanocomposite structures of PANI@MnO2/GNs (PMGNs) are further proved by X-ray diffraction (XRD), FT-IR, field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), thermogravimetric analysis (TGA), and X-ray photoelectron spectroscopy (XPS). The electrochemical characteristics of the electrodes made of the hierarchical structured PMGNs materials are determined by the CV and galvanostatic measurements. These electrochemical tests indicate that electrodes made of the nanostructured PMGNs exhibit an improved reversible capacitance of 695 F g-1 after 1000 cycles at a high current density of 4 A g-1. The ternary composites possess higher electrochemical capacitance than each individual component as supercapacitor electrode materials. Such intriguing electrochemical performance is mainly attributed to the synergistic effects of MnO2, PANI and graphene. The hierarchical ternary nanocomposites show excellent electrochemical properties for energy storage applications, which evidence their potential application as supercapacitors.

Microemulsion-mediated solvothermal synthesis of tin(IV) hydrogen phosphate rose-like three-dimensional nanostructures and their electrochemical properties

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

Yang Hui; He Xiaoyan; Cao Minhua

2009-03-05

Novel rose-like three-dimensional Sn(HPO{sub 4}){sub 2}.H{sub 2}O nanostructures self-assembled by tightly stacked nanopetals were successfully synthesized by a simple cetyltrimethylammonium bromide (CTAB)/water/cyclohexane/n-pentanol microemulsion system under solvothermal conditions for the first time. A series of compared experiments were carried out to investigate the factors that influence the morphology and size of the products. It was found that the molar ratio of water to CTAB and the concentration of SnCl{sub 4} aqueous solution play important roles in the formation of the rose-like nanostructures. A possible formation mechanism of rose-like nanostructures was proposed, which may be related to the crystal structure of Sn(HPO{submore » 4}){sub 2}.H{sub 2}O and the spherical micelles formed by the microemulsion. The electrochemical properties of Sn(HPO{sub 4}){sub 2}.H{sub 2}O were investigated through cyclic voltammetry (CV) measurements. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and field-emission scanning electron microscope (FE-SEM) were used to characterize the products.« less

Photocatalytic ability of Bi6Ti3WO18 nanoparticles with a mix-layered Aurivillius structure

NASA Astrophysics Data System (ADS)

Mi, Longqing; Feng, Yongyi; Cao, Lei; Xue, Mingqiang; Qin, Chuanxiang; Huang, Yanlin; Qin, Lin; Seo, Hyo Jin

2018-01-01

Aurivillius phase layered perovskites Bi6Ti3WO18 was prepared by the sol-gel citrate-complexation synthesis. The sample developed into the plate-like nanoparticles with the exposed (001) facets. The phase formation and structure have been verified via X-ray polycrystalline powder diffraction (XRD) Rietveld refinements. The nanoparticles were investigated via the measurements such as FE-SEM, TEM, EDS, and the surface analyses. UV-Vis absorption data revealed that the Aurivillius compound has a direct band characteristic with the band energy of 2.214 eV. The band structure of Bi6Ti3WO18 nanoparticles was discussed on the base of the experiments and theoretical calculation. Bi3+-containing Aurivillius Bi6Ti3WO18 shows efficient photocatalytic degradation for rhodamine B dye (RhB) with the visible light irradiation ( λ > 420 nm). Dynamic characteristic of the light-created excitons was measured by the luminescence and decay lifetime. The multivalent properties of W and Ti ions in the Aurivillius-like lattices of Bi6Ti3WO18 photocatalyst were discussed.

Fe-polyaniline composite nanofiber catalyst for chemoselective hydrolysis of oxime.

PubMed

Mahato, Sanjit Kumar; Bhaumik, Madhumita; Maji, Arun; Dutta, Abhijit; Maiti, Debabrata; Maity, Arjun

2018-03-01

A facile chemoselective one-pot strategy for the deprotection of oxime has been developed using Fe 0 -polyaniline composite nanofiber (Fe 0 -PANI), as a catalyst. Nano material based Fe 0 -PANI catalyst has been synthesized via in-situ polymerization of ANI monomer and followed by reductive deposition of Fe 0 onto PANI matrix. The catalyst was characterized by FE-SEM, HR-TEM, BET, XRD, ATR-FTIR, XPS and VSM techniques. The scope of the transformation was studied for aryl, alkyl and heteroarylketoxime with excellent chemoselectivity (>99%). Mechanistic investigations suggested the involvement of a cationic intermediate with Fe 3+ active catalytic species. Substituent effect showed a linear free energy relationship. The activation energy (E a ) was calculated to be 17.46 kJ mol -1 for acetophenone oxime to acetophenone conversion. The recyclability of the catalyst demonstrated up to 10 cycles without any significant loss of efficiency. Based on the preliminary experiments a plausible mechanism has been proposed involving a carbocationic intermediate. Copyright © 2017 Elsevier Inc. All rights reserved.

Modified WO3 nanorod with Pt nanoparticle as retrievable materials in catalytic and photocatalytic aerobic oxidation of alcohols

NASA Astrophysics Data System (ADS)

Hosseini, Farnaz; Safaei, Elham; Mohebbi, Sajjad

2017-07-01

This study has focused on catalytic and photocatalytic oxidation of aromatic alcohols using WO3 nanorod and a series of Pt/WO3 nanocomposite Pt nanoparticles was loaded on WO3 nanorod with several mass ratios 0.1, 0.2, and 0.3 via a photoreduction process (PRP) and characterized by TEM, FE-SEM imaging, EDAX, XRD, DRS, ICP, and XPS. WO3 nanorods were obtained monodispersed with average 40-nm diameter and square cross section without significant size change by the loading of platinum nanoparticles on it. Progress of oxidation reaction was monitored by GC and the yield of aerobic photocatalytic oxidation of alcohols reached up to 98% for Pt/WO3 and 69% for WO3 while, no oxidation was detected in the absence of light. The highest photocatalytic performance was obtained for mass ratio 0.2 with the selectivity >99%. So, this nanocomposite has potentials to be used as high-performance heterogeneous catalyst and photocatalyst under visible light irradiation with advantages of high activity, high selectivity, and reusability.

Fabrication and Characterization of New Composite Tio2 Carbon Nanofiber Anodic Catalyst Support for Direct Methanol Fuel Cell via Electrospinning Method

NASA Astrophysics Data System (ADS)

Abdullah, N.; Kamarudin, S. K.; Shyuan, L. K.; Karim, N. A.

2017-12-01

Platinum (Pt) is the common catalyst used in a direct methanol fuel cell (DMFC). However, Pt can lead towards catalyst poisoning by carbonaceous species, thus reduces the performance of DMFC. Thus, this study focuses on the fabrication of a new composite TiO2 carbon nanofiber anodic catalyst support for direct methanol fuel cells (DMFCs) via electrospinning technique. The distance between the tip and the collector (DTC) and the flow rate were examined as influencing parameters in the electrospinning technique. To ensure that the best catalytic material is fabricated, the nanofiber underwent several characterizations and electrochemical tests, including FTIR, XRD, FESEM, TEM, and cyclic voltammetry. The results show that D18, fabricated with a flow rate of 0.1 mLhr-1 and DTC of 18 cm, is an ultrafine nanofiber with the smallest average diameter, 136.73 ± 39.56 nm. It presented the highest catalyst activity and electrochemical active surface area value as 274.72 mAmg-1 and 226.75m2 g-1 PtRu, respectively, compared with the other samples.

Synthesis, characterization and properties of carbon nanotubes microspheres from pyrolysis of polypropylene and maleated polypropylene

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

Zhang, Junhao, E-mail: jhzhang6@mail.ustc.edu.cn; Department of Chemistry, University of Science and Technology of China, Heifei, Anhui 230026; Du, Jin

Microspheres assembled from carbon nanotubes (MCNTs), with the diameters ranging from 5.5 to 7.5 {mu}m, were synthesized by means of pyrolysis of polypropylene and maleated polypropylene in an autoclave. The characterization of structure and morphology was carried out by X-ray diffractometer (XRD), field-emission scanning electron microscopy (FESEM), (high resolution) transmission electron microscope [(HR)TEM)], selected-area electron diffraction (SAED) and Raman spectrum. As a typical morphology, the possible growth process of MCNTs was also investigated and discussed. The results of nitrogen adsorption-desorption indicate that the Brunauer-Emett-Teller (BET) surface area (140.6 m{sup 2}/g) of the MCNTs obtained at 600 {sup o}C is aboutmore » twice as that (74.5 m{sup 2}/g) of carbon nanotubes obtained at 700 {sup o}C. The results of catalytic experiment show that MCNTs based catalyst has higher catalytic activity than the carbon nanotubes based catalyst for the preparation of methanol and dimethoxy-ethane by oxidation of dimethyl ether.« less

Synthesis and characterization of the NiFe2O4@TEOS-TPS@Ag nanocomposite and investigation of its antibacterial activity

NASA Astrophysics Data System (ADS)

Allafchian, Ali R.; Jalali, S. A. H.; Amiri, R.; Shahabadi, Sh.

2016-11-01

In this study, the NiFe2O4 was embedded in (3-mercaptopropyl) trimethoxysilane (TPS) and tetraethyl orthosilicate (TEOS) using the sol-gel method. These compounds were used as the support of Ag nanoparticles (Ag NPs). The NiFe2O4@TEOS-TPS@Ag nanocomposites were obtained with the development of bonding between the silver atoms of Ag NPs and the sulfur atoms of TPS molecule. Field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) were used for the characterization of the Ag nanocomposites. Also, the magnetic properties of these nanocomposites were studied by using a vibrating sample magnetometer (VSM) technique. The disk diffusion, minimum inhibition concentration (MIC) and minimum bactericidal concentrations (MBC) tests were used for the investigation of the antibacterial effect of this nanocomposite against bacterial strains. The synthesized nanocomposite presented high reusability and good antibacterial activity against gram-positive and gram-negative bacteria. Remarkably, this nanocomposite could be easily removed from the disinfected media by magnetic decantation.

Nd2O3-SiO2 nanocomposites: A simple sonochemical preparation, characterization and photocatalytic activity.

PubMed

Zinatloo-Ajabshir, Sahar; Mortazavi-Derazkola, Sobhan; Salavati-Niasari, Masoud

2018-04-01

Nd 2 O 3 -SiO 2 nanocomposites with enhanced photocatalytic activity have been obtained through simple and rapid sonochemical route in presence of putrescine as a new basic agent, for the first time. The influence of the mole ratio of Si:Nd, basic agent and ultrasonic power have been optimized to obtain the best Nd 2 O 3 -SiO 2 nanocomposites on shape, size and photocatalytic activity. The produced Nd 2 O 3 -SiO 2 nanocomposites have been characterized utilizing XRD, EDX, TEM, FT-IR, DRS and FESEM. Application of the as-formed Nd 2 O 3 -SiO 2 nano and bulk structures as photocatalyst with photodegradation of methyl violet contaminant under ultraviolet illumination was compared. Results demonstrated that SiO 2 has remarkable effect on catalytic performance of Nd 2 O 3 photocatalyst for decomposition. By introducing of SiO 2 to Nd 2 O 3 , decomposition efficiency of Nd 2 O 3 toward methyl violet contaminant under ultraviolet illumination was increased. Copyright © 2017 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2015-09-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-10-01

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

Micelle-Assisted Synthesis of Al2O3 ·CaO Nanocatalyst: Optical Properties and Their Applications in Photodegradation of 2,4,6-Trinitrophenol

PubMed Central

Imtiaz, Ayesha; Khaleeq-ur-rahman, Muhammad; Adnan, Rohana

2013-01-01

Calcium oxide (CaO) nanoparticles are known to exhibit unique property due to their high adsorption capacity and good catalytic activity. In this work the CaO nanocatalysts were prepared by hydrothermal method using anionic surfactant, sodium dodecyl sulphate (SDS), as a templating agent. The as-synthesized nanocatalysts were further used as substrate for the synthesis of alumina doped calcium oxide (Al2O3 ·CaO) nanocatalysts via deposition-precipitation method at the isoelectric point of CaO. The Al2O3 ·CaO nanocatalysts were characterized by FTIR, XRD, TGA, TEM, and FESEM techniques. The catalytic efficiencies of these nanocatalysts were studied for the photodegradation of 2,4,6-trinitrophenol (2,4,6-TNP), which is an industrial pollutant, spectrophotometrically. The effect of surfactant and temperature on size of nanocatalysts was also studied. The smallest particle size and highest percentage of degradation were observed at critical micelle concentration of the surfactant. The direct optical band gap of the Al2O3 ·CaO nanocatalyst was found as 3.3 eV. PMID:24311980

Synthesis of Fluorinated Graphene/CoAl-Layered Double Hydroxide Composites as Electrode Materials for Supercapacitors.

PubMed

Peng, Weijun; Li, Hongqiang; Song, Shaoxian

2017-02-15

CoAl-layered double hydroxide/fluorinated graphene (CoAl-LDH/FGN) composites were fabricated via a two-step hydrothermal method. The synthesized CoAl-LDH/FGN composites have been characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and electrochemical measurements. The results indicated that the fluorinated carbon with various configuration forms were grafted onto the framework of graphene, and the C-F bond configuration and fluorine content could be tuned by the fluorination time. Most of semi-ionic C-F bonds were formed at an appropriate fluorination time and, then, converted into fluorine rich surface groups (such as CF 2 , CF 3 , etc.) which were electrochemically inactive as the fluorination time prolonged. Moreover, the CoAl-LDH/FGN composites prepared at the optimal fluorination time exhibited the highest specific capacitance (1222 F/g at 1 A/g), the best rate capability, and the most stable capacitance retention, which offered great promise as electrode materials for supercapacitors.

Humidity sensing behavior of tin-loaded 3-D cubic mesoporous silica

NASA Astrophysics Data System (ADS)

Poonia, Ekta; Dahiya, Manjeet S.; Tomer, Vijay K.; Kumar, Krishan; Kumar, Sunil; Duhan, Surender

2018-07-01

The present scientific investigation deals with template synthesis of 3D-cubic mesoporous KIT-6 with in-situ loading of SnO2 to obtain a material with enhanced number of surface active sites. The structural insights have been reported through analysis of XRD, TEM, FESEM, N2 sorption and mid-IR absorption data. X-ray diffraction confirmed 3D-cubic mesoporous structure of silica with Ia 3 bar d symmetry and existence of anatase SnO2 species. A decrease in surface area on loading of SnO2 nanoparticles is revealed via analysis of N2 adsorption-desorption isotherms. Rapid response time of 15 s and super rapid recovery time of 2 s (with response > 100) have been exhibited by sensor based on sample containing 1 wt% of SnO2. Further investigation on sensing performance of nanocomposite with 1 wt% of SnO2 confirmed its ohmic behavior (with negligible V-I hysteresis), excellent cycle stability, outstanding long term stability and very low hysteresis (1.4% at 53% RH).

Synthesis and luminescence properties of cinnamide based nanohybrid materials containing Eu (II) ions

NASA Astrophysics Data System (ADS)

Kiran Kumar, A. B. V.; Jayasimhadri, M.; Cha, Hyeongrae; Chen, Kuangcai; Lim, Jae-Min; Lee, Yong-Ill

2011-07-01

In the present work, the cinnamide based organic-inorganic hybrid luminescent materials were prepared by using sol-gel technique, in which both the components are covalently linked via Si-C bonds. The organic precursor N-(3-(triethoxysilyl)propyl)cinnamide (Cn-Si) was synthesized by (3-aminopropyl) triethoxysilane being reacted with cinnamoyal chloride. Finally, novel hybrid materials were prepared successfully through hydrolysis and polycondensation processes between the alkoxide groups of precursors Cn-Si and tetraethylorthosilane (TEOS) in the presence of europium nitrate. We have characterized thoroughly the prepared samples using FT-IR, thermal analysis (TGA/DTA), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), energy-dispersive spectroscopy (EDS) and photoluminescence (PL) spectroscopy. The results indicate that these materials exhibit the excellent thermal stability up to 350 °C. The X-ray diffraction patterns confirmed the amorphous nature of the developed materials. The rare-earth doped hybrid materials have exhibited an intense green emission at 530 nm with CIE chromaticity coordinates (0.4801, 0.4669). Whereas, the un-doped one gives some remarkable blue emission properties under UV excitation.

Facile synthesis of Nb2O5 nanobelts assembled from nanorods and their applications in lithium ion batteries

NASA Astrophysics Data System (ADS)

Liu, Xiaodi; Liu, Guangyin; Chen, Hao; Ma, Jianmin; Zhang, Ruixue

2017-12-01

Hierarchical 1D Nb2O5 nanobelts are successfully synthesized via a facile solvothermal method and following thermal treatment. The as-formed Nb2O5 nanobelts are characterized by XRD, FESEM, TEM, and BET, and the results indicate that they possess pseudohexagonal structure and are composed of ultranarrow nanorods with an average diameter of ca. 15 nm. When used as anodic materials for lithium ion batteries, the obtained Nb2O5 nanobelts can deliver initial discharge capacities of 209.3 mAh g-1 at the current density of 0.5 C. In addition, the Nb2O5 nanobelts exhibit a reversible capacity of 95.8 mAh g-1 after 200 cycles at relatively high current density of 5 C. The good electrochemical performance of the Nb2O5 nanobelts may be ascribed to their good monodispersity, high specific surface areas, and narrow rod-like building blocks. The Nb2O5 nanobelts can be developed as promising anodes for high-rate 2 V LIBs with good safety.

Fe2O3/ZnO/ZnFe2O4 composites for the efficient photocatalytic degradation of organic dyes under visible light

NASA Astrophysics Data System (ADS)

Li, Xiaojuan; Jin, Bo; Huang, Jingwen; Zhang, Qingchun; Peng, Rufang; Chu, Shijin

2018-06-01

In this study, novel ternary Fe2O3/ZnO/ZnFe2O4 (ZFO) composites were successfully prepared through a simple hydrothermal reaction with subsequent thermal treatment. The as-prepared products were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Brunauer-Emmett-Teller (BET) analysis, Barrett-Joyner-Halenda (BJH) measurement, and UV-vis diffuse reflectance spectroscopy (UV-vis DRS). The photocatalytic degradation of rhodamine B (Rh B) under visible light irradiation indicated that the ZFO composites calcined at 500 °C has the best photocatalytic activity (the photocatalytic degradation efficiency can reach up to 95.7% within 60 min) and can maintain a stable photocatalytic degradation efficiency for at least three cycles. In addition, the photocatalytic activity of ZFO composites toward dye decomposition follows the order cationic Rh B > anionic methyl orange. Finally, using different scavengers, superoxide and hydroxyl radicals were identified as the primary active species during the degradation reaction of Rh B.

Doping effect on SILAR synthesized crystalline nanostructured Cu-doped ZnO thin films grown on indium tin oxide (ITO) coated glass substrates and its characterization

NASA Astrophysics Data System (ADS)

Dhaygude, H. D.; Shinde, S. K.; Velhal, Ninad B.; Takale, M. V.; Fulari, V. J.

2016-08-01

In the present study, a novel chemical route is used to synthesize the undoped and Cu-doped ZnO thin films in aqueous solution by successive ionic layer adsorption and reaction (SILAR) method. The synthesized thin films are characterized by x-ray diffractometer (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive x-ray analysis (EDAX), contact angle goniometer and UV-Vis spectroscopic techniques. XRD study shows that the prepared films are polycrystalline in nature with hexagonal crystal structure. The change in morphology for different doping is observed in the studies of FE-SEM. EDAX spectrum shows that the thin films consist of zinc, copper and oxygen elements. Contact angle goniometer is used to measure the contact angle between a liquid and a solid interface and after detection, the nature of the films is initiated from hydrophobic to hydrophilic. The optical band gap energy for direct allowed transition ranging between 1.60-2.91 eV is observed.

Facile synthesis of one dimensional ZnO nanostructures for DSSC applications

NASA Astrophysics Data System (ADS)

Marimuthu, T.; Anandhan, N.

2016-05-01

Development of zinc oxide (ZnO) nanostructure based third generation dye sensitized solar cell is interesting compared to conventional silicon solar cells. ZnO nanostructured thin films were electrochemically deposited onto fluorine doped tin oxide (FTO) glass substrate. The effect of ethylene-diamine-tetra-acetic acid (EDTA) on structural, morphological and optical properties is investigated using X-ray diffraction (XRD) meter, field emission scanning electron microscope (FE-SEM) and micro Raman spectroscopy. XRD patterns reveal that the prepared nanostructures are hexagonal wutrzite structures with (101) plane orientation, the nanostructure prepared using EDTA exhibits better crystallinity. FE-SEM images illustrate that the morphological changes are observed from nanorod structure to cauliflower like structure as EDTA is added. Micro Raman spectra predict that cauliflower like structure possesses a higher crystalline nature with less atomic defects compared to nanorod structures. Dye sensitized solar cell (DSSC) is constructed for the optimized cauliflower structure, and open circuit voltage, short circuit density, fill factor and efficiency are estimated from the J-V curve.

Assessment of morphology and property of graphene oxide-hydroxypropylmethylcellulose nanocomposite films.

PubMed

Ghosh, Tapas Kumar; Gope, Shirshendu; Mondal, Dibyendu; Bhowmik, Biplab; Mollick, Md Masud Rahaman; Maity, Dipanwita; Roy, Indranil; Sarkar, Gunjan; Sadhukhan, Sourav; Rana, Dipak; Chakraborty, Mukut; Chattopadhyay, Dipankar

2014-05-01

Graphene oxide (GO) was synthesized by Hummer's method and characterized by using Fourier transform infrared spectroscopy and Raman spectroscopy. The as synthesized GO was used to make GO/hydroxypropylmethylcellulose (HPMC) nanocomposite films by the solution mixing method using different concentrations of GO. The nanocomposite films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and thermo-gravimetric analysis. Mechanical properties, water absorption property and water vapor transmission rate were also measured. XRD analysis showed the formation of exfoliated HPMC/GO nanocomposites films. The FESEM results revealed high interfacial adhesion between the GO and HPMC matrix. The tensile strength and Young's modulus of the nanocomposite films containing the highest weight percentage of GO increased sharply. The thermal stability of HPMC/GO nanocomposites was slightly better than pure HPMC. The water absorption and water vapor transmission rate of HPMC film was reduced with the addition of up to 1 wt% GO. Copyright © 2014 Elsevier B.V. All rights reserved.

Sol-gel synthesis and characterizations of crystalline NaGd(WO4)2 powder for anisotropic transparent ceramic laser application

NASA Astrophysics Data System (ADS)

Durairajan, A.; Thangaraju, D.; Balaji, D.; Moorthy Babu, S.

2013-02-01

NaGd(WO4)2 powders were synthesized at different pH (3.5, 4.5, 5.5, 6.5 and 7.5) values by conventional Pechini method. Sodium and gadolinium nitrate salts and ammonium paratungstate are used as starting precursors. Metal cations were chelated by citric acid and individual citrates were bound together with ethylene glycol. Synthesized gel was analyzed using differential thermal analysis (DTA), thermo gravimetric (TG) and FT-IR spectroscopy to understand the degradation of gel and formation of metal citrates. Calcined powders (250, 600, 700 and 800 °C) were characterized by powder XRD, FT-IR, Raman and FE-SEM analysis. The temperature dependent phase formation was examined by powder XRD. The morphological changes at different pH derived powders were observed with FE-SEM micrographs. Stepwise organic liberation with respect to temperature and presence of carbon content in the pre-fired powder were analyzed using FT-IR analysis. Raman spectrum reveals disordered tungstate vibrations in the NGW matrix.

Electrical properties of Mg doped ZnO nanostructure annealed at different temperature

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

Mohamed, R., E-mail: ruziana12@gmail.com; Mamat, M. H., E-mail: hafiz-030@yahoo.com; Rusop, M., E-mail: nanouitm@gmail.com

In this work, ZincOxide (ZnO) nanostructures doped with Mg were successfully grown on the glass substrate. Magnesium (Mg) metal element was added in the ZnO host which acts as a doping agent. Different temperature in range of 250°C to 500°C was used in order to investigate the effect of annealing temperature of ZnO thin films. Field Emission Scanning Electron Microscopy (FESEM) was used to investigate the physical characteristic of ZnO thin films. FESEM results have revealed that ZnO nanorods were grown vertically aligned. The structural properties were determined by using X-Ray Diffraction (XRD) analysis. XRD results showed Mg doped ZnOmore » thin have highest crystalinnity at 500°C annealing temperature. The electrical properties were investigating by using Current-Voltage (I-V) measurement. I-V measurement showed the electrical properties were varied at different annealing temperature. The annealing temperature at 500°C has the highest electrical conductance properties.« less

Influence of etching current density on microstructural, optical and electrical properties of porous silicon (PS):n-Si heterostructure

NASA Astrophysics Data System (ADS)

Das, M.; Nath, P.; Sarkar, D.

2016-02-01

In this article effect of etching current density (J) on the microstructural, optical and electrical properties of photoelectrochemically prepared heterostructure is reported. Prepared samples are characterized by FESEM, XRD, UV-Visible, Raman and photoluminescence (PL) spectra and current-voltage (I-V) characteristics. FESEM shows presence of mixture of randomly distributed meso- and micro-pores. Porous layer thickness determined by cross section view of SEM is proportional to J. XRD shows crystalline nature but gradually extent of crystallinity decreases with increasing J. Raman spectra show large red-shift and asymmetric broadening with respect to crystalline silicon (c-Si). UV-visible reflectance and PL show blue shift in peaks with increasing J. The I-V characteristics are analyzed by the conventional thermionic emission (TE) model and Cheung's model to estimate the barrier height (φb), ideality factor (n) and series resistance (Rs) for comparison between the two models. The latter model is found to fit better.

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

NASA Astrophysics Data System (ADS)

Shariati, Mohsen

2015-07-01

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

Metal copper films deposited on cenosphere particles by magnetron sputtering method

NASA Astrophysics Data System (ADS)

Yu, Xiaozheng; Xu, Zheng; Shen, Zhigang

2007-05-01

Metal copper films with thicknesses from several nanometres to several micrometres were deposited on the surface of cenosphere particles by the magnetron sputtering method under different working conditions. An ultrasonic vibrating generator equipped with a conventional magnetron sputtering apparatus was used to prevent the cenosphere substrates from accumulating during film growth. The surface morphology, the chemical composition, the average grain size and the crystallization of cenosphere particles were characterized by field emission scanning electron microscopy (FE-SEM), inductively coupled plasma-atom emission spectrometer, x-ray photoelectron spectroscopy and x-ray diffraction (XRD) analysis, respectively, before and after the plating process. The results indicate that the copper films were successfully deposited on cenosphere particles. It was found from the FE-SEM results that the films were well compacted and highly uniform in thickness. The XRD results show that the copper film coated on cenospheres has a face centred cubic structure and the crystallization of the film sample increases with increasing sputtering power.

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

NASA Astrophysics Data System (ADS)

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

2016-07-01

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

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

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

Don Pellinen and Michael Griffin

2009-01-23

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

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

Silver Trees: Chemistry on a TEM Grid

EPA Science Inventory

The copper/carbon substrate of a TEM grid reacted with aqueous silver nitrate solution within minutes to yield spectacular tree-like silver dendrites, without using any added capping or reducing reagents. These results demonstrate a facile, aqueous, room temperature synthesis of...

Design of binary SnO{sub 2}-CuO nanocomposite for efficient photocatalytic degradation of malachite green dye

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

Kumar, Aniket; Rout, Lipeeka; Achary, L. Satish Kumar

2016-04-13

Semiconductor mediated photocatalysis has got enormous consideration as it has shown immense potential in addressing the overall energy and environmental issues. To overcome the earlier drawbacks concerning quick charge recombination and limited visible-light absorption of semiconductor photocatalysts, numerous methods have been produced in the past couple of decades and the most broadly utilized one is to develop the photocatalytic heterojunctions. In our work, a series of SnO{sub 2}-CuO nanocomposites of different compositions were synthesized by a combustion method and have been investigated in detail by various characterization techniques, such as wide angle X-ray diffraction (XRD), UV-vis spectroscopy, transmission electron microscopymore » (TEM), and field emission scanning electron microscopy (FE-SEM). The results revealed that the crystal structure and optical properties of the nanocomposites were almost same for all the compositions. FE-SEM images showed that the shape of SnO{sub 2}-CuO was spherical in nature and the 1: 1 Sn/Cu sample had a well-proportioned morphology. The malachite green dye was used for the photocatalytic studies in a photoreactor and monitored with a UV-visible spectrometer for different composition ratio of metal (Sn: Cu) such as 1:1, 1:2, 2:1, 1:0.5 and 0.5:1. The 1:1 ratio nanocomposite showed excellent photocatalytic degradation of 96 % compared to pure SnO{sub 2} and CuO. The mechanism of degradation and charge separation ability of the nanocomposite are also explored using photocurrent measurement study.« less

Definitive Mineralogical Analysis of Mars Analog Rocks Using the CheMin XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Blake, D. F.; Sarrazin, P.; Bish, D. L.; Feldman, S.; Chipera, S. J.; Vaniman, D. T.; Collins, S.

2004-01-01

Mineral identification is a critical component of Mars Astrobiological missions. Chemical or elemental data alone are not definitive because a single elemental or chemical composition or even a single bonding type can represent a range of substances or mineral assemblages. Minerals are defined as unique structural and compositional phases that occur naturally. There are about 15,000 minerals that have been described on Earth, all uniquely identifiable via diffraction methods. There are likely many minerals yet undiscovered on Earth, and likewise on Mars. If an unknown phase is identified on Mars, it can be fully characterized by structural (X-ray Diffraction, XRD) and elemental analysis (X-ray Fluorescence, XRF) without recourse to other data because XRD relies on the principles of atomic arrangement for its determinations. XRD is the principal means of identification and characterization of minerals on Earth.

Comparison between measured and predicted turbulence frequency spectra in ITG and TEM regimes

NASA Astrophysics Data System (ADS)

Citrin, J.; Arnichand, H.; Bernardo, J.; Bourdelle, C.; Garbet, X.; Jenko, F.; Hacquin, S.; Pueschel, M. J.; Sabot, R.

2017-06-01

The observation of distinct peaks in tokamak core reflectometry measurements—named quasi-coherent-modes (QCMs)—are identified as a signature of trapped-electron-mode (TEM) turbulence (Arnichand et al 2016 Plasma Phys. Control. Fusion 58 014037). This phenomenon is investigated with detailed linear and nonlinear gyrokinetic simulations using the Gene code. A Tore-Supra density scan is studied, which traverses through a linear (LOC) to saturated (SOC) ohmic confinement transition. The LOC and SOC phases are both simulated separately. In the LOC phase, where QCMs are observed, TEMs are robustly predicted unstable in linear studies. In the later SOC phase, where QCMs are no longer observed, ion-temperature-gradient (ITG) modes are identified. In nonlinear simulations, in the ITG (SOC) phase, a broadband spectrum is seen. In the TEM (LOC) phase, a clear emergence of a peak at the TEM frequencies is seen. This is due to reduced nonlinear frequency broadening of the underlying linear modes in the TEM regime compared with the ITG regime. A synthetic diagnostic of the nonlinearly simulated frequency spectra reproduces the features observed in the reflectometry measurements. These results support the identification of core QCMs as an experimental marker for TEM turbulence.

Wild 2 grains characterized combining MIR/FIR/Raman micro-spectroscopy and FE-SEM/EDS analyses

NASA Astrophysics Data System (ADS)

Ferrari, M.; Rotundi, A.; Rietmeijer, F. J. M.; Della Corte, V.; Baratta, G. A.; Brunetto, R.; Dartois, E.; Djouadi, Z.; Merouane, S.; Borg, J.; Brucato, J. R.; Le Sergeant d'Hendecourt, L.; Mennella, V.; Palumbo, M. E.; Palumbo, P.

We present the results of the analyses \\cite{Rotundi14} of two bulk terminal particles (TPs), C2112,7,171,0,0 (TP2) and C2112,9,171,0,0 (TP3), derived from the Jupiter-Family comet 81P/Wild 2 returned by the NASA Stardust mission \\cite{Brownlee06}. Each particle, embedded in a slab of silica aerogel, was pressed in a diamond cell. Aerogel is usually cause of problems when characterizing the minerals and organic materials present in the embedded particles. We overcame this common issue by means of the combination of FE-SEM/EDS, IR and Raman mu -spectroscopy, three non-destructive analytical techniques, which provided bulk mineralogical and organic information on TP2 and TP3. This approach proved to be a practical solution for preliminary characterization, i.e. scanning particles for chemical and mineralogical heterogeneity. Using this type of bulk characterization prior to more detailed studies, could be taken into account as a standard procedure to be followed for selecting Stardust particles-of-interest. TP2 and TP3 are dominated by Ca-free and low-Ca, Mg-rich, Mg,Fe-olivine. The presence of melilite in both particles is supported by IR mu -spectroscopy and corroborated by FE-SEM/EDS analyses, but is not confirmed by Raman mu -spectroscopy possibly because the amount of this mineral is too small to be detected. TP2 and TP3 show similar silicate mineral compositions, but Ni-free, low-Ni, sub-sulfur (Fe,Ni)S grains are present only in TP2. TP2 contains indigenous amorphous carbon hot spots, while no indigenous carbon was identified in TP3. These non-chondritic particles probably originated in a differentiated body. The presence of high temperature melilite group minerals (incl. gehlenite) in TP2 and TP3 reinforces the notion that collisionally-ejected refractory debris from differentiated asteroids may be common in Jupiter-Family comets. This raises the question whether similar debris and other clearly asteroidal particles could be present in Halley-type comets

Synthesis and characterization of nano-hydroxyapatite using Sapindus Mukorossi extract

NASA Astrophysics Data System (ADS)

Subha, B.; Prasath, P. Varun; Abinaya, R.; Kavitha, R. J.; Ravichandran, K.

2015-06-01

Nano-Hydroxyapatite (HAP) powders were successfully synthesised by hydrothermal method using Sapindus Mukorossi extract as an additive. The structural and morphological analyses of thus synthesised powders were carried out using FT-IR, XRD and FESEM/EDX. The FT-IR spectra confirm the presence of phosphate and hydroxyl groups corresponding to HAP. The XRD analysis reveals the formation of HAP phase and found to reduce the crystallite size with addition of Sapindus Mukorossi extract. The morphology changes from sphere to flake shape by the influence of extract.

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Tsuda, H.; Halbig, M. C.; Singh, M.; Hasegawa, Y; Mori, S.; Asthana, R.

2017-01-01

Silicon Carbide (SiC) is a promising material for thermostructural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, Mo-B and TiCu. In this presentation, we report the microstructure of diffusion bonded SA-THX mainly with TiCu interlayers obtained by TEM observations, and the influence of metallic interlayers on the joint microstructure and microhardness will be discussed.

Geoelectrical characterization by joint inversion of VES/TEM in Paraná basin, Brazil

NASA Astrophysics Data System (ADS)

Bortolozo, C. A.; Couto, M. A.; Almeida, E. R.; Porsani, J. L.; Santos, F. M.

2012-12-01

For many years electrical (DC) and transient electromagnetic (TEM) soundings have been used in a great number of environmental, hydrological and mining exploration studies. The data of both methods are interpreted usually by individual 1D models resulting in many cases in ambiguous models. This can be explained by how the two different methodologies sample the subsurface. The vertical electrical sounding (VES) is good on marking very resistive structures, while the transient electromagnetic sounding (TEM) is very sensitive to map conductive structures. Another characteristic is that VES is more sensitive to shallow structures, while TEM soundings can reach deeper structures. A Matlab program for joint inversion of VES and TEM soundings, by using CRS algorithm was developed aiming explore the best of the both methods. Initially, the algorithm was tested with synthetic data and after it was used to invert experimental data from Paraná sedimentary basin. We present the results of a re-interpretation of 46 VES/TEM soundings data set acquired in Bebedouro region in São Paulo State - Brazil. The previous interpretation was based in geoelectrical models obtained by single inversion of the VES and TEM soundings. In this work we present the results with single inversion of VES and TEM sounding inverted by the Curupira Program and a new interpretation based in the joint inversion of both methodologies. The goal is increase the accuracy in determining the underground structures. As a result a new geoelectrical model of the region is obtained.

A Combined XRD/XRF Instrument for Lunar Resource Assessment

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Bish, D. L.; Chipera, S. J.; Blacic, J. D.

1992-01-01

Robotic surface missions to the Moon should be capable of measuring mineral as well as chemical abundances in regolith samples. Although much is already known about the lunar regolith, our data are far from comprehensive. Most of the regolith samples returned to Earth for analysis had lost the upper surface, or it was intermixed with deeper regolith. This upper surface is the part of the regolith most recently exposed to the solar wind; as such it will be important to resource assessment. In addition, it may be far easier to mine and process the uppermost few centimeters of regolith over a broad area than to engage in deep excavation of a smaller area. The most direct means of analyzing the regolith surface will be by studies in situ. In addition, the analysis of the impact-origin regolith surfaces, the Fe-rich glasses of mare pyroclastic deposits, are of resource interest, but are inadequately known; none of the extensive surface-exposed pyroclastic deposits of the Moon have been systematically sampled, although we know something about such deposits from the Apollo 17 site. Because of the potential importance of pyroclastic deposits, methods to quantify glass as well as mineral abundances will be important to resource evaluation. Combined x ray diffraction (XRD) and x ray fluorescence (XRF) analysis will address many resource characterization problems on the Moon. XRF methods are valuable for obtaining full major-element abundances with high precision. Such data, collected in parallel with quantitative mineralogy, permit unambiguous determination of both mineral and chemical abundances where concentrations are high enough to be of resource grade. Collection of both XRD and XRF data from a single sample provides simultaneous chemical and mineralogic information. These data can be used to correlate quantitative chemistry and mineralogy as a set of simultaneous linear equations, the solution of which can lead to full characterization of the sample. The use of

Effect of bismuth doping on the structural and magnetic properties of zinc-ferrite nanoparticles prepared by a microwave combustion method

NASA Astrophysics Data System (ADS)

Shoushtari, Morteza Zargar; Emami, Akram; Ghahfarokhi, Seyed Ebrahim Mosavi

2016-12-01

In this study, we examine the bismuth doping effect on the structural, magnetic and microstructural properties of zinc-ferrite nanoparticles (ZnFe2-xBixO4 with x=0.0, 0.02, 0.04, 0.06, 0.1, 0.15) which have been prepared by a microwave combustion method. The structural, morphological and electromagnetic properties and also Curie temperature of the samples were examined by x-ray powder diffraction (XRD), field emission scanning electron microscope (FESEM), vibrating sample magnetometer (VSM), and LCR meter, respectively. In order to measure the energy band gap, the FTIR spectra of the samples were also considered. The XRD patterns of the samples revealed that all of them are ZnFe2O4 structure and no additional peak was observed in their patterns. This implied that the samples were single-phase up to bismuth solubility of 0.15 in Zinc-Ferrite. The results of XRD patterns also showed that the value lattice parameter increases with increasing the bismuth doping. The FESEM results revealed an ascending trend in the size of the nanoparticles. Also considering the VSM results characterized that an increasing the bismuth doping leads to lower the saturation magnetization. The Curie temperatures of the samples were reduced as a result of increasing the amount of bismuth.

Synthesis and characterization of flower-like CuIn{sub 1-x}Ga{sub x}S{sub 2} (x = 0.3) microspheres

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

Zhong, Jiasong; Xiang, Weidong, E-mail: xiangweidong001@126.com; College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325035

Graphical abstract: In this paper, flower-like CuIn{sub 1-x}Ga{sub x}S{sub 2} (x = 0.3) microspheres were prepared via biomolecule-assisted solvothermal rate with CuCl{sub 2}{center_dot}2H{sub 2}O, GaCl{sub 3}, InCl{sub 3} and L-cystine as raw materials. UV-vis absorption spectrum showed that the band gap of CuIn{sub 0.7}Ga{sub 0.3}S{sub 2} microspheres was about 2.427 eV. Highlights: Black-Right-Pointing-Pointer We reported a small biomolecule-assisted route to synthesis CuIn{sub 0.3}Ga{sub 0.7}S{sub 2}. Black-Right-Pointing-Pointer The possible mechanisms of flower-like CuIn{sub 0.3}Ga{sub 0.7}S{sub 2} microspheres were proposed. Black-Right-Pointing-Pointer The as-prepared CuIn{sub 0.3}Ga{sub 0.7}S{sub 2} products were investigated by XRD, XPS, FESEM and TEM. Black-Right-Pointing-Pointer The optical properties were investigatedmore » by UV-vis spectroscopy and Raman spectrum. -- Abstract: We report the formation and characterization of the flower-like CuIn{sub 1-x}Ga{sub x}S{sub 2} (x = 0.3) microspheres using CuCl{sub 2}{center_dot}2H{sub 2}O, GaCl{sub 3}, InCl{sub 3} and L-cystine in the mixed solvent of ethylene glycol and distilled water (1:2, v/v) at 200 Degree-Sign C for 24 h. XRD results indicated that the CuIn{sub 0.7}Ga{sub 0.3}S{sub 2} nanostructures have a (1 1 2) preferred orientation. The EDS and XPS analyses of the sample revealed that Cu, In, Ga and S were present in an atomic ratio of approximately 1:0.7:0.3:2. FESEM and TEM images showed that the product was microspheres, consisting of nanoplates with the thickness of about 20 nm. The optical properties were investigated by ultraviolet-visible (UV-vis) absorption spectroscopy and Raman spectroscopy. UV-vis absorption spectrum indicated that the band gap of as-synthesized flower-like CuIn{sub 0.7}Ga{sub 0.3}S{sub 2} microspheres was about 2.427 eV. Raman spectrum of the obtained CuIn{sub 0.7}Ga{sub 0.3}S{sub 2} exhibited a high-intensity peak at 302 cm{sup -1} could be assigned as A1-mode.« less

Minimum depth of investigation for grounded-wire TEM due to self-transients

NASA Astrophysics Data System (ADS)

Zhou, Nannan; Xue, Guoqiang

2018-05-01

The grounded-wire transient electromagnetic method (TEM) has been widely used for near-surface metalliferous prospecting, oil and gas exploration, and hydrogeological surveying in the subsurface. However, it is commonly observed that such TEM signal is contaminated by the self-transient process occurred at the early stage of data acquisition. Correspondingly, there exists a minimum depth of investigation, above which the observed signal is not applicable for reliable data processing and interpretation. Therefore, for achieving a more comprehensive understanding of the TEM method, it is necessary to perform research on the self-transient process and moreover develop an approach for quantifying the minimum detection depth. In this paper, we first analyze the temporal procedure of the equivalent circuit of the TEM method and present a theoretical equation for estimating the self-induction voltage based on the inductor of the transmitting wire. Then, numerical modeling is applied for building the relationship between the minimum depth of investigation and various properties, including resistivity of the earth, offset, and source length. It is guide for the design of survey parameters when the grounded-wire TEM is applied to the shallow detection. Finally, it is verified through applications to a coal field in China.

Reduction of Off-Boresight Fields for a TEM Horn Antenna

DTIC Science & Technology

1994-12-01

model predicts the tapers will reduce the diffraction. Experimental results verify the TPS’s ability to reduce the peak off-hureslht ld& for a. TElL horn...diffractin. Experimental results verify the PS’s ability to reduce the fields foi a T14 horn anitnna xi Reduction of Off-Boresight Fields for a TEM Horn...geometry, has a constant amplitude response. Two simple models repiesent a TEM horn - a high frequency model and a low frequency model [5). At high

Characterization of CuCl quantum dots grown in NaCl single crystals via optical measurements, X-ray diffraction, and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Miyajima, Kensuke; Akatsu, Tatsuro; Itoh, Ken

2018-05-01

We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs) embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and transmission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work will play an important role in progressing the study of optical phenomena originating from assembled semiconductor QDs.

Binding of TEM-1 beta-lactamase to beta-lactam antibiotics by frontal affinity chromatography.

PubMed

Chen, Xiu; Li, Yuhua; Zhang, Yan; Yang, Jianting; Bian, Liujiao

2017-04-15

TEM-1 beta-lactamases can accurately catalyze the hydrolysis of the beta-lactam rings in beta-lactam antibiotics, which make beta-lactam antibiotics lose its activity, and the prerequisite for the hydrolysis procedure in the binding interaction of TEM-1 beta-lactamases with beta-lactam antibiotics is the beta-lactam rings in beta-lactam antibiotics. Therefore, the binding of TEM-1 beta-lactamase to three beta-lactam antibiotics including penicillin G, cefalexin as well as cefoxitin was explored here by frontal affinity chromatography in combination with fluorescence spectra, adsorption and thermodynamic data in the temperature range of 278-288K under simulated physiological conditions. The results showed that all the binding of TEM-1 beta-lactamase to the three antibiotics were spontaneously exothermic processes with the binding constants of 8.718×10 3 , 6.624×10 3 and 2.244×10 3 (mol/L), respectively at 288K. All the TEM-1 beta-lactamases were immobilized on the surface of the stationary phase in the mode of monolayer and there existed only one type of binding sites on them. Each TEM-1 beta-lactamase bound with only one beta-lactam antibiotic and hydrogen bond interaction and Van der Waals force were the main forces between them. This work provided an insight into the binding interactions between TEM-1 beta-lactamases and beta-lactam antibiotics, which may be beneficial for the designing and developing of new substrates resistant to TEM-1 beta-lactamases. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparative investigation of Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) in the determination of cotton fiber crystallinity.

PubMed

Liu, Yongliang; Thibodeaux, Devron; Gamble, Gary; Bauer, Philip; VanDerveer, Don

2012-08-01

Despite considerable efforts in developing curve-fitting protocols to evaluate the crystallinity index (CI) from X-ray diffraction (XRD) measurements, in its present state XRD can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous fraction in a sample. The greatest barrier to establishing quantitative XRD is the lack of appropriate cellulose standards, which are needed to calibrate the XRD measurements. In practice, samples with known CI are very difficult to prepare or determine. In a previous study, we reported the development of a simple algorithm for determining fiber crystallinity information from Fourier transform infrared (FT-IR) spectroscopy. Hence, in this study we not only compared the fiber crystallinity information between FT-IR and XRD measurements, by developing a simple XRD algorithm in place of a time-consuming and subjective curve-fitting process, but we also suggested a direct way of determining cotton cellulose CI by calibrating XRD with the use of CI(IR) as references.

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

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

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

2016-01-15

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

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

NASA Astrophysics Data System (ADS)

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

2001-01-01

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

TEM in situ cube-corner indentation analysis using ViBe motion detection algorithm

NASA Astrophysics Data System (ADS)

Yano, K. H.; Thomas, S.; Swenson, M. J.; Lu, Y.; Wharry, J. P.

2018-04-01

Transmission electron microscopic (TEM) in situ mechanical testing is a promising method for understanding plasticity in shallow ion irradiated layers and other volume-limited materials. One of the simplest TEM in situ experiments is cube-corner indentation of a lamella, but the subsequent analysis and interpretation of the experiment is challenging, especially in engineering materials with complex microstructures. In this work, we: (a) develop MicroViBE, a motion detection and background subtraction-based post-processing approach, and (b) demonstrate the ability of MicroViBe, in combination with post-mortem TEM imaging, to carry out an unbiased qualitative interpretation of TEM indentation videos. We focus this work around a Fe-9%Cr oxide dispersion strengthened (ODS) alloy, irradiated with Fe2+ ions to 3 dpa at 500 °C. MicroViBe identifies changes in Laue contrast that are induced by the indentation; these changes accumulate throughout the mechanical loading to generate a "heatmap" of features in the original TEM video that change the most during the loading. Dislocation loops with b = ½ <111> identified by post-mortem scanning TEM (STEM) imaging correspond to hotspots on the heatmap, whereas positions of dislocation loops with b = <100> do not correspond to hotspots. Further, MicroViBe enables consistent, objective quantitative approximation of the b = ½ <111> dislocation loop number density.

Luminescent properties of YVO4:Eu/SiO2 core-shell composite particles

NASA Astrophysics Data System (ADS)

Bao, Amurisana; Lai, Hua; Yang, Yuming; Liu, Zhilong; Tao, Chunyan; Yang, Hua

2010-02-01

We report an efficient process for preparing monodisperse SiO2@Y0.95Eu0.05VO4 core-shell phosphors using a simple citrate sol-gel method and without the use of surface-coupling silane agents or large stabilizers. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and photoluminescence (PL) spectra were used to characterize the resulting SiO2@Y0.95Eu0.05VO4 core-shell phosphors. The XRD results demonstrate that the Y0.95Eu0.05VO4 particles crystallization on the surface of SiO2 annealing at 800 °C is perfectly and the crystallinity increases with raising the annealing temperature. The obtained core-shell phosphors have a near perfect spherical shape with narrow size distribution (average size ca. 500 nm and an average thickness of 50 nm), are not agglomerated, and have a smooth surface. The thickness of the YVO4:Eu3+ shells on the SiO2 cores could be easily tailored by changing the mass ratio of shell to core ( W = [YVO4]/[SiO2]) ( 50 nm for W = 30%). The Eu3+ shows a strong PL luminescence (dominated by 5D0 - 7F2 red emission at 618 nm) under the excitation of 320 nm UV light. The PL intensity of Eu3+ increases with increasing the annealing temperature and the values of W.

Photocatalytic degradation of malathion using Zn2+-doped TiO2 nanoparticles: statistical analysis and optimization of operating parameters

NASA Astrophysics Data System (ADS)

Nasseri, Simin; Omidvar Borna, Mohammad; Esrafili, Ali; Rezaei Kalantary, Roshanak; Kakavandi, Babak; Sillanpää, Mika; Asadi, Anvar

2018-02-01

A Zn2+-doped TiO2 is successfully synthesized by a facile photodeposition method and used in the catalytic photo-degradation of organophosphorus pesticide, malathion. The obtained photocatalysts are characterized in detail by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). XRD results confirm the formation of the anatase and rutile phases for the Zn2+-doped TiO2 nanoparticles, with crystallite sizes of 12.9 nm. Zn2+-doped TiO2 that was synthesized by 3.0%wt Zn doping at 200 °C exhibited the best photocatalytic activity. 60 sets of experiments were conducted using response surface methodology (RSM) by adjusting five operating parameters, i.e. initial malathion concentration, catalyst dose, pH, reaction time at five levels and presence or absence of UV light. The analysis revealed that all considered parameters are significant in the degradation process in their linear terms. The optimum values of the variables were found to be 177.59 mg/L, 0.99 g/L, 10.99 and 81.04 min for initial malathion concentration, catalyst dose, pH and reaction time, respectively, under UV irradiation (UV ON). Under the optimized conditions, the experimental values of degradation and mineralization were 98 and 74%, respectively. Moreover, the effects of competing anions and H2O2 on photocatalyst process were also investigated.

Enhanced Ethanol Gas Sensing Properties of SnO2-Core/ZnO-Shell Nanostructures

PubMed Central

Tharsika, T.; Haseeb, A. S. M. A.; Akbar, Sheikh A.; Sabri, Mohd Faizul Mohd; Hoong, Wong Yew

2014-01-01

An inexpensive single-step carbon-assisted thermal evaporation method for the growth of SnO2-core/ZnO-shell nanostructures is described, and the ethanol sensing properties are presented. The structure and phases of the grown nanostructures are investigated by field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. XRD analysis indicates that the core-shell nanostructures have good crystallinity. At a lower growth duration of 15 min, only SnO2 nanowires with a rectangular cross-section are observed, while the ZnO shell is observed when the growth time is increased to 30 min. Core-shell hierarchical nanostructures are present for a growth time exceeding 60 min. The growth mechanism for SnO2-core/ZnO-shell nanowires and hierarchical nanostructures are also discussed. The sensitivity of the synthesized SnO2-core/ZnO-shell nanostructures towards ethanol sensing is investigated. Results show that the SnO2-core/ZnO-shell nanostructures deposited at 90 min exhibit enhanced sensitivity to ethanol. The sensitivity of SnO2-core/ZnO-shell nanostructures towards 20 ppm ethanol gas at 400 °C is about ∼5-times that of SnO2 nanowires. This improvement in ethanol gas response is attributed to high active sensing sites and the synergistic effect of the encapsulation of SnO2 by ZnO nanostructures. PMID:25116903

Synthesis and Raman scattering of GaN nanorings, nanoribbons and nanowires

NASA Astrophysics Data System (ADS)

Li, Z. J.; Chen, X. L.; Li, H. J.; Tu, Q. Y.; Yang, Z.; Xu, Y. P.; Hu, B. Q.

Low-dimensional GaN materials, including nanorings, nanoribbons and smooth nanowires have been synthesized by reacting gallium and ammonia using Ag particles as a catalyst on the substrate of MgO single crystals. They were characterized by field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). EDX, XRD indicated that the low-dimensional nanomaterials were wurtzite GaN. New features are found in Raman scatterings for these low-dimensional GaN materials, which are different from the previous observations of GaN materials.

'How I do it': TEM for tumors of the rectum.

PubMed

Collinson, Rowan J; McC Mortensen, Neil J

2009-02-01

Transanal endoscopic microsurgery (TEM) has an established role in the management of benign rectal tumors. It also has an expanding role in the management of malignant tumors, which is more demanding for the clinician. It requires accurate histological and radiological assessment and draws on an expert understanding of the nature of local recurrence, metastasis, and the place of adjuvant therapies. A multidisciplinary approach is recommended. This paper discusses our institutional approach to TEM for benign and malignant tumors and covers some of the current management controversies.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Chitin butyrate coated electrospun nylon-6 fibers for biomedical applications

NASA Astrophysics Data System (ADS)

Pant, Hem Raj; Kim, Han Joo; Bhatt, Lok Ranjan; Joshi, Mahesh Kumar; Kim, Eun Kyo; Kim, Jeong In; Abdal-hay, Abdalla; Hui, K. S.; Kim, Cheol Sang

2013-11-01

In this study, we describe the preparation and characterizations of chitin butyrate (CB) coated nylon-6 nanofibers using single-spinneret electrospinning of blends solution. The physicochemical properties of nylon-6 composite fibers with different proportions of CB to nylon-6 were determined using FE-SEM, TEM, FT-IR spectroscopy, and water contact angle measurement. FE-SEM and TEM images revealed that the nylon-6 and CB were immiscible in the as-spun nanofibers, and phase separated nanofiber morphology becomes more pronounced with increasing amounts of CB. The bone formation ability of composite fibers was evaluated by incubating in biomimetic simulated body fluid. In order to assay the cytocompatibility and cell behavior on the composite scaffolds, osteoblast cells were seeded on the matrix. Results suggest that the deposition of CB layer on the surface of nylon-6 could increase its cell compatibility and bone formation ability. Therefore, as-synthesized nanocomposite fibrous mat has great potentiality in hard tissue engineering.

Experimental investigation of the effects of different liquid environments on the graphene oxide produced by laser ablation method

NASA Astrophysics Data System (ADS)

Ghavidel, Elham; Sari, Amir Hossein; Dorranian, Davoud

2018-07-01

In this work, the effects of liquid environments on the characteristics and optical properties of carbon nanostructures - in particular, Graphene Oxide (GO) - prepared by pulsed laser ablation were studied experimentally. The second harmonic beam of a Q-switched Nd:YAG laser of 532 nm wavelength at 6 ns pulse width and 0.7 J/cm2 fluence was employed to irradiate the graphite target in liquid nitrogen, deionized water, and 0.01 M CTAB solution under the same initial experimental conditions. Produced nanostructures were characterized by Raman scattering spectrum, FE-SEM and TEM images, Photoluminescence, and UV-Vis-NIR spectrum. TEM and FE-SEM images show sheet-like morphology with few square micrometer area graphenes in all samples. Raman and UV-Vis-NIR analyses show that graphene is oxidized due to the presence of oxygen molecules in ablation environment. Results demonstrate that the graphene nanosheets produced in deionized water are multilayer, contains the largest sp2 domain size, the least defects and the lowest possibility of aggregation.

High temperature XRD of Cu2.1Zn0.9SnSe4

NASA Astrophysics Data System (ADS)

Chetty, Raju; Mallik, Ramesh Chandra

2014-04-01

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

Identification of TEM-135 β-Lactamase in Neisseria gonorrhoeae Strains Carrying African and Toronto Plasmids in Argentina

PubMed Central

Gianecini, R.; Oviedo, C.; Littvik, A.; Mendez, E.; Piccoli, L.; Montibello, S.

2014-01-01

One hundred forty-three penicillinase-producing Neisseria gonorrhoeae (PPNG) isolates obtained in Argentina from 2008 and 2012 were examined to detect blaTEM-135 genes and to investigate plasmid profiles and multiantigen sequence types. Forty-two PPNG isolates were found to carry TEM-135, and two contained a new TEM derivative characterized as TEM-220. The blaTEM-135 allele was carried by the Toronto/Rio and African plasmids. Molecular epidemiology revealed that two blaTEM-135 isolates were related to previously described isolates from Thailand and China, indicating a common evolutionary origin. PMID:25367903

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

PubMed Central

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

2000-01-01

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

TEM Study of Internal Crystals in Supernova Graphites

NASA Astrophysics Data System (ADS)

Croat, T. K.; Bernatowicz, T.; Stadermann, F. J.; Messenger, S.; Amari, S.

2003-03-01

A coordinated TEM and isotopic study of ten supernova (SN) graphites from the Murchison meteorite has revealed many internal grains, mostly titanium carbides (TiCs) and TiC-kamacite composite grains, which were accreted during the graphite growth.

[Study on Hydrothermal Preparation and Luminescence Properties of Luminescent Material BaSrMg(PO₄)₂:Eu³⁺].

PubMed

Hu, Qing-song; Zhu, Cheng-jing; Xia, Yue-yi; Wang, Li-li; Liu, Wen-han; Pan, Zai-fa

2016-02-01

Eu³⁺ doped BaSrMg (PO₄)₂ were prepared by a hydrothermal method. The crystal structure and morphology of BaSrMg(PO₄)₂:Eu³⁺ phosphor were characterized by X-ray powder diffraction (XRD) and field emission scanning electron microscopy (FESEM). The effects of different pH values (5, 6, 7 and 8) and different reaction temperatures (120, 140, 160, 180 and 200 °C) on the crystal structure and morphology of BaSrMg(PO₄)₂:Eu³⁺ phosphor were studied in this paper. The results of XRD indicate that diffraction peaks are sharp and strong only when pH value is 6, meanwhile the FESEM shows the morphology is regular-shaped. The XRD patterns show amorphous halos superimposed with several weak sharp peaks for the samples preparing under the pH values of 5, 7 and 8. It indicates that these three samples are solid solution or mixed phases, which are in accord with the results of FESEM. From the fluorescence spectra, the peaks in the excitation spectra were assigned to the transition from ⁷F₀ to ⁵D₄, ⁵L₈, ⁵L₆ and ⁵D₂, while the peaks of emission spectra corresponding to the transition of ⁵D₁ --> ⁷F₁ and ⁵D₀-->⁷Fj (J = 0, 1, 2, 3 and 4). The strongest emission peak of the optimized phosphor located at 613 nm (⁵D0--> ⁷F₂), excited by the main excitation peak with wavelength of 394 nm. The splitting of the emission peaks changes depends on pH values and temperatures, which indicating that luminescence properties is closely related to the crystal structure and morphology of particles.

VES/TEM 1D joint inversion by using Controlled Random Search (CRS) algorithm

NASA Astrophysics Data System (ADS)

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

2015-01-01

Electrical (DC) and Transient Electromagnetic (TEM) soundings are used in a great number of environmental, hydrological, and mining exploration studies. Usually, data interpretation is accomplished by individual 1D models resulting often in ambiguous models. This fact can be explained by the way as the two different methodologies sample the medium beneath surface. Vertical Electrical Sounding (VES) is good in marking resistive structures, while Transient Electromagnetic sounding (TEM) is very sensitive to conductive structures. Another difference is VES is better to detect shallow structures, while TEM soundings can reach deeper layers. A Matlab program for 1D joint inversion of VES and TEM soundings was developed aiming at exploring the best of both methods. The program uses CRS - Controlled Random Search - algorithm for both single and 1D joint inversions. Usually inversion programs use Marquadt type algorithms but for electrical and electromagnetic methods, these algorithms may find a local minimum or not converge. Initially, the algorithm was tested with synthetic data, and then it was used to invert experimental data from two places in Paraná sedimentary basin (Bebedouro and Pirassununga cities), both located in São Paulo State, Brazil. Geoelectric model obtained from VES and TEM data 1D joint inversion is similar to the real geological condition, and ambiguities were minimized. Results with synthetic and real data show that 1D VES/TEM joint inversion better recovers simulated models and shows a great potential in geological studies, especially in hydrogeological studies.

Novel Co{sub 3}O{sub 4} porous polyhedrons derived from metal–organic framework toward high performance for electrochemical energy devices

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

Chen, Youcun, E-mail: chenyc@aqtc.edu.cn; Hu, Lin

2016-07-15

Co{sub 3}O{sub 4} polyhedrons with porous structure have been synthesized simply by annealing Prussian blue analogue (PBA) Co{sub 3}[Co(CN){sub 6}]{sub 2} polyhedrons at 400 °C in air. The product was characterized by a series of techniques, such as X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), Transmission Electron Microscopy (TEM), High-resolution TEM (HRTEM), X-ray Photoelectron Spectroscopy (XPS), and Brunauer–Emmett–Teller (BET) gas adsorption. Interestingly, when evaluated as an anode material for lithium-ion batteries (LIBs), the Co{sub 3}O{sub 4} porous polyhedrons manifested high reversible capacity (about 1200 mAh g{sup −1} at 50 mA g{sup −1}) and excellent cycling performance. Moreover, theymore » also exhibited a high specific capacitance of 110 Fg{sup −1} when used as an electrode in the supercapacitor. It is suggested that the special morphology and porous nanostructure lead to the promising electrochemical properties. - Graphical abstract: Novel and complicated mesoporous architectures of Co{sub 3}O{sub 4} have been fabricated by thermal decomposition of Prussian Blue Analog (PBA) Co{sub 3}[Co(CN){sub 6}]{sub 2} polyhedrons which obtained at the room temperature. When Co{sub 3}O{sub 4} product was evaluated for Li-ion batteries (LIBs), they exhibited high reversible capacity of 1000 mAh g{sup −1} with excellent cycle life because of the hollow/porous structure. Display Omitted.« less

Beyond the job exposure matrix (JEM): the task exposure matrix (TEM).

PubMed

Benke, G; Sim, M; Fritschi, L; Aldred, G

2000-09-01

The job exposure matrix (JEM) has been employed to assign cumulative exposure to workers in many epidemiological studies. In these studies, where quantitative data are available, all workers with the same job title and duration are usually assigned similar cumulative exposures, expressed in mgm(-3)xyears. However, if the job is composed of multiple tasks, each with its own specific exposure profile, then assigning all workers within a job the same mean exposure can lead to misclassification of exposure. This variability of exposure within job titles is one of the major weaknesses of JEMs. A method is presented for reducing the variability in the JEM methodology, which has been called the task exposure matrix (TEM). By summing the cumulative exposures of a worker over all the tasks worked within a job title, it is possible to address the variability of exposure within the job title, and reduce possible exposure misclassification. The construction of a TEM is outlined and its application in the context of a study in the primary aluminium industry is described. The TEM was found to assign significantly different cumulative exposures to the majority of workers in the study, compared with the JEM and the degree of difference in cumulative exposure between the JEM and the TEM varied greatly between contaminants.

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

NASA Astrophysics Data System (ADS)

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

2016-05-01

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

Effect of deacetylation on property of electrospun chitosan/PVA nanofibrous membrane and removal of methyl orange, Fe(III) and Cr(VI) ions.

PubMed

Habiba, Umma; Siddique, Tawsif A; Talebian, Sepehr; Lee, Jacky Jia Li; Salleh, Areisman; Ang, Bee Chin; Afifi, Amalina M

2017-12-01

In this study, effect of degree of deacetylation on property and adsorption capacity of chitosan/polyvinyl Alcohol electrospun membrane has been investigated. Resulting nanofibers were characterized by FESEM, FTIR, XRD, TGA, tensile testing, weight loss test and adsorption test. FESEM result shows, finer nanofiber was fabricated from 42h hydrolyzed chitosan and PVA blend solution. FTIR and XRD result showed a strong interaction between chitosan and polyvinyl alcohol. Higher tensile strength was observed for the nanofiber having 42h hydrolyzed chitosan. Blend solution of chitosan/PVA having low DD chitosan had higher viscosity. The nanofibrous membrane was stable in distilled water, acidic and basic medium. The isotherm study shows that the adsorption capacity (q m ) of nanofiber containing higher DD chitosan was higher for Cr(VI). In contrary, the membrane containing chitosan with lower DD showed the higher adsorption capacity for Fe(III) and methyl orange. Moreover, the effect of DD on removal percentage of adsorbate was dependent on the initial concentration of the adsorbate. Copyright © 2017 Elsevier Ltd. All rights reserved.

Development of bimetal oxide doped multifunctional polymer nanocomposite for water treatment

NASA Astrophysics Data System (ADS)

Saxena, Swati; Saxena, Umesh

2016-08-01

Bimetal oxide doped polymer nanocomposite was developed using Alumina and Iron (III) Oxide as nanoparticles with Nylon 6, 6 and Poly (sodium-4-styrenesulphonate) as polymer matrix for removal of pollutants from water. The blend sample of polymers was prepared by well established solution blending technique and their nanocomposite samples were prepared through dispersion technique during the solution casting of blend sample. The fabricated composites were characterized adopting FTIR, XRD, FESEM and EDX techniques. XRD and FESEM were used for morphological characterization of nano phase, while FTIR and EDX analysis were adopted for characterization of chemical moieties in composites. In the study of pollutant removal capacities of prepared composites, 6 % nanocomposite provided the best results. It exhibited the maximum removal of all parameters. The removal of total alkalinity was 66.67 %, total hardness 42.85 %, calcium 66.67 %, magnesium 25 %, chloride 58.66 %, nitrate 34.78 %, fluoride 63.85 %, TDS 41.27 % and EC was up to the level of 41.37 % by this composite. The study is a step towards developing multifunctional, cost-effective polymer nanocomposites for water remediation applications.

Strontium hexaferrite (SrFe12O19) based composites for hyperthermia applications

NASA Astrophysics Data System (ADS)

Rashid, Amin Ur; Southern, Paul; Darr, Jawwad A.; Awan, Saifullah; Manzoor, Sadia

2013-10-01

Mixed phase composites of SrFe12O19/MgFe2O4/ZrO2 were prepared via the citrate gel technique as potential candidate materials for magnetic hyperthermia. Structural and magnetic properties of the samples were studied using powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and a vibrating sample magnetometer. XRD and FE-SEM data confirm that magnesium ferrite and zirconium oxide phases increased with increasing Mg and Zr content in the precursors. Magnetization loops for the composites were measured at room temperature and showed significant variation of saturation magnetization, coercivity and remanence depending on the amount of the highly anisotropic Sr-hexaferrite phase. The sample with the highest Mg and Zr content had the lowest coercivity (80 Oe) and saturation magnetization (41 emu/g). The composite samples each were exposed to a 214 kHz alternating magnetic field of amplitude 22 Oe and a significant heating effect was observed in selected samples, which suggests potential for use in magnetic hyperthermia.

Fabrication of TiO2 nanostructures on porous silicon for thermoelectric application

NASA Astrophysics Data System (ADS)

Fahrizal, F. N.; Ahmad, M. K.; Ramli, N. M.; Ahmad, N.; Fakhriah, R.; Mohamad, F.; Nafarizal, N.; Soon, C. F.; Ameruddin, A. S.; Faridah, A. B.; Shimomura, M.; Murakami, K.

2017-09-01

Nowadays, technology is moving by leaps and bounds over the last several decades. This has created new opportunities and challenge in the research fields. In this study, the experiment is about to investigate the potential of Titanium Dioxide (TiO2) nanostructures that have been growth onto a layer of porous silicon (pSi) for their thermoelectric application. Basically, it is divided into two parts, which is the preparation of the porous silicon (pSi) substrate by electrochemical-etching process and the growth of the Titanium Dioxide (TiO2) nanostructures by hydrothermal method. This sample have been characterize by Field Emission Scanning Electron Microscopy (FESEM) to visualize the morphology of the TiO2 nanostructures area that formed onto the porous silicon (pSi) substrate. Besides, the sample is also used to visualize their cross-section images under the FESEM microscopy. Next, the sample is characterized by the X-Ray Diffraction (XRD) machine. The XRD machine is used to get the information about the chemical composition, crystallographic structure and physical properties of materials.

Size-dependent photocatalytic activity of La0.8Sr0.2MnO3 nanoparticles prepared by hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Rahmani Afje, F.; Ehsani, M. H.

2018-04-01

Synthesize of La0.8Sr0.2MnO3 (LSMO) manganite were carried out in different particle sizes by hydrothermal method. Structural and optical properties of the prepared specimens were studied by x-ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), and UV–vis spectroscopy. The XRD study, coupled with the Rietveld refinement, exhibited rhombohedral structure with R-3C space group. Using the FT-IR and FESEM analyses, the perovskite structure of the samples with Nano-rod-like morphologies were inferred. Furthermore, the average sizes of 48.11, 70.99 and 111.45 nm were obtained for the ones sintered at 800, 900, and 1000 °C temperatures, respectively. The optical research showed that band gap energy is about 2.13 eV, being suitable in visible-light photocatalytic activity for water purification from dyes and toxic organic materials. The photo-degradation efficiency for decolorizing methyl orange solution (10 ppm) for various samples (100 ppm) were systematically probed and a strong relation is concluded between particle size and photocatalytic activity.

Morphology and phase identification of synthesized precipitated calcium carbonate from acetylene gas industry waste

NASA Astrophysics Data System (ADS)

Sabri, Siti Noorzidah Mohd; Othman, Rohaya; Othman, Anuar

2017-12-01

Precipitated calcium carbonate (PCC) is also known as synthetic calcium carbonate. In this paper, PCC was synthesized from carbide lime, which is the by-product from acetylene gas industry. The method used to produce PCC from carbide lime waste was ionic sucrose precipitation technique. The experiments were performed by varying the stirring rate. In this technique, carbide lime was first dissolved in ionic sucrose solution and then chilled at 10 °C for 24 hours before carbon dioxide gasses was introduced into the solution. The carbonation and precipitation process was took place and PCC was formed. The PCC was further filtered to obtain the solid PCC. The sample was then further characterised by using FESEM and XRD to determine the morphology and to identify the phase that exists in the synthesized compound respectively. The XRD and FESEM results clearly shown that the PCC obtained has mixed phases of calcite and vaterite, with mixtures of spherical and irregular shape morphologies formed. The irregular shapes corresponded to vaterite formation, meanwhile spherical shapes corresponded to calcite formation.

Influence of Iron Doping on Structural, Optical and Magnetic Properties of TiO2 Nanoparticles

NASA Astrophysics Data System (ADS)

Zahid, R.; Manzoor, M.; Rafiq, A.; Ikram, M.; Nafees, M.; Butt, A. R.; Hussain, S. G.; Ali, S.

2018-05-01

In this study, various concentrations of Fe doped TiO2 nanoparticles have been successfully synthesized using the sol-gel method. A variety of characterization techniques as ultra-violet visible (UV-Vis) spectroscopy, X-ray diffractometer (XRD), vibrating sample magnetometry (VSM) and field emission scanning electron microscopy (FESEM) were employed to analyze the prepared nanopowders. XRD measurement confirmed the substitution of Fe ion without disturbing the tetragonal crystal system of TiO2. The crystallite size was found to decrease and lattice strain increases upon doping estimated by Williamson Hall plot. Furthermore, the average grain size calculated by FESEM found was between 10 and 30 nm for pure and doped TiO2. UV-Vis spectroscopy showed an increase in absorption accompanied red shift and increase in band gap energies from 3.36 to 3.62 eV with the addition of Fe. The FTIR spectroscopy was employed to confirm the presence of functional groups in the fabricated nanopowders. Upon mixing the saturation magnetization (Ms) varying from (2.12 to 1.51)10-2 emu/g was observed.

"One-sample concept" micro-combinatory for high throughput TEM of binary films.

PubMed

Sáfrán, György

2018-04-01

Phases of thin films may remarkably differ from that of bulk. Unlike to the comprehensive data files of Binary Phase Diagrams [1] available for bulk, complete phase maps for thin binary layers do not exist. This is due to both the diverse metastable, non-equilibrium or instable phases feasible in thin films and the required volume of characterization work with analytical techniques like TEM, SAED and EDS. The aim of the present work was to develop a method that remarkably facilitates the TEM study of the diverse binary phases of thin films, or the creation of phase maps. A micro-combinatorial method was worked out that enables both preparation and study of a gradient two-component film within a single TEM specimen. For a demonstration of the technique thin Mn x Al 1- x binary samples with evolving concentration from x = 0 to x = 1 have been prepared so that the transition from pure Mn to pure Al covers a 1.5 mm long track within the 3 mm diameter TEM grid. The proposed method enables the preparation and study of thin combinatorial samples including all feasible phases as a function of composition or other deposition parameters. Contrary to known "combinatorial chemistry", in which a series of different samples are deposited in one run, and investigated, one at a time, the present micro-combinatorial method produces a single specimen condensing a complete library of a binary system that can be studied, efficiently, within a single TEM session. That provides extremely high throughput for TEM characterization of composition-dependent phases, exploration of new materials, or the construction of phase diagrams of binary films. Copyright © 2018 Elsevier B.V. All rights reserved.

Identification of TEM-135 β-lactamase in Neisseria gonorrhoeae strains carrying African and Toronto plasmids in Argentina.

PubMed

Gianecini, R; Oviedo, C; Littvik, A; Mendez, E; Piccoli, L; Montibello, S; Galarza, P

2015-01-01

One hundred forty-three penicillinase-producing Neisseria gonorrhoeae (PPNG) isolates obtained in Argentina from 2008 and 2012 were examined to detect blaTEM-135 genes and to investigate plasmid profiles and multiantigen sequence types. Forty-two PPNG isolates were found to carry TEM-135, and two contained a new TEM derivative characterized as TEM-220. The blaTEM-135 allele was carried by the Toronto/Rio and African plasmids. Molecular epidemiology revealed that two blaTEM-135 isolates were related to previously described isolates from Thailand and China, indicating a common evolutionary origin. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

A joint TEM-HLEM geophysical approach to borehole sitting in deeply weathered granitic terrains.

PubMed

Meju, M A; Fontes, S L; Ulugergerli, E U; La Terra, E F; Germano, C R; Carvalho, R M

2001-01-01

The accurate location of aquiferous fracture zones in granite beneath a > 50 m thick weathered mantle in semi-arid regions is a major hydrogeological problem. It is expected that the zone of intensive fracturing will be more susceptible to weathering and thus be characterized by the thickest development of saprolite, a good electrically conductive target for deep-probing electromagnetic systems. The single-loop transient electromagnetic (TEM) technique is well known to have the capability for detecting concealed steep mineralized targets in mining environments and can be adapted to this hydrogeological problem. We propose that combining the conventional frequency-domain horizontal-loop electromagnetic (HLEM) and single-loop TEM is an effective practical approach to locating concealed aquiferous fracture zones. In the supporting case studies presented here, we deployed multifrequency HLEM profiling (with 50 m transmitter-receiver separation) and TEM soundings with contiguous 10 or 20 m sided loops along the survey lines in a granitic terrain affected by deep (> 50 m) weathering in northeast Brazil. A somewhat layered structure consisting of resistive hardpan/leached zone, conductive saprolite, and resistive basement is identifiable in the typical TEM depth sounding data. We obtained coincident HLEM and TEM anomalies at all the sites, enabling a relatively straightforward selection of potential drilling positions. Simple resistivity-depth transformation of the TEM data was done for each site, yielding an approximate section from which drilling depths were estimated. All of the boreholes located were successful. Although our results appear to indicate that the single-loop TEM method could be used independently for borehole sitting in deeply weathered granitic terrains and that the weathering profile over granite can be mapped using TEM depth soundings of appropriate observational bandwidth, we recommend a joint electromagnetic approach for optimal well sitting.

Structure and Dynamics of Domains in Ferroelectric Nanostructures. In-situ TEM Studies

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

Pan, Xiaoqing

2015-06-30

The goal of this project was to explore the structure and dynamic behaviors of ferroelectric domains in ferroelectric thin films and nanostructures by advanced transmission electron microscopy (TEM) techniques in close collaboration with phase field modeling. The experimental techniques used include aberration-corrected sub-Å resolution TEM and in-situ TEM using a novel scanning tunneling microscopy (STM) - TEM holder that allows the direct observation of nucleation and dynamic evolution of ferroelectric domains under applied electric field. Specifically, this project was aimed to (1) to study the roles of static electrical boundary conditions and electrical charge in controlling the equilibrium domain structuresmore » of BiFeO 3 thin films with controlled substrate constraints, (2) to explore the fundamental mechanisms of ferroelectric domain nucleation, growth, and switching under an applied electric field in both uniform thin films and nanostructures, and to understand the roles of crystal defects such as dislocations and interfaces in these processes, (3) to understand the physics of ferroelectric domain walls and the influence of defects on the electrical switching of ferroelectric domains.« less

cisTEM, user-friendly software for single-particle image processing.

PubMed

Grant, Timothy; Rohou, Alexis; Grigorieff, Nikolaus

2018-03-07

We have developed new open-source software called cis TEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cis TEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k - 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cis TEM is available for download from cistem.org. © 2018, Grant et al.

cisTEM, user-friendly software for single-particle image processing

PubMed Central

2018-01-01

We have developed new open-source software called cisTEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cisTEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k – 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cisTEM is available for download from cistem.org. PMID:29513216

Size determination of Acipenser ruthenus spermatozoa in different types of electron microscopy.

PubMed

Psenicka, Martin; Tesarová, Martina; Tesitel, Jakub; Nebesárová, Jana

2010-07-01

In this study three types of scanning electron microscopes were used for the size determination of spermatozoa of sterlet Acipenser ruthenus - high vacuum scanning electron microscope (SEM, JEOL 6300), environmental scanning electron microscope (ESEM, Quanta 200 FEG), field emission scanning electron microscope (FESEM, JEOL 7401F) with cryoattachment Alto 2500 (Gatan) and transmission electron microscope (TEM, JEOL 1010). The use of particular microscopes was tied with different specimen preparation techniques. The aim of this study was to evaluate to what degree the type of used electron microscope can influence the size of different parts of spermatozoa. For high vacuum SEM the specimen was prepared using two slightly different procedures. After chemical fixation with 2.5% glutaraldehyde in 0.1M phosphate buffer and post-fixation by 1% osmium tetroxide, the specimen was dehydrated by acetone series and dried either by critical point method or by means of t-butylalcohol. For ESEM fresh, unfixed material was used, which was dropped on microscopic copper grids. In FESEM working in cryo-mode the specimen was observed in a frozen state. Ultrathin sections from chemically fixed and Epon embedded specimens were prepared for TEM observation. Distinct parts of sterlet spermatozoa were measured in each microscope and the data obtained was statistically processed. Results confirmed that the classical chemical procedure of specimen preparation for SEM including critical point drying method led to a significant contraction of all measured values, which could deviate up to 30% in comparison with values measured on the fresh chemically untreated specimen in ESEM. Surprisingly sperm dimensions determinated on ultrathin sections by TEM are comparable with values obtained in ESEM or FESEM. Copyright 2010 Elsevier Ltd. All rights reserved.

Synchronizing flash-melting in a diamond cell with synchrotron X ray diffraction (XRD)

NASA Astrophysics Data System (ADS)

Karandikar, Amol; Boehler, Reinhard; Meng, Yue; Rod, Eric; Shen, Guoyin

2013-06-01

The major challenges in measuring melting temperatures in laser heated diamond cells are sample instability, thermal runaway and chemical reactions. To circumvent these problems, we developed a ``flash heating'' method using a modulated CW fiber laser and fast X ray detection capability at APS (Pilatus 1M detector). As an example, Pt spheres of 5 micron diameter were loaded in a single crystal sapphire encapsulation in the diamond cell at 65 GPa and heated in a single flash heating event for 20 ms to reach a desired temperature. A CCD spectrometer and the Pilatus were synchronized to measure the temperature and the XRD signal, respectively, when the sample reached the thermal steady state. Each successive flash heating was done at a higher temperature. The integrated XRD pattern, collected during and after (300 K) each heating, showed no chemical reaction up to 3639 K, the highest temperature reached in the experiment. Pt111 and 200 peak intensity variation showed gradual recrystalization and complete diminishing at about 3600 K, indicating melting. Thus, synchronized flash heating with novel sample encapsulation circumvents previous notorious problems and enables accurate melting temperature measurement in the diamond cell using synchrotron XRD probe. Affiliation 2: Geowissenschaeften, Goethe-Universitaet, Altenhoeferallee 1, D-60438 Frankfurt a.M., Germany.

Preparation of high-quality planar FeRh thin films for in situ TEM investigations

NASA Astrophysics Data System (ADS)

Almeida, Trevor P.; McGrouther, Damien; Pivak, Yevheniy; Perez Garza, Hector Hugo; Temple, Rowan; Massey, Jamie; Marrows, Christopher H.; McVitie, Stephen

2017-10-01

The preparation of a planar FeRh thin film using a focused ion beam (FIB) secondary electron microscope (SEM) for the purpose of in situ transmission electron microscopy (TEM) is presented. A custom SEM stub with 45° faces allows for the transfer and milling of the sample on a TEM heating chip, whilst Fresnel imaging within the TEM revealed the presence of the magnetic domain walls, confirming the quality of the FIB-prepared sample.

1D Cole-Cole inversion of TEM transients influenced by induced polarization

NASA Astrophysics Data System (ADS)

Seidel, Marc; Tezkan, Bülent

2017-03-01

Effects of induced polarization (IP) can have an impact on time-domain electromagnetic measurements (TEM) and may lead to sign reversals in the recorded transients. To study these IP effects on TEM data, a new 1D inversion algorithm was developed for both, the central-loop and the separate-loop TEM configurations using the Cole-Cole relaxation model. 1D forward calculations for a homogeneous half-space were conducted with the aim of analyzing the impacts of the Cole-Cole parameters on TEM transients with respect to possible sign reversals. The forward modelings showed that the variation of different parameters have comparable effects on the TEM transients. This leads to an increasing number of equivalent models as a result of inversion calculations. Subsequently, 1D inversions of synthetic data were performed to study the potentials and limitations of the algorithm regarding the resolution of the Cole-Cole parameters. In order to achieve optimal inversion results, it was essential to error-weight the data points in the direct vicinity of sign reversals. The obtained findings were eventually adopted on the inversion of real field data which contained considerable IP signatures such as sign reversals. One field data set was recorded at the Nakyn kimberlite field in Western Yakutiya, Russia, in the central-loop configuration. Another field data set originates from a waste site in Cologne, Germany, and was measured utilizing the separate-loop configuration.

Coexistence of SHV-4- and TEM-24-Producing Enterobacter aerogenes Strains before a Large Outbreak of TEM-24-Producing Strains in a French Hospital

PubMed Central

Mammeri, H.; Laurans, G.; Eveillard, M.; Castelain, S.; Eb, F.

2001-01-01

In 1996, a monitoring program was initiated at the teaching hospital of Amiens, France, and carried out for 3 years. All extended-spectrum β-lactamase (ESBL)-producing Enterobacter aerogenes isolates recovered from clinical specimens were collected for investigation of their epidemiological relatedness by pulsed-field gel electrophoresis and enterobacterial repetitive intergenic consensus PCR (ERIC-PCR) and determination of the type of ESBL harbored by isoelectric focusing and DNA sequencing. Molecular typing revealed the endemic coexistence, during the first 2 years, of two clones expressing, respectively, SHV-4 and TEM-24 ESBLs, while an outbreak of the TEM-24-producing strain raged in the hospital during the third year, causing the infection or colonization of 165 patients. Furthermore, this strain was identified as the prevalent clone responsible for outbreaks in many French hospitals since 1996. This study shows that TEM-24-producing E. aerogenes is an epidemic clone that is well established in the hospital's ecology and able to spread throughout wards. The management of the outbreak at the teaching hospital of Amiens, which included the reinforcement of infection control measures, failed to obtain complete eradication of the clone, which has become an endemic pathogen. PMID:11376055

Effects of SPORL and dilute acid pretreatment on substrate morphology, cell physical and chemical wall structures, and subsequent enzymatic hydrolysis of lodgepole pine

Treesearch

Xinping Li; Xiaolin Luo; Kecheng Li; J.Y. Zhu; J. Dennis Fougere; Kimberley Clarke

2012-01-01

The effects of pretreatment by dilute acid and sulfite pretreatment to overcome recalcitrance of lignocellulose (SPORL) on substrate morphology, cell wall physical and chemical structures, along with the subsequent enzymatic hydrolysis of lodgepole pine substrate were investigated. FE-SEM and TEM images of substrate structural morphological changes showed that SPORL...

TEM Analysis of Interfaces in Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Tsuda, H.; Halbig, M. C.; Singh, M.; Hasegawa, Y.; Mori, S.; Asthana R.

2016-01-01

Silicon Carbide (SiC) is a promising material for thermo-structural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, and Mo-B. In this presentation, the result of microstructural analysis obtained by TEM observations and the influence of metallic interlayers and fiber orientation of SA-THX on the joint microstructure will be discussed.

Challenges in quantitative crystallographic characterization of 3D thin films by ACOM-TEM.

PubMed

Kobler, A; Kübel, C

2017-02-01

Automated crystal orientation mapping for transmission electron microscopy (ACOM-TEM) has become an easy to use method for the investigation of crystalline materials and complements other TEM methods by adding local crystallographic information over large areas. It fills the gap between high resolution electron microscopy and electron back scatter diffraction in terms of spatial resolution. Recent investigations showed that spot diffraction ACOM-TEM is a quantitative method with respect to sample parameters like grain size, twin density, orientation density and others. It can even be used in combination with in-situ tensile or thermal testing. However, there are limitations of the current method. In this paper we discuss some of the challenges and discuss solutions, e.g. we present an ambiguity filter that reduces the number of pixels with a '180° ambiguity problem'. For that an ACOM-TEM tilt series of nanocrystalline Pd thin films with overlapping crystallites was acquired and analyzed. Copyright © 2017. Published by Elsevier B.V.

Cross section TEM characterization of high-energy-Xe-irradiated U-Mo

DOE PAGES

Ye, B.; Jamison, L.; Miao, Y.; ...

2017-03-09

U-Mo alloys irradiated with 84 MeV Xe ions to various doses were characterized with transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) techniques. The TEM thin foils were prepared perpendicular to the irradiated surface to allow a direct observation of the entire region modified by ions. Furthermore, depth-selective microstructural information was revealed. Varied irradiation-induced phenomena such as gas bubble formation, phase reversal, and recrystallization were observed at different ion penetration depths in U-Mo.

[Transanal endocopic microsurgery (TEM) in advanced rectal cancer disease treatment].

PubMed

Paci, Marcello; Scoglio, Daniele; Ursi, Pietro; Barchetti, Luciana; Fabiani, Bernardina; Ascoli, Giada; Lezoche, Giovanni

2010-01-01

After Heald's revolution in 1982, who introduced the total mesorectal excision, for improve the results in terms of recurrance and survival rate, there is a need to explore new therapeutic options in treatment of sub-peritoneal rectal cancer. In particular, local excision represent more often a valid technique for non advanced rectal cancer treatment in comparison with the more invasive procedure, especially in elderly and/or in poor health patients. The introduction of TEM by Buess (transanal endoscopy microsurgery), has extended the local treatment also to classes of patients who would normally have been candidates for TME. The author gives literature's details and his experience in the use of TEM for early rectal cancer sub-peritoneal. The aim of the study is to analyze short and long term results in terms of local recurrence and survival rate comparing TEM technique with the other transanal surgery in rectal cancer treatment. Preoperative Chemio-Radio therapy and rigorous Imaging Staging are the first steps to planning surgery. It's time, for local rectal cancer, has come to make the devolution a few decades ago has been accomplished in the treatment of breast cancer

Nanominerals and potentially hazardous elements from coal cleaning rejects of abandoned mines: Environmental impact and risk assessment.

PubMed

Fdez-Ortiz de Vallejuelo, Silvia; Gredilla, Ainara; da Boit, Kátia; Teixeira, Elba C; Sampaio, Carlos H; Madariaga, Juan Manuel; Silva, Luis F O

2017-02-01

Soils around coal mining are important reservoir of hazardous elements (HEs), nanominerals, and ultrafine compounds. This research reports and discusses the soil concentrations of HEs (As, Cd, Cr, Cu, Ni, Pb, and Zn) in coal residues of abandoned mines. To assess differences regarding environmental impact and risk assessment between coal abandoned mines from the Santa Catarina state, eighteen coal cleaning rejects with different mineralogical and chemical composition, from eight abandoned mines were collected. Nanominerals and ultra-fine minerals from mining-contaminated areas were analyzed by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and high-resolution transmission electron microscope (HR-TEM), providing new information on the mineralogy and nano-mineralogy of these coal residues. The total contents of 57 elements (HEs, alkali metals, and rare earth elements) were analyzed by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The calculation of NWACs (Normalized Average Weighted Concentration), together with the chemometric analysis by Principal component analysis (PCA) confirmed the variability of the samples regarding their city and their mine of origin. Moreover, the results confirmed the existence of hotspots in mines near urban areas. Copyright © 2016 Elsevier Ltd. All rights reserved.

Influence of Annealing Duration on the Growth of V2O5 Nanorods Synthesized by Spray Pyrolysis Technique

NASA Astrophysics Data System (ADS)

Abd-Alghafour, N. M.; Ahmed, Naser M.; Hassan, Z.; Abubakar, D.; Bououdina, M.

2016-06-01

This paper deals with the investigation of annealing effects on the structural, morphological and optical properties of V2O5 nanorods (NRs) grown on the glass substrates by using chemical spray pyrolysis technique. The as-prepared samples were annealed at 500∘ for 40, 60 and 120 min in a quartz tube furnace. The high resolution X-ray diffraction (XRD) analysis revealed V2O5 NRs with preferred orientation along (001) plane. The crystallite size of the V2O5 NRs was increased by increasing the annealing duration. The morphological observations using field emission scanning electron microscope (FESEM) displayed NRs structures whose diameter and length were found to increase with increase of the annealing duration. The transmission electron microscopy (TEM) analysis confirmed the orthorhombic structures of the NRs. The AFM measurements indicated an increase of the average surface roughness by increasing the annealing time. The Raman spectroscopy revealed V-O-V phonon mode in the NRs annealed for 120 min. The optical bandgap was found in the range 2.6-2.58eV and observed to decrease with various duration annealed.

Microwave-assisted preparation of flower-like cobalt phosphate and its application as a new heterogeneous Fenton-like catalyst

NASA Astrophysics Data System (ADS)

Hu, Xiaoxia; Li, Rong; Zhao, Shuyu; Xing, Yanjun

2017-02-01

A novel flower-like 3D hierarchical cobalt phosphate Co3(PO4)2·8H2O (fCoP), and a plate-like cobalt phosphate (pCoP) were successfully synthesized via a microwave-assisted method at low temperature under atmospheric pressure using hexamethylene tetramine (HMTA) or urea as a template. All CoPs were characterized using XRD, FESEM, TEM, DRS and surface photovoltage spectra (SPS). The performance of the photocatalytic degradation of Rhodamine B (RhB) via a Fenton-like process on CoPs was evaluated both in the dark and under illumination. The results showed that the morphology and composition of the CoPs affected the RhB degradation. The flower-like hierarchical fCoP favored the photo degradation of RhB. fCoP was also confirmed to have the merits of easy recycling and good stability based on successive degradation experiments. The active species trapping experiments showed that the superoxide radical (rad O2-) was the dominant active species in the Fenton-like process. The catalytic activation was confirmed to be related to both the Co(II) on the surface and the fCoP framework.

Ultrasonic-assisted hydrothermal synthesis and catalytic behavior of a novel SAPO-34/Clinoptilolite nanocomposite catalyst for high propylene demand in MTO process

NASA Astrophysics Data System (ADS)

Moradiyan, Eshagh; Halladj, Rouein; Askari, Sima; Moghimpour Bijani, Parisa

2017-08-01

SAPO-34 as a catalyst has high selectivity and hydrothermal stability, but it is rapidly deactivated by the formation of coke in its micropores. Evaluating the natural Clinoptilolite capability as a binder in nanocomposite catalysts is of interest because of its low cost, and accelerating the reaction. The SAPO-34/Clinoptilolite (S/C) nanocomposite catalysts were synthesized via ultrasonic-assisted hydrothermal method using Clinoptilolite as a binder. Subsequent performance of the catalyst was investigated in the methanol to olefins (MTO) reaction. The structures of synthesized nanocomposite were characterized with several methods such as XRD, XRF, FESEM, TEM, NH3-TPD, FT-IR, and nitrogen adsorption techniques. The modified Clinoptilolite was attained using nitric acid treatment. Although the physicochemical analysis indicated that HNO3-treatment decreases the crystallinity of the Clinoptilolite, the specific surface area of natural zeolite enhances considerably from 20.07 to 187.8 m2/g. The nanocomposite catalysts showed high selectivity toward light olefins with 100% conversion and 90% selectivity to light olefins as desired products at 450 °C. Nanocomposite with the additional diffusion paths for mass transfer provided by binder-filled space ascend to higher catalytic lifetimes in compare with free SAPO-34 catalyst.

A new analytical device incorporating a nitrogen doped lanthanum metal oxide with reduced graphene oxide sheets for paracetamol sensing.

PubMed

Ponnaiah, Sathish Kumar; Prakash, Periakaruppan; Vellaichamy, Balakumar

2018-06-01

The novel N-CeO 2 nanoparticles decorated on reduced graphene oxide (N-CeO 2 @rGO) composite has been synthesized by sonochemical method. The characterization of as prepared nanocomposite was intensely performed by UV-Vis, FT-IR, EDX, FE-SEM, HR-TEM, XRD, and TGA analysis. The synthesized nanomaterial was further investigated for its selective and sensitive sensing of paracetamol (PM) based on a N-CeO 2 @rGO modified glassy carbon electrode. A distinct and improved reversible redox peak of PM is obtained at N-CeO 2 @rGO nanocomposite compared to the electrodes modified with N-CeO 2 and rGO. It displays a very good performance with a wide linear range of 0.05-0.600 μM, a very low detection limit of 0.0098 μM (S/N = 3), a high sensitivity of 268 μA µM -1  cm -2 and short response time (<3 s). Also, the fabricated sensor shows a good sensibleness for the detection of PM in various tablet samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Construction of NiO/MnO2/CeO2 hybrid nanoflake arrays as platform for electrochemical energy storage

NASA Astrophysics Data System (ADS)

Cui, Lihua; Cui, Jiewu; Zheng, Hongmei; Wang, Yan; Qin, Yongqiang; Shu, Xia; Liu, Jiaqin; Zhang, Yong; Wu, Yucheng

2017-09-01

Rational design and fabrication of novel electrode materials are of great importance for developing supercapacitors with remarkable capacitance and enhanced cycling stability. In this paper, we present a simple one-pot hydrothermal deposition followed by calcinations process for the in situ construction of homogeneous NiO/MnO2/CeO2 (NMC) nanoflake arrays on Ni foam substrate, which could be directly adopted as the binder-free electrode materials for high performance supercapacitors. The field-emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDX) are carried out to investigate the morphology, microstructure and composition of NMC nanoflake arrays. As-prepared hierarchical NMC nanoflake arrays exhibit the specific capacitance of 1027.8 F g-1 at a current density of 3.1 A g-1 and excellent cycling stability of 97.8% after 5000 charge/discharge cycles. This facile, cost-effective and controllable fabrication route and the robust supercapacitive activity suggest that the ordered NMC nanoflake arrays could be promising candidate electrode materials for high performance electrochemical energy storage devices.

Facile room-temperature synthesis of carboxylated graphene oxide-copper sulfide nanocomposite with high photodegradation and disinfection activities under solar light irradiation

PubMed Central

Yu, Shuyan; Liu, Jincheng; Zhu, Wenyu; Hu, Zhong-Ting; Lim, Teik-Thye; Yan, Xiaoli

2015-01-01

Carboxylic acid functionalized graphene oxide-copper (II) sulfide nanoparticle composite (GO-COOH-CuS) was prepared from carboxylated graphene oxide and copper precursor in dimethyl sulfoxide (DMSO) by a facile synthesis process at room temperature. The high-effective combination, the interaction between GO-COOH sheets and CuS nanoparticles, and the enhanced visible light absorption were confirmed by transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermo gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra (DRS) and Photoluminescence (PL) spectra. The as-synthesized GO-COOH-CuS nanocomposite exhibited excellent photocatalytic degradation performance of phenol and rhodamine B, high antibacterial activity toward E. coli and B. subtilis, and good recovery and reusability. The influence of CuS content, the synergistic reaction between CuS and GO-COOH, and the charge-transfer mechanism were systematically investigated. The facile and low-energy synthesis process combined with the excellent degradation and antibacterial performance signify that the GO-COOH-CuS has a great potential for water treatment application. PMID:26553709

Optical properties of pure and PbSe doped TiS2 nanodiscs

NASA Astrophysics Data System (ADS)

Parvaz, M.; Islamuddin; Khan, Zishan H.

2018-06-01

Titanium disulfide, being one of the popular transition-metal dichalcogenide (TMD) materials, shows wonderful properties owing to tunable optical band gap. Pure and PbSe doped titanium disulfide nanodiscs have been synthesized by solid-state reaction method. FESEM, TEM and Raman images confirm the synthesis of nanodiscs. XRD spectra suggest the polycrystalline structure of as-prepared as well as PbSe doped TiS2 nanodiscs. PL spectra of the as-synthesized nanodiscs has been studied in the wavelength range of (300–550 nm), at room temperature. The position of the peak shifts towards the lower wavelength (blue shift) and intensity of the PL increases after the doping of PbSe, which may be due to a broadening of the optical band gap. UV–vis spectra has been used to calculate optical band gap of pure and PbSe doped titanium disulfide nanodiscs. The calculated value are found to be 1.93 eV and 2.03 eV respectively. Various optical constants such as n and k have been calculated. The value of extinction coefficient (k) of pure and doped titanium disulfide increases while the value of the refractive index (n) decreases with increase in photon energy.

Synthesis of SnO_2 nanoparticles by electrooxidation of tin in quaternary ammonium salt for application in dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Abrari, Masoud; Ghanaatshoar, Majid; Hosseiny Davarani, Saied Saeed; Moazami, Hamid Reza; Kazeminezhad, Iraj

2017-05-01

A facile synthetic route has been employed to prepare tin oxide nanoparticles. The route comprises anodic dissolution of metallic tin in the presence of tetramethylammonium chloride called electrooxidation. The effect of experimental parameters was investigated with special focus on solution pH. The obtained nanostructures have been characterized by XRD, EDS, TEM, FESEM, FTIR and UV-visible studies. The results show that the solution pH has a critical influence on the nanoparticles properties. The hydrophilic feature of nanoparticles decreases with pH growth, whereas their mean size increases. On the other hand, the size distribution is much uniform for the samples prepared at low pH. Having achieved the nanoparticles by electrooxidation, the dye-sensitized solar cells based on the produced SnO_2 nanoparticles were fabricated and the influence of nanoparticles on their performance was investigated. By variation in solution pH, we prepared nanoparticles with different particle sizes and photoanodes with various dye-loading abilities. The dye absorption and consequently current density of cells increased in acidic case, and therefore, power conversion efficiency grew up by 33% in acidic synthetic environment.

Synthesis and characterization of Cu0.3Zn0.5Mg0.2Fe2O4 nanoparticles as a magnetic drug delivery system

NASA Astrophysics Data System (ADS)

Ansari, Mohammad; Bigham, Ashkan; Hassanzadeh-Tabrizi, S. A.; Abbastabar Ahangar, H.

2017-10-01

Mixed spinel ferrite nanoparticles are being applied in biomedical applications due to their biocompatibility, antibacterial activity, particular magnetic and electronic properties with chemical and thermal stabilities. The Cu0.3Zn0.5Mg0.2Fe2O4 nanoparticles are synthesized through the thermal treatment method. Polyvinyl alcohol (PVA) is used as the capping agent to stabilize the particles and prevent their agglomeration. The synthesized nanoparticles are characterized through X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), N2 adsorption-desorption, field emission scanning electron microscopy (FESEM), and transmission electron microscope (TEM). The magnetic characterization is made on a vibrating sample magnetometer (VSM), which displayed super-paramagnetic behavior of the synthesized sample. Potential application of the Cu0.3Zn0.5Mg0.2Fe2O4 nanoparticles as a drug delivery agent is assessed in vitro by estimating their release properties. The obtained results indicate that the amount of ibuprofen (IBU) adsorbed into the nanocarrier of Cu0.3Zn0.5Mg0.2Fe2O4 is 104 mg/g and the drug release is sustained up to 72 h.

Synthesis of ZnFe2O4/SiO2 composites derived from a diatomite template.

PubMed

Liu, Zhaoting; Fan, Tongxiang; Zhou, Han; Zhang, Di; Gong, Xiaolu; Guo, Qixin; Ogawa, Hiroshi

2007-03-01

A novel porous ZnFe2O4/SiO2 composite product has been generated with a template-directed assembly method from porous diatomite under different synthesis conditions, such as precursor concentrations (metallic nitrates), calcination temperature and diatomite type. The phase composition and morphology of all the materials were examined by x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The results indicated that an inherited hierarchical porous structure from the diatomite template can be obtained, and the synthesis conditions were found to have clear effects on the formation of the ZnFe2O4/SiO2 composite. The ideal composite of ZnFe2O4/SiO2 can be obtained through optimization of diatomite template type, precursor solution and calcination temperature. Furthermore, the adsorption abilities of two types of diatomites were analyzed in detail using FTIR spectra and nitrogen adsorption measurements etc, which proved that A-diatomite (Shengzhou-diatomite) is better than B-diatomite (Changbai-diatomite) on the aspect of adsorbing Zn and Fe ions, and of forming the ZnFe2O4.

High frequency electromagnetic reflection loss performance of substituted Sr-hexaferrite nanoparticles/SWCNTs/epoxy nanocomposite

NASA Astrophysics Data System (ADS)

Gordani, Gholam Reza; Ghasemi, Ali; saidi, Ali

2015-10-01

In this study, the electromagnetic properties of a novel nanocomposite material made of substituted Sr-hexaferrite nanoparticles and different percentage of single walled carbon nanotube have been studied. The structural, magnetic and electromagnetic properties of samples were studied as a function of volume percentage of SWCNTs by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, vibrating sample magnetometer and vector network analysis. Well suitable crystallinity of hexaferrite nanoparticles was confirmed by XRD patterns. TEM and FESEM micrographs were shown the good homogenity and high level of dispersivity of SWCNTs and Sr-hexaferrite nanoparticles in nanocomposite samples. The VSM results shown that with increasing in amount of CNTs (0-6 vol%), the saturation of magnetization decreased up to 11 emu/g for nanocomposite sample contains of 6 vol% of SWCNTs. The vector network analysis results show that the maximum value of reflection loss was -36.4 dB at the frequency of 11 GHz with an absorption bandwidth of more than 4 GHz (<-20 dB). The results indicate that, this nanocomposite material with appropriate amount of SWCNTs hold great promise for microwave device applications.

In-situ self-assembly of plant polyphenol-coated Fe3O4 particles for oleaginous microalgae harvesting.

PubMed

Wang, Xiaoyu; Zhao, Yuan; Jiang, Xiaoxue; Liu, Lijun; Li, Xue; Li, Huixian; Liang, Wenyan

2018-05-15

Plant polyphenol (PP), a natural polymer from the Larix gmelinii, was selected as the surfactant to synthesize Fe 3 O 4 . The Fe 3 O 4 -PP composite was prepared by in-situ self-assembly in solvothermal synthesis, and characterized using FE-SEM, TEM, XRD, FTIR, XPS, TGA, and VSM. The harvesting efficiency of Chlorella vulgaris was investigated under different parameters, including algal organic matter, dosage, and pH. The results showed that the core-shell sphere of Fe 3 O 4 -PP (∼150 nm) was coated by ∼50 nm PP with a saturated magnetization of 40.0 emu/g. The Fe 3 O 4 -PP could be directly applied to the culture broth (1.5 g dry cell weight/L, pH = 9.03), achieving 93.0% of harvesting efficiency at 20 g/L. Cells were detached from the harvested aggregates by adjusting pH value to 9.80 and with ultrasonication, which achieved 95.6% of recovery efficiency. The recycled Fe 3 O 4 -PP showed high stabilities in surface properties, maintaining more than 87.5% of harvesting efficiency after five recycles. Copyright © 2018 Elsevier Ltd. All rights reserved.

Synthesis of hierarchical flower-like Co3O4 superstructure and its excellent catalytic property for ammonium perchlorate decomposition

NASA Astrophysics Data System (ADS)

Li, Gang; Bai, Weiyang

2018-04-01

Hierarchical flower-like cobalt tetroxide (Co3O4) was successfully synthesized via a facile precipitation method in combination with heat treatment of the cobalt oxalate precursor. The samples were systematically characterized by thermo gravimetric analysis and derivative thermo gravimetric analysis (TGA-DTG), X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and N2 adsorption-desorption measurements. The results indicate that the as-fabricated Co3O4 exhibits uniform flower-like morphologies with diameters of 8-12 μm, which are constructed by one-dimensional nanowires. Furthermore, catalytic effect of this hierarchical porous Co3O4 on ammonium perchlorate (AP) pyrolysis was investigated using differential scanning calorimetry (DSC) techniques. It is found that the pyrolysis temperature of AP shifts 142 °C downward with a 2 wt% addition content of Co3O4. Meanwhile, the addition of Co3O4 results in a dramatic reduction of the apparent activation energy of AP pyrolysis from 216 kJ mol-1 to 152 kJ mol-1, determined by the Kissinger correlation. The results endorse this material as a potential catalyst in AP decomposition.

Effect of heavy tempering on microstructure and yield strength of 28CrMo48VTiB martensitic steel

NASA Astrophysics Data System (ADS)

Sun, Yu; Gu, Shunjie; Wang, Qian; Wang, Huibin; Wang, Qingfeng; Zhang, Fucheng

2018-02-01

The 28CrMo48VTiB martensitic steel for sulfide stress cracking (SSC) resistance oil country tubular goods (OCTG) of C110 grade was thermally processed through quenching at 890 °C and tempering at 600 °C-720 °C for 30-90 min. The microstructures of all samples were characterized using field emission scanning electron microscopy (FESEM), electron backscattering diffraction (EBSD), transmission electron microscopy (TEM) and x-ray diffractometry (XRD). Also, the tensile properties were measured. The results indicated that the yield strength (YS) decreased as both the tempering temperature and duration increased, due to the coarsening of martensitic packet/block/lath structures, the reduction of dislocation density, as well as the increase of both the volume fraction and average diameter of the precipitates. The martensitic lath width was the key microstructural parameter controlling the YS of this heavily-tempered martensitic steel, whereas the corresponding relationship was in accordance with the Langford-Cohen model. Furthermore, the martensitic structure boundary and the solid solution strengthening were the two most significant factors dominating the YS, in comparison with the dislocation and precipitation strengthening.

One-step in situ synthesis of graphene–TiO{sub 2} nanorod hybrid composites with enhanced photocatalytic activity

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

Sun, Mingxuan, E-mail: mingxuansun@sues.edu.cn; Li, Weibin; Sun, Shanfu

2015-01-15

Chemically bonded graphene/TiO{sub 2} nanorod hybrid composites with superior dispersity were synthesized by a one-step in situ hydrothermal method using graphene oxide (GO) and TiO{sub 2} (P25) as the starting materials. The as-prepared samples were characterized by XRD, XPS, TEM, FE-SEM, EDX, Raman, N{sub 2} adsorption, and UV–vis DRS techniques. Enhanced light absorption and a red shift of absorption edge were observed for the composites in the ultraviolet–visible diffuse reflectance spectroscopy (UV–vis DRS). Their effective photocatalytic activity was evaluated by the photodegradation of methylene blue under visible light irradiation. An enhancement of photocatalytic performance was observed over graphene/TiO{sub 2} nanorodmore » hybrid composite photocatalysts, as 3.7 times larger than that of pristine TiO{sub 2} nanorods. This work demonstrated that the synthesis of TiO{sub 2} nanorods and simultaneous conversion of GO to graphene “without using reducing agents” had shown to be a rapid, direct and clean approach to fabricate chemically bonded graphene/TiO{sub 2} nanorod hybrid composites with enhanced photocatalytic performance.« less

Fabrication of meso-porous BiOI sensitized zirconia nanoparticles with enhanced photocatalytic activity under simulated solar light irradiation

NASA Astrophysics Data System (ADS)

Vignesh, K.; Suganthi, A.; Min, Bong-Ki; Kang, Misook

2015-01-01

In this present work, BiOI sensitized zirconia (BiOI-ZrO2) nanoparticles were fabricated using a precipitation-deposition method. The physicochemical characteristics of BiOI/ZrO2 were studied through X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), BET-surface area, X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (UV-vis-DRS) and photoluminescence (PL) spectroscopy techniques. The absorption maximum of ZrO2 was shifted to the visible region after sensitization with BiOI. BET-surface area results inferred that the prepared hetero-junctions were meso-porous in nature. The photocatalytic activity of BiOI-ZrO2 for the degradation of methyl violet (MV) dye under simulated solar light irradiation was investigated in detail. 3% BiOI-ZrO2 exhibited the highest photocatalytic performance (98% of MV degradation) when compared with ZrO2 and BiOI. The enhancement in the photocatalytic activity of BiOI-ZrO2 is ascribed to the sensitization effect of BiOI, suppression of electron-hole recombination and the formation of p-n hetero-junction.

Heterogeneous Fenton-like discoloration of methyl orange using Fe3O4/MWCNTs as catalyst: combination mechanism and affecting parameters

NASA Astrophysics Data System (ADS)

Xu, Huan-Yan; Wang, Yuan; Shi, Tian-Nuo; Zhao, Hang; Tan, Qu; Zhao, Bo-Chao; He, Xiu-Lan; Qi, Shu-Yan

2018-03-01

Multi-walled carbon nanotubes (MWCNTs) can act not only as a support for Fe3O4 nanoparticles (NPs) but also as a coworker with synergistic effect, accordingly improving the heterogeneous Fenton-like efficiency of Fe3O4 NPs. In this study, Fe3O4 NPs were in situ anchored onto MWCNTs by a moderate co-precipitation method and the as-prepared Fe3O4/MWCNTs nanocomposites were employed as the highly efficient Fenton-like catalysts. The analyses of XRD, FTIR, Raman, FESEM, TEM and HRTEM results indicated the formation of Fe3O4 crystals in Fe3O4/MWCNTs nanocomposites prepared at different conditions and the interaction between Fe3O4 NPs and MWCNTs. Over a wide pH range, the surface of modified MWCNTs possessed negative charges. Based on these results, the possible combination mechanism between Fe3O4 NPs and MWCNTs was discussed and proposed. Moreover, the effects of preparation and catalytic conditions on the Fenton-like catalytic efficiency were investigated in order to gain further insight into the heterogeneous Fenton-like reaction catalyzed by Fe3O4/MWCNTs nanocomposites.

Preparation and characterization of nanostructured Pt/TiO2 thin films treated using electron beam.

PubMed

Shin, Joong-Hyeok; Woo, Hee-Gweon; Kim, Bo-Hye; Lee, Byung Cheol; Jun, Jin

2010-05-01

Pt nanoparticle-doped titanium dioxide (Pt/TiO2) thin films were prepared on a silicon wafer substrate by sol-gel spin coating process. The prepared thin films were treated with electron beam (EB at 1.1 MeV, 100, 200, 300 kGy) at air atmosphere. The effect of EB-irradiation on the composition of the treated thin films, optical properties and morphology of thin films were investigated by various analytical techniques such as X-ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The crystal structure of the TiO2 layer was found to be an anatase phase and the size of TiO2 particles was determined to be about 13 nm. Pt nanoparticles with diameter of 5 nm were observed on surface of the films. A new layer (presumed to be Pt-Ti complex and/or PtO2 compound) was created in the Pt/TiO2 thin film treated with EB (300 kGy). The transmittance of thin film decreased with EB treatment whereas the refractive index increased.

Core-shell structured SiO2@YVO4:Dy3+/Sm3+ phosphor particles: sol-gel preparation and characterization.

PubMed

Wang, H; Yu, M; Lin, C K; Lin, J

2006-08-01

Spherical SiO(2) particles have been coated with YVO(4):Dy(3+)/Sm(3+) phosphor layers by a Pechini sol-gel process, leading to the formation of core-shell structured SiO(2)@YVO(4):Dy(3+)/Sm(3+) particles. X-ray diffraction (XRD), Fourier-transform IR spectroscopy, field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting SiO(2)@YVO(4):Dy(3+)/Sm(3+) core-shell phosphors. The obtained core-shell phosphors have perfect spherical shape with narrow size distribution (average size ca. 300 nm), smooth surface and non-agglomeration. The thickness of shells could be easily controlled by changing the number of deposition cycles (20 nm for one deposition cycle). The core-shell particles show strong characteristic emission from Dy(3+) for SiO(2)@YVO(4):Dy(3+) and from Sm(3+) for SiO(2)@YVO(4):Sm(3+) due to an efficient energy transfer from YVO(4) host to them. The PL intensity of Dy(3+) and Sm(3+) increases with raising the annealing temperature and the number of coating cycles.

Simple sonochemical synthesis of Ho2O3-SiO2 nanocomposites as an effective photocatalyst for degradation and removal of organic contaminant.

PubMed

Zinatloo-Ajabshir, Sahar; Mortazavi-Derazkola, Sobhan; Salavati-Niasari, Masoud

2017-11-01

In this work, highly photocatalytically active Ho 2 O 3 -SiO 2 nanocomposites have been designed and applied for decomposition of methylene blue pollutant. Ho 2 O 3 -SiO 2 nanocomposites have been produced by new, quick and facile sonochemical process with the aid of tetramethylethylenediamine as a novel basic agent for the first time. The effect of the kind of basic agent, ultrasonic time and dosage of Ho source on the grain size, photocatalytic behavior and shape of the Ho 2 O 3 -SiO 2 nanocomposites have been evaluated for optimization the production condition. FESEM, EDX, FT-IR, DRS, XRD and TEM have been applied to characterize the as-produced Ho 2 O 3 -SiO 2 nanocomposites. Use of the as-produced Ho 2 O 3 -SiO 2 nanocomposites as photocatalyst via destruction of methylene blue pollutant under UV illumination has been compared. It was observed that SiO 2 has notable impact on catalytic activity of holmium oxide photocatalyst for destruction. Introducing of SiO 2 to holmium oxide can enhance destruction efficiency of holmium oxide to methylene blue pollutant under ultraviolet light. Copyright © 2017 Elsevier B.V. All rights reserved.

β-cyclodextrin functionalized poly (5-amidoisophthalicacid) grafted Fe3O4 magnetic nanoparticles: A novel biocompatible nanocomposite for targeted docetaxel delivery

NASA Astrophysics Data System (ADS)

Tarasi, Roghayeh; Khoobi, Mehdi; Niknejad, Hassan; Ramazani, Ali; Ma'mani, Leila; Bahadorikhalili, Saeed; Shafiee, Abbas

2016-11-01

Thiol-lactam initiated radical polymerization (TLIRP) was successfully employed to prepare poly-N-5-acrylamidoisophthalicacid grafted onto Fe3O4 magnetic nanoparticles (MNPs@PAIP). β-Cyclodextrin (CD) was then conjugated to the carboxylic groups of the prepared MNPs via carbodiimide activation. Subsequently, tumor-targeting folic acid (FA) was attached to the hydroxyl groups of CD on the surface of the latter MNPs to increase the site-specific intracellular delivery. The prepared MNPs were fully characterized by FTIR, VSM, TGA, XRD, FE-SEM and TEM. Docetaxel (DTX) as hydrophobic anticancer drug was loaded via host-guest inclusion complexation with CD and the release profile of the system was studied at different pH. The effect of MNPs on the cell viability was evaluated for the human embryonic kidney normal cell line (HEK293) as well as HeLa and MDA-MB-231 cancerous cell lines and the results did not show any apparent cytotoxic effect. In comparison, DTX loaded MNPs reduced the growth of HeLa and MDA-MB-231 cells more than free DTX. Intracellular uptake ability of DTX loaded MNPs was also studied using fluorescent microscopy and showed cellular uptake about 90% after 4 h treatment.

A hydro/organo/hybrid gelator: a peptide lipid with turning aspartame head groups.

PubMed

Mukai, Masaru; Minamikawa, Hiroyuki; Aoyagi, Masaru; Asakawa, Masumi; Shimizu, Toshimi; Kogiso, Masaki

2013-04-01

This work presents a novel bola-type peptide lipid which can gelate water, organic solvents, and water/organic-solvent mixtures. In its molecular structure, an amphiphilic dipeptide aspartame (L-α-aspartyl-L-phenylalanine methyl ester) is connected at both ends of an alkylene linker. The different morphologies in the hydrogel (helical nanotapes) and the organogel (tape-like nanostructures) were visualized by energy-filtering transmission electron microscopy (EF-TEM) and energy-filtering scanning electron microscopy (FE-SEM), and the molecular arrangement was examined using X-ray diffraction (XRD), infrared (IR) spectroscopy, and circular dichroism (CD) spectroscopy. Possessing a hydrophilic aspartic acid group and a (relatively) hydrophobic phenylalanine methyl ester group, the dipeptide head group can turn about in response to solvent polarity. As a consequence, the solvent condition changed the molecular packing of the gelator and affected the overall supramolecular structure of the gel. It is noted that the peptide lipid gelated mixed solvents of water and organic solvents such as dichloromethane, liquid-paraffin, olive-oil, silicone-oils, and so on. The present hybrid gel can simultaneously hold hydrophilic and hydrophobic functional materials. Copyright © 2013 Elsevier Inc. All rights reserved.

High-pressure homogenization associated hydrothermal process of palygorskite for enhanced adsorption of Methylene blue

NASA Astrophysics Data System (ADS)

Zhang, Zhifang; Wang, Wenbo; Wang, Aiqin

2015-02-01

Palygorskite (PAL) was modified by a high-pressure homogenization assisted hydrothermal process. The effects of modification on the morphology, structure and physicochemical properties of PAL were systematically investigated by Field-emission scanning electron microscopy (FESEM), Transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FTIR), Brunauer-Emmett-Teller (BET) analysis, X-ray diffraction (XRD) and Zeta potential analysis techniques, and the adsorption properties were systematically evaluated using Methylene blue (MB) as the model dye. The results revealed that the crystal bundles were disaggregated and the PAL nanorods became more even after treated via associated high-pressure homogenization and hydrothermal process, and the crystal bundles were dispersed as nanorods. The intrinsic crystal structure of PAL was remained after hydrothermal treatment, and the pore size calculated by the BET method was increased. The adsorption properties of PAL for MB were evidently improved (from 119 mg/g to 171 mg/g) after modification, and the dispersion of PAL before hydrothermal reaction is favorable to the adsorption. The desorption evaluation confirms that the modified PAL has stronger affinity with MB, which is benefit to fabricate a stable organic-inorganic hybrid pigment.

From the iron boring scraps to superparamagnetic nanoparticles through an aerobic biological route.

PubMed

Daneshvar, Majid; Hosseini, Mohammad Raouf

2018-06-15

A straightforward, highly efficient, and low-cost biological route was introduced for the synthesis of magnetic nanoparticles. Three urease-positive bacteria namely, Bacillus subtilis, B. pasteurii, and B. licheniformis were used to biosynthesize ammonia and biosurfactants required for the nanoparticle production. Also, the features of the applied biological approach was compared with a chemical co-precipitation method. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), dynamic light scattering (DLS), vibrating-sample magnetometer (VSM), and Fourier transform infrared spectroscopy (FTIR) were applied to characterize the synthesized nanoparticles. Results indicated that the biologically fabricated powders had a single domain structure, and their mean particle size was in the range of 37 to 97 nm. The production capacity of the biological processes was double the chemical method, and the biosynthesized superparamagnetic nanoparticles had higher saturation magnetization up to 132 emu/g. Finally, the removal of Cr(VI) from a synthetic solution was investigated using the four products. The maximum elimination of chromium (over 99%) was achieved by the particles synthesized by B. pasteurii, with the adsorption capacity of 190 mg/g. Copyright © 2018 Elsevier B.V. All rights reserved.

Synthesis and optimization of the magnetic properties of aligned strontium ferrite nanowires

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

Ebrahimi, Fatemeh, E-mail: F.Ebrahimi@ma.iut.ac.ir; Bakhshi, Saeed Reza; Ashrafizadeh, Fakhreddin

Highlights: • Dip coating method was used to synthesize strontium ferrite nanowires in template. • Size of nanowires was controlled via anodization parameters. • Fe/Sr ratio was optimized in precursor. • Magnetic properties of nanowires and nanopowders were compared. - Abstract: High aspect ratio strontium hexaferrite nanowires were fabricated by dip coating in alumina template. Fe/Sr ratio was changed from 10 to 12 in precursor, and the samples were annealed at a range of temperatures 500–900 °C in order to optimize the magnetic properties of strontium ferrite in the form of nanowires. Field emission scanning electron microscope (FESEM) proved themore » formation of nanowires in the templates, while TEM images revealed a high degree of crystallinity. The ferrites were further characterized by X-ray diffraction (XRD) and energy dispersive X-ray spectrometer (EDS). Magnetic properties of the specimens were studied by a SQUID at 10–300 K. The results showed that the coercivity of packed density nanowires in the template was much less than that of the nanopowders. On the other hand, the coercivity of nanowires at ambient temperature was less than low temperature coercivity.« less

Magnesium ferrite nanocrystal clusters for magnetorheological fluid with enhanced sedimentation stability

NASA Astrophysics Data System (ADS)

Wang, Guangshuo; Ma, Yingying; Li, Meixia; Cui, Guohua; Che, Hongwei; Mu, Jingbo; Zhang, Xiaoliang; Tong, Yu; Dong, Xufeng

2017-01-01

In this study, magnesium ferrite (MgFe2O4) nanocrystal clusters were synthesized using an ascorbic acid-assistant solvothermal method and evaluated as a candidate for magnetorheological (MR) fluid. The morphology, microstructure and magnetic properties of the MgFe2O4 nanocrystal clusters were investigated in detail by field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), thermogravimetric analyzer (TGA), X-ray diffraction (XRD) and superconducting quantum interference device (SQUID). The MgFe2O4 nanocrystal clusters were suspended in silicone oil to prepare MR fluid and the MR properties were tested using a Physica MCR301 rheometer fitted with a magneto-rheological module. The prepared MR fluid showed typical Bingham plastic behavior, changing from a liquid-like to a solid-like structure under an external magnetic field. Compared with the conventional carbonyl iron particles, MgFe2O4 nanocrystal clusters-based MR fluid demonstrated enhanced sedimentation stability due to the reduced mismatch in density between the particles and the carrier medium. In summary, the as-prepared MgFe2O4 nanocrystal clusters are regarded as a promising candidate for MR fluid with enhanced sedimentation stability.

Field emission and photoluminescence of ZnO nanocombs

NASA Astrophysics Data System (ADS)

Wang, B.; Wu, H. Y.; Zheng, Z. Q.; Yang, Y. H.

2013-11-01

Three kinds of new comb-shape nanostructures of ZnO have been grown on single silicon substrates without catalyst-assisted thermal evaporation of Zn and active carbon powders. The morphology and structure of the prepared nanorods are determined on the basis of field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and x-ray diffraction (XRD). The growth mechanism of the ZnO nanocombs can be explained on the basis of the vapor-solid (VS) processes. In nanocombs 1 and nanocombs 2, the comb teeth grow along [0001] and the comb stem grows along [], while in nanocombs 3, nanoteeth grow along [] and stem grows along [0001]. The photoluminescence and field-emission properties of ZnO nanocombs 1-3 have been investigated. The turn-on electric field of ZnO nanocombs 1-3, which is defined as the field required to producing a current density of 10 μA/cm2, is 9, 7.7 and 7.1 V/μm, respectively. The field-emission performance relies not only on the tip’s radius of curvature and field enhancement factor, but also on the factor evaluating the degree of the screening effect.

Conversion of CH4/CO2 to syngas over Ni-Co/Al2O3-ZrO2 nanocatalyst synthesized via plasma assisted co-impregnation method: Surface properties and catalytic performance

NASA Astrophysics Data System (ADS)

Rahemi, Nader; Haghighi, Mohammad; Akbar Babaluo, Ali; Fallah Jafari, Mahdi; Khorram, Sirous

2013-09-01

Ni/Al2O3 catalyst promoted by Co and ZrO2 was prepared by co-impregnation method and treated with glow discharge plasma. The catalytic activity of the synthesized nanocatalysts has been tested toward conversion of CH4/CO2 to syngas. The physicochemical characterizations like XRD, EDX, FESEM, TEM, BET, FTIR, and XPS show that plasma treatment results in smaller particle size, more surface concentration, and uniform morphology. The dispersion of nickel in plasma-treated nanocatalyst was also significantly improved, which was helpful for controlling the ensemble size of active phase atoms on the support surface. Improved physicochemical properties caused 20%-30% enhancement in activity of plasma-treated nanocatalyst that means to achieve the same H2 or CO yield, the plasma-treated nanocatalyst needed about 100 °C lower reaction temperature. The H2/CO ratio got closer to 1 at higher temperatures and finally at 850 °C H2/CO = 1 is attained for plasma-treated nanocatalyst. Plasma-treated nanocatalyst due to smaller Ni particles and strong interaction between active phase and support has lower tendency to keep carbon species on its structure and hence excellent stability can be observed for this catalyst.

Controlled release and long-term antibacterial activity of reduced graphene oxide/quaternary ammonium salt nanocomposites prepared by non-covalent modification.

PubMed

Ye, Xiaoli; Feng, Jin; Zhang, Jingxian; Yang, Xiujiang; Liao, Xiaoyan; Shi, Qingshan; Tan, Shaozao

2017-01-01

In order to control the long-term antibacterial property of quaternary ammonium salts, dodecyl dimethyl benzyl ammonium chloride (rGO-1227) and rGO-bromohexadecyl pyridine (rGO-CPB) were self-assembled on surfaces of reduced graphene oxide (rGO) via π-π interactions. The obtained rGO-1227 and rGO-CPB nanocompounds were characterized by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM).The antibacterial activities were evaluated on Gram-negative Escherichia coli and Gram-positive Staphylococcus aureus. Both rGO-CPB and rGO-1227 reduced the cytotoxicity of the pure antimicrobial agents and presented strong antimicrobial properties. Especially, CPB could be loaded efficiently on the surface of rGO via π-π conjugate effect, which resulted in a nanocomposite presenting a long-term antibacterial capability due to the more important quantity of free π electrons compared to that of 1227. When comparing the advantages of both prepared nanocomposites, rGO-CPB displayed a better specific-targeting capability and a longer-term antibacterial property. Copyright © 2016 Elsevier B.V. All rights reserved.

Electrocatalytic behavior of a nanocomposite of Ni/Pd supported by carbonized PVA nanofibers towards formic acid, ethanol and urea oxidation: A physicochemical and electro-analysis study

NASA Astrophysics Data System (ADS)

Mohamed, Ibrahim M. A.; Yasin, Ahmed S.; Barakat, Nasser A. M.; Song, Seung A.; Lee, Ha Eun; Kim, Seong Su

2018-03-01

A nanocomposite of Ni/Pd supported by carbonized poly-vinyl alcohol (PVA) nanofibers (NFs) was synthesized via electrospinning followed by calcination under an argon atmosphere. The as-synthesized NFs were studied using physicochemical analyses, such as field-emission scanning electron microscopy (FESEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTsbnd IR) and X-ray photoelectron spectroscopy (XPS), to investigate the morphology, crystallinity, effect of carbonization and surface chemistry of the NFs, respectively. Cyclic voltammetry (CV) and chronoamperometry (CA) were utilized to study the performance of the NFs towards electrooxidation reactions. The designed NFs present superior electrocatalytic behavior in an acid medium towards formic acid oxidation, as well as urea and ethanol oxidation in an alkaline medium. The electrocatalytic performance of the bimetallic NFs appears to arise from the assembly of bimetallic Ni/Pd@NFs based on PVA, which has hydroxyl groups. These hydroxyl groups can decrease the negative processes that occur as a result of metal-metal interactions, such as the aggregation process. This study introduces a novel non-precious electrocatalyst to facilitate the commercialization of fuel cells based on formic acid, urea and ethanol.

Hydrothermal Synthesis Au-Bi2Te3 Nanocomposite Thermoelectric Film with a Hierarchical Sub-Micron Antireflection Quasi-Periodic Structure.

PubMed

Tian, Junlong; Zhang, Wang; Zhang, Yuan; Xue, Ruiyang; Wang, Yuhua; Zhang, Zhijian; Zhang, Di

2015-06-03

In this work, Au-Bi(2)Te(3) nanocomposite thermoelectric film with a hierarchical sub-micron antireflection quasi-periodic structure was synthesized via a low-temperature chemical route using Troides helena (Linnaeus) forewing (T_FW) as the biomimetic template. This method combines chemosynthesis with biomimetic techniques, without the requirement of expensive equipment and energy intensive processes. The microstructure and the morphology of the Au-Bi(2)Te(3) nanocomposite thermoelectric film was analyzed by X-ray diffraction (XRD), field-emission scanning-electron microscopy (FESEM), and transmission electron microscopy (TEM). Coupled the plasmon resonances of the Au nanoparticles with the hierarchical sub-micron antireflection quasi-periodic structure, the Au-Bi(2)Te(3) nanocomposite thermoelectric film possesses an effective infrared absorption and infrared photothermal conversion performance. Based on the finite difference time domain method and the Joule effect, the heat generation and the heat source density distribution of the Au-Bi(2)Te(3) nanocomposite thermoelectric film were studied. The heterogeneity of heat source density distribution of the Au-Bi(2)Te(3) nanocomposite thermoelectric film opens up a novel promising technique for generating thermoelectric power under illumination.

Characterization of modified SiC@SiO2 nanocables/MnO2 and their potential application as hybrid electrodes for supercapacitors.

PubMed

Zhang, Yujie; Chen, Junhong; Fan, Huili; Chou, Kuo-Chih; Hou, Xinmei

2015-12-14

In this research, we demonstrate a simple route for preparing SiC@SiO2 core-shell nanocables and furthermore obtain SiC@SiO2 nanocables/MnO2 as hybrid electrodes for supercapacitors using various modified methods. The modified procedure consists of mild modifications using sodium hydroxide as well as UV light irradiation and deposition of MnO2. The morphology and microstructural characteristics of the composites are investigated using XRD, XPS, FE-SEM with EDS and TEM. The results indicate that the surfaces of modified SiC@SiO2 nanocables are uniformly coated with a MnO2 thin layer. The electrochemical behaviors of the hybrid electrodes are systematically measured in a three-electrode system using cyclic voltammetry, galvanostatic charge/discharge and electrochemical impedance spectroscopy. The resultant electrode presents a superb charge storage characteristic with a large specific capacitance of 276.3 F g(-1) at the current density of 0.2 A g(-1). Moreover, the hybrid electrode also displays a long cycle life with a good capacitance retention (∼92.0%) after 1000 CV cycles, exhibiting a promising potential for supercapacitors.

New Route for Synthesis of Fluorescent SnO₂ Nanoparticles for Selective Sensing of Fe(III) in Aqueous Media.

PubMed

Vyas, Gaurav; Kumar, Anshu; Bhatt, Madhuri; Bhatt, Shreya; Paul, Parimal

2018-06-01

A simple new route for synthesis of fluorescent SnO2 and its application as an efficient sensing material for Fe3+ in aqueous media is reported. The fluorescent SnO2 nanoparticles were obtained by oxidation of SnCl2, which when used as reducing agent for the reduction of organic nitro compounds to corresponding amino compounds in ethanol. The SnO2 nanoparticles have been characterized on the basis of powder-XRD, IR, UV-Vis, TEM, FESEM and EDX analysis and found that this material is highly fluorescent in aqueous media. Detail study revealed that this material functions as a selective probe for Fe3+ out of a large number of metal ions used. The oxygen vacancies (defects) generated on the surface of the SnO2 during synthesis, are the source of emission due to recombination of electrons with the photo-excited hole in the valance bond. The quenching of emission intensity in presence of Fe3+ is due to the nonradiative recombination of electrons and holes at the surface. This material is used for estimation of Fe3+ in real samples such as drinking water, tap water and soil.

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Hasegawa, Y.; Tsuda, H.; Mori, S.; Halbig, M. C.; Asthana, R.; Singh, M.

2017-01-01

SiC fiber-bonded ceramics (SA-Tyrannohex: SA-THX) diffusion-bonded with TiCu metallic interlayers were investigated. Thin samples of the ceramics were prepared with a focused ion beam (FIB) and the interfacial microstructure of the prepared samples was studied by transmission electron microscopy (TEM) and scanning TEM (STEM). In addition to conventional microstructure observation, for detailed analysis of reaction compounds in diffusion-bonded area, we performed STEM-EDS measurements and selected area electron diffraction (SAD) experiments. The TEM and STEM experiments revealed the diffusion-bonded area was composed of only one reaction layer, which was characterized by TiC precipitates in Cu-Si compound matrix. This reaction layer was in good contact with the SA-THX substrates, and it is concluded that the joint structure led to the excellent bonding strength.

Effects of diagnostic ionizing radiation on pregnancy via TEM

NASA Astrophysics Data System (ADS)

Mohammed, W. H.; Artoli, A. M.

2008-08-01

In Sudan, X-rays are routinely used at least once for measurements of pelvis during the gestation period, though this is highly prohibited worldwide, except for a few life threatening cases. To demonstrate the effect of diagnostic ionizing radiation on uterus, fetus and neighboring tissues to the ovaries, two independent experiments on pregnant rabbits were conducted. The first experiment was a proof of concept that diagnostic ionizing radiation is hazardous throughout the gestation period. The second experiment was done through Transmission Electron Microscopy (TEM) to elucidate the morphological changes in the ultra structure of samples taken from irradiated pregnant rabbits. This study uses TEM to test the effect of diagnostic radiation of less than 0.6 Gray on the cellular level. Morphological changes have been captured and the images were analyzed to quantify these effects.

TEM1 expression in cancer-associated fibroblasts is correlated with a poor prognosis in patients with gastric cancer

PubMed Central

Fujii, Satoshi; Fujihara, Ayano; Natori, Kei; Abe, Anna; Kuboki, Yasutoshi; Higuchi, Youichi; Aizawa, Masaki; Kuwata, Takeshi; Kinoshita, Takahiro; Yasui, Wataru; Ochiai, Atsushi

2015-01-01

The cancer stroma, including cancer-associated fibroblasts (CAFs), is known to contribute to cancer cell progression and metastasis, suggesting that functional proteins expressed specifically in CAFs might be candidate molecular targets for cancer treatment. The purpose of the present study was to explore the possibility of using TEM1 (tumor endothelial marker 1), which is known to be expressed in several types of mesenchymal cells, as a molecular target by examining the impact of TEM1 expression on clinicopathological factors in gastric cancer patients. A total of 945 consecutive patients with gastric cancer who underwent surgery at the National Cancer Center Hospital East between January 2003 and July 2007 were examined using a tissue microarray approach. TEM1 expression in CAFs or vessel-associated cells was determined using immunohistochemical staining. Three items (CAF-TEM1-positivity, CAF-TEM1-intensity, and vessel-TEM1-intensity) were then examined to determine the correlations between the TEM1 expression status and the recurrence-free survival (RFS), overall survival (OS), cancer-related survival (COS), and other clinicopathological factors. Significant correlations between CAF-TEM1-positivity or CAF-TEM1-intensity and RFS, OS, or COS were observed (P < 0.001, Kaplan–Meier curves); however, no significant correlation between vessel-TEM1-intensity and RFS, OS, or COS was observed. A univariate analysis showed that CAF-TEM1-positivity and CAF-TEM1-intensity were each correlated with a scirrhous subtype, tumor depth, nodal status, distant metastasis, serosal invasion, lymphatic or venous vessel infiltrations, and pTMN stage. This study suggests that the inhibition of TEM1 expression specifically in the CAFs of gastric carcinoma might represent a new strategy for the treatment of gastric cancer. PMID:26336878

Plasmonic characterization of photo-induced silver nanoparticles extracted from silver halide based TEM film

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

Sudheer,, E-mail: sudheer@rrcat.gov.in; Tiwari, P.; Rai, V. N.

The plasmonic responses of silver nanoparticles extracted from silver halide based electron microscope film are investigated. Photo-reduction process is carried out to convert the silver halide grains into the metallic silver. The centrifuge technique is used for separating the silver nanoparticles from the residual solution. Morphological study performed by field emission scanning electron microscope (FESEM) shows that all the nanoparticles have an average diameter of ~120 nm with a high degree of mono dispersion in size. The localized surface plasmon resonance (LSPR) absorption peak at ~537 nm confirms the presence of large size silver nanoparticles.

Ultrasonic assisted synthesis of Bikitaite zeolite: A potential material for hydrogen storage application.

PubMed

Roy, Priyanka; Das, Nandini

2017-05-01

Li containing Bikitaite zeolite has been synthesized by an ultrasound-assisted method and used as a potential material for hydrogen storage application. The Sonication energy was varied from 150W to 250W and irradiation time from 3h to 6h. The Bikitaite nanoparticles were characterized by X-ray diffraction (XRD), infrared (IR) spectral analysis, and field-emission scanning electron microscopy (FESEM) thermo-gravimetrical analysis and differential thermal analysis (TGA, DTA). XRD and IR results showed that phase pure, nano crystalline Bikitaite zeolites were started forming after 3h irradiation and 72h of aging with a sonication energy of 150W and nano crystalline Bikitaite zeolite with prominent peaks were obtained after 6h irradiation of 250W sonic energy. The Brunauer-Emmett-Teller (BET) surface area of the powder by N 2 adsorption-desorption measurements was found to be 209m 2 /g. The TEM micrograph and elemental analysis showed that desired atomic ratio of the zeolite was obtained after 6h irradiation. For comparison, sonochemical method, followed by the hydrothermal method, with same initial sol composition was studied. The effect of ultrasonic energy and irradiation time showed that with increasing sonication energy, and sonication time phase formation was almost completed. The FESEM images revealed that 50nm zeolite crystals were formed at room temperature. However, agglomerated particles having woollen ball like structure was obtained by sonochemical method followed by hydrothermal treatment at 100°C for 24h. The hydrogen adsorption capacity of Bikitaite zeolite with different Li content, has been investigated. Experimental results indicated that the hydrogen adsorption capacities were dominantly related to their surface areas as well as total pore volume of the zeolite. The hydrogen adsorption capacity of 143.2c.c/g was obtained at 77K and ambient pressure of (0.11MPa) for the Bikitaite zeolite with 100% Li, which was higher than the reported values for

Sb:SnO2 thin films-synthesis and characterization

NASA Astrophysics Data System (ADS)

Bhadrapriya B., C.; Varghese, Anitta Rose; Amarendra, G.; Hussain, Shamima

2018-04-01

Transparent thin films of antimony doped SnO2 have been synthesized and characterized using optical spectroscopy, XRD, RAMAN and FESEM. The band gap of Sb doped tin oxide thin film samples were found to vary from 3.26 eV to 3.7 eV. The XRD peaks showed prominent rutile SnO2 peaks with diminished intensity due to antimony doping. A wide band in the range 550-580 cm-1 was observed in raman spectra and is a feature of nano-sized SnO2. SEM images showed flower-like structures on thin film surface, a characteristic feature of antimony.

Technical Evaluation Motor 3 (TEM-3)

NASA Technical Reports Server (NTRS)

Garecht, Diane

1989-01-01

A primary objective of the technical evaluation motor program is to recover the case, igniter and nozzle hardware for use on the redesigned solid rocket motor flight program. Two qualification objectives were addressed and met on TEM-3. The Nylok thread locking device of the 1U100269-03 leak check port plug and the 1U52295-04 safe and arm utilizing Krytox grease on the barrier-booster shaft O-rings were both certified. All inspection and instrumentation data indicate that the TEM-3 static test firing conducted 23 May 1989 was successful. The test was conducted at ambient conditions with the exception of the field joints (set point of 121 F, with a minimum of 87 F at the sensors), igniter joint (set point at 122 F with a minimum of 87 F at sensors) and case-to-nozzle joint (set point at 114 F with a minimum of 87 F at sensors). Ballistics performance values were within specification requirements. Nozzle performance was nominal with typical erosion. The nozzle and the case joint temperatures were maintained at the heaters controlling set points while electrical power was supplied. The water and the CO2 quench systems prevented damage to the metal hardware. All other test equipment performed as planned, contributing to a successful motor firing. All indications are that the test was a success, and all expected hardware will be refurbished for the RSRM program.

Detecting single-electron events in TEM using low-cost electronics and a silicon strip sensor.

PubMed

Gontard, Lionel C; Moldovan, Grigore; Carmona-Galán, Ricardo; Lin, Chao; Kirkland, Angus I

2014-04-01

There is great interest in developing novel position-sensitive direct detectors for transmission electron microscopy (TEM) that do not rely in the conversion of electrons into photons. Direct imaging improves contrast and efficiency and allows the operation of the microscope at lower energies and at lower doses without loss in resolution, which is especially important for studying soft materials and biological samples. We investigate the feasibility of employing a silicon strip detector as an imaging detector for TEM. This device, routinely used in high-energy particle physics, can detect small variations in electric current associated with the impact of a single charged particle. The main advantages of using this type of sensor for direct imaging in TEM are its intrinsic radiation hardness and large detection area. Here, we detail design, simulation, fabrication and tests in a TEM of the front-end electronics developed using low-cost discrete components and discuss the limitations and applications of this technology for TEM.

Comprehensive analysis of TEM methods for LiFePO4/FePO4 phase mapping: spectroscopic techniques (EFTEM, STEM-EELS) and STEM diffraction techniques (ACOM-TEM).

PubMed

Mu, X; Kobler, A; Wang, D; Chakravadhanula, V S K; Schlabach, S; Szabó, D V; Norby, P; Kübel, C

2016-11-01

Transmission electron microscopy (TEM) has been used intensively in investigating battery materials, e.g. to obtain phase maps of partially (dis)charged (lithium) iron phosphate (LFP/FP), which is one of the most promising cathode material for next generation lithium ion (Li-ion) batteries. Due to the weak interaction between Li atoms and fast electrons, mapping of the Li distribution is not straightforward. In this work, we revisited the issue of TEM measurements of Li distribution maps for LFP/FP. Different TEM techniques, including spectroscopic techniques (energy filtered (EF)TEM in the energy range from low-loss to core-loss) and a STEM diffraction technique (automated crystal orientation mapping (ACOM)), were applied to map the lithiation of the same location in the same sample. This enabled a direct comparison of the results. The maps obtained by all methods showed excellent agreement with each other. Because of the strong difference in the imaging mechanisms, it proves the reliability of both the spectroscopic and STEM diffraction phase mapping. A comprehensive comparison of all methods is given in terms of information content, dose level, acquisition time and signal quality. The latter three are crucial for the design of in-situ experiments with beam sensitive Li-ion battery materials. Furthermore, we demonstrated the power of STEM diffraction (ACOM-STEM) providing additional crystallographic information, which can be analyzed to gain a deeper understanding of the LFP/FP interface properties such as statistical information on phase boundary orientation and misorientation between domains. Copyright © 2016 Elsevier B.V. All rights reserved.

Appendix B: Summary of TEM Particle Size Distribution Datasets

EPA Pesticide Factsheets

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

Structural investigations in helium charged titanium films using grazing incidence XRD and EXAFS spectroscopy

NASA Astrophysics Data System (ADS)

Wan, Chubin; Zhou, Xiaosong; Wang, Yuting; Li, Shina; Ju, Xin; Peng, Shuming

2014-01-01

The crystal structure and local atomic arrangements surrounding Ti atoms were determined for He-charged hexagonal close-packed (hcp) Ti films and measured at glancing angles by synchrotron radiation X-ray diffraction (XRD) and extended X-ray absorption fine structure (EXAFS) spectroscopy, respectively. The charged specimens were prepared by direct current magnetron sputtering with a He/Ar mixture. He atoms with a relatively medium concentration (He/Ti atomic ratio as high as 17 at.%) were incorporated evenly in the deposited films. XRD results showed the changes in the peak intensities in Ti films with different He contents. EXAFS Fourier Transform analysis indicated that the average Ti-Ti distance decreased significantly, and proved the existence of phase transition.

Dispersion of Co/CNTs via strong electrostatic adsorption method: Thermal treatment effect

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

Akbarzadeh, Omid, E-mail: omid.akbarzadeh63@gmail.com; Abdullah, Bawadi, E-mail: bawadi-abdullah@petronas.com.my; Subbarao, Duvvuri, E-mail: duvvuri-subbarao@petronas.com.my

The effect of different thermal treatment temperature on the structure of multi-walled carbon nanotubes (MWCNTs) and Co particle dispersion on CNTs support is studied using Strong electrostatic adsorption (SEA) method. The samples tested by N{sub 2}-adsorption, field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). N{sub 2}-adsorption results showed BET surface area increased using thermal treatment and TEM images showed that increasing the thermal treatment temperature lead to flaky CNTs and defects introduced on the outer surface and Co particle dispersion increased.

Surface morphology and electrochemical studies on polyaniline/CuO nano composites

NASA Astrophysics Data System (ADS)

Ashokkumar, S. P.; Vijeth, H.; Yesappa, L.; Niranjana, M.; Vandana, M.; Basappa, M.; Devendrappa, H.

2018-05-01

An electrochemically synthesized Polyaniline (PANI) and Polyaniline/copper oxide (PCN) nano composite have studied the morphology and electrochemical properties. The composite is characterized by X-ray diffraction (XRD) and surface morphology was studied using FESEM and electrochemical behavior is studied using cyclic voltammetry (CV) technique. The CV curves shows rectangular shaped curve and they have contribution to electrical double layer capacitance (EDCL).

Quantitative energy-filtered TEM imaging of interfaces

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

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

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

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

PubMed

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

2015-12-16

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

Distortion of DNA Origami on Graphene Imaged with Advanced TEM Techniques.

PubMed

Kabiri, Yoones; Ananth, Adithya N; van der Torre, Jaco; Katan, Allard; Hong, Jin-Yong; Malladi, Sairam; Kong, Jing; Zandbergen, Henny; Dekker, Cees

2017-08-01

While graphene may appear to be the ultimate support membrane for transmission electron microscopy (TEM) imaging of DNA nanostructures, very little is known if it poses an advantage over conventional carbon supports in terms of resolution and contrast. Microscopic investigations are carried out on DNA origami nanoplates that are supported onto freestanding graphene, using advanced TEM techniques, including a new dark-field technique that is recently developed in our lab. TEM images of stained and unstained DNA origami are presented with high contrast on both graphene and amorphous carbon membranes. On graphene, the images of the origami plates show severe unwanted distortions, where the rectangular shape of the nanoplates is significantly distorted. From a number of comparative control experiments, it is demonstrated that neither staining agents, nor screening ions, nor the level of electron-beam irradiation cause this distortion. Instead, it is suggested that origami nanoplates are distorted due to hydrophobic interaction of the DNA bases with graphene upon adsorption of the DNA origami nanoplates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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

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

2013-11-13

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

Joint TEM and MT aquifer study in the Atacama Desert, North Chile

NASA Astrophysics Data System (ADS)

Ruthsatz, Alexander D.; Sarmiento Flores, Alvaro; Diaz, Daniel; Reinoso, Pablo Salazar; Herrera, Cristian; Brasse, Heinrich

2018-06-01

The Atacama Desert represents one of the driest regions on earth, and despite the absence of sustainable clean water reserves the demand has increased drastically since 1970 as a result of growing population and expanding mining activities. Magnetotelluric (MT) and Transient Electromagnetic (TEM) measurements were carried out for groundwater exploration in late 2015 in the area of the Profeta Basin at the western margin of the Chilean Precordillera. Both methods complement each other: While MT in general attains larger penetration depths, TEM allows better resolution of near surface layers; furthermore TEM is free from galvanic distortion. Data were collected along three profiles, enabling a continuous resistivity image from the surface to at least several hundred meters depth. TEM data were inverted in a 1-D manner, consistently yielding a poorly conductive near-surface layer with a thickness of approximately 30 m and below a well-conducting layer which we interpret as the aquifer with resistivities around 10 Ωm. At marginal sites of the main SW-NE-profile the resistive basement was found in 150 m. These depths are confirmed by interpretation of the MT soundings. Those were firstly inverted with a 2-D approach and then by 3-D inversion as clear indications of three-dimensionality exist. Several modeling runs were performed with different combinations of transfer functions and smoothing parameters. Generally, MT and TEM results agree reasonably well and an overall image of the resistivity structures in the Profeta Basin could be achieved. The aquifer reaches depths of more than 500 m in parts and, by applying Archie's law, resistivities of 1 Ωm can be assumed, indicating highly saline fluids from the source region of the surrounding high Andes under persisting arid conditions.

Investigating Processes of Materials Formation via Liquid Phase and Cryogenic TEM

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

De Yoreo, James J.; Sommerdijk, Nico

2016-06-14

The formation of materials in solutions is a widespread phenomenon in synthetic, biological and geochemical systems, occurring through dynamic processes of nucleation, self-assembly, crystal growth, and coarsening. The recent advent of liquid phase TEM and advances in cryogenic TEM are transforming our understanding of these phenomena by providing new insights into the underlying physical and chemical mechanisms. The techniques have been applied to metallic and semiconductor nanoparticles, geochemical and biological minerals, electrochemical systems, macromolecular complexes, and selfassembling systems, both organic and inorganic. New instrumentation and methodologies currently on the horizon promise new opportunities for advancing the science of materials synthesis.

Characterization of some biological specimens using TEM and SEM

NASA Astrophysics Data System (ADS)

Ghosh, Nabarun; Smith, Don W.

2009-05-01

The advent of novel techniques using the Transmission and Scanning Electron Microscopes improved observation on various biological specimens to characterize them. We studied some biological specimens using Transmission and Scanning Electron Microscopes. We followed negative staining technique with Phosphotungstic acid using bacterial culture of Bacillus subtilis. Negative staining is very convenient technique to view the structural morphology of different samples including bacteria, phage viruses and filaments in a cell. We could observe the bacterial cell wall and flagellum very well when trapped the negative stained biofilm from bacterial culture on a TEM grid. We cut ultra thin sections from the fixed root tips of Pisum sativum (Garden pea). Root tips were pre fixed with osmium tetroxide and post fixed with uranium acetate and placed in the BEEM capsule for block making. The ultrathin sections on the grid under TEM showed the granular chromatin in the nucleus. The protein bodies and large vacuoles with the storage materials were conspicuous. We followed fixation, critical point drying and sputter coating with gold to view the tissues with SEM after placing on stubs. SEM view of the leaf surface of a dangerous weed Tragia hispida showed the surface trichomes. These trichomes when break on touching releases poisonous content causing skin irritation. The cultured tissue from in vitro culture of Albizia lebbeck, a tree revealed the regenerative structures including leaf buds and stomata on the tissue surface. SEM and TEM allow investigating the minute details characteristic morphological features that can be used for classroom teaching.

Atom-counting in High Resolution Electron Microscopy:TEM or STEM - That's the question.

PubMed

Gonnissen, J; De Backer, A; den Dekker, A J; Sijbers, J; Van Aert, S

2017-03-01

In this work, a recently developed quantitative approach based on the principles of detection theory is used in order to determine the possibilities and limitations of High Resolution Scanning Transmission Electron Microscopy (HR STEM) and HR TEM for atom-counting. So far, HR STEM has been shown to be an appropriate imaging mode to count the number of atoms in a projected atomic column. Recently, it has been demonstrated that HR TEM, when using negative spherical aberration imaging, is suitable for atom-counting as well. The capabilities of both imaging techniques are investigated and compared using the probability of error as a criterion. It is shown that for the same incoming electron dose, HR STEM outperforms HR TEM under common practice standards, i.e. when the decision is based on the probability function of the peak intensities in HR TEM and of the scattering cross-sections in HR STEM. If the atom-counting decision is based on the joint probability function of the image pixel values, the dependence of all image pixel intensities as a function of thickness should be known accurately. Under this assumption, the probability of error may decrease significantly for atom-counting in HR TEM and may, in theory, become lower as compared to HR STEM under the predicted optimal experimental settings. However, the commonly used standard for atom-counting in HR STEM leads to a high performance and has been shown to work in practice. Copyright © 2017 Elsevier B.V. All rights reserved.

Elucidation of reaction mechanism involved in the formation of LaNiO3 from XRD and TG analysis

NASA Astrophysics Data System (ADS)

Dharmadhikari, Dipti V.; Athawale, Anjali A.

2013-06-01

The present work is focused on the synthesis and elucidation of reaction mechanism involved in the formation of LaNiO3 with the help of X-ray diffraction (XRD) and thermogravimetric (TG) analysis. LaNiO3 was synthesized by hydrothermal method by heating at 160°C under autogenous pressure for 6h. Pure phase product was obtained after calcining the hydrothermally activated product for 6h at 700°C. The various phases of the product obtained after hydrothermal treatment and calcination followed by the formation of pure phase nanocrystalline lanthanum nickel oxide could be determined from XRD analysis of the samples. The reaction mechanism and phase formation temperature has been interpreted by thermogravimetric analysis of the hydrothermally synthesized product and XRD analysis.

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

NASA Astrophysics Data System (ADS)

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

2013-10-01

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

An investigation of down-conversion luminescence properties of rare earth doped CaMoO4 phosphors for solar cell application

NASA Astrophysics Data System (ADS)

Verma, Akta; Sharma, S. K.

2018-05-01

In the present work, we have synthesized a CaMoO4:(1%)Er3+,(1%)Yb3+ down-converting phosphor by hydrothermal method. The primary goal of studying down-conversion is to enhance the conversion efficiency of Si-solar cell by converting one high energy (UV) photon into two low energy (NIR) photons. The various characterization such as XRD, FESEM and Photoluminescence (PL) were carried out. The X-ray diffraction (XRD) pattern exhibit tetragonal crystal structure and has a space group of I41a (88). The FESEM microphotograph shows surface morphology having a abundance of particles in spherical shape. The PL emission spectra were recorded both in Visible and NIR regions. There is hypertensive emission peak at 555 nm in the visible region due to 4S3/2 → 4I15/2 transition of Er3+ ions and an emission at 980 nm (2F5/2 → 2F7/2) due to Yb3+ ions. The result shows a demand of this down-converting material in the field of solar energy to improve the efficiency of Si-solar-cell.

A study on the structural and mechanical properties of nanocrystalline CuS thin films grown by chemical bath deposition technique

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

Mukherjee, Nillohit; Sinha, Arijit; Khan, Gobinda Gopal

2011-01-15

We report a chemical route for the deposition of nanocrystalline thin films of CuS, using aqueous solutions of Cu(CH{sub 3}COO){sub 2}, SC(NH{sub 2}){sub 2} and N(CH{sub 2}CH{sub 2}OH){sub 3} [triethanolamine, i.e. TEA] in proper concentrations and ratios. The films were structurally characterized using X-ray diffraction technique (XRD), field emission scanning electron microscopy (FESEM) and optical analysis [both photo luminescence (PL) and ultraviolet-visible (UV-vis)]. Optical studies showed a large blue shift in the band gap energy of the films due to quantum confinement effect exerted by the nanocrystals. From both XRD and FESEM analyses, formation of CuS nanocrystals with sizes withinmore » 10-15 nm was evident. A study on the mechanical properties was carried out using nanoindentation and nanoscratch techniques, which showed good mechanical stability and high adherence of the films with the bottom substrate. Such study on the mechanical properties of the CuS thin films is being reported here for the first time. Current-voltage (I-V) measurements were also carried out for the films, which showed p-type conductivity.« less

Upconversion luminescence of Er3+/Yb3+ doped Sr5(PO4)3OH phosphor powders

NASA Astrophysics Data System (ADS)

Mokoena, P. P.; Swart, H. C.; Ntwaeaborwa, O. M.

2018-04-01

Sr5(PO4)3OH co-doped with Er3+and Yb3+ powder phosphors were synthesized by urea combustion method. The crystal structure was analyzed using X-ray diffraction (XRD). Particle morphology was analyzed using a Jeol JSM 7800F thermal field emission scanning electron microscope (FE-SEM) and the chemical composition analysis was carried out using an Oxford Instruments AzTEC energy dispersive spectrometer (EDS) attached to the FE-SEM. Upconversion emission was measured by using a FLS980 Spectrometer equipped with a 980 nm NIR laser as the excitation source, and a photomultiplier (PMT) detector. The XRD data of the Sr5(PO4)3OH powder exhibited characteristic diffraction patterns of the hexagonal structure referenced in the standard JCPDS card number 00-033-1348. The sharp peaks revealed the formation of crystalline Sr5(PO4)3OH. The powders were made up of hexagonal nanospheres. The enhanced red emission due to the 4F9/2 → 4I15/2 transitions of Er3+ was observed and was attributed to up conversion (UC) energy transfer from Yb3+. The upconversion energy transfer mechanism from Yb3+ to Er3+ is discussed.

Controlled synthesis, characterization and photoluminescence property of olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3}

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

Zhang, Youjin, E-mail: zyj@ustc.edu.cn; Zheng, Ao; Yang, Xiaozhi

2012-09-15

Highlights: ► The olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3} was gained with EDTA assisted hydrothermal method. ► The product was characterized by XRD, XPS, FTIR, FESEM, and PL. ► The possible formation mechanism for olive-like α-Nd{sub 2}(MoO{sub 4}){sub 3} was proposed. ► The PL in visible region of the olive-like α-Nd{sub 2}(MoO{sub 4}){sub 3} was studied. -- Abstract: The olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3} was obtained by a convenient and facile complex agent assisted hydrothermal method. The product was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectroscopy, field-emission scanning electron microscopy (FESEM) andmore » photoluminescence (PL). The possible formation mechanism of the olive-like α-Nd{sub 2}(MoO{sub 4}){sub 3} was proposed. The photoluminescence property in visible region of the olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3} was studied.« less

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

NASA Astrophysics Data System (ADS)

Mirzaee, Majid; Dolati, Abolghasem

2015-03-01

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

Performance assessment of MCM-48 ceramic composite membrane by separation of AlCl3 from aqueous solution.

PubMed

Kumar Basumatary, Ashim; Kumar Ghoshal, Aloke; Pugazhenthi, G

2016-12-01

Three dimensional ordered mesoporous MCM-48 membrane was fabricated on a circular shaped ceramic support by in-situ hydrothermal method. The synthesized MCM-48 powder and MCM-48 ceramic composite membrane were characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA) and field emission scanning electron microscopy (FESEM). The porosity and pore size of the composite membrane are reduced considerably by the deposition of MCM-48 on the support. The formation of MCM-48 is verified by the XRD analysis. Three stepwise mechanisms for surfactant removal are observed by TGA analysis. FESEM images clearly signify the deposition of MCM-48 on the ceramic support. The pure water flux of the support and MCM-48 composite membrane is found to be 3.63×10 -6 and 4.18×10 -8 m 3 /m 2 skPa, respectively. The above prepared MCM-48 ceramic composite membrane is employed for the removal of AlCl 3 from aqueous solution and the highest rejection of 81% is obtained at an applied pressure of 276kPa with salt concentration of 250ppm. Copyright © 2015 Elsevier Inc. All rights reserved.

MoTe2, A novel anode material for sodium ion battery

NASA Astrophysics Data System (ADS)

Panda, Manas Ranjan; Anish Raj, K.; Bao, Qiaoliang; Mitra, Sagar

2018-04-01

2D layered transition metal dichalcogenides are considered as a potential anode for sodium-ion batteries due to their high specific capacity, structural stability and its well-developed two-dimensional layers. 2D layered structure Molybdenum ditelluride (MoTe2) provides a superior Na-ion storage properties in sodium ion battery due to its comparative more interlayer spacing (0.699 nm). In the current study MoTe2 polycrystalline powder sample has been prepared by solid state reaction process, the structural and morphological studies have been carried out by XRD, FE-SEM and EDS etc. XRD study revealsthe well crystalline structure of the material having hexagonal structure. FE-SEM and EDS studies depict the uniformflakes like structure of the material. When it is tested as sodium-ion battery anode by applying a potential window 0.1-2.5 V, the material demonstrates a high capacity and high power performances. The as prepared MoTe2 shows an initial discharge capacity of 376 mA h g-1 and a corresponding discharge capacity of 303 mA h g-1 after the 50th cycle at a current density of 500 mA g-1.

Co-precipitation synthesis of nano-composites consists of zinc and tin oxides coatings on glass with enhanced photocatalytic activity on degradation of Reactive Blue 160 KE2B.

PubMed

Habibi, Mohammad Hossein; Mardani, Maryam

2015-02-25

Nano-composite containing zinc oxide-tin oxide was obtained by a facile co-precipitation route using tin chloride tetrahydrate and zinc chloride as precursors and coated on glass by Doctor Blade deposition. The crystalline structure and morphology of composites were evaluated by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The XRD results showed peaks relative to zinc oxide with hexagonal wurtzite structure and tin oxide with tetragonal structure. FESEM observations showed that the nano-composite consisted of aggregates of particles with an average particle size of 18 nm. The photocatalytic activity of the pure SnO2, pure ZnO, ZnSnO3-Zn2SnO4 and ZnO-SnO2 nano-structure thin films was examined using the degradation of a textile dye Reactive Blue 160 (KE2B). ZnO-SnO2 nano-composite showed enhanced photo-catalytic activity than the pure zinc oxide and tin oxide. The enhanced photo-catalytic activity of the nano-composite was ascribed to an improved charge separation of the photo-generated electron-hole pairs. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrochemical synthesis of nanostructured Se-doped SnS: Effect of Se-dopant on surface characterizations

NASA Astrophysics Data System (ADS)

Kafashan, Hosein; Azizieh, Mahdi; Balak, Zohre

2017-07-01

SnS1-xSex nanostructures with different Se-dopant concentrations were deposited on fluorine doped tin oxide (FTO) substrate through cathodic electrodeposition technique. The pH, temperature, applied potential (E), and deposition time remained were 2.1, 60 °C, -1 V, and 30 min, respectively. SnS1-xSex nanostructures were characterized using X-ray diffraction (XRD), field emission scanning electron microcopy (FESEM), energy dispersive X-ray spectroscopy (EDX), room temperature photoluminescence (PL), and UV-vis spectroscopy. The XRD patterns revealed that the SnS1-xSex nanostructures were polycrystalline with orthorhombic structure. FESEM showed various kinds of morphologies in SnS1-xSex nanostructures due to Se-doping. PL and UV-vis spectroscopy were used to evaluate the optical properties of SnS1-xSex thin films. The PL spectra of SnS1-xSex nanostructures displayed four emission peaks, those are a blue, a green, an orange, and a red emission. UV-vis spectra showed that the optical band gap energy (Eg) of SnS1-xSex nanostructures varied between 1.22-1.65 eV, due to Se-doping.

Spherical nanocrystalline cellulose (NCC) from oil palm empty fruit bunch pulp via ultrasound assisted hydrolysis.

PubMed

Zianor Azrina, Z A; Beg, M Dalour H; Rosli, M Y; Ramli, Ridzuan; Junadi, Norhafzan; Alam, A K M Moshiul

2017-04-15

Nanocrystalline cellulose (NCC) was isolated from oil palm empty fruit bunch pulp (EFBP) using ultrasound assisted acid hydrolysis. The obtained NCC was analysed using FESEM, XRD, FTIR, and TGA, and compared with raw empty fruit bunch fibre (REFB), empty fruit bunch pulp (EFBP), and treated empty fruit bunch pulp (TEFBP). Based on FESEM analysis, it was found that NCC has a spherical shaped after acid hydrolysis with the assistance of ultrasound. This situation was different compared to previous studies that obtained rod-like shaped of NCC. Furthermore, the crystallinity of NCC is higher compared to REFB and EFBP. According to thermal stability, the NCC obtained shows remarkable sign of high thermal stability compared to REFB and EFBP. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

NASA Technical Reports Server (NTRS)

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

2015-01-01

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

Ceftazidime-Resistant Enterobacteriaceae Isolates from Three Polish Hospitals: Identification of Three Novel TEM- and SHV-5-Type Extended-Spectrum β-Lactamases

PubMed Central

Gniadkowski, Marek; Schneider, Ines; Jungwirth, Renate; Hryniewicz, Waleria; Bauernfeind, Adolf

1998-01-01

Twelve ceftazidime-resistant isolates of the family Enterobacteriaceae (11 Klebsiella pneumoniae isolates and 1 Escherichia coli isolate) were collected in 1995 from three Polish hospitals located in different cities. All were identified as producers of extended-spectrum β-lactamases (ESBLs). Detailed analysis of their β-lactamase contents revealed that six of them expressed SHV-5-like ESBLs. The remaining six were found to produce three different TEM enzymes, each characterized by a pI value of 6.0 and specified by new combinations of amino acid substitutions. The amino acid substitutions compared to the TEM-1 β-lactamase sequence were Gly238Ser, Glu240Lys, and Thr265Met for TEM-47; Leu21Phe, Gly238Ser, Glu240Lys, and Thr265Met for TEM-48; and Leu21Phe, Gly238Ser, Glu240Lys, Thr265Met, and Ser268Gly for TEM-49. The new TEM β-lactamases, TEM-47, TEM-48, and TEM-49, belong to a subfamily of TEM-2-related enzymes. Genes coding for TEM-47 and TEM-49 could have originated from the TEM-48-encoding sequence by various single genetic events. The new TEM derivatives probably document the already advanced microevolution of ESBLs ongoing in Polish hospitals, in a majority of which no monitoring of ESBL producers was performed before 1996. PMID:9517925

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

PubMed

Ostrooumov, Mikhail; Hernández-Bernal, Maria del Sol

2011-12-01

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

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

Liu, Shuling, E-mail: liusl8888@yahoo.com.cn; Li, Honglin; Yan, Lu

Graphical abstract: - Highlights: • 3D urchin-like ZnS/CdS composites were synthesized via a two-step method. • The CdS nanoparticles were assembled on the thorns of 3D ZnS urchins. • The ZnS/CdS composites show excellent photocatalytic degradation activities. • The modification of CdS on ZnS is responsible for the enhanced property. - Abstract: Urchin-like ZnS/CdS semiconductor composites were successfully synthesized by combining solvothermal route with homogeneous precipitation process. The as-obtained samples were characterized by means of XRD, EDX, TEM, HR-TEM, ED and FE-SEM techniques. The results show that the as-obtained composites were comprised of the hexagonal structure ZnS and CdS, andmore » CdS nanoparticles were assembled on the surfaces of the thorns of urchin-like ZnS. In addition, the optical properties and photocatalytic activities of the as-prepared ZnS/CdS composites toward some organic dyes (such as Methyl Orange, Pyronine B, Rhodamine B and Methylene Blue) were separately investigated. It is found that the ZnS/CdS composites exhibit excellent photocatalytic degradation activity for these dyes under UV irradiation, as compared to corresponding pure ZnS urchins and commercial anatase TiO{sub 2} (P-25). This enhanced activity may be related to the modification of CdS nanoparticles on the surfaces of thorns of ZnS urchins and a tentative mechanism for the enhanced photocatalytic degradation activities of the ZnS/CdS composite catalyst was proposed.« less

Amorphous V-O-C composite nanofibers electrospun from solution precursors as binder- and conductive additive-free electrodes for supercapacitors with outstanding performance.

PubMed

Chen, Xia; Zhao, Bote; Cai, Yong; Tadé, Moses O; Shao, Zongping

2013-12-21

Flexible V-O-C composite nanofibers were fabricated from solution precursors via electrospinning and were investigated as free-standing and additive-free film electrodes for supercapacitors. Specifically, composite nanofibers (V0, V5, V10 and V20) with different vanadyl acetylacetonate (VO(acac)2) contents of 0, 5, 10 and 20 wt% with respect to polyacrylonitrile (PAN) were prepared. The composite nanofibers were comparatively studied using XRD, Raman spectroscopy, XPS, N2 adsorption-desorption, FE-SEM, TEM and S-TEM. The vanadium element was found to be well-dispersed in the carbon nanofibers, free from the formation of an aggregated crystalline phase, even in the case of V20. A specific surface area of 587.9 m(2) g(-1) was reached for V10 after calcination, which is approximately twice that of the vanadium-free carbon nanofibers (V0, 300.9 m(2) g(-1)). To perform as an electrode for supercapacitors in an aqueous electrolyte, the V10 film delivered a specific capacitance of 463 F g(-1) at 1 A g(-1). V10 was also able to retain a specific capacitance of 380 F g(-1), even at a current density of 10 A g(-1). Additionally, very stable cycling stability was achieved, maintaining an outstanding specific capacitance of 400 F g(-1) at 5 A g(-1) after charge-discharge cycling 5000 times. Thus, V-O-C composite nanofibers are highly attractive electrode materials for flexible, high-power, thin film energy storage devices and applications.

Preparation method of Ni@Pt/C nanocatalyst affects the performance of direct borohydride-hydrogen peroxide fuel cell: Improved power density and increased catalytic oxidation of borohydride.

PubMed

Hosseini, Mir Ghasem; Mahmoodi, Raana

2017-08-15

The Ni@Pt/C electrocatalysts were synthesized using two different methods: with sodium dodecyl sulfate (SDS) and without SDS. The metal loading in synthesized nanocatalysts was 20wt% and the molar ratio of Ni: Pt was 1:1. The structural characterizations of Ni@Pt/C electrocatalysts were investigated by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HR-TEM). The electrocatalytic activity of Ni@Pt/C electrocatalysts toward BH 4 - oxidation in alkaline medium was studied by means of cyclic voltammetry (CV), chronopotentiometry (CP), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS). The results showed that Ni@Pt/C electrocatalyst synthesized without SDS has superior catalytic activity toward borohydride oxidation (22016.92Ag Pt -1 ) in comparison with a catalyst prepared in the presence of SDS (17766.15Ag Pt -1 ) in NaBH 4 0.1M at 25°C. The Membrane Electrode Assembly (MEA) used in fuel cell set-up was fabricated with catalyst-coated membrane (CCM) technique. The effect of Ni@Pt/C catalysts prepared with two methods as anode catalyst on the performance of direct borohydride-hydrogen peroxide fuel cell was studied. The maximum power density was obtained using Ni@Pt/C catalyst synthesized without SDS at 60°C, 1M NaBH 4 and 2M H 2 O 2 (133.38mWcm -2 ). Copyright © 2017 Elsevier Inc. All rights reserved.

Improvement of energy conversion efficiency and power generation in direct borohydride-hydrogen peroxide fuel cell: The effect of Ni-M core-shell nanoparticles (M = Pt, Pd, Ru)/Multiwalled Carbon Nanotubes on the cell performance

NASA Astrophysics Data System (ADS)

Hosseini, M. G.; Mahmoodi, R.

2017-12-01

In this study, core@shell nanoparticles with Ni as a core material and Pt, Pd and Ru as shell materials are synthesized on multiwalled carbon nanotube (MWCNT) as catalyst support using the sequence reduction method. The influence of Ni@Pt, Ni@Pd and Ni@Ru core@shell nanoparticles on MWCNT toward borohydride oxidation in alkaline solution is investigated by various three-electrode electrochemical techniques. Also, the impact of these anodic electrocatalysts on the performance of direct borohydride-hydrogen peroxide fuel cell (DBHPFC) is evaluated. The structural and morphological properties of electrocatalysts are studied by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS). The results of three electrode investigations show that Ni@Pd/MWCNT has excellent catalytic activity since borohydride oxidation current density on Ni@Pd/MWCNT (34773.27 A g-1) is 1.37 and 9.19 times higher than those of Ni@Pt/MWCNT (25347.27 A g-1) and Ni@Ru/MWCNT (3782.83 A g-1), respectively. Also, the energy conversion efficiency and power density of DBHPFC with Ni@Pd/MWCNT (246.82 mW cm-2) increase to 34.27% and 51.53% respect to Ni@Pt/MWCNT (162.24 mW cm-2) and Ni@Ru/MWCNT (119.62 mW cm-2), respectively. This study reveals that Ni@Pd/MWCNT has highest activity toward borohydride oxidation and stability in fuel cell.

Processing grounded-wire TEM signal in time-frequency-pseudo-seismic domain: A new paradigm

NASA Astrophysics Data System (ADS)

Khan, M. Y.; Xue, G. Q.; Chen, W.; Huasen, Z.

2017-12-01

Grounded-wire TEM has received great attention in mineral, hydrocarbon and hydrogeological investigations for the last several years. Conventionally, TEM soundings have been presented as apparent resistivity curves as function of time. With development of sophisticated computational algorithms, it became possible to extract more realistic geoelectric information by applying inversion programs to 1-D & 3-D problems. Here, we analyze grounded-wire TEM data by carrying out analysis in time, frequency and pseudo-seismic domain supported by borehole information. At first, H, K, A & Q type geoelectric models are processed using a proven inversion program (1-D Occam inversion). Second, time-to-frequency transformation is conducted from TEM ρa(t) curves to magneto telluric MT ρa(f) curves for the same models based on all-time apparent resistivity curves. Third, 1-D Bostick's algorithm was applied to the transformed resistivity. Finally, EM diffusion field is transformed into propagating wave field obeying the standard wave equation using wavelet transformation technique and constructed pseudo-seismic section. The transformed seismic-like wave indicates that some reflection and refraction phenomena appear when the EM wave field interacts with geoelectric interface at different depth intervals due to contrast in resistivity. The resolution of the transformed TEM data is significantly improved in comparison to apparent resistivity plots. A case study illustrates the successful hydrogeophysical application of proposed approach in recovering water-filled mined-out area in a coal field located in Ye county, Henan province, China. The results support the introduction of pseudo-seismic imaging technology in short-offset version of TEM which can also be an useful aid if integrated with seismic reflection technique to explore possibilities for high resolution EM imaging in future.

XRD and SEM study of alumina silicate porcelain insulator

NASA Astrophysics Data System (ADS)

Duddi, Dharmender; Singh, G. P.; Kalra, Swati; Shekhawat, M. S.; Tak, S. K.

2018-05-01

Higher strength electrical porcelain is a requirement of industry. This will be achieved by a specific composition of raw materials, which is consisted of clays and feldspars. Water absorption, particle size and insulating properties are of special interest now a day. China clay, Ball clay and Quartz are widely used by ceramic industries in Bikaner district of Rajasthan. Sample for present study were prepared by mixing of above clay, feldspar with MnO2, then shrinkage is observed. Bar shaped samples were prepared and heated up to a temperature of about 1185° C to observe shrinkage. For phase study of XRD and SEM are observed.

Effect of content silver and heat treatment temperature on morphological, optical, and electrical properties of ITO films by sol-gel technique

NASA Astrophysics Data System (ADS)

Mirzaee, Majid; Dolati, Abolghasem

2014-09-01

Silver-doped indium tin oxide thin films were synthesized using sol-gel dip-coating technique. The influence of different silver-dopant contents and annealing temperature on the electrical, optical, structural, and morphological properties of the films were characterized by means of four-point probe, UV-Vis spectroscopy, X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscope (XPS). XRD analysis confirmed the formation of cubic bixbyte structure of In2O3 with silver nanoparticles annealed at 350 °C. XPS analysis showed that divalent tin transformed to tetravalent tin through oxidization, and silver nanoparticles embedded into ITO matrix covered with silver oxide shell, resulting in high quality nanocomposite thin films. The embedment of polyvinylpyrrolidone inhibited the growth of silver nanoparticles and ITO annealed at 350 °C. Delafossite structure of tin-doped AgInO2 was found at higher annealing temperatures. XRD analysis and FESEM micrographs showed that the optimum temperature to prevent the formation of AgInO2 is 350 °C. The embedment of silver particles (5-10 nm) from reduction of silver ion in ITO thin films improved the electrical conductivity and optical transmittance of ITO nanolayers. The lowest stable sheet resistance of 1,952 Ω/Sq for a 321 nm thick and an average optical transmittance of 91.8 % in the visible region with a band gap of 3.43 eV were achieved for silver-doping content of 0.04 M.

An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments

NASA Technical Reports Server (NTRS)

Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.

1993-01-01

By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

The Synthesis and Photoluminescent Properties of CaMoO₄:Eu³⁺ Nanocrystals by a Soft Chemical Route.

PubMed

Li, Fuhai; Yu, Lixin; Sun, Jiaju; Li, Songchu; Wei, Shuilin

2017-04-01

In this paper, the CaMoO4:Eu3+ phosphors were prepared by a simple hydrothermal method assisted by the citric acid as the surfactant, and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and fluorescent spectrophotometry. The results of XRD show that the as-prepared samples are single phase. The process of the Ostwald ripening is controlled by the content of the citric acid in the hydrothermal reaction. The pH value of the precursor affects the shift of the charge transition band (CTB) in the excitation spectra. The reaction condition can strongly affect the luminescent intensity of the samples.

Structural and optical studies of Mg doped nanoparticles of chromium oxide (Cr2O3) synthesized by co-precipitation method

NASA Astrophysics Data System (ADS)

Singh, Jarnail; Verma, Vikram; Kumar, Ravi

2018-04-01

We present here the synthesization, structural and optical studies of Mg doped nanoparticles of Chromium oxide (Cr2O3) prepared using co-precipitation method. These samples were characterized using powder X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Raman spectroscopy and UV-Vis spectroscopy techniques. We have demonstrated that there is negligible change in optical band gap with the Mg doping. The prepared Cr2O3 nanoparticles are spherical in shape, but they are transformed into platelets when doped with Mg. The XRD studies reveal that the Mg doping in Cr2O3 doesn't affect the structure of Chromium oxide (Cr2O3).

Methanol conversion to light olefins over nanostructured CeAPSO-34 catalyst: Thermodynamic analysis of overall reactions and effect of template type on catalytic properties and performance

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

Aghamohammadi, Sogand; Reactor and Catalysis Research Center; Haghighi, Mohammad, E-mail: haghighi@sut.ac.ir

2014-02-01

Graphical abstract: In this research nanostructured CeAPSO-34 was synthesized to explore the effect of TEAOH and morpholine on its physiochemical properties and MTO performance. Prepared catalysts were characterized with XRD, FESEM, BET, FTIR and NH3-TPD techniques. The results indicated that the nature of the template determines the physiochemical properties of CeAPSO-34 due to different rate of crystal growth. The catalyst obtained by using morpholine showed longer life time as well as sustaining light olefins selectivity at higher values. Furthermore, a comprehensive thermodynamic analysis of overall reactions network was carried out to address the major channels of methanol to olefins conversion.more » - Highlights: • Introduction of Ce into SAPO-34 framework. • Comparison of CeAPSO-34 synthesized using morpholine and TEAOH. • The nature of the template determines the physiochemical properties of CeAPSO-34. • Morpholine enhances catalyst lifetime in MTO process. • Presenting a complete reaction network for MTO process. - Abstract: TEAOH and morpholine were employed in synthesis of nanostructured CeAPSO-34 molecular sieve and used in methanol to olefins conversion. Prepared samples were characterized by XRD, FESEM, EDX, BET, FTIR and NH{sub 3}-TPD techniques. XRD patterns reflected the higher crystallinity of the catalyst synthesized with morpholine. The FESEM results indicated that the nature of the template determines the morphology of nanostructured CeAPSO-34 due to different rate of crystal growth. There was a meaningful difference in the strength of both strong and weak acid sites for CeAPSO-34 catalysts synthesized with TEAOH and morpholine templates. The catalyst synthesized with morpholine showed higher desorption temperature of both weak and strong acid sites evidenced by NH{sub 3}-TPD characterization. The catalyst obtained using morpholine template had the longer lifetime and sustained desired light olefins at higher values. A

Coordinated Isotopic and TEM Studies of Presolar Graphites from Murchison

NASA Astrophysics Data System (ADS)

Croat, T. K.; Stadermann, F. J.; Zinner, E.; Bernatowicz, T. J.

2004-03-01

TEM and NanoSIMS investigations of the same presolar Murchison KFC graphites revealed high Zr, Mo, and Ru content in refractory carbides within the graphites. Along with isotopically light carbon, these suggest a low-metallicity AGB source.

Validation of TOF-SIMS and FE-SEM/EDS Techniques Combined with Sorption and Desorption Experiments to Check Competitive and Individual Pb2+ and Cd2+ Association with Components of B Soil Horizons

PubMed Central

Andrade, María Luisa; Vega, Flora A.

2015-01-01

Sorption and desorption experiments were performed by the batch method on the B horizons of five natural soils: Umbric Cambisol, Endoleptic Luvisol, Mollic Umbrisol, Dystric Umbrisol, and Dystric Fluvisol. Individual and competitive sorption and desorption capacity and hysteresis were determined. The results showed that Pb2+ was sorbed and retained in a greater quantity than Cd2+ and that the hysteresis of the first was greater than that of the second. The most influential characteristics of the sorption and retention of Pb2+ were pH, ECEC, Fe and Mn oxides and clay contents. For Cd2+ they were mainly pH and, to a lesser extent, Mn oxides and clay content. The combined use of TOF-SIMS, FE-SEM/EDS and sorption and desorption analyses was suitable for achieving a better understanding of the interaction between soil components and the two heavy metals. They show the preferential association of Pb2+ with vermiculite, chlorite, Fe and Mn oxides, and of Cd2+ with the same components, although to a much lesser extent and intensity. This was due to the latter’s higher mobility as it competed unfavourably with the Pb2+ sorption sites. TOF-SIMS and FE-SEM/EDS techniques confirmed the results of the sorption experiments, and also provided valuable information on whether the soil components (individually or in association) retain Cd2+ and / or Pb2+; this could help to propose effective measures for the remediation of contaminated soils. PMID:25893518

Effect of intrinsic zinc oxide coating on the properties of Al-doped zinc oxide nanorod arrays

NASA Astrophysics Data System (ADS)

Saidi, S. A.; Mamat, M. H.; Ismail, A. S.; Malek, M. F.; Yusoff, M. M.; Sin, N. D. Md.; Zoolfakar, A. S.; Khusaimi, Z.; Rusop, M.

2018-05-01

The aim of this study was to explore the influence of intrinsic zinc oxide (ZnO) coating fabricated by a simple immersion method. X-ray powder diffraction (XRD) analysis indicated that the Al-doped ZnO nanorod arrays films had a hexagonal wurtzite structure, similar to that of an intrinsic ZnO coating. Structural properties of the samples were characterised using field emission scanning electron microscopy (FESEM; JEOL JSM-7600F) and optical properties using X-ray diffraction (XRD). The XRD results showed that all films were crystallized under hexagonal wurtzite structure and presented a preferential orientation along the c-axis (002) was obtained. The XRD results showed that the intrinsic ZnO coating material had a strong orientation, whereas the ZnO was randomly oriented. Overall these results indicate that intrinsic ZnO coating are pontetial for the creation of functional materials such as barrier protection, optoelectronic devices, humidity sensor and ultraviolet photoconductive sensor.

Helicopter TEM parameters analysis and system optimization based on time constant

NASA Astrophysics Data System (ADS)

Xiao, Pan; Wu, Xin; Shi, Zongyang; Li, Jutao; Liu, Lihua; Fang, Guangyou

2018-03-01

Helicopter transient electromagnetic (TEM) method is a kind of common geophysical prospecting method, widely used in mineral detection, underground water exploration and environment investigation. In order to develop an efficient helicopter TEM system, it is necessary to analyze and optimize the system parameters. In this paper, a simple and quantitative method is proposed to analyze the system parameters, such as waveform, power, base frequency, measured field and sampling time. A wire loop model is used to define a comprehensive 'time constant domain' that shows a range of time constant, analogous to a range of conductance, after which the characteristics of the system parameters in this domain is obtained. It is found that the distortion caused by the transmitting base frequency is less than 5% when the ratio of the transmitting period to the target time constant is greater than 6. When the sampling time window is less than the target time constant, the distortion caused by the sampling time window is less than 5%. According to this method, a helicopter TEM system, called CASHTEM, is designed, and flight test has been carried out in the known mining area. The test results show that the system has good detection performance, verifying the effectiveness of the method.

TEM measurement in a low resistivity overburden performed by using low temperature SQUID

NASA Astrophysics Data System (ADS)

Ji, Yanju; Du, Shangyu; Xie, Lijun; Chang, Kai; Liu, Yang; Zhang, Yi; Xie, Xiaoming; Wang, Yuan; Lin, Jun; Rong, Liangliang

2016-12-01

Exploration of areas with thick low resistivity overburden is still a challenge for time domain transient electromagnetic method (TEM). We report modeling of a sandwich-layered earth by simulating the B field response with different conductive target layer thicknesses, thus obtaining a relationship between the resolution of the B field and the exploration depth. A low temperature Superconducting Quantum Interference Device (SQUID) is an ideal sensor for measuring the secondary magnetic field B in TEM measurements, because its sensitivity of several fT/√Hz is independent of frequency. In our TEM experiments, we utilized two different coils as receivers, a simple SQUID system, and a large transmitter loop of 200 × 200 m2 to compare the detected decay curves. At some measurement points, a decay signal of more than 300 ms duration was obtained by using the SQUID. Apparent resistivity profiles of about 9 km length are presented.

Strain mapping in TEM using precession electron diffraction

DOEpatents

Taheri, Mitra Lenore; Leff, Asher Calvin

2017-02-14

A sample material is scanned with a transmission electron microscope (TEM) over multiple steps having a predetermined size at a predetermined angle. Each scan at a predetermined step and angle is compared to a template, wherein the template is generated from parameters of the material and the scanning. The data is then analyzed using local mis-orientation mapping and/or Nye's tensor analysis to provide information about local strain states.

Mössbauer and XRD study of novel quaternary Sn-Fe-Co-Ni electroplated alloy

NASA Astrophysics Data System (ADS)

Kuzmann, E.; Sziráki, L.; Stichleutner, S.; Homonnay, Z.; Lak, G. B.; El-Sharif, M.; Chisholm, C. U.

2017-11-01

Constant current electrochemical deposition technique was used to obtain quaternary alloys of Sn-Fe-Co-Ni from a gluconate electrolyte, which to date have not been reported in the literature. For the characterization of electroplated alloys, 57Fe and 119Sn Conversion Electron Mössbauer Spectroscopy (CEMS), XRD and SEM/EDAX were used. XRD revealed the amorphous character of the novel Sn-Fe-Co-Ni electrodeposited alloys. 57Fe Mössbauer spectrum of quaternary deposit with composition of 37.0 at% Sn, 38.8 at% Fe, 16.8 at% Co and 7.4 at% Ni displayed a magnetically split sextet (B = 28.9T) with broad lines typical of iron bearing ferromagnetic amorphous alloys. Magnetically split 119Sn spectra reflecting a transferred hyperfine field (B = 2.3T) were also observed. New quaternary Sn-Fe-Co-Ni alloys were successfully prepared.

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

PubMed

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

2014-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2013-12-01

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

Network Analysis of Sequence-Function Relationships and Exploration of Sequence Space of TEM β-Lactamases.

PubMed

Zeil, Catharina; Widmann, Michael; Fademrecht, Silvia; Vogel, Constantin; Pleiss, Jürgen

2016-05-01

The Lactamase Engineering Database (www.LacED.uni-stuttgart.de) was developed to facilitate the classification and analysis of TEM β-lactamases. The current version contains 474 TEM variants. Two hundred fifty-nine variants form a large scale-free network of highly connected point mutants. The network was divided into three subnetworks which were enriched by single phenotypes: one network with predominantly 2be and two networks with 2br phenotypes. Fifteen positions were found to be highly variable, contributing to the majority of the observed variants. Since it is expected that a considerable fraction of the theoretical sequence space is functional, the currently sequenced 474 variants represent only the tip of the iceberg of functional TEM β-lactamase variants which form a huge natural reservoir of highly interconnected variants. Almost 50% of the variants are part of a quartet. Thus, two single mutations that result in functional enzymes can be combined into a functional protein. Most of these quartets consist of the same phenotype, or the mutations are additive with respect to the phenotype. By predicting quartets from triplets, 3,916 unknown variants were constructed. Eighty-seven variants complement multiple quartets and therefore have a high probability of being functional. The construction of a TEM β-lactamase network and subsequent analyses by clustering and quartet prediction are valuable tools to gain new insights into the viable sequence space of TEM β-lactamases and to predict their phenotype. The highly connected sequence space of TEM β-lactamases is ideally suited to network analysis and demonstrates the strengths of network analysis over tree reconstruction methods. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

Validation of enhanced stabilization of municipal solid waste under controlled leachate recirculation using FTIR and XRD.

PubMed

Sethi, Sapna; Kothiyal, N C; Nema, Arvind K

2012-07-01

Leachate recirculation at neutral PH accompanied with buffer/nutrients addition has been used successfully in earlier stabilization of municipal solid waste in bioreactor landfills. In the present study, efforts were made to enhance the stabilization rate of municipal solid waste (MSW) and organic solid waste (OSW) in simulated landfill bioreactors by controlling the pH of recirculated leachate towards slightly alkaline side in absence of additional buffer and nutrients addition. Enhanced stabilization in waste samples was monitored with the help of analytical tools like Fourier Transform Infrared Spectroscopy (FTIR) and X-Ray Diffraction (XRD). Predominance of bands assigned to inorganic compounds and comparatively lower intensities of bands for organic compounds in the FTIR spectra of waste samples degraded with leachate recirculation under controlled pH confirmed higher rate of biodegradation and mineralization of waste than the samples degraded without controlled leachate recirculation. XRD spectra also confirmed to a greater extent of mineralization in the waste samples degraded under leachate recirculation with controlled pH. Comparison of XRD spectra of two types of wastes pointed out higher degree of mineralization in organic solid waste as compared to municipal solid waste.

[Study on the vibrational spectra and XRD characters of Huanglong jade from Longling County, Yunnan Province].

PubMed

Pei, Jing-cheng; Fan, Lu-wei; Xie, Hao

2014-12-01

Based on the conventional test methods, the infrared absorption spectrum, Raman spectrum and X-ray diffraction (XRD) were employed to study the characters of the vibration spectrum and mineral composition of Huanglong jade. The testing results show that Huanglong jade shows typical vibrational spectrum characteristics of quartziferous jade. The main infrared absorption bands at 1162, 1076, 800, 779, 691, 530 and 466 cm(-1) were induced by the asymmetric stretching vibration, symmetrical stretching vibration and bending vibration of Si-O-Si separately. Especially the absorption band near 800 cm(-1) is split, which indicates that Huanglong jade has good crystallinity. In Raman spectrum, the main strong vibration bands at 463 and 355 cm(-1) were attributed to bending vibration of Si-O-Si. XRD test confirmed that Quartz is main mineral composition of Huanglong jade and there is a small amount of hematite in red color samples which induced the red color of Huanglong jade. This is the first report on the infrared, Raman and XRD spectra feature of Huanglong jade. It will provide a scientific basis for the identification, naming and other research for huanglong jade.

Studying dynamic processes in liquids by TEM/STEM/DTEM

NASA Astrophysics Data System (ADS)

Abellan, Patricia; Evans, James; Woehl, Taylor; Jungjohann, Katherine; Parent, Lucas; Arslan, Ilke; Ristenpart, William; Browning, Nigel; Mater. Sci. Group Team; Microsc. Group Team; Catal. Sci. Group Collaboration; Ristenpart Res. Group Collaboration

2013-03-01

In order to study dynamic phenomena such as corrosion or catalysis, extreme environmental conditions must be reproduced around the specimen - these include high-temperatures, high-pressures, specific oxidizing/reducing atmospheres or a liquid environment. The use of environmental stages specifically designed to fit in any transmission electron microscope (TEM) allows us to apply the distinct capabilities of each instrument to study dynamic processes. Localized gas/fluid conditions are created around the sample and separated from the high vacuum inside the microscope using hermetically sealed windowed-cells. Advanced capabilities of these techniques include spatial resolutions of ~1 Angstrom or better in aberration corrected instruments or temporal resolutions in the microsecond-nanosecond range in a dynamic TEM (DTEM). Here, unique qualities of the DTEM that benefit the in-situ experiments with gas/fluid environmental cells will be discussed. We also present our results with a liquid stage allowing atomic resolution imaging of nanomaterials in a colloidal suspension, core EEL spectra acquisition, continuous flow, controlled growth of nanocrystals and systematic calibration of the effect of the electron dose on silver nuclei formation.

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

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

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

2014-04-24

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

Synthesis of Silver and Gold Nanoparticles Using Antioxidants from Blackberry, Blueberry, Pomegranate, and Turmeric Extracts

EPA Science Inventory

Greener synthesis of Ag and Au nanoparticles is described using antioxidants from blackberry, blueberry, pomegranate, and turmeric extracts. The synthesized particles were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution TEM (HR...

TEM-induced gene mutations at enzyme loci in the mouse.

PubMed

Soares, E R

1979-01-01

Strain DBA/2J male mice were treated with triethylenemelamine (TEM) and subsequently mated to strain C57BL/6J females. Tissues from F1 progeny produced in these crosses were then examined using starch gel electrophoresis for the presence of presumed induced mutations at a series of 11 specific enzyme loci. In the course of this study, four heritable mutations were identified at the following loci: Es-1, Ldh-1, Pgm-1, and Gpi-1. Of these four, the first two were apparently segregating in parental males and were not TEM-induced. Both of these are viable and fertile in the heterozygous and homozygous condition, and neither confers any readily apparent deleterious effect to the animal. The latter mutations (Pgm-1 and Gpi-1) are presumably induced. Although viable and fertile in the heterozygous state, we have not recovered any offsping homozygous for either of these two mutations.

Development of an analytical environmental TEM system and its application.

PubMed

Kishita, Keisuke; Sakai, Hisashi; Tanaka, Hiromochi; Saka, Hiroyasu; Kuroda, Kotaro; Sakamoto, Masayuki; Watabe, Akira; Kamino, Takeo

2009-12-01

Many automotive materials, such as catalysts and fuel cell materials, undergo significant changes in structure or properties when subjected to temperature change or the addition of a gas. For this reason, in the development of these materials, it is important to study the behavior of the material under controlled temperatures and gaseous atmospheres. Recently, a new environmental transmission electron microscope (TEM) has been developed for observation with a high resolution at high temperatures and under gaseous atmospheres, thus making it possible to analyze reaction processes in details. Also, the new TEM provides a high degree of reproducibility of observation conditions, thus making it possible to compare and validate observation of various specimens under a given set of conditions. Furthermore, easiness of gas condition and temperature control can provide a powerful tool for the studying of the mechanism of material change, such as oxidation and reduction reactions.

Mineralogical Composition of the Mexican Ordinary Chondrite Type Meteorite: A Raman, Infrared and XRD Study

NASA Astrophysics Data System (ADS)

Ostrooumov, M.

2016-08-01

The Raman microprobe (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of seven mexican meteorites: Aldama, Cosina, El Pozo, Escalon, Nuevo Mercurio,Pacula, Zapotitlan Salinas.

Effect of annealing temperature on physical properties of solution processed nickel oxide thin films

NASA Astrophysics Data System (ADS)

Sahoo, Pooja; Thangavel, R.

2018-05-01

In this report, NiO thin films were prepared at different annealing temperatures from nickel acetate precursor by sol-gel spin coating method. These films were characterized by different analytical techniques to obtain their structural, optical morphological and electrical properties using X-ray diffractometer (XRD), Field emission scanning electron microscopy (FESEM), UV-Vis NIR double beam spectrophotometer and Keithley 2450 source meter respectively. FESEM images clearly indicates the formation of a homogenous and porous films. Due to their porosity, they can be used in sensing applications. The optical absorption spectra elucidated that the films are highly transparent and have a suitable band gap which are in similar agreement with earlier reports. The current enhancement under illumination shows the suitability of nanostructured NiO thin films in its application in photovoltaics.

Comparative investigation of Fourier Transform Infrared (FT-IR) spectroscopy and X-ray Diffraction (XRD) in the determination of cotton fiber crystallinity

USDA-ARS?s Scientific Manuscript database

Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI) from the X-ray diffraction (XRD) measurement, in its present state XRD procedure can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous po...

[NIR and XRD analysis of drill-hole samples from Zhamuaobao iron-graphite deposit, Inner Mongolia].

PubMed

Li, Ying-kui; Cao, Jian-jin; Wu, Zheng-quan; Dai, Dong-le; Lin, Zu-xu

2015-01-01

The author analyzed the 4202 drill-hole samples from Zhamuaobao iron-graphite deposit by using near infrared spectroscopy(NIR) and X-ray diffraction(XRD) measuring and testing techniques, and then compared and summarized the results of two kinds of testing technology. The results indicate that some difference of the mineral composition exists among different layers, the lithology from upper to deeper is the clay gravel layer of tertiary and quaternary, mudstone, mica quartz schist, quartz actinolite scarn, skarnization marble, iron ore deposits, graphite deposits and mica quartz schist. The petrogenesis in different depth also shows difference, which may indicate the geological characteristic to some extent. The samples had mainly undergone such processes as oxidization, carbonation, chloritization and skarn alteration. The research results can not only improve the geological feature of the mining area, but also have great importance in ore exploration, mining, mineral processing and so on. What's more, as XRD can provide preliminary information about the mineral composition, NIR can make further judgement on the existence of the minerals. The research integrated the advantages of both NIR and XRD measuring and testing techniques, put forward a method with two kinds of modern testing technology combined with each other, which may improve the accuracy of the mineral composition identification. In the meantime, the NIR will be more wildly used in geography on the basis of mineral spectroscopy.

Dopant concentration dependent growth of Fe:ZnO nanostructures

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

Sahai, Anshuman; Goswami, Navendu, E-mail: navendugoswami@gmail.com

2016-05-23

Systematic investigations of structural properties of 1-10% Fe doped ZnO nanostructure (Fe:ZnO NS) prepared via chemical precipitation method have been reported. Structural properties were probed thoroughly employing scanning electron microscope (SEM) and transmission electron microscope (TEM), energy dispersive X-ray (EDAX) analysis and X-ray diffraction (XRD). Morphological transformation of nanostructures (NS) with Fe incorporation is evident in SEM/TEM images. Nanoparticles (NP) obtained with 1% Fe, evolve to nanorods (NR) for 3% Fe; NR transform to nanocones (NC) (for 5% and 7% Fe) and finally NC transform to nanoflakes (NF) at 10% Fe. Morover, primary phase of Zn{sub 1-x}Fe{sub x}O along withmore » secondary phases of ZnFe{sub 2}O{sub 4} and Fe{sub 2}O{sub 3} were also revealed through XRD measurements. Based on collective XRD, SEM, TEM, and EDAX interpretations, a model for morphological evolution of NS was proposed and the pivotal role of Fe dopant was deciphered.« less

On the structural affinity of macromolecules with different biological properties: molecular dynamics simulations of a series of TEM-1 mutants.

PubMed

Giampaolo, Alessia Di; Mazza, Fernando; Daidone, Isabella; Amicosante, Gianfranco; Perilli, Mariagrazia; Aschi, Massimiliano

2013-07-12

Molecular Dynamics simulations have been carried out in order to provide a molecular rationalization of the biological and thermodynamic differences observed for a class of TEM β-lactamases. In particular we have considered the TEM-1(wt), the single point mutants TEM-40 and TEM-19 representative of IRT and ESBL classes respectively, and TEM-1 mutant M182T, TEM-32 and TEM-20 which differ from the first three for the additional of M182T mutation. Results indicate that most of the thermodynamic, and probably biological behaviour of these systems arise from subtle effects which, starting from the alterations of the local interactions, produce drastic modifications of the conformational space spanned by the enzymes. The present study suggests that systems showing essentially the same secondary and tertiary structure may differentiate their chemical-biological activity essentially (and probably exclusively) on the basis of the thermal fluctuations occurring in their physiological environment. Copyright © 2013 Elsevier Inc. All rights reserved.

[Analysis of XRD spectral characteristics of soil clay mineral in two typical cultivated soils].

PubMed

Zhang, Zhi-Dan; Luo, Xiang-Li; Jiang, Hai-Chao; Li, Qiao; Shen, Cong-Ying; Liu, Hang; Zhou, Ya-Juan; Zhao, Lan-Po; Wang, Ji-Hong

2014-07-01

The present paper took black soil and chernozem, the typical cultivated soil in major grain producing area of Northeast, as the study object, and determinated the soil particle composition characteristics of two cultivated soils under the same climate and location. Then XRD was used to study the composition and difference of clay mineral in two kinds of soil and the evolutionary mechanism was explored. The results showed that the two kinds of soil particles were composed mainly of the sand, followed by clay and silt. When the particle accumulation rate reached 50%, the central particle size was in the 15-130 microm interval. Except for black soil profile of Shengli Xiang, the content of clay showed converse sequence to the central particle in two soils. Clay accumulated under upper layer (18.82%) in black soil profile while under caliche layer (17.41%) in chernozem profile. Clay content was the least in parent material horizon except in black profile of Quanyanling. Analysis of clay XRD atlas showed that the difference lied in not only the strength of diffraction peak, but also in the mineral composition. The main contents of black soil and chernozem were both 2 : 1 clay, the composition of black soil was smectite/illite mixed layer-illite-vermiculite and that of chernozem was S/I mixture-illite-montmorillonite, and both of them contained little kaolinite, chlorite, quartz and other primary mineral. This paper used XRD to determine the characteristics of clay minerals comprehensively, and analyzed two kinds of typical cultivated soil comparatively, and it was a new perspective of soil minerals study.

Cdc15 integrates Tem1 GTPase-mediated spatial signals with Polo kinase-mediated temporal cues to activate mitotic exit.

PubMed

Rock, Jeremy M; Amon, Angelika

2011-09-15

In budding yeast, a Ras-like GTPase signaling cascade known as the mitotic exit network (MEN) promotes exit from mitosis. To ensure the accurate execution of mitosis, MEN activity is coordinated with other cellular events and restricted to anaphase. The MEN GTPase Tem1 has been assumed to be the central switch in MEN regulation. We show here that during an unperturbed cell cycle, restricting MEN activity to anaphase can occur in a Tem1 GTPase-independent manner. We found that the anaphase-specific activation of the MEN in the absence of Tem1 is controlled by the Polo kinase Cdc5. We further show that both Tem1 and Cdc5 are required to recruit the MEN kinase Cdc15 to spindle pole bodies, which is both necessary and sufficient to induce MEN signaling. Thus, Cdc15 functions as a coincidence detector of two essential cell cycle oscillators: the Polo kinase Cdc5 synthesis/degradation cycle and the Tem1 G-protein cycle. The Cdc15-dependent integration of these temporal (Cdc5 and Tem1 activity) and spatial (Tem1 activity) signals ensures that exit from mitosis occurs only after proper genome partitioning.

3D TEM reconstruction and segmentation process of laminar bio-nanocomposites

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

Iturrondobeitia, M., E-mail: maider.iturrondobeitia@ehu.es; Okariz, A.; Fernandez-Martinez, R.

2015-03-30

The microstructure of laminar bio-nanocomposites (Poly (lactic acid)(PLA)/clay) depends on the amount of clay platelet opening after integration with the polymer matrix and determines the final properties of the material. Transmission electron microscopy (TEM) technique is the only one that can provide a direct observation of the layer dispersion and the degree of exfoliation. However, the orientation of the clay platelets, which affects the final properties, is practically immeasurable from a single 2D TEM image. This issue can be overcome using transmission electron tomography (ET), a technique that allows the complete 3D characterization of the structure, including the measurement ofmore » the orientation of clay platelets, their morphology and their 3D distribution. ET involves a 3D reconstruction of the study volume and a subsequent segmentation of the study object. Currently, accurate segmentation is performed manually, which is inefficient and tedious. The aim of this work is to propose an objective/automated segmentation methodology process of a 3D TEM tomography reconstruction. In this method the segmentation threshold is optimized by minimizing the variation of the dimensions of the segmented objects and matching the segmented V{sub clay} (%) and the actual one. The method is first validated using a fictitious set of objects, and then applied on a nanocomposite.« less

Scalable pumping approach for extracting the maximum TEM(00) solar laser power.

PubMed

Liang, Dawei; Almeida, Joana; Vistas, Cláudia R

2014-10-20

A scalable TEM(00) solar laser pumping approach is composed of four pairs of first-stage Fresnel lens-folding mirror collectors, four fused-silica secondary concentrators with light guides of rectangular cross-section for radiation homogenization, four hollow two-dimensional compound parabolic concentrators for further concentration of uniform radiations from the light guides to a 3 mm diameter, 76 mm length Nd:YAG rod within four V-shaped pumping cavities. An asymmetric resonator ensures an efficient large-mode matching between pump light and oscillating laser light. Laser power of 59.1 W TEM(00) is calculated by ZEMAX and LASCAD numerical analysis, revealing 20 times improvement in brightness figure of merit.

[Infrared spectroscopy and XRD studies of coral fossils].

PubMed

Chen, Quan-li; Zhou, Guan-min; Yin, Zuo-wei

2012-08-01

Coral fossil is an old remain of multicellular animal on the earth, and formed by various geological processes. The structural characteristics and compositions of the coral fossils with different color and radial texture on the surface were studied by infrared absorption spectroscopy and X-ray powder diffraction analyses. The results show that the studied coral fossils mainly are composed of SiO2, and the radial microstructure characterized by the calcareous coral cross-section is preserved. It is formed by metasomatism by SiO2. The infrared absorption spectra of the coral fossil with different color and texture are essentially the same, showing typical infrared absorption spectra of the quartz jade. XRD analysis shows that the main components of the coral fossils with different color and texture are consistent and mainly composed of SiO2 with a trace amount of other minerals and without CaCO3.

Silk fibroin/gold nanocrystals: a new example of biopolymer-based nanocomposites

NASA Astrophysics Data System (ADS)

Noinville, S.; Garnier, A.; Courty, A.

2017-05-01

The dispersion of nanoparticles in ordered polymer nanostructures can provide control over particle location and orientation, and pave the way for tailored nanomaterials that have enhanced mechanical, electrical, or optical properties. Here we used silk fibroin, a natural biopolymer, to embed gold nanocrystals (NCs), so as to obtain well-ordered structures such as nanowires and self-assembled triangular nanocomposites. Monodisperse gold NCs synthesized in organic media are mixed to silk fibroin and the obtained nanocomposites are characterized by UV-visible spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (FE-SEM), atomic force microscopy (AFM) and Infrared spectroscopy. The optical properties study of gold NCs and silk-gold nanocomposites shows that the Surface Plasmon band is blue shifted compared to gold NCs. The size and shape of NCs gold superlattices can be well controlled by the presence of silk fibroin giving nanowires and also self-assembled triangular nanocomposites as characterized by TEM, FE-SEM and AFM. The strong interaction between gold NCs and silk fibroin is also revealed by the conformation change of silk protein in presence of gold NCs, as shown by FTIR analysis. The formation of such ordered nanocomposites (gold NCs/silk fibroin) will provide new nanoplasmonic devices.

Facile construction of vertically aligned EuS-ZnO hybrid core shell nanorod arrays for visible light driven photocatalytic properties

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

Ranjith, K. S.; Kumar, D. Ranjith; Kumar, R. T. Rajendra, E-mail: rtrkumar@buc.edu.in

2015-06-24

We demonstrated the development of coupled semiconductor in the form of hybrid heterostructures for significant advancement in catalytic functional materials. In this article, we report the preparation of vertically aligned core shell ZnO-EuS nanorod photocatalyst arrays by a simple chemical solution process followed by sulfudation process. The XRD pattern confirmed formation of the hexagonal wurtzite structure of ZnO and cubic nature of the EuS. Cross sectional FESEM images show vertical rod array structure, and the size of the nanorods ranges from 80 to 120 nm. UV-Vis DRS spectra showed that the optical absorption of ZnO was significantly enhanced to the visiblemore » region by modification with EuS surfaces. TEM study confirmed that the surface of ZnO was drastically improved by the modification with EuS nanoparticle. The catalytic activity of EuS−ZnO core shell nanorod arrays were evaluated by the photodegradation of Methylene Blue (MB) dye under visible irradiation. The results revealed that the photocatalytic activity of EuS−ZnO was much higher than that of ZnO under natural sunlight. EuS−ZnO was found to be stable and reusable without appreciable loss of catalytic activity up to four consecutive cycles.« less

Thermal stability, optical and Photoluminescence properties of spherical Ce x Zr1‑x O2 (x = 0.05) crystalline blue-emitting nanophosphors synthesized by microwave method

NASA Astrophysics Data System (ADS)

Manjunatha, S.; Dharmaprakash, M. S.

2018-03-01

Nanocrystalline ZrO2 based material is an impressive candidate for the various functional applications owing to their ease of preparation and high thermal stability. This paper reports the synthesis, structural and optical characterization of thermally stable monodispersed CexZr1‑xO2 (x = 0.05) nanoparticles. This method is based on the fact that, microwave irradiation allows the formation of size controlled and single phase cubic ZrO2 nanoparticles containing Ce+4 as a dopant. The XRD and Rietveld analysis revealed the formation of the crystalline cubic fluorite phase. The formation of nanoparticles was confirmed by FTIR. The morphology of the nanophosphors was characterised by FESEM and TEM. The optical band gap was calculated from the UV–visible absorption spectra and was found to vary from 3.93 to 4.25 eV with calcination temperature. It shows the decrease in the optical band gap from the pristine ZrO2. The particle size was measured by using HRTEM, and the average particle size was found to be 22 nm. Under the 268 nm Ultra Violet irradiation excitation a blue emission at 443 nm was observed at room temperature. The possible luminescence mechanism of CexZr1‑xO2 nanophosphor under UV excitation is discussed.

Synthesis of colloidal silver iron oxide nanoparticles--study of their optical and magnetic behavior.

PubMed

Kumar, Anil; Singhal, Aditi

2009-07-22

Silver iron oxide nanoparticles of fairly small size (average diameter approximately 1 nm) with narrow size distribution have been synthesized by the interaction of colloidal beta- Fe2O3 and silver nanoparticles. The surface morphology and size of these particles have been analyzed by using atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Their structural analysis has been carried out by employing x-ray diffraction (XRD), selected-area electron diffraction (SAED), optical and infrared (IR) spectroscopic techniques. The ageing of these particles exhibits the formation of self-assembly, possibly involving weak supramolecular interactions between Ag(I)O4 and Fe(III)O4 species. These particles display the onset of absorption in the near-infrared region and have higher absorption coefficient in the visible range compared to that of its precursors. Magnetic measurements reveal an interesting transition in their magnetic behavior from diamagnetic to superparamagnetic. The magnetic moment of these particles attains a limiting value of about 0.19 emu cm(-2), which is more than two times higher than that of colloidal beta- Fe2O3. With enhanced optical and magnetic properties, this system is suggested to have possible applications in optoelectronic and magnetic devices.

Adenine-functionalized Spongy Graphene for Green and High-Performance Supercapacitors

PubMed Central

El-Gendy, Dalia M.; Ghany, Nabil A. Abdel; El Sherbini, E. E. Foad; Allam, Nageh K.

2017-01-01

A simple method is demonstrated to prepare spongy adenine-functionalized graphene (SFG) as interconnected, porous 3-dimensional (3D) network crinkly sheets. Such 3D network structure provides better contact at the electrode/electrolyte interface and facilitates the charge transfer kinetics. The fabricated SFG was characterized by X-ray diffraction (XRD), FTIR, scanning electron microscopy (FESEM), Raman spectroscopy, thermogravimetric analysis (TGA), UV−vis absorption spectroscopy, and transmission electron microscopy (TEM). The synthesized materials have been evaluated as supercapacitor materials in 0.5 M H2SO4 using cyclic voltammetry (CV) at different potential scan rates, and galvanostatic charge/discharge tests at different current densities. The SFG electrodes showed a maximum specific capacitance of 333 F/g at scan rate of 1 mV/s and exhibited excellent cycling retention of 102% after 1000 cycles at 200 mV/s. The energy density was 64.42 Wh/kg with a power density of 599.8 W/kg at 1.0 A/g. Those figures of merit are much higher than those reported for graphene-based materials tested under similar conditions. The observed high performance can be related to the synergistic effects of the spongy structure and the adenine functionalization. PMID:28216668

A top-down method to fabricate SrAl2O4:Eu2+,Dy3+ nanosheets from commercial blocky phosphors

NASA Astrophysics Data System (ADS)

Zhang, Haoran; Xue, Zhiping; Lei, Bingfu; Dong, Hanwu; Zhang, Haiming; Deng, Suqing; Zheng, Mingtao; Liu, Yingliang; Xiao, Yong

2014-09-01

By using commercial SrAl2O4:Eu2+,Dy3+ phosphor as raw material, we have developed a novel and simple top-down method to fabricate SrAl2O4:Eu2+,Dy3+ nanosheets that are useful for potential practical applications, especially as fluorescent labels for biomolecules and mechano-optical nano-devices. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDX) results demonstrate that the treated samples are still pure-phase of SrAl2O4:Eu2+,Dy3+. The field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) results indicate that the treated SrAl2O4:Eu2+,Dy3+ phosphors are built up by nanosheets bundles. Excitation and emission spectra, afterglow emission spectra and decay curves are used to analyze the luminescence properties of SrAl2O4:Eu2+,Dy3+ nanosheets, and the results show that, compared with commercial samples, the treated samples show similar spectra characteristic including the spectra shapes and the band position. Furthermore, the fluorescence and afterglow intensity of SrAl2O4:Eu2+,Dy3+ nanosheets can be tuned linearly by changing the circumstance temperatures, which further indicates its potential applications in fiber-optical thermometer materials.

Preparation, characterization, and antibacterial activity of NiFe2O4/PAMA/Ag-TiO2 nanocomposite

NASA Astrophysics Data System (ADS)

Allafchian, Alireza; Jalali, Seyed Amir Hossein; Bahramian, Hamid; Ahmadvand, Hossein

2016-04-01

We have described a facile fabrication of silver deposited on the TiO2, Poly Acrylonitrile Co Maleic Anhydride (PAMA) polymer and nickel ferrite composite (NiFe2O4/PAMA/Ag-TiO2) through a three-step procedure. A pre-synthesized NiFe2O4 was first coated with PAMA polymer and then Ag-TiO2 was deposited on the surface of PAMA polymer shell. After the characterization of this three-component composite by various techniques, such as FTIR, XRD, FESEM, BET, TEM and VSM, it was impregnated in standard antibiotic discs. The antibacterial activity of NiFe2O4/PAMA/Ag-TiO2 nanocomposite was investigated against some gram positive and gram negative bacteria by employing disc diffusion assay and then compared with that of naked NiFe2O4, NiFe2O4/Ag, AgNPs and NiFe2O4/PAMA. The results demonstrated that the AgNPs, when embedded in TiO2 and combined with NiFe2O4/PAMA, became an excellent antibacterial agent. The NiFe2O4/PAMA/Ag-TiO2 nanocomposite could be readily separated from water solution after the disinfection process by applying an external magnetic field.

Microwave synthesis and photocatalytic activities of ZnO bipods with different aspect ratios

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

Sun, Fazhe; Zhao, Zengdian; Qiao, Xueliang, E-mail: xuelqiao@163.com

2016-02-15

Highlights: • We synthesized linked ZnO nanorods by a facile microwave method. • The effect of reaction parameters on ZnO was investigated. • ZnO bipods with different aspect ratios were prepared. • The photocatalytic performance of ZnO bipods was evaluated. - Abstract: Linked ZnO nanorods have been successfully prepared via a facile microwave method without any post-synthesis treatment. The X-ray diffraction (XRD) patterns indicated the precursor had completely transformed into the pure ZnO crystal. The images of field emitting scanning electron microscope (FESEM) and transmission electron microscope (TEM) showed that linked ZnO nanorods consisted predominantly of ZnO bipods. The formationmore » process of the ZnO bipods was clearly discussed. ZnO bipods with different aspect ratios have been obtained by tuning the concentrations of reagents and microwave power. Moreover, the photocatalytic performance of ZnO bipods with different aspect ratios for degradation of methylene blue was systematically evaluated. The results of photocatalytic experiments showed that the photocatalytic activity increased with the aspect ratios of ZnO bipods increased. The reason is that ZnO bipods with larger aspect ratio have higher surface area, which can absorb more MB molecules to react with ·OH radicals.« less

Enhanced NO2 sensing characteristics of Au modified porous silicon/thorn-sphere-like tungsten oxide composites

NASA Astrophysics Data System (ADS)

Yuan, Lin; Hu, Ming; Wei, Yulong; Ma, Wenfeng

2016-12-01

The thorn-sphere-like tungsten oxide (WO3) made up by 1D nanorods has been successfully synthesized through hydrothermal method on the Au-modified porous silicon (PS) substrates with seed-layer induction. By using XRD, EDS, FESEM and TEM techniques, we tested and verified that the crystal structure and morphology evolution of WO3 hierarchical nanostructure on the Au-modified PS strongly depend on the Au-sputtering time and hydrothermal reaction time. In addition, by comparing the NO2-sensing properties of the prepared products, we found that the 10 s-Au decorated PS/WO3-3 h (sputtering Au for 10 s and hydrothermal reaction for 3 h) composites sensor behaving as a typical p-type semiconductor and operating at room temperature (RT) exhibits high sensitivity and response characteristics even to ppb-level NO2, which makes this kind of sensor a competitive candidate for NO2-sensing applications. Moreover, the enhanced response may not only due to the high specific surface area but the Au nanoparticles acting as promoters for the spillover effect and forming metal-semiconductor heterojunctions with the PS and WO3. The transmission of electrons and holes in the heterogeneous interface generated among PS, WO3 and Au is proposed to illustrate the p-type response mechanism.

A high-performance nonenzymatic glucose sensor made of CuO-SWCNT nanocomposites.

PubMed

Quoc Dung, Nguyen; Patil, Dewyani; Jung, Hyuck; Kim, Dojin

2013-04-15

Nanocomposites of CuO and single-wall carbon nanotubes (SWCNTs) were synthesized using an arc-discharging graphite rod that contained copper wires. Simultaneous arc discharges produced a CuO-SWCNT composite network. The crystalline structure and morphology of the CuO-SWCNT composite films were investigated using XRD, Raman spectroscopy, FE-SEM and TEM. The electrochemical properties were investigated by cyclic voltammogram and amperometric measurements in a 0.1 M NaOH solution. The CuO content in the CuO-SWCNT nanocomposites was optimized for nonenzymatic glucose detection. The glucose sensing properties of the optimized CuO-SWCNT electrode showed good stability, selectivity, and linear glucose detection that ranged from 0.05 to 1800 μM with a higher sensitivity of 1610 μA cm⁻² mM⁻¹, a quick response time of 1-2 s, and the lowest limit of detection at 50 nM. The sensing performance was better than the pure CuO and SWCNT sensors, and the synergetic effect of the composite sensor was attributed to the high conductivity network of highly porous nanowires. The sensor also showed a good response in a human serum sample, which proves its high potential towards a commercial nonenzymatic glucose sensor. Copyright © 2012 Elsevier B.V. All rights reserved.

Thermal and ultrasonic influence in the formation of nanometer scale hydroxyapatite bio-ceramic

PubMed Central

Poinern, GJE; Brundavanam, R; Le, X Thi; Djordjevic, S; Prokic, M; Fawcett, D

2011-01-01

Hydroxyapatite (HAP) is a widely used biocompatible ceramic in many biomedical applications and devices. Currently nanometer-scale forms of HAP are being intensely investigated due to their close similarity to the inorganic mineral component of the natural bone matrix. In this study nano-HAP was prepared via a wet precipitation method using Ca(NO3)2 and KH2PO4 as the main reactants and NH4OH as the precipitator under ultrasonic irradiation. The Ca/P ratio was set at 1.67 and the pH was maintained at 9 during the synthesis process. The influence of the thermal treatment was investigated by using two thermal treatment processes to produce ultrafine nano-HAP powders. In the first heat treatment, a conventional radiant tube furnace was used to produce nano-particles with an average size of approximately 30 nm in diameter, while the second thermal treatment used a microwave-based technique to produce particles with an average diameter of 36 nm. The crystalline structure and morphology of all nanoparticle powders produced were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR). Both thermal techniques effectively produced ultrafine powders with similar crystalline structure, morphology and particle sizes. PMID:22114473

Mechanical Alloying of W-Mo-V-Cr-Ta High Entropy Alloys

NASA Astrophysics Data System (ADS)

Das, Sujit; Robi, P. S.

2018-04-01

Recent years have seen the emergence of high-entropy alloys (HEAs) consisting of five or more elements in equi-atomic or near equi-atomic ratios. These alloys in single phase solid solution exhibit exceptional mechanical properties viz., high strength at room and elevated temperatures, reasonable ductility and stable microstructure over a wide range of temperatures making it suitable for high temperature structural materials. In spite of the attractive properties, processing of these materials remains a challenge. Reports regarding fabrication and characterisation of a few refractory HEA systems are available. The processing of these alloys have been carried out by arc melting of small button sized materials. The present paper discusses the development of a novel refractory W-Mo-V-Cr-Ta HEA powder based on a new alloy design concept. The powder mixture was milled for time periods up to 64 hours. Single phase alloy powder having body centred cubic structure was processed by mechanical alloying. The milling characteristics and extent of alloying during the ball milling were characterized using X-ray diffractiometre (XRD), field emission scanning electron microscope (FESEM) and transmission electron microscope (TEM). A single phase solid solution alloy powder having body-centred cubic (BCC) structure with a lattice parameter of 3.15486 Å was obtained after milling for 32 hours.

Self-assembled chiral helical nanofibers by amphiphilic dipeptide derived from d- or l-threonine and application as a template for the synthesis of Au and Ag nanoparticles.

PubMed

Zhang, Han; Xin, Xia; Sun, Jichao; Zhao, Liupeng; Shen, Jinglin; Song, Zhaohua; Yuan, Shiling

2016-12-15

The discovery of a class of self-assembling peptides that spontaneously undergo self-organization into well-ordered structures opened a new avenue for molecular fabrication of biological materials. In this paper, the structure controlled helical nanofibers were prepared by two artificial β-sheet dipeptides with long alkyl chains derived from l- and d-threonine (Thr) and sodium hydroxide (NaOH). These helical nanofibers have been characterized using transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), circular dichroism (CD), Fourier transform infrared (FT-IR) spectroscopy, and X-ray powder diffraction (XRD). It was demonstrated that the helicity of the nanofibers could be easily controlled by changing the chirality of the constituent amino acids in the peptide species (d- or l-threonine). Moreover, the hydrogen bonding interactions between the amide groups as well as the hydrophobic interactions among the alkyl chains play important roles in the self-assembly process. It also can be observed that with the passage of time, the hydrogen bonding interactions between the individual nanofiber induced the conversion from nanofibers to nanobelts. Particularly, gold and silver nanoparticles performed good catalytic ability were synthesized using the assembled nanofibers as template. Copyright © 2016 Elsevier Inc. All rights reserved.

Efficient decomposition of formaldehyde at room temperature over Pt/honeycomb ceramics with ultra-low Pt content.

PubMed

Nie, Longhui; Zheng, Yingqiu; Yu, Jiaguo

2014-09-14

Pt/honeycomb ceramic (Pt/HC) catalysts with ultra-low Pt content (0.005-0.055 wt%) were for the first time prepared by an impregnation of honeycomb ceramics with Pt precursor and NaBH4-reduction combined method. The microstructures, morphologies and textural properties of the resulting samples were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). The obtained Pt/HC catalysts were used for catalytic oxidative decomposition of formaldehyde (HCHO) at room temperature. It was found that the as-prepared Pt/HC catalysts can efficiently decompose HCHO in air into CO2 and H2O at room temperature. The catalytic activity of the Pt/HC catalysts increases with increasing the Pt loading in the range of 0.005-0.013 wt%, and the further increase of the Pt loading does not obviously improve catalytic activity. From the viewpoint of cost and catalytic performance, 0.013 wt% Pt loading is the optimal Pt loading amount, and the Pt/HC catalyst with 0.013 wt% Pt loading also exhibited good catalytic stability. Considering practical applications, this work will provide new insights into the low-cost and large-scale fabrication of advanced catalytic materials for indoor air purification.

Photoluminescent properties of spider silk coated with Eu-doped nanoceria

NASA Astrophysics Data System (ADS)

Dmitrović, Svetlana; Nikolić, Marko G.; Jelenković, Branislav; Prekajski, Marija; Rabasović, Mihailo; Zarubica, Aleksandra; Branković, Goran; Matović, Branko

2017-02-01

Spider dragline silk was coated with pure as well as Eu-doped ceria nanopowders at the room temperature. The treatment was done by immersion of the spider silk mesh into aqueous solutions of cerium nitrate (Ce(NO3)3) and ammonium hydroxide (NH4OH). Depending on the relationship between Ce3+ ion and ammonium hydroxide concentration, coated fibers exhibited a different thickness. Obtained materials were studied by means of FESEM. It was found that ceria nanoparticles of average size of 3 nm were coated along spider thread. X-ray diffraction (XRD) and selected-area electron diffraction (SAED) confirmed crystal nature of nanoparticle coating of spider silk. By using Williamson-Hall plots, crystallite size and strain were estimated. EDS measurement confirmed the presence of Eu in spider-Eu-doped ceria composite, and according to FTIR analysis, the interaction between CeO2 and spider silk was proposed. The morphology of obtained composite was observed by TEM. The photoluminescence emission spectra of spider silk coated with Eu-doped ceria were measured with two different excitations of 385 and 466 nm. The two-photon excited auto-fluorescence of spider silk coated with Eu-doped ceria was detected using a nonlinear laser scanning microscope. Obtained composite has a potential as a fluorescent labeling material in diverse applications.

Metal organic framework g-C3N4/MIL-53(Fe) heterojunctions with enhanced photocatalytic activity for Cr(VI) reduction under visible light

NASA Astrophysics Data System (ADS)

Huang, Wenyuan; Liu, Ning; Zhang, Xiaodong; Wu, Minghong; Tang, Liang

2017-12-01

In this study, hybrid nanocomposites based on Fe-based MOF and graphitic carbon nitride (g-C3N4) were developed by a facile solvothermal method. The as-prepared materials were characterized by XRD, FESEM, TEM, XPS and PL analysis. It was showed that the introduction of a certain amount of g-C3N4 on the surface of MIL-53(Fe) would improve the separation and migration rate of photo-induced charges, consequently resulting in the boost of photocatalytic efficiency. Compared with g-C3N4 and MIL-53(Fe), the CMFe composites displayed more excellent visible light-resposive photocatalytic activity for the reduction of Cr(VI). The optimal doping content of g-C3N4 in g-C3N4/MIL-53(Fe) composite was determined to be 3.0 wt%, and it showed about 2.1 and 2.0 times as high photocatalytic efficiency for the reduction of Cr(VI) as that of pure g-C3N4 and MIL-53(Fe), respectively. Meanwhile, the composite exhibited good reusability and stability in the process of cyclic experiments. A possible photocatalytic reaction mechanism was also investigated in detail by the related electrochemical analysis.

Preparation of porous palladium nanowire arrays and their catalytic performance for hydrogen peroxide electroreduction in acid medium

NASA Astrophysics Data System (ADS)

Wang, Xin; Ye, Ke; Gao, Yinyi; Zhang, Hongyu; Cheng, Kui; Xiao, Xue; Wang, Guiling; Cao, Dianxue

2016-01-01

Nanoporous palladium supported on the carbon coated titanium carbide (C@TiC) nanowire arrays (Pd NP/C@TiC) are successfully prepared by a facile chemical vapor deposition of three-dimensional (3D) C@TiC substrate, followed by electrochemical codeposition of Pd-Ni and removal of Ni via dealloying. The structure and morphology of the obtained Pd NP/C@TiC electrodes are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Cyclic voltammetry (CV), linear sweep voltammetry (LSV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) are used to examine the catalytic performances of the electrodes for H2O2 electroreduction in H2SO4 solution. The Pd NP/C@TiC electrode exhibits a largely effective specific surface area owing to its open nanoporous structure allowing the full utilization of Pd surface active sites. At the potential of 0.2 V in 2.0 mol L-1 H2O2 and 2 mol L-1 H2SO4 solutions, the reduction current density reaches 3.47 A mg-1, which is significantly higher than the catalytic activity of H2O2 electroreduction achieved previously with precious metals as catalysts.

Manipulation of partially oriented hydroxyapatite building blocks to form flowerlike bundles without acid-base regulation.

PubMed

Wen, Zhenliang; Wang, Zihao; Chen, Jingdi; Zhong, Shengnan; Hu, Yimin; Wang, Jianhua; Zhang, Qiqing

2016-06-01

The application of hydroxyapatite (HAP) in different fields depends greatly on its morphology, composition and structure. Besides, the main inorganic building blocks of human bones and teeth are also HAP. Therefore, accurate shape and aggregation control and of hydroxyapatite particles will be of great interest. Herein, oriented bundles of flowerlike HAP nanorods were successfully prepared through hydrothermal treatment without acid-base regulation, with the mono-alkyl phosphate (MAP) and sodium citrate as surfactant and chelating agent, respectively. The prepared samples were characterized by the X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and zeta potential, the pH value and conductivity value of suspension were characterized by pH meter and conductivity measurement. The results showed that the MAP and citrate play an important role in assembly of HAP nanorods without acid-base regulation. Citrate calcium complex could decompose slowly and release citrate ions at hydrothermal conditions. Besides, the further decomposition of citrate ions could release aconitic acid as the reaction time prolongs. Moreover, the possible scheme for the formation process was discussed in detail. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis of inorganic fullerene-like WS2 nanoparticles and their lubricating performance

NASA Astrophysics Data System (ADS)

Yang, Haibin; Liu, Shikai; Li, Jixue; Li, Minghui; Peng, Gang; Zou, Guangtian

2006-03-01

A facile, large-scale and low-cost route was used to synthesize inorganic fullerene-like (IF) WS2 nanoparticles by the reaction of sulfur powder (S) and as-prepared WO3 nanoparticles in a hydrogen atmosphere at a heating temperature of 500-650 °C. The as-synthesized IF-WS2 nanoparticles are of a closed hollow cage structure with an average size of about 50 nm. The composition, morphology and structure of the products were characterized by XRD, TEM, FE-SEM, and HRTEM. The influences of the main reaction conditions were investigated and the possible growth mechanism are proposed. It is worth noting that through changing the amount of as-prepared composite powder (WO3 and S) and the content of hydrogen, yields of IF-WS2 in larger scales can accordingly be easily obtained, and such a synthetic route may also be used in the synthesis of other transition IF metal dichalcogenides. Furthermore, tribological experiments emphasized the important role played by these as-synthesized IF-WS2 nanoparticles in providing excellent lubricating performance, which may bring a much brighter future for their applications in the lubricating field, or even arouse great interest of both scientists and industrialists for their many other important applications.

Cost-effective single-step carbon nanotube synthesis using microwave oven

NASA Astrophysics Data System (ADS)

Algadri, Natheer A.; Ibrahim, K.; Hassan, Z.; Bououdina, M.

2017-08-01

This paper reports the characterization of carbon nanotubes (CNTs) synthesised using a conventional microwave oven method, offering several advantages including fast, simple, low cost, and solvent free growth process. The procedure involves flattening of graphite/ferrocene mixture catalyst inside the microwave oven under ambient conditions for a very short duration of 5 s, which inhibits the loss factor of graphite and ferrocene. The effect of graphite/ferrocene mixture ratio for the synthesis of CNTs is investigated by transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), x-ray diffraction (XRD), Raman spectroscopy and UV-NIR-Vis measurements. The samples produced using the different ratios contain nanotubes with an average diameter in the range 44-79 nm. The highest yield of CNTs is attained with graphite/ferrocene mixture ratio of 70:30. The lowest I D/I G ratio intensity as identified by Raman spectroscopy for 70:30 ratio indicates the improved crystallinity of CNTs. Due to the capillary effect of CNTs, Fe nanoparticles are found to be encapsulated inside the tubes at different positions along the tube length. The obtained results showed that the smaller the diameter of graphite and ferrocene favors the synthesis of graphene oxide upon microwave radiation.

TiO2 Nanotube-Carbon (TNT-C) as Support for Pt-based Catalyst for High Methanol Oxidation Reaction in Direct Methanol Fuel Cell.

PubMed

Abdullah, M; Kamarudin, S K; Shyuan, L K

2016-12-01

In this study, TiO 2 nanotubes (TNTs) were synthesized via a hydrothermal method using highly concentrated NaOH solutions varying from 6 to 12 M at 180 °C for 48 h. The effects of the NaOH concentration and the TNT crystal structure on the performance for methanol oxidation were investigated to determine the best catalyst support for Pt-based catalysts. The results showed that TNTs produced with 10 M NaOH exhibited a length and a diameter of 550 and 70 nm, respectively; these TNTs showed the best nanotube structure and were further used as catalyst supports for a Pt-based catalyst in a direct methanol fuel cell. The synthesized TNT and Pt-based catalysts were analysed by FESEM, TEM, BET, EDX, XRD and FTIR. The electrochemical performance of the catalysts was investigated using cyclic voltammetry (CV) and chronoamperometric (CA) analysis to further understand the methanol oxidation in the direct methanol fuel cell (DMFC). Finally, the result proves that Pt-Ru/TNT-C catalyst shows high performance in methanol oxidation as the highest current density achieved at 3.3 mA/cm 2 (normalised by electrochemically active surface area) and high catalyst tolerance towards poisoning species was established.

Graphene nanosheets preparation using magnetic nanoparticle assisted liquid phase exfoliation of graphite: The coupled effect of ultrasound and wedging nanoparticles.

PubMed

Hadi, Alireza; Zahirifar, Jafar; Karimi-Sabet, Javad; Dastbaz, Abolfazl

2018-06-01

This study aims to investigate a novel technique to improve the yield of liquid phase exfoliation of graphite to graphene sheets. The method is based on the utilization of magnetic Fe 3 O 4 nanoparticles as "particle wedge" to facilitate delamination of graphitic layers. Strong shear forces resulted from the collision of Fe 3 O 4 particles with graphite particles, and intense ultrasonic waves lead to enhanced exfoliation of graphite. High quality of graphene sheets along with the ease of Fe 3 O 4 particle separation from graphene solution which arises from the magnetic nature of Fe 3 O 4 nanoparticles are the unique features of this approach. Initial graphite flakes and produced graphene sheets were characterized by various methods including field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Raman spectroscopy, atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and Zeta potential analysis. Moreover, the effect of process factors comprising initial graphite concentration, Fe 3 O 4 nanoparticles concentration, sonication time, and sonication power were investigated. Results revealed that graphene preparation yield and the number of layers could be manipulated by the presence of magnetic nanoparticles. Copyright © 2018 Elsevier B.V. All rights reserved.

Bayesian resolution of TEM, CSEM and MT soundings: a comparative study

NASA Astrophysics Data System (ADS)

Blatter, D. B.; Ray, A.; Key, K.

2017-12-01

We examine the resolution of three electromagnetic exploration methods commonly used to map the electrical conductivity of the shallow crust - the magnetotelluric (MT) method, the controlled-source electromagnetic (CSEM) method and the transient electromagnetic (TEM) method. TEM and CSEM utilize an artificial source of EM energy, while MT makes use of natural variations in the Earth's electromagnetic field. For a given geological setting and acquisition parameters, each of these methods will have a different resolution due to differences in the source field polarization and the frequency range of the measurements. For example, the MT and TEM methods primarily rely on induced horizontal currents and are most sensitive to conductive layers while the CSEM method generates vertical loops of current and is more sensitive to resistive features. Our study seeks to provide a robust resolution comparison that can help inform exploration geophysicists about which technique is best suited for a particular target. While it is possible to understand and describe a difference in resolution qualitatively, it remains challenging to fully describe it quantitatively using optimization based approaches. Part of the difficulty here stems from the standard electromagnetic inversion toolkit, which makes heavy use of regularization (often in the form of smoothing) to constrain the non-uniqueness inherent in the inverse problem. This regularization makes it difficult to accurately estimate the uncertainty in estimated model parameters - and therefore obscures their true resolution. To overcome this difficulty, we compare the resolution of CSEM, airborne TEM, and MT data quantitatively using a Bayesian trans-dimensional Markov chain Monte Carlo (McMC) inversion scheme. Noisy synthetic data for this study are computed from various representative 1D test models: a conductive anomaly under a conductive/resistive overburden; and a resistive anomaly under a conductive/resistive overburden. In

Strains on the nano- and microscale in nickel-titanium: An advanced TEM study

NASA Astrophysics Data System (ADS)

Tirry, Wim

2007-12-01

A general introduction to shape memory behavior and the martensitic transformation is given in chapter 1, with speck information concerning the NiTi material. The technique used to study the material is transmission electron microscopy (TEM) of which the basics are explained in chapter 2 as well as information concerning the NiTi material. The main goal was to apply more advanced TEM techniques in order to measure some aspects in a quantitative way rather than qualitative, which is mostly the case in conventional TEM. (1) Quantitative electron diffraction was used to refine the structure of Ni4Ti3 precipitates, this was done by using the MSLS method in combination with density functional theory (DFT) calculations. (2) These Ni4Ti3 precipitates are (semi-)coherent which results in a strain field in the matrix close to the precipitate. High resolution TEM (HRTEM) in combination with image processing techniques was used to measure these strain fields. The obtained results are compared to the Eshelby model for elliptical inclusions, and major difference is an underestimation of the strain magnitude by the model. One of the algorithms used to extract strain information from HRTEM images is the geometric phase method. (3) The Ni4Ti3-Ni4Ti3 and Ni4Ti3-precipitate interface was investigated with HRTEM showing that the Ni4Ti3-precipitate interface might be diffuse over a range of 3nm. (4) In-situ straining experiments were performed on single crystalline and superelastic polycrystalline NiTi samples. It seems that the strain induced martensite planes in the polycrystalline sample show no sign of twinning. This is in contradiction to what is expected and is discussed in the view of the crystallographic theory of martensite, in addition a first model explaining this behavior is proposed. In this dissertation the main attention is divided over the material aspects of NiTi and on how to apply these more advanced TEM techniques.

Development and Application of Operando TEM to a Ruthenium Catalyst for CO Oxidation

NASA Astrophysics Data System (ADS)

Miller, Benjamin Kyle

Operando transmission electron microscopy (TEM) is an extension of in-situ TEM in which the performance of the material being observed is measured simultaneously. This is of great value, since structure-performance relationships lie at the heart of materials science. For catalyst materials, like the SiO2-supported Ru nanoparticles studied, the important performance metric, catalyst activity, is measured inside the microscope by determining the gas composition during imaging. This is accomplished by acquisition of electron energy loss spectra (EELS) of the gas in the environmental TEM while catalysis is taking place. In this work, automated methods for rapidly quantifying low-loss and core-loss EELS of gases were developed. A new sample preparation method was also established to increase catalytic conversion inside a differentially-pumped environmental TEM, and the maximum CO conversion observed was about 80%. A system for mixing gases and delivering them to the environmental TEM was designed and built, and a method for locating and imaging nanoparticles in zone axis orientations while minimizing electron dose rate was determined. After atomic resolution images of Ru nanoparticles observed during CO oxidation were obtained, the shape and surface structures of these particles was investigated. A Wulff model structure for Ru particles was compared to experimental images both by manually rotating the model, and by automatically determining a matching orientation using cross-correlation of shape signatures. From this analysis, it was determined that most Ru particles are close to Wulff-shaped during CO oxidation. While thick oxide layers were not observed to form on Ru during CO oxidation, thin RuO2 layers on the surface of Ru nanoparticles were imaged with atomic resolution for the first time. The activity of these layers is discussed in the context of the literature on the subject, which has thus far been inconclusive. We conclude that disordered oxidized ruthenium

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Multivariate analysis of DSC-XRD simultaneous measurement data: a study of multistage crystalline structure changes in a linear poly(ethylene imine) thin film.

PubMed

Kakuda, Hiroyuki; Okada, Tetsuo; Otsuka, Makoto; Katsumoto, Yukiteru; Hasegawa, Takeshi

2009-01-01

A multivariate analytical technique has been applied to the analysis of simultaneous measurement data from differential scanning calorimetry (DSC) and X-ray diffraction (XRD) in order to study thermal changes in crystalline structure of a linear poly(ethylene imine) (LPEI) film. A large number of XRD patterns generated from the simultaneous measurements were subjected to an augmented alternative least-squares (ALS) regression analysis, and the XRD patterns were readily decomposed into chemically independent XRD patterns and their thermal profiles were also obtained at the same time. The decomposed XRD patterns and the profiles were useful in discussing the minute peaks in the DSC. The analytical results revealed the following changes of polymorphisms in detail: An LPEI film prepared by casting an aqueous solution was composed of sesquihydrate and hemihydrate crystals. The sesquihydrate one was lost at an early stage of heating, and the film changed into an amorphous state. Once the sesquihydrate was lost by heating, it was not recovered even when it was cooled back to room temperature. When the sample was heated again, structural changes were found between the hemihydrate and the amorphous components. In this manner, the simultaneous DSC-XRD measurements combined with ALS analysis proved to be powerful for obtaining a better understanding of the thermally induced changes of the crystalline structure in a polymer film.

Poly (N-ethyl aniline)/Ag Nanocomposite as Humidity Sensor

NASA Astrophysics Data System (ADS)

Pande, Nishigandh S.; Jaspal, Dipika; Ambekar, Jalindar

Poly (N-ethyl aniline)/Ag organic-inorganic composite has been synthesized by a single step in situ chemical oxidative polymerization method. The synthesis of Poly (N-ethyl aniline)/Ag nanocomposite has been confirmed by X-ray diffraction (XRD), Ultraviolet-Vis Spectroscopy (UV-visible), Fourier transform infrared analysis (FTIR) and FE-SEM investigations. XRD spectral study exhibited major diffraction in the range 20-80∘ (2θ) and indicated the semicrystalline nature of poly (N-ethyl aniline)/Ag nanocomposite. Characteristic peaks in UV-visible and FTIR spectra of poly (N-ethyl aniline) switched to higher wave numbers in poly (N-ethyl aniline)/Ag nanocomposite. Peaks at 1789cm-1, 1595cm-1, 667cm-1 and 501cm-1 in FTIR spectrum confirmed the formation of poly (N-ethyl aniline)/Ag nanocomposite. FE-SEM photographs reported agglomerated granular particulate nature of poly (N-ethyl aniline)/Ag nanocomposite. Synthesized poly (N-ethyl aniline)/Ag nanocomposite exhibited a high response to humidity, good reproducibility and stability at room temperature. An appreciable response was shown in the presence of 40% humid atmosphere for up to successive four cycles. Composite sensitivity has been found to increase with the increasing concentration of humidity, at room temperature.

Synthesis of Hierarchical Self-Assembled CuO and Their Structure-Enhanced Photocatalytic Performance

NASA Astrophysics Data System (ADS)

Wang, Dagui; Yan, Bing; Song, Caixiong; Ye, Ting; Wang, Yongqian

2018-01-01

Hierarchical self-assembled CuO hollow microspheres with superior photocatalytic performance are synthesized via a simple hydrothermal process in the presence of cationic surfactants (cetyltrimethylammonium bromide, CTAB). The structure, morphology, and optical absorption performance of CuO samples prepared with different surfactants including CTAB, nonionic surfactant (polyvinylpyrrolidone, PVP) and anionic surfactant (sodium dodecyl sulfate, SDS) are characterized by x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), ultraviolet-visible (UV-vis) absorption spectra. Moreover, the photocatalytic performances of the CuO samples are evaluated by the photo-degradation of a simulative contaminant methylene blue. The XRD patterns and FESEM images demonstrate that the category of surfactants have effects on the phase structure and morphology of CuO. Compared with bulk CuO (1.20 eV at room temperature), the band gap of CuO microspheres prepared with different surfactants including CTAB, PVP and SDS are measured at 2.16 eV, 2.29 eV, 2.44 eV, respectively, which exhibits a blue shift in the UV-vis spectra. The synthesized hierarchical self-assembled CuO hollow microspheres reveal commendable photocatalytic activity, in which the photo-degradation rate could rise to 94.1%. Additionally, a reasonable growth mechanism of CuO microspheres synthesized with different surfactants is discussed in detail.

Structure, glass transition temperature and spectroscopic properties of 10Li2O-xP2O5-(89-x)TeO2-1CuO (5≤x≤25 mol%) glass system.

PubMed

Upender, G; Babu, J Chinna; Mouli, V Chandra

2012-04-01

X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), energy dispersive X-ray spectrometry (EDS), differential scanning calorimetry (DSC), infrared (IR), Raman, electron paramagnetic resonance (EPR) and optical absorption studies on 10Li2O-xP2O5-(89-x)TeO2-1CuO glasses (where x=5, 10, 15, 20 and 25 mol%) have been carried out. The amorphous nature of the glasses was confirmed using XRD and FESEM measurements. The glass transition temperature (Tg) of glass samples have been estimated from DSC traces and found that the Tg increases with increasing P2O5 content. Both the IR and Raman studies have been showed that the present glass system consists of [TeO3], [TeO4], [PO3] and [PO4] units. The spin-Hamiltonian parameters such as g∥, g⊥, and A∥ have been determined from EPR spectra and it was found that the Cu2+ ion is present in tetragonal distorted octahedral site with [Formula: see text] as the ground state. Bonding parameters and bonding symmetry of Cu2+ ions have been calculated by correlating EPR and optical data and were found to be composition dependent. Copyright © 2012 Elsevier B.V. All rights reserved.

Effects of swift heavy ion irradiation on structural, optical and photocatalytic properties of ZnO–CuO nanocomposites prepared by carbothermal evaporation method

PubMed Central

Kuriakose, Sini; Avasthi, D K

2015-01-01

Summary ZnO–CuO nanocomposite thin films were prepared by carbothermal evaporation of ZnO and Cu, combined with annealing. The effects of 90 MeV Ni7+ ion irradiation on the structural and optical properties of ZnO–CuO nanocomposites were studied by using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), UV–visible absorption spectroscopy and Raman spectroscopy. XRD studies showed the presence of ZnO and CuO nanostructures in the nanocomposites. FESEM images revealed the presence of nanosheets and nanorods in the nanocomposites. The photocatalytic activity of ZnO–CuO nanocomposites was evaluated on the basis of degradation of methylene blue (MB) and methyl orange (MO) dyes under sun light irradiation and it was observed that swift heavy ion irradiation results in significant enhancement in the photocatalytic efficiency of ZnO–CuO nanocomposites towards degradation of MB and MO dyes. The possible mechanism for the enhanced photocatalytic activity of ZnO–CuO nanocomposites is proposed. We attribute the observed enhanced photocatalytic activity of ZnO–CuO nanocomposites to the combined effects of improved sun light utilization and suppression of the recombination of photogenerated charge carriers in ZnO–CuO nanocomposites. PMID:25977864

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

Hlaing, Nwe Ni, E-mail: nwenihlaing76@gmail.com; Department of International Development Engineering, Tokyo Institute of Technology, 2-12-1 Ookayama, Meguro-ku, Tokyo; Department of Physics, University of Yangon, 11041 Kamayut, Yangon

Recent years, CaO-based synthetic materials have been attracted attention as potential adsorbents for CO{sub 2} capture mainly due to their high CO{sub 2} adsorption capacity. In this study, micro/nanostructured aragonite CaCO{sub 3} was synthesized by a simple hydrothermal method with using polyacrylamide (PAM). The structural, morphological and thermal properties of the synthesized sample were investigated by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and thermogravimetry analysis (TG-DTA). The XRD and FESEM results showed that the obtained sample was aragonite CaCO{sub 3} with aggregated nanorods and microspheres composed of nanorods. A TG-DTA apparatus with Thermoplus 2 software was used tomore » investigate the effect of carbonation temperature on the CO{sub 2} adsorption capacity of CaO derived from aragonite CaCO{sub 3} sample. At 300 °C, the sample reached the CO{sub 2} adsorption capacity of 0.098 g-CO{sub 2}/g-adsorbent, whereas the sample achieved the highest capacity of 0.682 g-CO{sub 2}/g-adsorbent at 700 °C. The results showed that the carbonation temperature significantly influenced on the CO{sub 2} adsorption capacity of the CaO derived from aragonite CaCO{sub 3}.« less

Passive optical limiting studies of nanostructured Cu doped ZnO-PVA composite thin films

NASA Astrophysics Data System (ADS)

Tamgadge, Y. S.; Sunatkari, A. L.; Talwatkar, S. S.; Pahurkar, V. G.; Muley, G. G.

2016-01-01

We prepared undoped and Cu doped ZnO semiconducting nanoparticles (NPs) by chemical co-precipitation method and obtained Cu doped ZnO-polyvinyl alcohol (PVA) nanocomposite thin films by spin coating to investigate third order nonlinear optical and optical limiting properties under cw laser excitation. Powder samples of NPs were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive spectroscopy, transmission electron microscopy, ultraviolet-visible (UV-vis) and Fourier transform infrared spectroscopy. XRD pattern and FE-SEM micrograph revealed the presence of hexagonal wurtzite phase ZnO NPs having uniform morphology with average particle size of 20 nm. The presence of excitons and absorption peaks in the range 343-360 nm, revealed by UV-vis study, were attributed to excitons in n = 1 quantum state. Third order NLO properties of all composite thin films were investigated by He-Ne continuous wave (cw) laser of wavelength 632.8 nm using Z-scan technique. Thermally stimulated enhanced values of nonlinear refraction and absorption coefficients were obtained which may be attributed to self-defocusing effect, reverse saturable absorption, weak free carrier absorption and surface states properties originated from thermo optic effect. Optical limiting properties have been studied using cw diode laser of wavelength 808 nm and results are presented.

A study on photoelectrochemical properties of ZnO@ZnS nanostructures synthesized via facile ion-exchange approach

NASA Astrophysics Data System (ADS)

Sharma, Akash; Sahoo, Pooja; Thangavel, R.

2018-05-01

In this work, ZnO nanorods (NRs) were fabricated, on cleaned ITO substrates by using sol-gel spin coating followed by hydrothermal technique. In order to coat zinc sulphide (ZnS) layers on the earlier prepared NRs a facile ion-exchange approach was adopted. The ZnO@ZnS nanostructures so prepared were characterised by using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), UV-visible spectroscopy and photoelectrochemical study. XRD spectra confirmed the hexagonal wurtzite structure of all the samples along with preferential c-axis orientation. Further it was also observed from the FESEM images that sulfidation process doesn't affect the structure of ZnO NRs arrays. From the absorption spectra it can be clearly observed that the light absorbing property has increased in within the visible range due to the formation of ZnS layer on the ZnO nanostructures, which is not possible for either of the material individually. The cyclic voltammetry results indicates the enhancement in photocurrent density after illumination for the synthesized nanostructures. The electrocatalytic behaviour of ZnO@ZnS electrodes have been studied using a 3-electrode system in presence of 0.1M NaOH electrolyte solution with respect to an Ag/AgCl reference electrode.

Synthesis and structural characterization of magnetic cadmium sulfide-cobalt ferrite nanocomposite, and study of its activity for dyes degradation under ultrasound

NASA Astrophysics Data System (ADS)

Farhadi, Saeed; Siadatnasab, Firouzeh

2016-11-01

Cadmium sulfide-cobalt ferrite (CdS/CFO) nanocomposite was easily synthesized by one-step hydrothermal decomposition of cadmium diethyldithiocarbamate complex on the CoFe2O4 nanoparticles at 200 °C. Spectroscopic techniques of powder X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), UV-visible spectroscopy, field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), Brunauer-Emmett-Teller (BET), and magnetic measurements were applied for characterizing the structure and morphology of the product. The results of FT-IR, XRD and EDX indicated that the CdS/CFO was highly pure. SEM and TEM results revealed that the CdS/CFO nanocomposite was formed from nearly uniform and sphere-like nanoparticles with the size of approximately 20 nm. The UV-vis absorption spectrum of the CdS/CFO nanocomposite showed the band gap of 2.21 eV, which made it suitable for sono-/photo catalytic purposes. By using the obtained CdS/CFO nanocomposite, an ultrasound-assisted advanced oxidation process (AOP) has been developed for catalytic degradation of methylene blue (MB), Rhodamine B (RhB), and methyl orange (MO)) in the presence of H2O2 as a green oxidant. CdS/CFO nanocomposite exhibited excellent sonocatalytic activity, so that, dyes were completely degraded in less than 10 min. The influences of crucial factors such as the H2O2 amount and catalyst dosage on the degradation efficiency were evaluated. The as-prepared CdS/CFO nanocomposite exhibited higher catalytic activity than pure CdS nanoparticles. Moreover, the magnetic property of CoFe2O4 made the nanocomposite recyclable.

Synthesis, characterization, and hydrogen uptake studies of magnesium nanoparticles by solution reduction method

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

Rather, Sami ullah, E-mail: rathersami@gmail.com

2014-12-15

Graphical abstract: X-ray diffraction (XRD) pattern of magnesium nanoparticles synthesized by solution reduction method with and without TOPO. - Highlights: • Simple and convenient method of preparing Mg nanoparticles. • Characterized by XRD, SEM, FESEM and TEM. • Trioctylphosphine oxide offers a greater control over the size of the particles. • Hydrogen uptake of samples at different temperatures and pressure of 4.5 MPa. - Abstract: Facile and simple, surfactant-mediated solution reduction method was used to synthesize monodisperse magnesium nanoparticles. Little amount of magnesium oxide nanoparticles were also formed due to the presence of TOPO and easy oxidation of magnesium, eventhough,more » all precautions were taken to avoid oxidation of the sample. Precise size control of particles was achieved by carefully varying the concentration ratio of two different types of surfactants, – trioctylphosphine oxide and hexadecylamine. Recrystallized magnesium nanoparticle samples with and without TOPO were analyzed by X-ray diffraction, scanning electron microscope, field emission scanning electron microscope, and transmission electron microscope. The peak diameters of particles were estimated from size distribution analysis of the morphological data. The particles synthesized in the presence and absence of TOPO found to have diameters 46.5 and 34.8 nm, respectively. This observed dependence of particle size on the presence of TOPO offers a convenient method to control the particle size by simply using appropriate surfactant concentrations. Exceptional enhancement in hydrogen uptake and kinetics in synthesized magnesium nanoparticles as compared to commercial magnesium sample was due to the smaller particle size and improved morphology. Overall hydrogen uptake not affected by the little variation in particle size with and without TOPO.« less

Thinning of Large Biological Cells for Cryo-TEM Characterization by Cryo-FIB Milling

PubMed Central

Strunk, Korrinn M.; Ke, Danxia; Gray, Jennifer L.; Zhang, Peijun

2013-01-01

SUMMARY Focused ion beam milling at cryogenic temperatures (cryo-FIB) is a valuable tool that can be used to thin vitreous biological specimens for subsequent imaging and analysis in a cryo-transmission electron microscope (cryo-TEM) in their frozen-hydrated state. This technique offers the potential benefit of eliminating the mechanical artifacts that are typically found with cryo-ultramicrotomy. However, due to the additional complexity in transferring samples in and out of the FIB, contamination and devitrification of the amorphous ice is commonly encountered. In order to address these problems, we have designed a new sample cryo-shuttle that specifically accepts Polara TEM cartridges directly in order to simplify the transfer process between the FIB and TEM. We used the quality of the ice in the sample as an indicator to test various parameters used the process, and demonstrated with successful milling of large mammalian cells. By comparing the results from larger HeLa cells to those from E. coli cells, we discuss some of the artifacts and challenges we have encountered using this technique. PMID:22906009

TEM in situ micropillar compression tests of ion irradiated oxide dispersion strengthened alloy

NASA Astrophysics Data System (ADS)

Yano, K. H.; Swenson, M. J.; Wu, Y.; Wharry, J. P.

2017-01-01

The growing role of charged particle irradiation in the evaluation of nuclear reactor candidate materials requires the development of novel methods to assess mechanical properties in near-surface irradiation damage layers just a few micrometers thick. In situ transmission electron microscopic (TEM) mechanical testing is one such promising method. In this work, microcompression pillars are fabricated from a Fe2+ ion irradiated bulk specimen of a model Fe-9%Cr oxide dispersion strengthened (ODS) alloy. Yield strengths measured directly from TEM in situ compression tests are within expected values, and are consistent with predictions based on the irradiated microstructure. Measured elastic modulus values, once adjusted for the amount of deformation and deflection in the base material, are also within the expected range. A pillar size effect is only observed in samples with minimum dimension ≤100 nm due to the low inter-obstacle spacing in the as received and irradiated material. TEM in situ micropillar compression tests hold great promise for quantitatively determining mechanical properties of shallow ion-irradiated layers.

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

PubMed

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

2017-01-01

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

Evolution of the substructure of a novel 12% Cr steel under creep conditions

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

Yadav, Surya Deo, E-mail: surya.yadav@tugraz.at; Kalácska, Szilvia, E-mail: kalacska@metal.elte.hu; Dománková, Mária, E-mail: maria.domankova@stuba.sk

2016-05-15

In this work we study the microstruture evolution of a newly developed 12% Cr martensitic/ferritic steel in as-received condition and after creep at 650 °C under 130 MPa and 80 MPa. The microstructure is described as consisting of mobile dislocations, dipole dislocations, boundary dislocations, precipitates, lath boundaries, block boundaries, packet boundaries and prior austenitic grain boundaries. The material is characterized employing light optical microscopy (LOM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). TEM is used to characterize the dislocations (mobile + dipole) inside the subgrains and XRD measurements are used tomore » the characterize mobile dislocations. Based on the subgrain boundary misorientations obtained from EBSD measurements, the boundary dislocation density is estimated. The total dislocation density is estimated for the as-received and crept conditions adding the mobile, boundary and dipole dislocation densities. Additionally, the subgrain size is estimated from the EBSD measurements. In this publication we propose the use of three characterization techniques TEM, XRD and EBSD as necessary to characterize all type of dislocations and quantify the total dislocation densty in martensitic/ferritic steels. - Highlights: • Creep properties of a novel 12% Cr steel alloyed with Ta • Experimental characterization of different types of dislocations: mobile, dipole and boundary • Characterization and interpretation of the substructure evolution using unique combination of TEM, XRD and EBSD.« less

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

NASA Astrophysics Data System (ADS)

Johns, Steve; Shin, Wontak; Kane, Joshua J.; Windes, William E.; Ubic, Rick; Karthik, Chinnathambi

2018-07-01

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. To ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ∼60 μm. Discs 3 mm in diameter were then oxidized at temperatures between 575 °C and 625 °C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575 °C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

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

Johns, Steve; Shin, Wontak; Kane, Joshua J.

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

DOE PAGES

Johns, Steve; Shin, Wontak; Kane, Joshua J.; ...

2018-04-03

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

X-Ray Diffraction (XRD) Characterization Methods for Sigma=3 Twin Defects in Cubic Semiconductor (100) Wafers

NASA Technical Reports Server (NTRS)

Park, Yeonjoon (Inventor); Kim, Hyun Jung (Inventor); Skuza, Jonathan R. (Inventor); Lee, Kunik (Inventor); Choi, Sang Hyouk (Inventor); King, Glen C. (Inventor)

2017-01-01

An X-ray defraction (XRD) characterization method for sigma=3 twin defects in cubic semiconductor (100) wafers includes a concentration measurement method and a wafer mapping method for any cubic tetrahedral semiconductor wafers including GaAs (100) wafers and Si (100) wafers. The methods use the cubic semiconductor's (004) pole figure in order to detect sigma=3/{111} twin defects. The XRD methods are applicable to any (100) wafers of tetrahedral cubic semiconductors in the diamond structure (Si, Ge, C) and cubic zinc-blend structure (InP, InGaAs, CdTe, ZnSe, and so on) with various growth methods such as Liquid Encapsulated Czochralski (LEC) growth, Molecular Beam Epitaxy (MBE), Organometallic Vapor Phase Epitaxy (OMVPE), Czochralski growth and Metal Organic Chemical Vapor Deposition (MOCVD) growth.

Appraisal of an Array TEM Method in Detecting a Mined-Out Area Beneath a Conductive Layer

NASA Astrophysics Data System (ADS)

Li, Hai; Xue, Guo-qiang; Zhou, Nan-nan; Chen, Wei-ying

2015-10-01

The transient electromagnetic method has been extensively used for the detection of mined-out area in China for the past few years. In the cases that the mined-out area is overlain by a conductive layer, the detection of the target layer is difficult with a traditional loop source TEM method. In order to detect the target layer in this condition, this paper presents a newly developed array TEM method, which uses a grounded wire source. The underground current density distribution and the responses of the grounded wire source TEM configuration are modeled to demonstrate that the target layer is detectable in this condition. The 1D OCCAM inversion routine is applied to the synthetic single station data and common middle point gather. The result reveals that the electric source TEM method is capable of recovering the resistive target layer beneath the conductive overburden. By contrast, the conductive target layer cannot be recovered unless the distance between the target layer and the conductive overburden is large. Compared with inversion result of the single station data, the inversion of common middle point gather can better recover the resistivity of the target layer. Finally, a case study illustrates that the array TEM method is successfully applied in recovering a water-filled mined-out area beneath a conductive overburden.

Effectiveness of Shield Termination Techniques Tested with TEM Cell and Bulk Current Injection

NASA Technical Reports Server (NTRS)

Bradley, Arthur T.; Hare, Richard J.

2009-01-01

This paper presents experimental results of the effectiveness of various shield termination techniques. Each termination technique is evaluated by two independent noise injection methods; transverse electromagnetic (TEM) cell operated from 3 MHz 400 MHz, and bulk current injection (BCI) operated from 50 kHz 400 MHz. Both single carrier and broadband injection tests were investigated. Recommendations as to how to achieve the best shield transfer impedance (i.e. reduced coupled noise) are made based on the empirical data. Finally, the noise injection techniques themselves are indirectly evaluated by comparing the results obtained from the TEM Cell to those from BCI.

A Structural Study of Escherichia coli Cells Using an In Situ Liquid Chamber TEM Technology.

PubMed

Wang, Yibing; Chen, Xin; Cao, Hongliang; Deng, Chao; Cao, Xiaodan; Wang, Ping

2015-01-01

Studying cell microstructures and their behaviors under living conditions has been a challenging subject in microbiology. In this work, in situ liquid chamber TEM was used to study structures of Escherichia coli cells in aqueous solutions at a nanometer-scale resolution. Most of the cells remained intact under electron beam irradiation, and nanoscale structures were observed during the TEM imaging. The analysis revealed structures of pili surrounding the E. coli cells; the movements of the pili in the liquid were also observed during the in situ tests. This technology also allowed the observation of features of the nucleoid in the E. coli cells. Overall, in situ TEM can be applied as a valuable tool to study real-time microscopic structures and processes in microbial cells residing in native aqueous solutions.

TEM Pump With External Heat Source And Sink

NASA Technical Reports Server (NTRS)

Nesmith, Bill J.

1991-01-01

Proposed thermoelectric/electromagnetic (TEM) pump driven by external source of heat and by two or more heat pipe radiator heat sink(s). Thermoelectrics generate electrical current to circulate liquid metal in secondary loop of two-fluid-loop system. Intended for use with space and terrestrial dual loop liquid metal nuclear reactors. Applications include spacecraft on long missions or terrestrial beacons or scientific instruments having to operate in remote areas for long times. Design modified to include multiple radiators, converters, and ducts, as dictated by particular application.

Trace elemental analysis of Indian natural moonstone gems by PIXE and XRD techniques.

PubMed

Venkateswara Rao, R; Venkateswarulu, P; Kasipathi, C; Sivajyothi, S

2013-12-01

A selected number of Indian Eastern Ghats natural moonstone gems were studied with a powerful nuclear analytical and non-destructive Proton Induced X-ray Emission (PIXE) technique. Thirteen elements, including V, Co, Ni, Zn, Ga, Ba and Pb, were identified in these moonstones and may be useful in interpreting the various geochemical conditions and the probable cause of their inceptions in the moonstone gemstone matrix. Furthermore, preliminary XRD studies of different moonstone patterns were performed. The PIXE technique is a powerful method for quickly determining the elemental concentration of a substance. A 3MeV proton beam was employed to excite the samples. The chemical constituents of moonstones from parts of the Eastern Ghats geological formations of Andhra Pradesh, India were determined, and gemological studies were performed on those gems. The crystal structure and the lattice parameters of the moonstones were estimated using X-Ray Diffraction studies, trace and minor elements were determined using the PIXE technique, and major compositional elements were confirmed by XRD. In the present work, the usefulness and versatility of the PIXE technique for research in geo-scientific methodology is established. © 2013 Elsevier Ltd. All rights reserved.

Facile synthesis of GO@SnO2/TiO2 nanofibers and their behavior in photovoltaics.

PubMed

Mohamed, Ibrahim M A; Dao, Van-Duong; Yasin, Ahmed S; Choi, Ho-Suk; Khalil, KhalilAbdelrazek; Barakat, Nasser A M

2017-03-15

Chemical doping is a widely-used strategy to improve the performance of TiO 2 for the dye-sensitized solar cells (DSCs). However, the effect of two efficient dopants has been rarely investigated. We present the synthesis of GO@SnO 2 /TiO 2 nanofibers (NFs) by a facile method using electrospinning and hydrothermal processes. The synthesized NFs are described in terms of morphology, crystallinity and chemistry through FESEM, TEM, HR-TEM, XRD, EDX, XPS, FT-IR and Raman spectra. As the results, the axial ratio and the average diameter of NFs decreased after the hydrothermal treatment and calcination process, respectively. The prepared Titania-based nanofibers have 81.82% anatase and 18.18% rutile-structure. The developed materials are applied as working electrodes of DSCs. The photovoltaic performances showed that the efficiency of the device employed GO@SnO 2 /TiO 2 photoanode gave 5.41%, which was higher than those of cells fabricated with SnO 2 /TiO 2 NFs (3.41%) and GO@TiO 2 NFs (4.52%) photoanodes. The photovoltaic parameters such as J sc , V oc , FF and R ct are calculated and found to be 11.19mAcm -2 , 0.72V, 0.67 and 9.26Ω, respectively. The high photovoltaic response of DSC based of GO@SnO 2 /TiO 2 NFs may be attributed to the large surface area of the NFs, and the low electron recombination. Furthermore, the start-stop switches of the cell devices with the developed photoanode affirmed the stability and photovoltaic performance of the cell. Copyright © 2016 Elsevier Inc. All rights reserved.

Extracellular red Monascus pigment-mediated rapid one-step synthesis of silver nanoparticles and its application in biomedical and environment.

PubMed

Koli, Sunil H; Mohite, Bhavana V; Suryawanshi, Rahul K; Borase, Hemant P; Patil, Satish V

2018-05-01

The development of a safe and eco-friendly method for metal nanoparticle synthesis has an increasing demand, due to emerging environmental and biological harms of hazardous chemicals used in existing nanosynthesis methods. The present investigation reports a rapid one-step, eco-friendly and green approach for the formation of nanosized silver particles (AgNPs) using extracellular non-toxic-colored fungal metabolites (Monascus pigments-MPs). The formation of nanosized silver particles utilizing Monascus pigments was confirmed after exposure of reaction mixture to sunlight, by visually color change and further established by spectrophotometric analysis. The size, shape, and topography of synthesized MPs-AgNPs were well-defined using different microscopic and spectroscopic techniques, i.e., FE-SEM, HR-TEM, and DLS. The average size of MPs-AgNPs was found to be 10-40 nm with a spherical shape which was highly stable and dispersed in the solution. HR-TEM and XRD confirmed crystalline nature of MPs-AgNPs. The biocidal potential of MPs-AgNPs was evaluated against three bacterial pathogens such as Pseudomonas aeruginosa, Escherichia coli, and Staphylococcus aureus and it was observed that the MPs-AgNPs significantly inhibited the growth of all three bacterial pathogens. The anti-biofilm activity of MPs-AgNPs was recorded against antibiotic-resistant P. aeruginosa. Besides, the colorimetric metal sensing using MPs-AgNPs was studied. Among the metals tested, the selective Hg 2+ -sensing potential at micromolar concentration was observed. In conclusion, this is the rapid one-step (within 12-15 min), environment-friendly method for synthesis of AgNPs and synthesized MPs-AgNPs could be used as a potential antibacterial agent against antibiotic-resistant bacterial pathogens.

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

NASA Astrophysics Data System (ADS)

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

Post Irradiation TEM Investigation of ZrN Coated U(Mo) Particles Prepared with FIB

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

Van Renterghem, W.; Leenaers, A.; Van den Berghe, S.

2015-10-01

In the framework of the Selenium project, two dispersion fuel plates were fabricated with Si and ZrN coated fuel particles and irradiated in the Br2 reactor of SCK•CEN to high burn-up. The first analysis of the irradiated plate proved the reduced swelling of the fuel plate and interaction layer growth up to 70% burn-up. The question was raised how the structure of the interaction layer had been affected by the irradiation and how the structure of the fuel particles had evolved. Hereto, samples from the ZrN coated UMo particles were prepared for transmission electron microscopy (TEM) using focused ion beammore » milling (FIB) at INL. The FIB technique allowed to precisely select the area of the interaction layer and/or fuel to produce a sample that is TEM transparent over an area of 20 by 20 µm. In this contribution, the first TEM results will be presented from the 66% burn-up sample.« less

GISAXS modelling of helium-induced nano-bubble formation in tungsten and comparison with TEM

NASA Astrophysics Data System (ADS)

Thompson, Matt; Sakamoto, Ryuichi; Bernard, Elodie; Kirby, Nigel; Kluth, Patrick; Riley, Daniel; Corr, Cormac

2016-05-01

Grazing-incidence small angle x-ray scattering (GISAXS) is a powerful non-destructive technique for the measurement of nano-bubble formation in tungsten under helium plasma exposure. Here, we present a comparative study between transmission electron microscopy (TEM) and GISAXS measurements of nano-bubble formation in tungsten exposed to helium plasma in the Large Helical Device (LHD) fusion experiment. Both techniques are in excellent agreement, suggesting that nano-bubbles range from spheroidal to ellipsoidal, displaying exponential diameter distributions with mean diameters μ=0.68 ± 0.04 nm and μ=0.6 ± 0.1 nm measured by TEM and GISAXS respectively. Depth distributions were also computed, with calculated exponential depth distributions with mean depths of 8.4 ± 0.5 nm and 9.1 ± 0.4 nm for TEM and GISAXS. In GISAXS modelling, spheroidal particles were fitted with an aspect ratio ε=0.7 ± 0.1. The GISAXS model used is described in detail.

Thermal behavior of polyhalite: a high-temperature synchrotron XRD study

DOE PAGES

Xu, Hongwu; Guo, Xiaofeng; Bai, Jianming

2016-09-17

As an accessory mineral in marine evaporites, polyhalite, K 2MgCa 2(SO 4) 4·2H 2O, coexists with halite (NaCl) in salt formations, which have been considered as potential repositories for permanent storage of high-level nuclear wastes. However, because of the heat generated by radioactive decays in the wastes, polyhalite may dehydrate, and the released water will dissolve its neighboring salt, potentially affecting the repository integrity. Thus, studying the thermal behavior of polyhalite is important. In this paper, a polyhalite sample containing a small amount of halite was collected from the Salado formation at the WIPP site in Carlsbad, New Mexico. Tomore » determine its thermal behavior, in situ high-temperature synchrotron X-ray diffraction was conducted from room temperature to 1066 K with the sample powders sealed in a silica-glass capillary. At about 506 K, polyhalite started to decompose into water vapor, anhydrite (CaSO 4) and two langbeinite-type phases, K 2Ca x Mg 2-x (SO 4) 3, with different Ca/Mg ratios. XRD peaks of the minor halite disappeared, presumably due to its dissolution by water vapor. With further increasing temperature, the two langbeinite solid solution phases displayed complex variations in crystallinity, composition and their molar ratio and then were combined into the single-phase triple salt, K 2CaMg(SO 4) 3, at ~919 K. Rietveld analyses of the XRD data allowed determination of structural parameters of polyhalite and its decomposed anhydrite and langbeinite phases as a function of temperature. Finally, from the results, the thermal expansion coefficients of these phases have been derived, and the structural mechanisms of their thermal behavior been discussed.« less

(S)TEM analysis of functional transition metal oxides

NASA Astrophysics Data System (ADS)

Chi, Miaofang

Perovskite vanadates (AVO3) form an ideal family to study the structure-property relationships in transition metal oxides because their physical properties can easily be tailored by varying the A-site cations. (S)TEM is an ideal tool for this type of study due to its capacity for simultaneous imaging and chemical analysis. Determination of the oxidation state of vanadium in complex oxides have been carried out by electron energy loss spectroscopy. SrVO3/LaAlO3 is then studied both experimentally and theoretically as a prototype system. Extra electrons have been detected on the interface layer, and further proven to originate mainly from a change in the local bonding configuration of V at the La-O terminated substrate surface. Cr-containing stainless steel deposited with a LaCrO3 thin-film layer is a promising interconnect material of Solid Oxide Fuel Cells (SOFC). Our investigation on its microstructural evolution reveals that the LaCrO 3 thin film plays a role in inhibiting the growth of an oxide layer on the metal surface and thus protects the surface of the stainless steel. Ca-doped LaCoO3 is a promising SOFC cathode material. The domain structures and the oxidation state of Co in Ca-doped LaCoO3, which are directly related to its mechanical properties and electronic conductivity, are investigated by in-situ TEM and EELS. The formation of microcracks is observed during thermal cycles. Ca-doping in LaCoO3 is shown to not only improve the electronic conductivity of the material, but is also likely to strengthen the grain boundaries. The realization of its application in SOFCs depends on depressing the ferroelastisity to reduce strain formation during thermal cycles. The application of the (S)TEM techniques used for studying the perovskite systems are further extended to other compounds containing transition metal elements. The refractory minerals from Comet 81 P/Wild-2 are studied to investigate the formation of the early solar system. A relatively high Ti3+/Ti 4

Synthesis and structural properties of Ba(1-x)LaxTiO3 perovskite nanoparticles fabricated by solvothermal synthesis route

NASA Astrophysics Data System (ADS)

Puli, Venkata Sreenivas; Adireddy, Shiva; Elupula, Ravinder; Molugu, Sudheer; Shipman, Josh; Chrisey, Douglas B.

2017-05-01

We report the successful synthesis and structural characterization of barium lanthanum titanate Ba(1-x)LaxTiO3 (x=0.003,0.006,0.010) nanoparticles. The colloidal nanoparticles were prepared with high yield by a solvothermal method at temperatures as low as 150°C for 24h. The as-prepared nanopowders were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. The XRD studies revealed pseudo-cubic crystalline structure, with no impurity phases at room temperature. However ferroelectric tetragonal modes were clearly observed using Raman spectroscopy measurements. From TEM measurements, uniformly sized BLT nanoparticles were observed. Selected area diffraction TEM images revealed polycrystalline perovskite ring patterns, identified as corresponding to the tetragonal phase.

TEM characterization of a silorane composite bonded to enamel/dentin.

PubMed

Mine, Atsushi; De Munck, Jan; Van Ende, Annelies; Cardoso, Marcio Vivan; Kuboki, Takuo; Yoshida, Yasuhiro; Van Meerbeek, Bart

2010-06-01

The low-shrinking composite composed of combined siloxane-oxirane technology (Filtek Silorane, 3M ESPE, Seefeld, Germany) required the development of a specific adhesive (Silorane System Adhesive, 3M ESPE), in particular because of the high hydrophobicity of the silorane composite. The purpose of this study was to characterize the interfacial ultra-structure at enamel and dentin using transmission electron microscopy (TEM). Non-demineralized/demineralized 70-90 nm sections were prepared following common TEM specimen processing procedures. TEM revealed a typical twofold build-up of the adhesive resin, resulting in a total adhesive layer thickness of 10-20 microm. At bur-cut enamel, a tight interface without distinct dissolution of hydroxyapatite was observed. At bur-cut dentin, a relatively thin hybrid layer of maximum a few hundreds of nanometer was formed without clear surface demineralization. No clear resin tags were formed. At fractured dentin, the interaction appeared very superficial (100-200 nm). Distinct resin tags were formed due to the absence of smear plugs. Silver-nitrate infiltration showed a varying pattern of both spot- and cluster-like appearance of nano-leakage. Traces of Ag were typically detected along some part of the enamel-adhesive interface and/or between the two adhesive resin layers. Substantially more Ag-infiltration was observed along the dentin-adhesive interface of bur-cut dentin, as compared to that of fractured dentin. The nano-interaction of Silorane System Adhesive should be attributed to its relatively high pH of 2.7. The obtained tight interface at both enamel and dentin indicates that the two-step self-etch adhesive effectively bridged the hydrophilic tooth substrate with the hydrophobic silorane composite. Copyright (c) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Studies of antibacterial efficacy of different biopolymer protected silver nanoparticles synthesized under reflux condition

NASA Astrophysics Data System (ADS)

Su, Chia Hung; Velusamy, Palaniyandi; Kumar, Govindarajan Venkat; Adhikary, Shritama; Pandian, Kannaiyan; Anbu, Periyasamy

2017-01-01

In the present study, a simple method to impregnate silver nanoparticles (AgNPs) into carboxymethyl cellulose (CMC) and sodium alginate (SA) is reported for the first time. Single step synthesis of carboxymethyl cellulose (CMC) and sodium alginate (SA) biopolymer protected silver nanoparticles (AgNPs) using aniline as a reducing agent under reflux conditions was investigated. The synthesized nanoparticles were characterized by UV-Vis spectrophotometry, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and field emission scanning electron microscopy (FESEM). The FESEM results of CMC@AgNPs and SA@AgNPs showed the formation of spherical nanoparticles sized 30-60 nm. Testing of the antibiofilm efficacy of the polymer protected AgNPs against different bacterial strains such as Klebsiella pneumoniae MTCC 4032 and Streptococcus pyogenes MTCC 1924 revealed that the biopolymer protected AgNPs had excellent antibiofilm activity.

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

PubMed

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.

XRD and EBSD analysis of anisotropic microstructure development in cold rolled F138 stainless steel

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

De Vincentis, N.S., E-mail: devincentis@ifir-conic

The microstructural characteristics of deformation-processed materials highly influence their mechanical properties. For a complete characterization of a microstructure both local and global information must be gathered, which requires the combination of different analysis techniques. X-ray and Electron Backscatter Diffraction were used in the present paper to characterize the deformation induced in a cold rolled F138 austenitic stainless steel sample. The results obtained using laboratory and synchrotron X-ray sources were compared and combined with EBSD quantitative results, allowing the global and local characterization and orientation dependence of the deformation microstructure. A particular behavior was observed in the XRD data corresponding tomore » the planes with < 220 >∥ ND, likely due to a smaller amount of defects accumulated in the crystals with that particular orientation. EBSD was used to separate the scans data into partitions and to calculate misorientation variables and parameters, showing that this behavior can be attributed to a combination of larger grain sizes, lower local boundary misorientations and dislocation densities for crystals having < 220 >∥ ND. Several conclusions, of general validity for the evaluation of microstructure anisotropy, can be extracted from the results. - Highlights: •Combined XRD and EBSD for studying microstructure gave a superb insight on anisotropic accumulation of defects. •W-H and CMWP methods were applied for checking consistency of results. •XRD showed that a smaller accumulation of defects occurred in crystals with < 220 >∥ ND. •High brilliance X-ray beam allowed to study the anisotropy of defect accumulation.« less

Simulation and analysis of the effect of ungrounded rectangular loop distributed parameters on TEM response

NASA Astrophysics Data System (ADS)

Shi, Zongyang; Liu, Lihua; Xiao, Pan; Geng, Zhi; Liu, Fubo; Fang, Guangyou

2018-02-01

An ungrounded loop in the shallow subsurface transient electromagnetic surveys has been studied as the transmission line model for early turn-off stage, which can accurately explicate the early turn-off current waveform inconsistency along the loop. In this paper, the Gauss-Legendre numerical integration method is proposed for the first time to simulate and analyze the transient electromagnetic (TEM) response considering the different early turn-off current waveforms along the loop. During the simulation, these integral node positions along the loop are firstly determined by solving these zero points of Legendre polynomial, then the turn-off current of each node position is simulated by using the transfer function of the transmission line. Finally, the total TEM response is calculated by using the Gauss-Legendre integral formula. In addition, the comparison and analysis between the results affected by the distributed parameters and that generated by lumped parameters are presented. It is found that the TEM responses agree well with each other after current is thoroughly switched off, while the transient responses in turn-off stage are completely different. It means that the position dependence of the early turn-off current should be introduced into the forward model during the early response data interpretation of the shallow TEM detection of the ungrounded loop. Furthermore, the TEM response simulations at four geometric symmetry points are made. It shows that early responses of different geometric symmetry points are also inconsistent. The research on the influence of turn-off current position dependence on the early response of geometric symmetry point is of great significance to guide the layout of the survey lines and the transmitter location.

TEM-187, a new extended-spectrum β-lactamase with weak activity in a Proteus mirabilis clinical strain.

PubMed

Corvec, Stéphane; Beyrouthy, Racha; Crémet, Lise; Aubin, Guillaume Ghislain; Robin, Frédéric; Bonnet, Richard; Reynaud, Alain

2013-05-01

A Proteus mirabilis clinical strain (7001324) was isolated from urine sample of a patient hospitalized in a long-term-care facility. PCR and cloning experiments performed with this strain identified a novel TEM-type β-lactamase (TEM-187) differing by four amino acid substitutions (Leu21Phe, Arg164His, Ala184Val, and Thr265Met) from TEM-1. This characterization provides further evidence for the diversity of extended-spectrum β-lactamases (ESBL) produced by P. mirabilis and for their potential spread to other Enterobacteriaceae due to a lack of sensitive detection methods used in daily practice.

In-situ XRD and EDS method study on the oxidation behaviour of Ni-Cu sulphide ore.

PubMed

Li, Guangshi; Cheng, Hongwei; Xiong, Xiaolu; Lu, Xionggang; Xu, Cong; Lu, Changyuan; Zou, Xingli; Xu, Qian

2017-06-12

The oxidation mechanism of sulfides is the key issue during the sulphide-metallurgy process. In this study, the phase transformation and element migration were clearly demonstrated by in-situ laboratory-based X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS), respectively. The reaction sequence and a four-step oxidation mechanism were proposed and identified. The elemental distribution demonstrated that at a low temperature, the Fe atoms diffused outward and the Ni/Cu atoms migrated toward the inner core, whereas the opposite diffusion processes were observed at a higher temperature. Importantly, the unique visual presentation of the oxidation behaviour provided by the combination of in-situ XRD and EDS might be useful for optimising the process parameters to improve the Ni/Cu extraction efficiency during Ni-Cu sulphide metallurgy.

Synthesis of nano-sized ZnO particles by co-precipitation method with variation of heating time

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

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro

Zinc oxide powders have been synthesized by a co-precipitation method at low temperature (85 °C), using zinc acetate dihydrate, ammonia, hydrochloric acid solutions as the reactants. A number of process parameters such as reaction temperature, solution basicity or pH and heating time are the main factors affecting the morphology and physical properties of the ZnO nanostructures. In this work the effect of heating time on the morphology and particles size were studied. The as-synthesized ZnO powders were characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The samples were also analyzed using Fourier transform infrared (FTIR). Rietveld refinementmore » of XRD data confirms that ZnO crystallizes in the hexagonal wurtzite structure with high degree of purity and the (101) plane predominant. The XRD results show that the average crystallite sizes were about 66, 27 and 12 nm for 3, 4 and 5 h of heating times, respectively. The XRD analysis indicated that a fraction of nano-sized ZnO powders were in the form of aggregates, which was also verified by TEM image. The TEM photograph demonstrated that the nano-sized ZnO particles were a pseudo-spherical shape.« less

Effect of sample moisture content on XRD-estimated cellulose crystallinity index and crystallite size

Treesearch

Umesh P. Agarwal; Sally A. Ralph; Carlos Baez; Richard S. Reiner; Steve P. Verrill

2017-01-01

Although X-ray diffraction (XRD) has been the most widely used technique to investigate crystallinity index (CrI) and crystallite size (L200) of cellulose materials, there are not many studies that have taken into account the role of sample moisture on these measurements. The present investigation focuses on a variety of celluloses and cellulose...

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

NASA Astrophysics Data System (ADS)

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.

A novel functional domain of Cdc15 kinase is required for its interaction with Tem1 GTPase in Saccharomyces cerevisiae.

PubMed Central

Asakawa, K; Yoshida, S; Otake, F; Toh-e, A

2001-01-01

Exit from mitosis requires the inactivation of cyclin-dependent kinase (CDK) activity. In the budding yeast Saccharomyces cerevisiae, a number of gene products have been identified as components of the signal transduction network regulating inactivation of CDK (called the MEN, for the mitotic exit network). Cdc15, one of such components of the MEN, is an essential protein kinase. By the two-hybrid screening, we identified Cdc15 as a binding protein of Tem1 GTPase, another essential regulator of the MEN. Coprecipitation experiments revealed that Tem1 binds to Cdc15 in vivo. By deletion analysis, we found that the Tem1-binding domain resides near the conserved kinase domain of Cdc15. The cdc15-LF mutation, which was introduced into the Tem1-binding domain, reduced the interaction with Cdc15 and Tem1 and caused temperature-sensitive growth.The kinase activity of Cdc15 was not so much affected by the cdc15-LF mutation. However, Cdc15-LF failed to localize to the SPB at the restrictive temperature. Our data show that the interaction with Tem1 is important for the function of Cdc15 and that Cdc15 and Tem1 function in a complex to direct the exit from mitosis. PMID:11290702

High temperature XRD of Cu2GeSe3

NASA Astrophysics Data System (ADS)

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

2015-06-01

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