Pt nanoparticle on La0.02Na0.98TaO3 catalyst for hydrogen evolution from glycerol aqueous solution

NASA Astrophysics Data System (ADS)

Husin, Husni; Adisalamun, Sy, Yuliana; Asnawi, Teku Muhammad; Hasfita, Fikri

2017-01-01

Pt nanoparticles on La-doped sodium tantalum oxide (La0.02Na0.98TaO3), which acts as an active co-catalyst for H2 evolution under UV light irradiation was successfully synthesized by photo-deposition method. The La0.02Na0.98TaO3 photocatalyst was obtained by the reaction of La(NO3)2.3H2O, TaCl5, and NaOH at ambient temperature. The catalyst produced was characterized by a scanning electron microscope (SEM) and a high-resolution transmission electron microscope (HRTEM). SEM images of the La0.02Na0.98TaO3 sample showing that its particles size is ranging between 50-150 nm. The Pt particles are detected from HRTEM images is around 2-4 nm. The Pt/La0.02Na0.98TaO3 samples prepared were applied for photocatalytic H2 production at 30°C. The photocatalyst performance was evaluated for hydrogen production from water combining with glycerol as an electron donor (sacrificial reagent). The reactions were carried out in a closed reactor with a gas circulation system, illuminated with mercury (Hg) lamp. The experimental results show that the presence of glycerol in the systems can not only improve the efficiency of photocatalytic hydrogen generation but can also be decomposed to hydrogen efficiently. The photocatalytic activity of La0.02Na0.98TaO3 is significantly enhanced when Pt was loaded onto its crystalline surface.

Particle Morphology From Wood-Burning Cook Stoves Emissions

NASA Astrophysics Data System (ADS)

Peralta, O.; Carabali, G.; Castro, T.; Torres, R.; Ruiz, L. G.; Molina, L. T.; Saavedra, I.

2013-12-01

Emissions from three wood-burning cook stoves were sampled to collect particles. Transmission electron microscope (TEM) copper grids were placed on the last two stages of an 8-stage MOUDI cascade impactor (d50= 0.32, and 0.18 μm). Samples were obtained on two heating stages of cooking, the first is a quick heating process to boil 1 liter of water, and the second is to keep the water at 90 C. Absorption coefficient, scattering coefficients, and particles concentration (0.01 - 2.5 μm aerodynamic diameter) were measured simultaneously using an absorption photometer (operated at 550 nm), a portable integrating nephelometer (at 530 nm), and a condensation particle counter connected to a chamber to dilute the wood stoves emissions. Transmission electron micrographic images of soot particles were acquired at different magnifications using a High Resolution Transmission Electron Microscope (HRTEM) JEOL HRTEM 4000EX operating at 200 kV, equipped with a GATAN digital micrograph system for image acquisition. The morphology of soot particles was analyzed calculating the border-based fractal dimension (Df). Particles sampled on the first heating stage exhibit complex shapes with high values of Df, which are present as aggregates formed by carbon ceno-spheres. The presence of high numbers of carbon ceno-spheres can be attributed to pyrolysis, thermal degradation, and others processes prior to combustion. Energy dispersive X-ray spectroscopy (EDS) was used to determine the elemental composition of particles. EDS analysis in particles with d50= 0.18 μm showed a higher content of carbonaceous material and relevant amounts of Si, S and K.

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.

Bio-inspired sustainable and green synthesis of plasmonic Ag/AgCl nanoparticles for enhanced degradation of organic compound from aqueous phase.

PubMed

Devi, Th Babita; Ahmaruzzaman, M

2016-09-01

In the current study, we report the utilization of the biogenic potential of Benincasa hispida (ash gourd) peel extract for the synthesis of Ag embedded AgCl nanoparticles nanoparticles (Ag/AgCl NPs) without the use of any external organic solvents. The appearance of dark brown color from the pale yellow color confirmed the formation of Ag/AgCl nanoparticles which was further validated by absorbance peak using UV-visible spectroscopy. The phytochemicals (flavones) present in the B. hispida peel extract acts as a reducing/stabilizing agents. The morphology and size of the synthesized NPs were characterized by transmission electron microscope (TEM), selected area electron microscope (SAED) and high resolution transmission electron microscope (HR-TEM). FT-IR spectra of the B. hispida peel extract and after the development of nanoparticles are determined to identify the functional groups responsible for the conversion of metal ions to metal nanoparticles. The synthesized nanoparticles showed an excellent photocatalytic property in the degradation of toxic dye like malachite green oxalate under sunlight irradiation. For the first time, malachite green oxalate dye was degraded by Ag/AgCl nanoparticles under sunlight irradiation.

Controlling dispersion of graphene nanoplatelets in aqueous solution by ultrasonic technique

NASA Astrophysics Data System (ADS)

Wang, Baomin; Jiang, Ruishuang; Song, Wanzeng; Liu, Hui

2017-08-01

The homogenous graphene nanoplatelets (GNP) suspension had been prepared through ultrasonic exfoliation in the presence of methylcellulose (MC) as dispersant. The influence of different sonication times on dispersing of aqueous GNP suspension was monitored by UV-Vis absorbance, sedimentation test, optical microscope and transmission electron microscope (TEM). The study of UV-Vis absorbance verifies that the minimum sonication time to break the 0.1 g/L concentration of bundled GNPs is 20 min; furthermore, the GNP suspension achieved the best dispersion, when sonication time increased up to 80 min. From optical microscope images of GNPs, the agglomeration of GNPs was broken by enough sonication energy, and the distribution of GNPs particles became more uniform. The dispersing mechanism had been discussed and simulated by HRTEM image. The bundled GNPs were exfoliated by cavitation effect of ultrasonic irradiation, meanwhile, the dispersant adsorbed on the surface of GNPs prevented re-entanglement by forming steric hindrance.

Nanoscale characterization of the thermal interface resistance of a heat-sink composite material by in situ TEM.

PubMed

Kawamoto, Naoyuki; Kakefuda, Yohei; Mori, Takao; Hirose, Kenji; Mitome, Masanori; Bando, Yoshio; Golberg, Dmitri

2015-11-20

We developed an original method of in situ nanoscale characterization of thermal resistance utilizing a high-resolution transmission electron microscope (HRTEM). The focused electron beam of the HRTEM was used as a contact-free heat source and a piezo-movable nanothermocouple was developed as a thermal detector. This method has a high flexibility of supplying thermal-flux directions for nano/microscale thermal conductivity analysis, and is a powerful way to probe the thermal properties of complex or composite materials. Using this method we performed reproducible measurements of electron beam-induced temperature changes in pre-selected sections of a heat-sink α-Al(2)O(3)/epoxy-based resin composite. Observed linear behavior of the temperature change in a filler reveals that Fourier's law holds even at such a mesoscopic scale. In addition, we successfully determined the thermal resistance of the nanoscale interfaces between neighboring α-Al(2)O(3) fillers to be 1.16 × 10(-8) m(2)K W(-1), which is 35 times larger than that of the fillers themselves. This method that we have discovered enables evaluation of thermal resistivity of composites on the nanoscale, combined with the ultimate spatial localization and resolution sample analysis capabilities that TEM entails.

Shape-controlled solvothermal synthesis of bismuth subcarbonate nanomaterials

NASA Astrophysics Data System (ADS)

Cheng, Gang; Yang, Hanmin; Rong, Kaifeng; Lu, Zhong; Yu, Xianglin; Chen, Rong

2010-08-01

Much effort has been devoted to the synthesis of novel nanostructured materials because of their unique properties and potential applications. Bismuth subcarbonate ((BiO) 2CO 3) is one of commonly used antibacterial agents against Helicobacter pylori ( H. pylori). Different (BiO) 2CO 3 nanostructures such as cube-like nanoparticles, nanobars and nanoplates, were fabricated from bismuth nitrate via a simple solvothermal method. The nanostructures were characterized by powder X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). It was found that the solvents and precursors have an influence on the morphologies of (BiO) 2CO 3 nanostructures. The possible formation mechanism of different (BiO) 2CO 3 nanostructures fabricated under different conditions was also discussed.

Bi2Te3 thin hexagonal nanoplatelets: Synthesis and its characterization studies

NASA Astrophysics Data System (ADS)

Vinoth, S.; Balaganapathi, T.; KaniAmuthan, B.; Arun, T.; Muthuselvam, I. Panneer; Chou, Fang-Cheng; Thilakan, P.

2017-08-01

Solvothermal synthesis and optimization of pure Bismuth telluride (Bi2Te3) hexagonal nanoplatelets was carried out from Bismuth Oxide (Bi2O3) and Tellurium dioxide (TeO2). XRD measurements revealed a sensitive change in crystallization behaviour in correlation with variation in Te/Bi stoichiometry identified through the exchange in intensities between (10 10 ̅) and (110) peaks. Further, Energy Dispersive X-ray (EDAX) analysis revealed the variation in Te/Bi ratio with respect to autoclave temperature. Field emission scanning electron Microscope (FESEM) and the high resolution transmission electron Microscope (HRTEM) studies show the complete growth of hexagonal nanoplatelets at 200 °C. Confocal Micro-Raman measurements revealed the occurrence of symmetry breaking in the synthesized hexagonal nanoplatelets. The electrical conductivity and the activation energy were recorded as 6.01×10-3 S/m and 0.042 eV respectively. Highest maximum absolute value of Seebeck coefficient of -355 μV/K was obtained for the hexagonal nanoplatelets.

Barrier properties of nano silicon carbide designed chitosan nanocomposites.

PubMed

Pradhan, Gopal C; Dash, Satyabrata; Swain, Sarat K

2015-12-10

Nano silicon carbide (SiC) designed chitosan nanocomposites were prepared by solution technique. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) were used for studying structural interaction of nano silicon carbide (SiC) with chitosan. The morphology of chitosan/SiC nanocomposites was investigated by field emission scanning electron microscope (FESEM), and high resolution transmission electron microscope (HRTEM). The thermal stability of chitosan was substantially increased due to incorporation of stable silicon carbide nanopowder. The oxygen permeability of chitosan/SiC nanocomposites was reduced by three folds as compared to the virgin chitosan. The chemical resistance properties of chitosan were enhanced due to the incorporation of nano SiC. The biodegradability was investigated using sludge water. The tensile strength of chitosan/SiC nanocomposites was increased with increasing percentage of SiC. The substantial reduction in oxygen barrier properties in combination with increased thermal stability, tensile strength and chemical resistance properties; the synthesized nanocomposite may be suitable for packaging applications. Copyright © 2015 Elsevier Ltd. All rights reserved.

Growth of single wall carbon nanotubes using PECVD technique: An efficient chemiresistor gas sensor

NASA Astrophysics Data System (ADS)

Lone, Mohd Yaseen; Kumar, Avshish; Husain, Samina; Zulfequar, M.; Harsh; Husain, Mushahid

2017-03-01

In this work, the uniform and vertically aligned single wall carbon nanotubes (SWCNTs) have been grown on Iron (Fe) deposited Silicon (Si) substrate by plasma enhanced chemical vapor deposition (PECVD) technique at very low temperature of 550 °C. The as-grown samples of SWCNTS were characterized by field emission scanning electron microscope (FESEM), high resolution transmission electron microscope (HRTEM) and Raman spectrometer. SWCNT based chemiresistor gas sensing device was fabricated by making the proper gold contacts on the as-grown SWCNTs. The electrical conductance and sensor response of grown SWCNTs have been investigated. The fabricated SWCNT sensor was exposed to ammonia (NH3) gas at 200 ppm in a self assembled apparatus. The sensor response was measured at room temperature which was discussed in terms of adsorption of NH3 gas molecules on the surface of SWCNTs. The achieved results are used to develope a miniaturized gas sensor device for monitoring and control of environment pollutants.

Effects of a common worldwide drink (Beer) on L-Phenylalanine and L-Tyrosine fibrillar assemblies

NASA Astrophysics Data System (ADS)

Banik, Debasis; Banerjee, Pavel; Sabeehuddin, Ghazi; Sarkar, Nilmoni

2017-11-01

In this letter, small amount of beer [0.42-2.08% (v/v)] is employed to investigate the fibril inhibition kinetics of 1 mM L-Phenylalanine and L-Tyrosine (relevant to disease condition) using Fluorescence Lifetime imaging Microscopy (FLIM), Field Emission Scanning Electron Microscopy (FESEM) and High Resolution Transmission Electron Microscopic (HR-TEM) techniques. Our results indicate that 1.67 and 0.42% of beer is sufficient for effective breakdown of L-Phe and L-Tyr assemblies, respectively. Quantitative information about fibril inhibition is obtained from Fluorescence Correlation Spectroscopic (FCS) measurements. We have shown that the morphology of L-Phe changes to L-Tyr in presence of 2,2‧-Bipyridine-3,3‧-diol (BP(OH)2).

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

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

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

An efficient adsorption of indigo carmine dye from aqueous solution on mesoporous Mg/Fe layered double hydroxide nanoparticles prepared by controlled sol-gel route.

PubMed

Ahmed, M A; Brick, A A; Mohamed, A A

2017-05-01

A new approach for removal of indigo carmine blue (IC) dye which is extensively used in jeans manufacture was successfully performed on novel mesoporous [LDH] nanoparticles prepared by sol-gel route using CTAB as shape and pore directing agent. The physicochemical features were monitored by X-ray diffraction (XRD), Fourier transformer infra-red (FTIR), N 2 adsorption-desorption isotherm, Field emission electron microscope (FESEM) and high resolution transmission electron microscope (HRTEM). The influence of reaction parameters affecting dye adsorption including contact time, initial dye concentration, pH and temperature were investigated. Textural analysis and HRTEM images indicate the existence of mesoporous spherical nanoparticles of size = 26 nm connected to each other's and embedded large numbers of mesopores of average pore radius = 43.5 Å. A successful adsorption of IC on LDH nanoparticles of surface area = 85.6 m 2 /g at various pH with maximum adsorption capacity = 62.8 mg/g at pH = 9.5. Langmuir model is more favorable to describe the adsorption of IC rather than Freundlich model which reflecting the preferential formation of monolayer on the surface of LDH. Both film diffusion and the intraparticle diffusion affect the dye adsorption. The values of enthalpy change (ΔH) for and (ΔS) are + 28.18 and + 0.118 kJ/mol, respectively indicating that the removal process is endothermic. The results indicated that LDH nanoparticles conserved a good activity even after five consecutive cycles of reuse. Our results suggest that mesoporous LDH nanoparticles are considered a potential novel adsorbent for remediation of wastewater containing IC. Copyright © 2017 Elsevier Ltd. All rights reserved.

High-performance antibacterial of montmorillonite decorated with silver nanoparticles using microwave-assisted method

NASA Astrophysics Data System (ADS)

Kheiralla, Zeinab Mohamed Hassan; Rushdy, Abeer Ahmed; Betiha, Mohamed Ahmed; Yakob, Naglaa Abdullah Nasif

2014-08-01

Syntheses of silver nanocomposites (AgNPs@MMT) were fabricated with different silver nanoparticles to montmorillonite clay (MMT) ratios using microwave-assisted synthesis method, and silver nitrate was used as the precursor of silver nanoparticles. The antibacterial activities of the nanocomposite were evaluated against Staphylococcus aureus and Pseudomonas aeruginosa bacteria by the disk diffusion and macrodilution broth techniques. The prepared nanocomposites were characterized by N2 adsorption-desorption isotherms, X-ray diffraction (XRD), field emission scanning electron microscope, high-resolution transmission electron microscope (HRTEM), X-ray fluorescence spectroscopy and Fourier transform infrared spectroscopy. The wide-angle XRD patterns and HRTEM images demonstrate that silver nanoparticles were fabricated on surface and within MMT channels. The diameters of the AgNPs were below 15 nm, as indicated by UV-Vis absorption, which effectively controlled by the pores of the MMT host. Data revealed that 5 % AgNP@MMT nanocomposite is much more effective than silver nitrate and shows strong antibacterial activities. The efficiency of antibiotics increased when combined with 5 % AgNP@MMT nanocomposite against both the tested strains. The increase in fold area was higher in case of P. aeruginosa than S. aureus. The highest percentage of fold increases was found for Sulfamethaxole/Trimethoprim and Oxacillin followed by Levofloxaci and Nalidixic acid against P.aeruginosa. On the other hand, Imipenem increases activity in presence of AgNP@MMT nanocomposite against S. aureus. Overall, the synergistic effect of antibiotics and nanoparticles clearly revealed that nanoparticles can be effectively used in combination with antibiotics in order to improve their efficiency against various pathogenic microbes. The suspensions of the synthesized nanocomposites were found to be stable over a long time without any sign of detachment of AgNPs.

Evaluation of stacking faults and associated partial dislocations in AlSb/GaAs (001) interface by aberration-corrected high-resolution transmission electron microscopy

NASA Astrophysics Data System (ADS)

Wen, C.; Ge, B. H.; Cui, Y. X.; Li, F. H.; Zhu, J.; Yu, R.; Cheng, Z. Y.

2014-11-01

The stacking faults (SFs) in an AlSb/GaAs (001) interface were investigated using a 300 kV spherical aberration-corrected high-resolution transmission electron microscope (HRTEM). The structure and strain distribution of the single and intersecting (V-shaped) SFs associated with partial dislocations (PDs) were characterized by the [110] HRTEM images and geometric phase analysis, respectively. In the biaxial strain maps ɛxx and ɛyy, a SF can be divided into several sections under different strain states (positive or negative strain values). Furthermore, the strain state for the same section of a SF is in contrast to each other in ɛxx and ɛyy strain maps. The modification in the strain states was attributed to the variation in the local atomic displacements for the SF in the AlSb film on the GaAs substrate recorded in the lattice image. Finally, the single SF was found to be bounded by two 30° PDs. A pair of 30° PDs near the heteroepitaxial interface reacted to form a Lomer-Cottrell sessile dislocation located at the vertices of V-shaped SFs with opposite screw components. The roles of misfit dislocations, such as the PDs, in strain relaxation were also discussed.

Effects of copper on the preparation and characterization of Na-Ca-P borate glasses.

PubMed

Shailajha, S; Geetha, K; Vasantharani, P; Sheik Abdul Kadhar, S P

2015-03-05

Glasses in the system Na2O-CaO-B2O3-P2O5: CuO have been prepared by melt quenching at 1200°C and rapidly cooling at room temperature. The structural, optical and thermal properties have been investigated using X-ray diffraction (XRD), ultraviolet-visible (UV-VIS) spectroscopy, thermogravimetric-differential thermal analysis (TG-DTA), Fourier transform infrared (FTIR) spectroscopy, high resolution scanning electron microscopy (HRSEM) with energy dispersive X-ray (EDX) spectroscopy and high resolution transmission electron microscope (HRTEM) with energy dispersive X-ray (EDAX). The amorphous and crystalline nature of these samples was verified by XRD. Glass transition, crystallization and thermal stability were determined by TG-DTA investigations. Direct optical energy band gaps before and after doping with different percents of copper oxide were evaluated from 4.81eV to 2.99eV indicated the role of copper in the glassy matrix by UV spectra. FTIR spectrum reveals characteristic absorption bands due to various groups of triangular and tetrahedral borate network. Due to the amorphous nature, the particles like agglomerates on the glass surface were investigated by the HRSEM analysis. The crystalline nature of the samples in XRD is confirmed by SAED pattern using HRTEM. Copyright © 2014 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2014-12-01

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

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

PubMed

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

2016-11-15

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

Twinning of cubic diamond explains reported nanodiamond polymorphs

NASA Astrophysics Data System (ADS)

Németh, Péter; Garvie, Laurence A. J.; Buseck, Peter R.

2015-12-01

The unusual physical properties and formation conditions attributed to h-, i-, m-, and n-nanodiamond polymorphs has resulted in their receiving much attention in the materials and planetary science literature. Their identification is based on diffraction features that are absent in ordinary cubic (c-) diamond (space group: Fd-3m). We show, using ultra-high-resolution transmission electron microscope (HRTEM) images of natural and synthetic nanodiamonds, that the diffraction features attributed to the reported polymorphs are consistent with c-diamond containing abundant defects. Combinations of {113} reflection and <011> rotation twins produce HRTEM images and d-spacings that match those attributed to h-, i-, and m-diamond. The diagnostic features of n-diamond in TEM images can arise from thickness effects of c-diamonds. Our data and interpretations strongly suggest that the reported nanodiamond polymorphs are in fact twinned c-diamond. We also report a new type of twin (<11> rotational), which can give rise to grains with dodecagonal symmetry. Our results show that twins are widespread in diamond nanocrystals. A high density of twins could strongly influence their applications.

Green Synthesis of Silver Nanoparticles by using Eucalyptus Globulus Leaf Extract

NASA Astrophysics Data System (ADS)

Balamurugan, Madheswaran; Saravanan, Shanmugam

2017-12-01

A single step eco-friendly, energy efficient and economically scalable green method was employed to synthesize silver nanoparticles. In this work, the synthesis of silver nanoparticles using Eucalyptus globulus leaf extract as reducing and capping agent along with water as solvent at normal room temperature is described. Silver nanoparticles were prepared from aqueous silver nitrate solution by adding the leaf extract. The prepared nanoparticles were characterized by using UV-visible Spectrophotometer, X-ray diffractometer, High Resolution Transmission Electron Microscope (HR-TEM) and Fourier Transform Infrared Spectroscope (FTIS). X-ray diffraction studies brought to light the crystalline nature and the face centered cubic structure of the silver nanoparticles. Using HR-TEM. the nano sizes and morphology of the particles were studied. The mean sizes of the prepared silver nanoparticles ranged from 30 to 36 nm. The density of the particles was tuned by varying the molar ratio of silver nitrate. FTIS studies showed the functional group of organic molecules which were located on the surface of the silver nanoparticles. Originating from the leaf extracts, these organic molecules reduced and capped the particles.

High-efficiency and conveniently recyclable photo-catalysts for dye degradation based on urchin-like CuO microparticle/polymer hybrid composites

NASA Astrophysics Data System (ADS)

Liu, Xiong; Cheng, Yuming; Li, Xuefeng; Dong, Jinfeng

2018-05-01

In this work, we developed a new type of photo-catalysts composed of the urchin-like cupric oxide (CuO) microparticle and polyvinylidene fluoride (PVDF) hybrid composites by the convenient organic-inorganic hybrid strategy, which show high-efficiency and conveniently recyclable for dye degradation including methylene blue (MB), Congo red (CR), and malachite green (MG) by visible light irradiation. The micro-structural characteristics of urchin-like CuO microparticles are crucial and dominant over the photo-degrading efficiency of hybrid catalyst because of their highly exposed {0 0 2} facet and larger specific surface area. Simultaneously, the intrinsic porous framework of PVDF membrane not only remains the excellent photo-catalytic activity of urchin-like CuO microparticles but also facilitates the enrichment of dyes on the membrane, and thereby synergistically contributing to the photo-catalytic efficiency. The microstructures of both urchin-like CuO microparticles and hybrid catalysts are systematically characterized by various techniques including scanning electron microscopy (SEM), transmission electron microscope (TEM), high-resolution transmission electron microscope (HRTEM), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), and nitrogen adsorption/desorption isotherms, which evidently support the mentioned mechanism.

ß-Ga2O3 nanorod synthesis with a one-step microwave irradiation hydrothermal method and its efficient photocatalytic degradation for perfluorooctanoic acid.

PubMed

Zhao, Baoxiu; Li, Xiang; Yang, Long; Wang, Fen; Li, Jincheng; Xia, Wenxiang; Li, Weijiang; Zhou, Li; Zhao, Colin

2015-01-01

ß-Ga2O3 nanorod was first directly prepared by the microwave irradiation hydrothermal way without any subsequent heat treatments, and its characterizations were analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM), high-resolution transmission electron microscope (HRTEM), UV-Vis diffuse reflection spectroscopy techniques, and also its photocatalytic degradation for perfluorooctanoic acid (PFOA) was investigated. XRD patterns revealed that ß-Ga2O3 crystallization increased with the enhancement of microwave power and the adding of active carbon (AC). PFOA, as an environmental and persistent pollutant, is hard decomposed by hydroxyl radicals (HO·); however, it is facilely destroyed by ß-Ga2O3 photocatalytic reaction in an anaerobic atmosphere. The important factors such as pH, ß-Ga2O3 dosage and bubbling atmosphere were researched, and the degradation and defluorination was 98.8% and 56.2%, respectively. Reductive atmosphere reveals that photoinduced electron may be the major reactant for PFOA. Furthermore, the degradation kinetics for PFOA was simulated and constant and half-life was calculated, respectively. © 2014 The American Society of Photobiology.

Copper and platinum doped titania for photocatalytic reduction of carbon dioxide

NASA Astrophysics Data System (ADS)

Ambrožová, Nela; Reli, Martin; Šihor, Marcel; Kuśtrowski, Piotr; Wu, Jeffrey C. S.; Kočí, Kamila

2018-02-01

The parent TiO2, platinum and copper doped TiO2 photocatalysts with 0.5-2 wt. % of Pt, 0.5-2 wt. % Cu and 1 wt. % Pt combined with 1 wt. % Cu were prepared by the sol-gel method. All the prepared photocatalysts were tested for the CO2 photocatalytic reduction in a stirred batch reactor. The main reaction product was methane, however, hydrogen and carbon monoxide were also detected. The textural, (micro)structural, optical and electronic properties of photocatalysts were characterized in detail by low-temperature nitrogen physisorption, X-ray powder diffraction, EDX, HRTEM, X-ray fluorescence, X-ray photon spectroscopy, scanning electron microscope, transmission electron microscope and diffuse reflectance UV-vis spectroscopy. The photoelectrochemical characteristics of the photocatalysts were determined using photoelectric spectrometry. The highest yields of CH4, H2 and CO were achieved in the presence of 2 wt. % Cu/TiO2, 0.5 wt. % Cu/TiO2 and pure, amorphous TiO2. Based on the conducted experiments it was suggested that both the amount of chemisorbed oxygen or/and hydroxyl species on the TiO2 surface and specific surface area of photocatalyst highly influence its photocatalytic activity.

Large-scale synthesis of coiled-like shaped carbon nanotubes using bi-metal catalyst

NASA Astrophysics Data System (ADS)

Krishna, Vemula Mohana; Somanathan, T.; Manikandan, E.; Umar, Ahmad; Maaza, M.

2018-02-01

Carbon nanomaterials (CNMs), especially carbon nanotubes (CNTs) with coiled structure exhibit scientifically fascinating. They may be projected as an innovative preference to future technological materials. Coiled carbon nanotubes (c-CNTs) on a large-scale were successfully synthesized with the help of bi-metal substituted α-alumina nanoparticles catalyst via chemical vapor deposition (CVD) technique. Highly spring-like carbon nanostructures were observed by field emission scanning electron microscope (FESEM) examination. Furthermore, the obtained material has high purity, which correlates the X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDX) analysis. Raman spectroscopy reveals that the carbon multi layers are well graphitized and crystalline, even if they have defects in its structure due to coiled morphology. High-resolution transmission electron microscope (HRTEM) describes internal structure and dia of the product. Ultimately, results support the activity of bi-metal impregnated α-alumina nanoparticles catalyst to determine the high yield, graphitization and internal structure of the material. We have also studied the purified c-CNTs magnetic properties at room temperature and will be an added advantage in several applications.

Time-dependent gel to gel transformation of a peptide based supramolecular gelator.

PubMed

Baral, Abhishek; Basak, Shibaji; Basu, Kingshuk; Dehsorkhi, Ashkan; Hamley, Ian W; Banerjee, Arindam

2015-06-28

A dipeptide with a long fatty acid chain at its N-terminus gives hydrogels in phosphate buffer in the pH range 7.0-8.5. The hydrogel with a gelator concentration of 0.45% (w/v) at pH 7.46 (physiological pH) provides a very good platform to study dynamic changes within a supramolecular framework as it exhibits remarkable change in its appearance with time. Interestingly, the first formed transparent hydrogel gradually transforms into a turbid gel within 2 days. These two forms of the hydrogel have been thoroughly investigated by using small angle X-ray scattering (SAXS), powder X-ray diffraction (PXRD), field emission scanning electron microscopic (FE-SEM) and high-resolution transmission electron microscopic (HR-TEM) imaging, FT-IR and rheometric analyses. The SAXS and low angle PXRD studies substantiate different packing arrangements for the gelator molecules for these two different gel states (the freshly prepared and the aged hydrogel). Moreover, rheological studies of these two gels reveal that the aged gel is stiffer than the freshly prepared gel.

Ex Situ Investigation of Anisotropic Interconnection in Silicon-Titanium-Nickel Alloy Anode Material

DOE PAGES

Cho, Jong -Soo; Alaboina, Pankaj Kumar; Kang, Chan -Soon; ...

2017-03-10

Herein we investigate the nanostructural evolution of Silicon-Titanium-Nickel (Si-Ti-Ni) ternary alloy material synthesized by melt spinning process for advanced lithium-ion battery anode. The synthesized material was found to have nano-Silicon particles dispersed in the Ti 4Ni 4Si 7 (STN) alloy buffering matrix and was characterized by X-ray diffraction (XRD), High resolution- transmission electron microscope (HR-TEM), Scanning transmission electron microscopes - energy dispersive X-ray spectrometer (STEM-EDS), and electrochemical performance test. The role of STN matrix is to accommodate the volume expansion stresses of the dispersed Si nanoparticles. However, an interesting behavior was observed during cycling. The Si nanoparticles were observed tomore » form interconnection channels growing through the weak STN matrix cracks and evolving to a network isolating the STN matrix into small puddles. In conclusion, this unique nanostructural evolution of Si particles and isolation of the STN matrix failing to offer significant buffering effect to the grown Si network eventually accelerates more volume expansions during cycling due to less mechanical confinement and leads to performance degradation and poor cycle stability.« less

Synthesis of BiOCl nanosheets with oxygen vacancies for the improved photocatalytic properties

NASA Astrophysics Data System (ADS)

Cai, Yujie; Li, Dongya; Sun, Jingyu; Chen, Mengdie; Li, Yirui; Zou, Zhongwei; Zhang, Hua; Xu, Haiming; Xia, Dongsheng

2018-05-01

The square-sharped BiOCl nanosheets with oxygen vacancies were successfully synthesized via a facile hydrothermal route using xylitol as surfactant. The as-prepared BiOCl samples were characterized by Powder X-ray Diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), UV-Vis diffuse reflectance spectra (DRS), Brunauer-Emmett-Teller (BET), X-ray photoelectron spectroscopy (XPS) and Electron spin resonance (ESR). The as-prepared samples were phase-pure with the width and the thickness were about 50-400 nm and 20-50 nm respectively. Besides, the photodegradation performances showed the BiOCl nanosheets with 0.1 g concentration of xylitol (BOC-1) had the best photocatalytic activity under visible light due to its special polycrystalline structure, grain boundary and an optimum concentration of oxygen vacancies. The h+ and radO2- were the two main active species during the photocatalytic process and the possible photocatalytic mechanism was proposed.

Colloidal Synthesis and Thermoelectric Properties of CuFeSe2 Nanocrystals

PubMed Central

Zhang, Bing-Qian; Zuo, Yong; Chen, Jing-Shuai; Niu, He-Lin; Mao, Chang-Jie

2017-01-01

Copper-based chalcogenides that contain abundant, low-cost and environmentally-friendly elements, are excellent materials for numerous energy conversion applications, such as photocatalysis, photovoltaics, photoelectricity and thermoelectrics (TE). Here, we present a high-yield and upscalable colloidal synthesis route for the production of monodisperse ternary I-III-VI2 chalcogenides nanocrystals (NCs), particularly stannite CuFeSe2, with uniform shape and narrow size distributions by using selenium powder as the anion precursor and CuCl2·2H2O and FeCl3 as the cationic precursors. The composition, the state of valence, size and morphology of the CuFeSe2 materials were examined by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), transmission electron microscope (TEM) and high resolution transmission electron microscope (HRTEM), respectively. Furthermore, the TE properties characterization of these dense nanomaterials compacted from monodisperse CuFeSe2 NCs by hot press at 623 K were preliminarily studied after ligand removal by means of hydrazine and hexane solution. The TE performances of the sintered CuFeSe2 pellets were characterized in the temperature range from room temperature to 653 K. Finally, the dimensionless TE figure of merit (ZT) of this Earth-abundant and intrinsic p-type CuFeSe2 NCs is significantly increased to 0.22 at 653 K in this work, which is demonstrated to show a promising TE materialand makes it a possible p-type candidate for medium-temperature TE applications. PMID:29278381

Comparison of nitrogen adsorption and transmission electron microscopy analyses for structural characterization of carbon nanotubes

NASA Astrophysics Data System (ADS)

Abbaslou, Reza Malek; Vosoughi, Vahid; Dalai, Ajay K.

2017-10-01

Carbon nanotubes (CNTs) are different from other porous substrates such as activated carbon due to their high external surfaces. This structural feature can lead in some uncertainties in the results of nitrogen adsorption analysis for characterization of CNTs. In this paper, the results of microscopic analyses and nitrogen adsorption method for characterization of carbon nanotubes were compared. Five different types of CNTs with different structures were either synthesized or purchased. The CNT samples were characterized by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM) and N2 adsorption analysis. The comparisons between the results from the microscopic analyses and N2 adsorption showed that the total pore volume and BET surface measurements include the internal and external porosity of CNTs. Therefore, the interpretation of N2 adsorption data required accurate TEM analysis. In addition, the evaluation of pore size distribution curves from all CNT samples in this study and several instances in the literature revealed the presence of a common peak in the range of 2-5 nm. This peak does not explain the inner pore size distribution. The presence of this common peak can be attributed to the strong adsorption of N2 on the junction of touched and crossed nanotubes.

Nanostructure investigation of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} synthesized by sol-gel method

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

Pransisco, Prengki, E-mail: prengkipransisco@gmail.com; Badan Lingkungan Hidup Derah Kabupaten Empat Lawang South of Sumatera; Shafie, Afza, E-mail: afza@petronas.com.my

2015-07-22

Magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} was successfully prepared by using sol-gel method. Heat treatment on material is always giving defect on properties of material. This paper investigates the effect of heat treatment on nanostructure of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4}. According to thermo gravimetric analysis (TGA) that after 600°C there is no more weight loss detected and it was decided as minimum calcination temperature. Intensity, crystallite size, structure, lattice parameter and d-spacing of the material were investigated by using X-ray diffraction (XRD). High resolution transmission electron microscope (HRTEM) was used to examine nanostructure, nanosize,more » shape and distribution particle of magnetic material Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} and variable pressure field emission scanning electron microscope (VP-FESEM) was used to investigate the surface morphology and topography of the material. The XRD result shows single-phase cubic spinel structure with average crystallite size in the range of 25.6-95.9 nm, the value of the intensity of the material was increased with increasing temperature, and followed by lattice parameter was increased with increasing calcination temperature, value of d-spacing was relatively decreased with accompanied increasing temperature. From HRTEM result the distribution of particles was tend to be agglomerates with particle size of 7.8-17.68 nm. VP-FESEM result shows that grain size of the material increases with increasing calcination temperature and the surface morphology shows that the material is in hexagonal shape and it was also proved by mapping result which showing the presence each of constituents inside the compound.« less

Oxygen vacancy effect on photoluminescence of KNb3O8 nanosheets

NASA Astrophysics Data System (ADS)

Li, Rui; Liu, Liying; Ming, Bangming; Ji, Yuhang; Wang, Ruzhi

2018-05-01

Fungus-like potassium niobate (KNb3O8) nanosheets have been synthesized on indium-doped tin oxide (ITO) glass substrates by a simple and environmental friendly two-step hydrothermal process. The prepared samples have been characterized by using X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), High Resolution Transmission Electron Microscope (HRTEM), Fourier Transform Infra-Red Spectroscopy (FTIR), Raman Spectroscopy and X-ray Photoelectron Spectroscopy (XPS). Furthermore, the photoluminescence (PL) of KNb3O8 nanosheets have been systematically studied. The results showed that the PL spectrum is between 300 and 645 nm with a 325 nm light excitation, which is divided into some sub-peaks. It is different from the perfect KNb3O8 nanosheets whose PL emission peaks located at near 433 nm. It should be originated from the effect of the oxygen (O) vacancies in the KNb3O8 nanosheets, which the PLs peaks can be found at about 490 nm and 530 nm by different position of O vacancy. The experimental results are in accordance with the first-principles calculations. Our results may present a feasible clue to estimate the defect position in KNb3O8 by the shape analysis of its spectrum of PLs.

Interfacial characteristics of diamond/aluminum composites with high thermal conductivity fabricated by squeeze-casting method

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

Jiang, Longtao, E-mail: longtaojiang@163.com; Wang, Pingping; Xiu, Ziyang

2015-08-15

In this work, aluminum matrix composites reinforced with diamond particles (diamond/aluminum composites) were fabricated by squeeze casting method. The material exhibited a thermal conductivity as high as 613 W / (m · K). The obtained composites were investigated by scanning electron microscope and transmission electron microscope in terms of the (100) and (111) facets of diamond particles. The diamond particles were observed to be homogeneously distributed in the aluminum matrix. The diamond{sub (111)}/Al interface was found to be devoid of reaction products. While at the diamond{sub (100)}/Al interface, large-sized aluminum carbides (Al{sub 4}C{sub 3}) with twin-crystal structure were identified. Themore » interfacial characteristics were believed to be responsible for the excellent thermal conductivity of the material. - Graphical abstract: Display Omitted - Highlights: • Squeeze casting method was introduced to fabricate diamond/Al composite. • Sound interfacial bonding with excellent thermal conductivity was produced. • Diamond{sub (111)}/ aluminum interface was firstly characterized by TEM/HRTEM. • Physical combination was the controlling bonding for diamond{sub (111)}/aluminum. • The growth mechanism of Al{sub 4}C{sub 3} was analyzed by crystallography theory.« less

Tribological improvements of carbon-carbon composites by infiltration of atomic layer deposited lubricious nanostructured ceramic oxides

NASA Astrophysics Data System (ADS)

Mohseni, Hamidreza

A number of investigators have reported enhancement in oxidation and wear resistant of carbon-carbon composites (CCC) in the presence of protective coating layers. However, application of a surface and subsurface coating system that can preserve its oxidation and wear resistance along with maintaining lubricity at high temperature remains unsolved. To this end, thermodynamically stable protective oxides (ZnO/Al2O3/ZrO2) have been deposited by atomic layer deposition (ALD) to infiltrate porous CCC and graphite foams in order to improve the thermal stability and wear resistance in low and high speed sliding contacts. Characterization of microstructural evolution was achieved by using energy dispersive x-ray spectroscopy (EDS) mapping in scanning electron microscope (SEM) coupled with focused ion beam (FIB), x-ray tomography, high resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy (STEM) and X-ray diffraction (XRD). Evaluation of the tribological properties of CCC coated with abovementioned ALD thin films were performed by employing low speed pure sliding tribometer and a high speed/frequency reciprocating rig to simulate the fretting wear behavior at ambient temperature and elevated temperatures of 400°C. It was determined with x-ray tomography imaging and EDS mapping that ALD ZnO/Al2O3/ZrO2 nanolaminates and baseline ZrO2 coatings exhibited excellent conformality and pore-filling capabilities down to ˜100 microm and 1.5 mm in the porous CCC and graphite foam, respectively, which were dependent on the exposure time of the ALD precursors. XRD and HRTEM determined the crystalline phases of {0002} textured ZnO (wurtzite), amorphous Al2O3, and {101}-tetragonal ZrO2. Significant improvements up to ˜65% in the sliding and fretting wear factors were determined for the nanolaminates in comparison to the uncoated CCC. A tribochemical sliding-induced mechanically mixed layer (MML) was found to be responsible for these improvements. HRTEM confirmed the presence of a high density of ZnO shear-induced basal stacking faults inside the wear tracks responsible for intrafilm shear velocity accommodation that mitigated friction and wear.

Effect of Ag and Cu Contents on the Age Hardning Behavior of Al-Zn-Mg Alloys

NASA Astrophysics Data System (ADS)

Watanabe, Katsumi; Kawabata, Tokimasa; Ikeno, Susumu; Yoshida, Tomoo; Murakami, Satoshi; Matsuda, Kenji

Al-Zn-Mg alloy has been known as one of the aluminum alloys with the good age-hardening ability and the high strength among commercial aluminum alloys. The mechanical property of the limited ductility, however, is required to further improvement. In this work, three alloys, which were added Cu or Ag into the Al-Zn-Mg-Si alloy, were prepared to compare the effect of the additional elements on the aging behavior. The content of Ag and Cu were 0.2 at.% and 0.2at.%, respectively. The age-hardening behavior and microstructures of those alloys were investigated by hardness measurement, high resolution transmission electron microscope (HRTEM) and selected area electron diffraction (SAED) technique. Ag or Cu added alloy showed higher peak hardness than Ag or Cu free alloy. According to addition of Ag or Cu, the number density of the precipitates increased than Ag or Cu free alloy.

HRTEM low dose: the unfold of the morphed graphene, from amorphous carbon to morphed graphenes.

PubMed

Calderon, H A; Okonkwo, A; Estrada-Guel, I; Hadjiev, V G; Alvarez-Ramírez, F; Robles Hernández, F C

We present experimental evidence under low-dose conditions transmission electron microscopy for the unfolding of the evolving changes in carbon soot during mechanical milling. The milled soot shows evolving changes as a function of the milling severity or time. Those changes are responsible for the transformation from amorphous carbon to graphenes, graphitic carbon, and highly ordered structures such as morphed graphenes, namely Rh6 and Rh6-II. The morphed graphenes are corrugated layers of carbon with cross-linked covalently nature and sp 2 - or sp 3 -type allotropes. Electron microscopy and numerical simulations are excellent complementary tools to identify those phases. Furthermore, the TEAM 05 microscope is an outstanding tool to resolve the microstructure and prevent any damage to the sample. Other characterization techniques such as XRD, Raman, and XPS fade to convey a true identification of those phases because the samples are usually blends or mixes of the mentioned phases.

Visible cathodoluminescence of Er ions in β-Ga(2)O(3) nanowires and microwires.

PubMed

Nogales, E; Méndez, B; Piqueras, J

2008-01-23

Erbium doped β-Ga(2)O(3) nanowires and microwires have been obtained by a vapour-solid process from an initial mixture of Ga(2)O(3) and Er(2)O(3) powders. X-ray diffraction (XRD) analysis reveals the presence of erbium gallium garnet as well as β-Ga(2)O(3) phases in the microwires. Scanning electron microscopy (SEM) images show that the larger microwires have a nearly rectangular cross-section. Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) analysis show good crystal quality of the β-Ga(2)O(3) nanowires. The nanostructures have been studied by means of the cathodoluminescence technique in the scanning electron microscope. Er intraionic blue, green and red emission lines are observed in luminescence spectra even at room temperature, which confirms the optical activity of the rare earth ions in the grown structures. Mapping of the main 555 nm emission intensity shows a non-homogeneous distribution of Er ions in the microstructures.

Response to the comment by C. Kisielowski, H.A. Calderon, F.R. Chen, S. Helveg, J.R. Jinschek, P. Specht, D. Van Dyck on the article "On the influence of the electron dose-rate on the HRTEM image contrast" by J. Barthel, M. Lentzen, A. Thust, Ultramicroscopy 176 (2017) 37-45.

PubMed

Barthel, Juri; Lentzen, Markus; Thust, Andreas

2017-08-01

In a recent article [1] we examined the influence of the applied electron dose rate on the magnitude of the image contrast in high-resolution transmission electron microscopy (HRTEM). We concluded that the magnitude of the image contrast is not substantially affected by the applied electron dose rate. This result is in obvious contradiction to numerous earlier publications by Kisielowski and coworkers [2-7], who commented our recent article due to this contradiction. The present short communication is a response to the comment of Kisielowski and coworkers on our recent article, where we provide additional arguments supporting our initial findings and conclusions on the magnitude of the image contrast in HRTEM. Copyright © 2017 Elsevier B.V. All rights reserved.

Experimental evidence and structural modeling of nonstoichiometric (010) surfaces coexisting in hydroxyapatite nano-crystals.

PubMed

Ospina, C A; Terra, J; Ramirez, A J; Farina, M; Ellis, D E; Rossi, A M

2012-01-01

High-resolution transmission electron microscopy (HRTEM) and ab initio quantum-mechanical calculations of electronic structure were combined to investigate the structure of the hydroxyapatite (HA) (010) surface, which plays an important role in HA interactions with biological media. HA was synthesized by in vitro precipitation at 37°C. HRTEM images revealed thin elongated rod nanoparticles with preferential growth along the [001] direction and terminations parallel to the (010) plane. The focal series reconstruction (FSR) technique was applied to develop an atomic-scale structural model of the high-resolution images. The HRTEM simulations identified the coexistence of two structurally distinct terminations for (010) surfaces: a rather flat Ca(II)-terminated surface and a zig-zag structure with open OH channels. Density functional theory (DFT) was applied in a periodic slab plane-wave pseudopotential approach to refine details of atomic coordination and bond lengths of Ca(I) and Ca(II) sites in hydrated HA (010) surfaces, starting from the HRTEM model. Copyright © 2011 Elsevier B.V. All rights reserved.

Chemically stabilized reduced graphene oxide/zirconia nanocomposite: synthesis and characterization

NASA Astrophysics Data System (ADS)

Sagadevan, Suresh; Zaman Chowdhury, Zaira; Enamul Hoque, Md; Podder, Jiban

2017-11-01

In this research, chemical method was used to fabricate reduced graphene oxide/zirconia (rGO/ZrO2) nanocomposite. X-ray Diffraction analysis (XRD) was carried out to examine the crystalline structure of the nanocomposites. The nanocomposite prepared here has average crystallite size of 14 nm. The surface morphology was observed using scanning electron microscopic analysis (SEM) coupled with electron dispersion spectroscopy (EDS) to detect the chemical element over the surface of the nanocomposites. High-resolution Transmission electron microscopic analysis (HR-TEM) was carried out to determine the particle size and shape of the nanocomposites. The optical property of the prepared samples was determined using UV-visible absorption spectrum. The functional groups were identified using FTIR and Raman spectroscopic analysis. Efficient, cost effective and properly optimized synthesis process of rGO/ZrO2 nanocomposite can ensure the presence of infiltrating graphene network inside the ZrO2 matrix to enhance the electrical properties of the hybrid composites up to a greater scale. Thus the dielectric constant, dielectric loss and AC conductivity of the prepared sample was measured at various frequencies and temperatures. The analytical results obtained here confirmed the homogeneous dispersion of ZrO2 nanostructures over the surface of reduced graphene oxide nanosheets. Overall, the research demonstrated that the rGO/ZrO2 nano-hybrid structure fabricated here can be considered as a promising candidate for applications in nanoelectronics and optoelectronics.

One-pot synthesis of Fe3O4@Chitosan-pSDCalix hybrid nanomaterial for the detection and removal of Hg2+ ion from aqueous media

NASA Astrophysics Data System (ADS)

Bhatti, Asif Ali; Oguz, Mehmet; Yilmaz, Mustafa

2018-03-01

New one pot mesoporous hybrid material containing iron nanoparticles fabricated with chitosan and p-sulfonato dansyl calix[4]arene composite (Fe3O4@Chitosan-pSDCalix) has been susccessfully synthesized. These mesoporous fluorescence iron nanoparticles were applied for the detection and removal of environmentally toxic Hg2+ ion from aqueous media. Different techniques were applied to confirm the preparation of Fe3O4@Chitosan-pSDCalix such as HRTEM, TGA/DTA, FTIR and XRD. Synthesized nanoparticles have average size of 17 nm with pore size of 0.19 nm as revealed from HRTEM images. Fluorescence study follow the photoinduced electron transfer process after addition of Hg2+ in the solution with decrease in intensity. Confocal microscope images were also acquired to confirm the presence of Hg2+ on nanoparticles. Adsorption study suggests that the removal of Hg2+ from aqueous media follows Langmuir adsorption isotherm. These studies suggest the synthesized Fe3O4@Chitosan-pSDCalix is an efficient hybrid material for the detection and removal of Hg2+ ion from aqueous media, and that it can also be used in biomolecules for the detection of toxic metal ions.

Microstructure and magnetic behavior of Mn doped GeTe chalcogenide semiconductors based phase change materials

NASA Astrophysics Data System (ADS)

Adam, Adam Abdalla Elbashir; Cheng, Xiaomin; Abuelhassan, Hassan H.; Miao, Xiang Shui

2017-06-01

Phase-change materials (PCMs) are the most promising candidates to be used as an active media in the universal data storage and spintronic devices, due to their large differences in physical properties of the amorphous-crystalline phase transition behavior. In the present study, the microstructure, magnetic and electrical behaviors of Ge0.94Mn0.06Te thin film were investigated. The crystallographic structure of Ge0.94Mn0.06Te thin film was studied sing X-ray diffractometer (XRD) and High Resolution Transmission Electron Microscope (HR-TEM). The XRD pattern showed that the crystallization structure of the film was rhombohedral phase for GeTe with a preference (202) orientation. The HR-TEM image of the crystalline Ge0.94Mn0.06Te thin film demonstrated that, there were two large crystallites and small amorphous areas. The magnetization as a function of the magnetic field analyses of both amorphous and crystalline states showed the ferromagnetic hysteretic behaviors. Then, the hole carriers concentration of the film was measured and it found to be greater than 1021 cm-3 at room temperature. Moreover, the anomalous of Hall Effect (AHE) was clearly observed for the measuring temperatures 5, 10 and 50 K. The results demonstrated that the magnitude of AHE decreased when the temperature was increasing.

Effect of calcination temperature on microstructure and magnetic properties of Ni{sub 0.5}Zn{sub 0.25}Cu{sub 0.25} Fe{sub 2}O{sub 4} nanoparticles synthesized by sol-gel method

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

Pransisco, Prengki, E-mail: prengkipransisco@gmail.com, E-mail: afza@petronas.com.my; Shafie, Afza, E-mail: prengkipransisco@gmail.com, E-mail: afza@petronas.com.my; Guan, Beh Hoe, E-mail: beh.hoeguan@petronas.com.my

2014-10-24

This paper examines the effect of calcination process on the structural and magnetic properties material nanostructure composite of Ni{sub 0Ð}œ‡{sub 5}Zn{sub 0Ð}œ‡{sub 25}Cu{sub 0.25} Fe{sub 2}O{sub 4} ferrites. The samples were successfully prepared by sol-gel method at different calcination temperature, which are 600°C, 700°C, 800°C and 900°C. Morphological investigation, average crystallite size and microstructure of the material were examined by using X-ray diffraction (XRD) and confirmed by high resolution transmission electron microscope (HRTEM) and field emission scanning electron microscope (FESEM). The effects of calcination temperature on the magnetic properties were calculated by using vibrating sample magnetometer (VSM). The XRD resultmore » shows single-phase cubic spinel structure with interval average size 5.9-38 nm, and grain size microstructure of the material was increasing with temperature increases. The highest magnetization saturation was reached at a temperature 800°C with value 53.89 emu/g, and the value coercive force (Hc) was inversely with the grain size.« less

Growth of ultrananocrystalline diamond film by DC Arcjet plasma enhanced chemical vapor deposition

NASA Astrophysics Data System (ADS)

Chen, G. C.; Li, B.; Yan, Z. Q.; Liu, J.; Lu, F. X.; Ye, H.

2012-06-01

Self-standing diamond films were grown by DC Arcjet plasma enhanced chemical vapor deposition (CVD). The feed gasses were Ar/H2/CH4, in which the flow ratio of CH4 to H2 (F/F) was varied from 5% to 20%. Two distinct morphologies were observed by scanning electron microscope (SEM), i.e. the "pineapple-like" morphology and the "cauliflower-like" morphology. It was found that the morphologies of the as-grown films are strongly dependent on the flow ratio of CH4 to H2 in the feed gasses. High resolution transmission electron microscope (HRTEM) survey results revealed that there were nanocrystalline grains within the "pineapple-like" films whilst there were ultrananocrystalline grains within "cauliflower-like" films. X-ray diffraction (XRD) results suggested that (110) crystalline plane was the dominant surface in the "cauliflower-like" films whilst (100) crystalline plane was the dominant surface in the "pineapple-like" films. Raman spectroscopy revealed that nanostructured carbon features could be observed in both types of films. Plasma diagnosis was carried out in order to understand the morphology dependent growth mechanism. It could be concluded that the film morphology was strongly influenced by the density of gas phases. The gradient of C2 radical was found to be different along the growth direction under the different growth conditions.

Synthesis and characterization of monodispersed silver nanoparticles

NASA Astrophysics Data System (ADS)

Jegatha Christy, A.; Umadevi, M.

2012-09-01

Synthesis of silver nanoparticles (NPs) has become a fascinating and important field of applied chemical research. In this paper silver NPs were prepared using silver nitrate (AgNO3), gelatin, and cetyl trimethyl ammonium bromide (CTAB). The prepared silver NPs were exposed under the laser ablation. In our photochemical procedure, gelatin acts as a biopolymer and CTAB acts as a reducing agent. The appearance of surface plasmon band around 410 nm indicates the formation of silver NPs. The nature of the prepared silver NPs in the face-centered cubic (fcc) structure are confirmed by the peaks in the x-ray diffraction (XRD) pattern corresponding to (111), (200), (220) and (311) planes. Monodispersed, stable, spherical silver NPs with diameter about 10 nm were obtained and confirmed by high-resolution transmission electron microscope (HRTEM).

Synthesis, characterization and photovoltaic performance of Mn-doped ZnS quantum dots- P3HT hybrid bulk heterojunction solar cells

NASA Astrophysics Data System (ADS)

Jabeen, Uzma; Adhikari, Tham; Shah, Syed Mujtaba; Pathak, Dinesh; Nunzi, Jean-Michel

2017-11-01

Zinc sulphide (ZnS) and transition metal-doped ZnS nanocrystals were synthesized by co-precipitation method. Further the synthesized nanocrystals were characterized by Field Emission Scanning Electron Microscope (FESEM), High Resolution Transmission Electron Microscope (HRTEM), Fluorescence, UV-Visible, X-ray diffraction (XRD) and Fourier Transformed Infra-red (FTIR) Spectrometer (FTIR). Scanning electron microscope supplemented with EDAX was employed to attain grain size and chemical composition of the nanomaterials. A considerable blue shift of absorption band was noted by the manganese concentration (0.5 M) in the doped sample in comparison with ZnS quantum dots because of the decrease in the size of nanoparticles which may be due to quantum confinement. The photoluminescence emission observed at 596 nm is due to the emission of divalent manganese and can be ascribed to a 4T1→6A1 transition within the 3d shell. Though, the broad blue emission band was observed at 424 nm which may originates from the radiative recombination comprising defect states in the un-doped zinc sulphide quantum dots. XRD analysis exhibited that the synthesized nanomaterial endured in cubic structure. The synthesized nanomaterial combined with organic polymer P3HT, poly (3-hexyl thiophene) and worked in the construction of inverted solar cells. The photovoltaic devices with un-doped zinc sulphide quantum dots showed power conversion efficiency of 0.48% without annealing and 0.52% with annealing. By doping with manganese, the efficiency was enhanced by a factor of 0.52 without annealing and 0.59 with annealing. The morphology and packing behavior of blend of nanocrystals with organic polymer were explored using Atomic Force Microscopy.

Green synthesis and characterization of Au@Pt core-shell bimetallic nanoparticles using gallic acid

NASA Astrophysics Data System (ADS)

Zhang, Guojun; Zheng, Hongmei; Shen, Ming; Wang, Lei; Wang, Xiaosan

2015-06-01

In this study, we developed a facile and benign green synthesis approach for the successful fabrication of well-dispersed urchin-like Au@Pt core-shell nanoparticles (NPs) using gallic acid (GA) as both a reducing and protecting agent. The proposed one-step synthesis exploits the differences in the reduction potentials of AuCl4- and PtCl62-, where the AuCl4- ions are preferentially reduced to Au cores and the PtCl62- ions are then deposited continuously onto the Au core surface as a Pt shell. The as-prepared Au@Pt NPs were characterized by transmission electron microscope (TEM); high-resolution transmission electron microscope (HR-TEM); scanning electron microscope (SEM); UV-vis absorption spectra (UV-vis); X-ray diffraction (XRD); Fourier transmission infrared spectra (FT-IR). We systematically investigated the effects of some experimental parameters on the formation of the Au@Pt NPs, i.e., the reaction temperature, the molar ratios of HAuCl4/H2PtCl6, and the amount of GA. When polyvinylpyrrolidone K-30 (PVP) was used as a protecting agent, the Au@Pt core-shell NPs obtained using this green synthesis method were better dispersed and smaller in size. The as-prepared Au@Pt NPs exhibited better catalytic activity in the reaction where NaBH4 reduced p-nitrophenol to p-aminophenol. However, the results showed that the Au@Pt bimetallic NPs had a lower catalytic activity than the pure Au NPs obtained by the same method, which confirmed the formation of Au@Pt core-shell nanostructures because the active sites on the surfaces of the Au NPs were covered with a Pt shell.

The synthesis of Ag/polypyrrole coaxial nanocables via ion adsorption method using different oxidants

NASA Astrophysics Data System (ADS)

Qiu, Teng; Xie, Huxiao; Zhang, Jiangru; Zahoor, Amad; Li, Xiaoyu

2011-03-01

Ag/polypyrrole (PPy) coaxial nanocables (NCs) were synthesized by an ion adsorption method. In this method, the pre-made Ag nanowires (NWs) were dispersed in the aqueous solution of copper acetate (Cu(Ac)2), and the Cu2+ ions adsorbed onto the surface of Ag NWs can oxidize pyrrole monomers to polymerize into uniform PPy sheath outside Ag NWs after the Cu(Ac)2-treated Ag NWs were re-dispersed in the aqueous solution of pyrrole. The morphology of NCs was characterized by transmission electron microscope (TEM) and scanning electron microscope (SEM). The relationship between the thickness of polymer sheath and the concentration of Cu(Ac)2 was established. As Cu(Ac)2 which served as the oxidant can also be replaced by AgNO3 in this synthesis, the differences on the structure of polymer sheath caused by different oxidants were studied by surface-enhanced Raman scattering (SERS), high-resolution transmission electron microscope (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS). Comparing with the characterization results of Ag/PPy NCs synthesized using AgNO3 as the oxidant which indicates the random arrangement of PPy chains at the interface between polymer sheath and Ag NWs, PPy chain oxidized by Cu2+ tends to show a relatively ordered conformation at the interface with the pyrrole rings identically taking the plane vertical to the surface of Ag NWs. In addition, although the main part of the polymer sheath was composed of PPy whatever kind of oxidant was used, the sheath of the NCs oxidized by Cu2+ is typical for the existence of Cu(I)-pyrrole coordinate structures with strong Cu(I)-N bond signal shown in XPS characterization.

Effective Pb2+ removal from water using nanozerovalent iron stored 10 months

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Bishay, Samiha T.; Ahmed, Fatma M.; El-Dek, S. I.

2017-10-01

Heavy metal removal from water required reliable and cost-effective considerations, fast separation as well as easy methodology. In this piece of research, nanozerovalent iron (NZVI) was prepared as ideal sorbent for Pb2+ removal. The sample was characterized using X-ray diffraction (XRD), high-resolution transmission electron microscope (HRTEM), and atomic force microscope (AFM-SPM). Batch experiments comprised the effect of pH value and contact time on the adsorption process. The same NZVI was stored for a shelf time (10 months) and the batch experiment was repeated. The outcomes of the investigation assured that NZVI publicized an extraordinary large metal uptake (98%) after a short contact time (10 h). The stored sample revealed the same effectiveness on Pb2+ removal under the same conditions. The results of the physical properties, magnetic susceptibility, and conductance were correlated with the adsorption efficiency. This work offers evidence that these NZVI particles could be potential candidate for Pb2+ removal in large scale, stored for a long time using a simple, green, and cost-effective methodology, and represent an actual feedback in waste water treatment.

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

Resolution Quality and Atom Positions in Sub-?ngstr?m Electron Microscopy

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

O'Keefe, Michael A.; Allard Jr, Lawrence Frederick; Blom, Douglas Allen

2005-01-01

John Cowley pioneered use of transmission electron microscopy (TEM) for high-resolution imaging and helped spur improvements in resolution that enabled researchers to pinpoint the positions of all but the lightest atoms within a crystal structure. Sub-{angstrom} capabilities allow imaging of even the lightest atoms. Initially achieved with software aberration correction (focal-series reconstruction of the specimen exit-surface wave), sub-{angstrom} imaging will become commonplace for next-generation electron microscopes with hardware-corrected lenses and monochromated electron beams. Currently, advanced HR-TEMs can image columns of light atoms (carbon, oxygen, nitrogen) in complex structures, including the lithium atoms present in battery materials. The ability to determinemore » whether an image peak represents one single atom (or atom column) instead of several depends on the resolution of the HR-(S)TEM. Rayleigh's resolution criterion, an accepted standard in optics, was derived as a means for judging when two image intensity peaks from two sources of light (stars) are distinguishable from a single source. Atom spacings closer than the Rayleigh limit have been resolved in HR-TEM, suggesting that it may be useful to consider other limits, such as the Sparrow resolution criterion. From the viewpoint of the materials scientist, it is important to be able to use the image to determine whether an image feature represents one or more atoms (resolution), and where the atoms (or atom columns) are positioned relative to one another (resolution quality). When atoms and the corresponding image peaks are separated by more than the Rayleigh limit of the HR-(S)TEM, it is possible to adjust imaging parameters so that relative peak positions in the image correspond to relative atom positions in the specimen. When atoms are closer than the Rayleigh limit, we must find the relationship of the peak position to the atom position by peak fitting or, if we have a suitable model, by image simulation.« 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

Blueish green photoluminescence from nitrided GaAs(100) surfaces

NASA Astrophysics Data System (ADS)

Shimaoka, Goro; Udagawa, Takashi

1999-04-01

Optical and structural studies were made on the Si-doped (100)GaAs surfaces nitrided at a temperature between 650° and 750°C for 15 min in the flowing NH 3 gas. The wavelength of photoluminescence (PL) spectra were observed to be shortened from 820 nm of the GaAs nitrided at 650°C with increasing nitridation temperature. Blueish green PL with wavelengths of approx. 490 nm and 470 nm were emitted from the nitrided surfaces at 700° and 750°C, respectively. Results of AES and SIMS indicated that the surfaces are nitrided as GaAs 1- xN x, (0< x≤1) alloy layer, and the nitrided region also tended to increase as the temperature raised. High-resolution transmission electron microscopic (HRTEM), transmission electron diffraction (TED) and energy dispersive X-ray (EDX) results showed that films peeled off from the nitrided surfaces consisted mainly of hexagonal, wurtzite-type gallium nitride (GaN) with stacking faults and microtwins.

CROSS-DISCIPLINARY PHYSICS AND RELATED AREAS OF SCIENCE AND TECHNOLOGY: Effect of polyacrylamide on morphology and electromagnetic properties of chrysanthemum-like ZnO particles

NASA Astrophysics Data System (ADS)

Yan, Jun-Feng; Zhang, Zhi-Yong; You, Tian-Gui; Zhao, Wu; Yun, Jiang-Ni; Zhang, Fu-Chun

2009-10-01

Through hydrothermal process, the chrysanthemum-like ZnO particles are prepared with zinc acetate dihydrate (Zn(CH3COO)2·2H2O) and sodium hydroxide (NaOH) used as main resources under the different concentrations of surfactant polyacrylamide (PAM). The microstructure, morphology and the electromagnetic properties of the as-prepared products are characterized by high-resolution transmissïon electron microscopy (HRTEM), field emission environment scanning electron microscope (FEESEM) and microwave vector network analyzer, respectively. The experimental results indicate that the as-prepared products are ZnO single crystalline with hexagona wurtzite structure, that the values of slenderness ratio Ld are different in different PAM concentrations, and that the good magnetic loss property is found in the ZnO products, and the average magnetic loss tangent tan δu increases with PAM concentration increasing, while the dielectric loss tangent tan δe decreases.

Wintertime Experimental investigation of Morphology, Mixing States and Columnar Optical Properties of Aerosols over a Desert location in India

NASA Astrophysics Data System (ADS)

Mishra, S.; Kumar, T.; Sharma, C.; Prasad, M. V. S. N.; Singh, S.; Agnihotri, R.; Arya, B. C.; Gupta, B.; Naaraayanan, T.; Gautam, S.; Kumar, D.; Sood, K. N.; Tawale, J. S.; Sharma, A. K.; Mitra, A. K.

2014-12-01

Indian Desert (The Thar Desert) is considered as the source of mineral dust in the Indo-Gangetic Plain (IGP) especially in pre-monsoon period due to large scale convective activities during hot summer. To study the physico-chemical characteristics of aerosols over the Thar Desert (Jaisalmer, Rajasthan) during winter (December, 2013), a field campaign has been carried out in Jaisalmer in Rajasthan state. Experiments were conducted inside the city as well as far from the city. The faraway location is close to international border of another country i.e. Pakistan. PM2.5 and PM10 were collected within the city while PM5 was collected far from the city. Particles were collected on Teflon filters for bulk analysis with Fourier Transform Infrared Spectroscopy (FTIR), on Tin substrate for individual particle morphology and elemental composition analysis with Scanning Electron Microscope (SEM) equipped with Energy Dispersive Spectrometer (EDS) and on the Cu-TEM grid for individual particle morphology and mixing state characterization using High Resolution-Transmission Electron Microscope (HRTEM). Together with this, aerosol size distribution observation and columnar spectral aerosol optical properties have been carried out with OPC (Optical Particle Counter, GRIMM Model 1.108) and hand held Microtops-II, respectively. HRTEM analysis reveals occurrence of carbonaceous fractals found in various mixing states 1) aged with some hygroscopic species 2) embedded in sulfate host 3) semi-externally mixed with sulfate and other species. Core-shell particles were also observed with varying core composition (carbon, typical mineral dust, and calcite) and shell thickness (shell comprising of water). The back trajectory analysis reveals the source of wind from Karachi and Islamabad from Pakistan which may be the potential source of carbonaceous species over the sampling site. SEM-EDS analysis reveals occurrence of mineral dust 1) pure mineral dust (Ca and Si rich) 2) polluted mineral dust (mixed with carbon and Cr) together with some pollutants (rich in carbon, S, K, Cl, Mo and Nb). Signatures of various organics were traced using FTIR. Aerosol columnar spectral optical properties, size distribution and meteorology in tandem with aforementioned aerosol properties will be discussed in detail during the presentation.

Nucleation of diamond by pure carbon ion bombardment—a transmission electron microscopy study

NASA Astrophysics Data System (ADS)

Yao, Y.; Liao, M. Y.; Wang, Z. G.; Lifshitz, Y.; Lee, S. T.

2005-08-01

A cross-sectional high-resolution transmission electron microscopy (HRTEM) study of a film deposited by a 1 keV mass-selected carbon ion beam onto silicon held at 800 °C is presented. Initially, a graphitic film with its basal planes perpendicular to the substrate is evolving. The precipitation of nanodiamond crystallites in upper layers is confirmed by HRTEM, selected area electron diffraction, and electron energy loss spectroscopy. The nucleation of diamond on graphitic edges as predicted by Lambrecht et al. [W. R. L. Lambrecht, C. H. Lee, B. Segall, J. C. Angus, Z. Li, and M. Sunkara, Nature, 364 607 (1993)] is experimentally confirmed. The results are discussed in terms of our recent subplantation-based diamond nucleation model.

HRTEM Analysis of Crystallographic Defects in CdZnTe Single Crystal

NASA Astrophysics Data System (ADS)

Yasar, Bengisu; Ergunt, Yasin; Kabukcuoglu, Merve Pinar; Parlak, Mehmet; Turan, Rasit; Kalay, Yunus Eren

2018-01-01

In recent years, CdZnTe has attracted much attention due to its superior electrical and structural properties for room-temperature operable gamma and x-ray detectors. However, CdZnTe (CZT) material has often suffered from crystallographic defects encountered during the growth and post-growth processes. The identification and structural characterization of these defects is crucial to synthesize defect-free CdZnTe single crystals. In this study, Cd0.95 Zn0.05 Te single crystals were grown using a three-zone vertical Bridgman system. The single crystallinity of the material was ensured by using x-ray diffraction measurements. High-resolution electron microscopy (HRTEM) was used to characterize the nano-scale defects on the CdZnTe matrix. The linear defects oriented along the ⟨211⟩ direction were examined by transmission electron microscopy (TEM) and the corresponding HRTEM image simulations were performed by using a quantitative scanning TEM simulation package.

Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

PubMed

Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

2015-06-01

This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

Nanouric acid or nanocalcium phosphate as central nidus to induce calcium oxalate stone formation: a high-resolution transmission electron microscopy study on urinary nanocrystallites

PubMed Central

Gao, Jie; Xue, Jun-Fa; Xu, Meng; Gui, Bao-Song; Wang, Feng-Xin; Ouyang, Jian-Ming

2014-01-01

Purpose This study aimed to accurately analyze the relationship between calcium oxalate (CaOx) stone formation and the components of urinary nanocrystallites. Method High-resolution transmission electron microscopy (HRTEM), selected area electron diffraction, fast Fourier transformation of HRTEM, and energy dispersive X-ray spectroscopy were performed to analyze the components of these nanocrystallites. Results The main components of CaOx stones are calcium oxalate monohydrate and a small amount of dehydrate, while those of urinary nanocrystallites are calcium oxalate monohydrate, uric acid, and calcium phosphate. The mechanism of formation of CaOx stones was discussed based on the components of urinary nanocrystallites. Conclusion The formation of CaOx stones is closely related both to the properties of urinary nanocrystallites and to the urinary components. The combination of HRTEM, fast Fourier transformation, selected area electron diffraction, and energy dispersive X-ray spectroscopy could be accurately performed to analyze the components of single urinary nanocrystallites. This result provides evidence for nanouric acid and/or nanocalcium phosphate crystallites as the central nidus to induce CaOx stone formation. PMID:25258530

Direct evidence on Ta-Metal Phases Igniting Resistive Switching in TaOx Thin Film

PubMed Central

Kyu Yang, Min; Ju, Hyunsu; Hwan Kim, Gun; Lee, Jeon-Kook; Ryu, Han-Cheol

2015-01-01

A Ta/TaOx/Pt stacked capacitor-like device for resistive switching was fabricated and examined. The tested device demonstrated stable resistive switching characteristics including uniform distribution of resistive switching operational parameters, highly promising endurance, and retention properties. To reveal the resistive switching mechanism of the device, micro structure analysis using high-resolution transmission electron microscope (HR-TEM) was performed. From the observation results, two different phases of Ta-metal clusters of cubic α-Ta and tetragonal β-Ta were founded in the amorphous TaOx mother-matrix after the device was switched from high resistance state (HRS) to low resistance state (LRS) by externally applied voltage bias. The observed Ta metal clusters unveiled the origin of the electric conduction paths in the TaOx thin film at the LRS. PMID:26365532

Direct evidence on Ta-Metal Phases Igniting Resistive Switching in TaOx Thin Film

NASA Astrophysics Data System (ADS)

Kyu Yang, Min; Ju, Hyunsu; Hwan Kim, Gun; Lee, Jeon-Kook; Ryu, Han-Cheol

2015-09-01

A Ta/TaOx/Pt stacked capacitor-like device for resistive switching was fabricated and examined. The tested device demonstrated stable resistive switching characteristics including uniform distribution of resistive switching operational parameters, highly promising endurance, and retention properties. To reveal the resistive switching mechanism of the device, micro structure analysis using high-resolution transmission electron microscope (HR-TEM) was performed. From the observation results, two different phases of Ta-metal clusters of cubic α-Ta and tetragonal β-Ta were founded in the amorphous TaOx mother-matrix after the device was switched from high resistance state (HRS) to low resistance state (LRS) by externally applied voltage bias. The observed Ta metal clusters unveiled the origin of the electric conduction paths in the TaOx thin film at the LRS.

Effects of aspect ratio of multi-walled carbon nanotubes on coal washery waste water treatment.

PubMed

Aliyu, Ahmed; Kariim, Ishaq; Abdulkareem, Saka Ambali

2017-11-01

The dependency of adsorption behaviour on the aspect ratio of multi-walled carbon nanotubes (MWCNTs) has been explored. In this study, effect of growth temperature on yield and aspect ratio of MWCNTs by catalytic chemical vapour deposition (CCVD) method is reported. The result revealed that yield and aspect ratio of synthesised MWCNTs strongly depend on the growth temperature during CCVD operation. The resulting MWCNTs were characterized by High Resolution Transmission Electron Microscope (HRTEM), Dynamic Light Scattering (DLS) and X-ray diffraction (XRD) techniques to determine it diameter, hydrodynamic diameter and crystallinity respectively. Aspect ratio and length of the grown MWCNTs were determined from the HRTEM images with the hydrodynamic diameter using the modified Navier-Stokes and Stokes-Einstein equations. The effect of the prepared MWCNTs dosage were investigated on the Turbidity, Iron (Fe) and Lead (Pb) removal efficiency of coal washery effluent. The MWCNTs with higher length (58.17 μm) and diameter (71 nm) tend to show high turbidity and Fe removal, while MWCNTs with lower length (38.87 μm) and diameter (45 nm) tend to show high removal of Pb. Hence, the growth temperature during CCVD operation shows a great effluence on the aspect ratio of MWCNTs which determines it area of applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Properties of CuInS₂ Nano-Particles on TiO₂ by Spray Pyrolysis for CuInS₂/TiO₂ Composite Solar Cell.

PubMed

Park, Gye-Choon; Li, Zhen-Yu; Yang, O-Bong

2017-04-01

In this letter, for the absorption layer of a CuInS₂/TiO₂ composite solar cell, I–III–VI2 chalcopyrite semiconductor CuInS₂ nano-particles were deposited by using spray pyrolysis method on TiO2 porous film. Their material characteristics including structural and optical properties of CuInS₂ nano-particles on TiO₂ nanorods were analyzed as a function of its composition ratios of Cu:In:S. Crystalline structure, surface morphology and crystalline size were also investigated by X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), and High-Resolution TEM (HRTEM), respectively. On the other hand, optical property was characterized by an UV-Visible Spectrophotometer. As a result, it was found that the size of CuInS₂ nano-particles, which was formed at 300±5 °C, was smaller than 16 nm from HRTEM analyses, and it was identified that the CuInS₂ particle size was increased as increasing the heat-treatment temperature and time. However, as the size of CuInS₂ nano-particle becomes smaller, optical absorption edge of ternary compound film tends to move to the blue wavelength band. It turns out that the optical energy-band gap of the compound films was ranging from 1.48 eV to 1.53 eV.

Asphaltene aggregation and impact of alkylphenols.

PubMed

Goual, Lamia; Sedghi, Mohammad; Wang, Xiaoxiao; Zhu, Ziming

2014-05-20

The main objective of this study was to provide novel insights into the mechanism of asphaltene aggregation in toluene/heptane (Heptol) solutions and the effect of alkylphenols on asphaltene dispersion through the integration of advanced experimental and modeling methods. High-resolution transmission electron microscope (HRTEM) images revealed that the onset of asphaltene flocculation occurs near a toluene/heptane volume ratio of 70:30 and that flocculates are well below 1 μm in size. To assess the impact of alkylphenols on asphaltene aggregation, octylphenol (OP) and dodecylphenol (DP) were evaluated by impedance analysis based on their ability to delay the precipitation onset and to reduce the size of nonflocculated asphaltene aggregates in 80:20 toluene/heptane solutions. Although a longer dispersant chain length did not affect the precipitation onset, it reduced the size of the aggregates. Molecular dynamics simulations were then performed to understand the mechanism of interaction between a model asphaltene and OP in heptane. OP molecules saturated the H-bonding sites of asphaltenes and prevented them from interacting laterally between themselves. This explained why OP favored the formation of flocculates with filamentary rather than globular structures, which were clearly observed by HRTEM. Although OP proved to be an effective dispersant, its effectiveness was hindered by its self-association and the fact that it interacted at the periphery of asphaltenes, leaving their aromatic cores uncovered.

High Resolution Transmission Electron Microscopy (HRTEM) of nanophase ferric oxides

NASA Technical Reports Server (NTRS)

Golden, D. C.; Morris, R. V.; Ming, D. W.; Lauer, H. V., Jr.

1994-01-01

Iron oxide minerals are the prime candidates for Fe(III) signatures in remotely sensed Martian surface spectra. Magnetic, Mossbauer, and reflectance spectroscopy have been carried out in the laboratory in order to understand the mineralogical nature of Martian analog ferric oxide minerals of submicron or nanometer size range. Out of the iron oxide minerals studied, nanometer sized ferric oxides are promising candidates for possible Martian spectral analogs. 'Nanophase ferric oxide (np-Ox)' is a generic term for ferric oxide/oxihydroxide particles having nanoscale (less than 10 nm) particle dimensions. Ferrihydrite, superparamagnetic particles of hematite, maghemite and goethite, and nanometer sized particles of inherently paramagnetic lepidocrocite are all examples of nanophase ferric oxides. np-Ox particles in general do not give X-ray diffraction (XRD) patterns with well defined peaks and would often be classified as X-ray amorphous. Therefore, different np-Oxs preparations should be characterized using a more sensitive technique e.g., high resolution transmission electron microscopy (HRTEM). The purpose of this study is to report the particle size, morphology and crystalline order, of five np-Ox samples by HRTEM imaging and electron diffraction (ED).

Screening of bacterial strains isolated from uranium mill tailings porewaters for bioremediation purposes.

PubMed

Sánchez-Castro, Iván; Amador-García, Ahinara; Moreno-Romero, Cristina; López-Fernández, Margarita; Phrommavanh, Vannapha; Nos, Jeremy; Descostes, Michael; Merroun, Mohamed L

2017-01-01

The present work characterizes at different levels a number of bacterial strains isolated from porewaters sampled in the vicinity of two French uranium tailing repositories. The 16S rRNA gene from 33 bacterial isolates, corresponding to the different morphotypes recovered, was almost fully sequenced. The resulting sequences belonged to 13 bacterial genera comprised in the phyla Firmicutes, Actinobacteria and Proteobacteria. Further characterization at physiological level and metals/metalloid tolerance provided evidences for an appropriate selection of bacterial strains potentially useful for immobilization of uranium and other common contaminants. By using High Resolution Transmission Electron Microscope (HRTEM), this potential ability to immobilize uranium as U phosphate mineral phases was confirmed for the bacterial strains Br3 and Br5 corresponding to Arthrobacter sp. and Microbacterium oxydans, respectively. Scanning Transmission Electron Microscope- High-Angle Annular Dark-Field (STEM-HAADF) analysis showed U accumulates on the surface and within bacterial cytoplasm, in addition to the extracellular space. Energy Dispersive X-ray (EDX) element-distribution maps demonstrated the presence of U and P within these accumulates. These results indicate the potential of certain bacterial strains isolated from porewaters of U mill tailings for immobilizing uranium, likely as uranium phosphates. Some of these bacterial isolates might be considered as promising candidates in the design of uranium bioremediation strategies. Copyright © 2016 Elsevier Ltd. All rights reserved.

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.

Functionalized carbon dot adorned coconut shell char derived green catalysts for the rapid synthesis of amidoalkyl naphthols.

PubMed

Narayanan, Divya P; Cherikallinmel, Sudha Kochiyil; Sankaran, Sugunan; Narayanan, Binitha N

2018-06-15

A one pot synthesis of carbon dot incorporated porous coconut shell char derived sulphonated catalyst is reported here for the first time and is effectively used in the multicomponent synthesis of amidoalkyl naphthol. Macroporous nature of the char is revealed from scanning electron microscopic (SEM) analysis, whereas the dispersion of carbon dots (CDs) on the porous coconut shell char is confirmed from the high resolution transmission electron microscopic (HRTEM) analysis. Fluorescence emission spectrum further confirmed the presence of CDs in the catalyst. Fourier-transform infrared (FTIR) spectral analysis of the materials indicated that sulphonation occurred both to the CD and to the porous char. X-ray photo electron spectroscopic (XPS) analysis of the most active catalyst confirmed the presence of both sulphonic acid and carboxylic acid groups in the catalyst. The coconut shell char derived materials prepared by varying the amount of H 2 SO 4 are successfully utilized as efficient alternative green catalysts for the multicomponent reaction, where excellent activity in amidoalkyl naphthol synthesis is obtained within short periods under solvent free reaction conditions. A maximum yield of 98% is obtained in the synthesis of N-[Phenyl-(2-hydroxy-naphthalen-1-yl)-methyl]-benzamide, the representative amidoalkyl naphthol, with the best catalyst within 3 min of reaction. The catalyst is highly active for the reactions carried out with varieties of aldehydes and amides with a product yield in the range of 88-98%. The best catalyst system retained more than 90% of its initial activity even upto 6 th repeated run. Copyright © 2018 Elsevier Inc. All rights reserved.

Photo-Catalytic Properties of TiO2 Supported on MWCNTs, SBA-15 and Silica-Coated MWCNTs Nanocomposites.

PubMed

Ramoraswi, Nteseng O; Ndungu, Patrick G

2015-12-01

Mesoporous silica, specifically SBA-15, acid-treated multi-walled carbon nanotubes and a hybrid nanocomposite of SBA-15 coated onto the sidewalls acid-treated multi-walled carbon nanotubes (CNTs) were prepared and used as supports for anatase TiO2. Sol-gel methods were adapted for the synthesis of selected supports and for coating the materials with selected wt% loading of titania. Physical and chemical properties of the supports and catalyst composite materials were investigated by powder X-ray diffraction (XRD), Raman spectroscopy, thermogravimetric analysis, scanning electron microscope (SEM), high-resolution transmission electron microscope (HRTEM), UV-vis diffuse reflectance spectroscopy and fluorescence spectroscopy. The photo-activity of the catalyst composites were evaluated on the decolorisation of methylene blue as a model pollutant. Coating CNTs with SBA-15 improved the thermal stability and textural properties of the nanotubes. All supported titania composites had high surface areas (207-301 m(2)/g), altered band gap energies and reduced TiO2 crystallite sizes. The TiO2/SBA-CNT composite showed enhanced photo-catalytic properties and activity than the TiO2/SBA-15 and TiO2/CNT composites. In addition, an interesting observation was noted with the TiO2/SBA-15 nanocomposites, which had a significantly greater photo-catalytic activity than the TiO2/CNT nanocomposites in spite of the high electron-hole recombination phenomena observed with the photoluminescence results. Discussions in terms of morphological, textural and physical-chemical aspects to account for the result are presented.

Photo-Catalytic Properties of TiO2 Supported on MWCNTs, SBA-15 and Silica-Coated MWCNTs Nanocomposites

NASA Astrophysics Data System (ADS)

Ramoraswi, Nteseng O.; Ndungu, Patrick G.

2015-10-01

Mesoporous silica, specifically SBA-15, acid-treated multi-walled carbon nanotubes and a hybrid nanocomposite of SBA-15 coated onto the sidewalls acid-treated multi-walled carbon nanotubes (CNTs) were prepared and used as supports for anatase TiO2. Sol-gel methods were adapted for the synthesis of selected supports and for coating the materials with selected wt% loading of titania. Physical and chemical properties of the supports and catalyst composite materials were investigated by powder X-ray diffraction (XRD), Raman spectroscopy, thermogravimetric analysis, scanning electron microscope (SEM), high-resolution transmission electron microscope (HRTEM), UV-vis diffuse reflectance spectroscopy and fluorescence spectroscopy. The photo-activity of the catalyst composites were evaluated on the decolorisation of methylene blue as a model pollutant. Coating CNTs with SBA-15 improved the thermal stability and textural properties of the nanotubes. All supported titania composites had high surface areas (207-301 m2/g), altered band gap energies and reduced TiO2 crystallite sizes. The TiO2/SBA-CNT composite showed enhanced photo-catalytic properties and activity than the TiO2/SBA-15 and TiO2/CNT composites. In addition, an interesting observation was noted with the TiO2/SBA-15 nanocomposites, which had a significantly greater photo-catalytic activity than the TiO2/CNT nanocomposites in spite of the high electron-hole recombination phenomena observed with the photoluminescence results. Discussions in terms of morphological, textural and physical-chemical aspects to account for the result are presented.

Controllable biosynthesis of gold nanoparticles from a Eucommia ulmoides bark aqueous extract

NASA Astrophysics Data System (ADS)

Guo, Mingxia; Li, Wei; Yang, Feng; Liu, Huihong

2015-05-01

The present work reports the green synthesis of gold nanoparticles (AuNPs) by water extract of Eucommia ulmoides (E. ulmoides) bark. The effects of various parameters such as the concentration of reactants, pH of the reaction mixture, temperature and the time of incubation were explored to the controlled formation of gold nanoparticles. The characterization through high resolution-transmission electron microscopic (HRTEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) infer that the as-synthesized AuNPs were spherical in shape with a face cubic crystal (FCC) structure. The results from zeta potential and dynamic light scattering (DLS) suggest the good stability and narrow size distribution of the AuNPs. This method for synthesis of AuNPs is simple, economic, nontoxic and efficient. The as-synthesized AuNPs show excellent catalytic activity for the catalytic reducing decoloration of model compounds of azo-dye: reactive yellow 179 and Congo red.

Structural and mechanical characterization of hybrid metallic-inorganic nanosprings

NASA Astrophysics Data System (ADS)

Habtoun, Sabrina; Houmadi, Said; Reig, Benjamin; Pouget, Emilie; Dedovets, Dmytro; Delville, Marie-Hélène; Oda, Reiko; Cristiano, Fuccio; Bergaud, Christian

2017-10-01

Silica nanosprings (NS) are fabricated by a sol-gel deposition of silica precursors onto a template made of self-assembled organic chiral nanostructures. They are deposited and assembled on microstructured silicon substrates, and then metallized and clamped in a single lithography-free step using a focused ion beam (FIB). The resulting suspended hybrid metallic/inorganic NS are then characterized with high-resolution transmission electron microscopy (HRTEM) and scanning TEM/energy-dispersive X-ray spectroscopy (STEM/EDX), showing the atomic structure of the metallic layer. Three-point bending tests are also carried out using an atomic force microscope (AFM) and supported by finite element method (FEM) simulation with COMSOL Multiphysics allowing the characterization of the mechanical behavior and the estimation of the stiffness of the resulting NS. The information obtained on the structural and mechanical properties of the NS is discussed for future nano-electro-mechanical system (NEMS) applications.

MICRO/NANO-STRUCTURAL EXAMINATION AND FISSION PRODUCT IDENTIFICATION IN NEUTRON IRRADIATED AGR-1 TRISO FUEL

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

van Rooyen, I. J.; Lillo, T. M.; Wen, H. M.

Advanced microscopic and microanalysis techniques were developed and applied to study irradiation effects and fission product behavior in selected low-enriched uranium oxide/uranium carbide TRISO-coated particles from fuel compacts in six capsules irradiated to burnups of 11.2 to 19.6% FIMA. Although no TRISO coating failures were detected during the irradiation, the fraction of Ag-110m retained in individual particles often varied considerably within a single compact and at the capsule level. At the capsule level Ag-110m release fractions ranged from 1.2 to 38% and within a single compact, silver release from individual particles often spanned a range that extended from 100% retentionmore » to nearly 100% release. In this paper, selected irradiated particles from Baseline, Variant 1 and Variant 3 type fueled TRISO coated particles were examined using Scanning Electron Microscopy, Atom Probe Tomography; Electron Energy Loss Spectroscopy; Precession Electron Diffraction, Transmission Electron Microscopy, Scanning Transmission Electron Microscopy (STEM), High Resolution Electron Microscopy (HRTEM) examinations and Electron Probe Micro-Analyzer. Particle selection in this study allowed for comparison of the fission product distribution with Ag retention, fuel type and irradiation level. Nano sized Ag-containing features were predominantly identified in SiC grain boundaries and/or triple points in contrast with only two sitings of Ag inside a SiC grain in two different compacts (Baseline and Variant 3 fueled compacts). STEM and HRTEM analysis showed evidence of Ag and Pd co-existence in some cases and it was found that fission product precipitates can consist of multiple or single phases. STEM analysis also showed differences in precipitate compositions between Baseline and Variant 3 fuels. A higher density of fission product precipitate clusters were identified in the SiC layer in particles from the Variant 3 compact compared with the Variant 1 compact. Trend analysis shows precipitates were randomly distributed along the perimeter of the IPyC-SiC interlayer but only weakly associated with kernel protrusion and buffer fractures. There has been no evidence that the general release of silver is related to cracks or significant degradation of the microstructure. The results presented in this paper provide new insights to Ag transport mechanism(s) in intact SiC layer of TRISO coated particles.« less

The extraction of gold nanoparticles from oat and wheat biomasses using sodium citrate and cetyltrimethylammonium bromide, studied by x-ray absorption spectroscopy, high-resolution transmission electron microscopy, and UV-visible spectroscopy.

PubMed

Armendariz, Veronica; Parsons, Jason G; Lopez, Martha L; Peralta-Videa, Jose R; Jose-Yacaman, Miguel; Gardea-Torresdey, Jorge L

2009-03-11

Gold (Au) nanoparticles can be produced through the interaction of Au(III) ions with oat and wheat biomasses. This paper describes a procedure to recover gold nanoparticles from oat and wheat biomasses using cetyltrimethylammonium bromide or sodium citrate. Extracts were analyzed using UV-visible spectroscopy, high-resolution transmission electron microscopy (HRTEM), and x-ray absorption spectroscopy. The HRTEM data demonstrated that smaller nanoparticles are extracted first, followed by larger nanoparticles. In the fourth extraction, coating of chelating agents is visible on the extracted nanoparticles.

One-Pot Green Synthesis of Graphene Nanosheets Encapsulated Gold Nanoparticles for Sensitive and Selective Detection of Dopamine

PubMed Central

Thirumalraj, Balamurugan; Rajkumar, Chellakannu; Chen, Shen-Ming; Palanisamy, Selvakumar

2017-01-01

We report a simple new approach for green preparation of gallic acid supported reduced graphene oxide encapsulated gold nanoparticles (GA-RGO/AuNPs) via one-pot hydrothermal method. The as-prepared composites were successfully characterized by using Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray powder diffraction techniques (XRD), scanning electron microscope (SEM), high resolution transmission electron microscopy (HRTEM) and elemental analysis. The GA-RGO/AuNPs modified electrode behaves as a hybrid electrode material for sensitive and selective detection of dopamine (DA) in presence of ascorbic acid (AA) and uric acid (UA). The GA-RGO/AuNPs modified electrode displays an excellent electrocatalytic activity towards the oxidation of DA and exhibits a wide linear response range over the DA concentrations from 0.01–100.3 μM with a detection limit (LOD) of 2.6 nM based on S/N = 3. In addition, the proposed sensor could be applied for the determination of DA in human serum and urine samples for practical analysis. PMID:28128225

One-Pot Green Synthesis of Graphene Nanosheets Encapsulated Gold Nanoparticles for Sensitive and Selective Detection of Dopamine

NASA Astrophysics Data System (ADS)

Thirumalraj, Balamurugan; Rajkumar, Chellakannu; Chen, Shen-Ming; Palanisamy, Selvakumar

2017-01-01

We report a simple new approach for green preparation of gallic acid supported reduced graphene oxide encapsulated gold nanoparticles (GA-RGO/AuNPs) via one-pot hydrothermal method. The as-prepared composites were successfully characterized by using Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray powder diffraction techniques (XRD), scanning electron microscope (SEM), high resolution transmission electron microscopy (HRTEM) and elemental analysis. The GA-RGO/AuNPs modified electrode behaves as a hybrid electrode material for sensitive and selective detection of dopamine (DA) in presence of ascorbic acid (AA) and uric acid (UA). The GA-RGO/AuNPs modified electrode displays an excellent electrocatalytic activity towards the oxidation of DA and exhibits a wide linear response range over the DA concentrations from 0.01-100.3 μM with a detection limit (LOD) of 2.6 nM based on S/N = 3. In addition, the proposed sensor could be applied for the determination of DA in human serum and urine samples for practical analysis.

The synthesis of Cu/Fe/Fe3O4 catalyst through the aqueous solution ball milling method assisted by high-frequency electromagnetic field

NASA Astrophysics Data System (ADS)

Yingzhe, Zhang; Yuxing, He; Qingdong, Qin; Fuchun, Wang; Wankun, Wang; Yongmei, Luo

2018-06-01

In this paper, nano-magnetic Cu/Fe/Fe3O4 catalyst was prepared by a new aqueous solution ball milling method assisted by high-frequency electromagnetic field at room temperature. The products were characterized by means of X-ray diffraction (XRD), high-resolution transmission electron microscope (HRTEM), selected area electron diffraction (SAED), and vibrating sample magnetometer (VSM). Microwave induced catalytic degradation of methylene blue (MB) was carried out in the presence of Cu/Fe/Fe3O4. The concentration of methylene blue was determined by UV-Vis spectrophotometry. The solid catalyst showed high catalytic activity of degrade MB and considerable saturation magnetization, lower remanence and coercivity. It indicate that the catalyst can be effectively separated for reuse by simply applying an external magnetic field and it can greatly promote their potential industrial application to eliminate organic pollutants from waste-water. Finally, we found that it is the non-thermal effect of microwave that activated the catalytic activity of Cu/Fe/Fe3O4 to degrade MB.

Electrodeposition of Ni and CeO₂/Ni Nanotubes for Hydrogen Evolution Reaction Electrode.

PubMed

Du, Xiaoqing; Yang, Yumeng; Yi, Chenxi; Chen, Yu; Cai, Chao; Zhang, Zhao

2018-07-01

Ni NTs and CeO2-Ni nanotubes (NTs) have been prepared by galvanostatic electrodeposition in anodic aluminum oxide (AAO) Templates. Scanning electron microscope (SEM), high resolution transmission electron microscopy (HRTEM), energy dispersive X-ray spectroscopic (EDS) and X-ray Diffraction (XRD) are used to characterize the prepared NTs. The results showed that the preparation process of CeO2-Ni NTs was accompanied by the formation of many new phases CeNix (x = 1, 2, 3.5 or 5) and preferential orientation crystal face of Ni in CeO2-Ni NTs is 〈111〉, which is different from that Ni 〈200〉 in Ni NTs. Then linear scan voltammetry (LSV) is applied to test the electrocatalytic activity for hydrogen revolution reaction (HER) of the two electrodes in 1 M NaCl aqueous solution and find that both of the two materials exhibited good performance. Finally, the kinetics analyses from the HER process showed that Tafel slope b was mainly dependent on phase composition and electric conductivity of the electrode, while j0 was mainly dependent on its real specific surface area.

Enhancement of efficiency by embedding ZnS and Mn-doped ZnS nanoparticles in P3HT:PCBM hybrid solid state solar cells

NASA Astrophysics Data System (ADS)

Jabeen, Uzma; Adhikari, Tham; Shah, Syed Mujtaba; Nunzi, Jean-Michel; Badshah, Amin; Ahmad, Iqbal

2017-06-01

Zinc sulphide (ZnS) and Mn-doped ZnS nanoparticles were synthesized by wet chemical method. The synthesized nanoparticles were characterized by UV-visible, fluorescence, X-ray diffraction (XRD), fourier transform infra-red (FTIR) spectrometer, field emission scanning electron microscope (FESEM) and high resolution transmission electron microscope (HRTEM). Scanning electron microscope (SEM) was used to find particle size while chemical composition of the synthesized materials was investigated by EDAX. UV-visible absorption spectrum of Mn-doped ZnS was slightly shifted to lower wavelength with respect to the un-doped zinc sulphide with decrease in the size of nanoparticles. Consequently, the band gap was tuned from 3.04 to 3.13 eV. The photoluminescence (PL) emission positioned at 597 nm was ascribed to 4T1 → 6A1 transition within the 3d shell of Mn2+. X-ray diffraction (XRD) analysis revealed that the synthesized nanomaterials existed in cubic crystalline state. The effect of embedding un-doped and doped ZnS nanoparticles in the active layer and changing the ratio of PCBM ([6, 6]-phenyl-C61-butyric acid methyl ester) to nanoparticles on the performance of hybrid solar cell was studied. The device with active layer consisting of poly(3-hexylthiophene) (P3HT), [6, 6]-phenyl-C61-butyric acid methyl ester (PCBM), and un-doped ZnS nanoparticles combined in the ratio of (1:0.5:0.5) attained an efficiency of 2.42% which was found 71% higher than the reference device under the same conditions but not containing nanoparticles. Replacing ZnS nanoparticles with Mn-doped ZnS had a little effect on the enhancement of efficiency. The packing behavior and morphology of blend of nanoparticles with P3HT:PCBM were examined using atomic force microscope (AFM) and XRD. Contribution to the topical issue "Materials for Energy harvesting, conversion and storage II (ICOME 2016)", edited by Jean-Michel Nunzi, Rachid Bennacer and Mohammed El Ganaoui

Interfacial scanning tunneling spectroscopy (STS) of chalcogenide/metal hybrid nanostructure

NASA Astrophysics Data System (ADS)

Saad, Mahmoud M.; Abdallah, Tamer; Easawi, Khalid; Negm, Sohair; Talaat, Hassan

2015-05-01

The electronic structure at the interface of chalcogenide/metal hybrid nanostructure (CdSe-Au tipped) had been studied by UHV scanning tunneling spectroscopy (STS) technique at room temperature. This nanostructure was synthesized by a phase transfer chemical method. The optical absorption of this hybrid nanostructure was recorded, and the application of the effective mass approximation (EMA) model gave dimensions that were confirmed by the direct measurements using the scanning tunneling microscopy (STM) as well as the high-resolution transmission electron microscope (HRTEM). The energy band gap obtained by STS agrees with the values obtained from the optical absorption. Moreover, the STS at the interface of CdSe-Au tipped hybrid nanostructure between CdSe of size about 4.1 ± 0.19 nm and Au tip of size about 3.5 ± 0.29 nm shows a band bending about 0.18 ± 0.03 eV in CdSe down in the direction of the interface. Such a result gives a direct observation of the electron accumulation at the interface of CdSe-Au tipped hybrid nanostructure, consistent with its energy band diagram. The presence of the electron accumulation at the interface of chalcogenides with metals has an important implication for hybrid nanoelectronic devices and the newly developed plasmon/chalcogenide photovoltaic solar energy conversion.

Structural, optical and photovoltaic properties of P3HT and Mn-doped CdS quantum dots based bulk hetrojunction hybrid layers

NASA Astrophysics Data System (ADS)

Jabeen, Uzma; Adhikari, Tham; Pathak, Dinesh; Shah, Syed Mujtaba; Nunzi, Jean-Michel

2018-04-01

Cadmium sulphide (CdS) and Mn-doped CdS nanocrystals were synthesized by co-precipitation method. The nanocrystals were characterized by Fluorescence, Fourier Transformed Infra-red Spectrometer (FTIR), UV-Visible, X-ray diffraction (XRD), X-ray photoelectron spectrometer (XPS), Field Emission Scanning Electron Microscope (FESEM), and High Resolution Transmission Electron Microscope (HRTEM). A considerable blue shift of absorption band with respect to the cadmium sulphide was observed by the Mn concentration (0.5 M) in the doped sample with decreasing the size of nanocrystals. Other reason for this may be Mn doping. Subsequently the band gap was altered from 2.11 to 2.21 eV due to quantum confinement effect. Scanning electron microscope supplemented with EDAX was operated to find grain size and chemical composition of the synthesized nanomaterials. The PL spectrum of Mn-doped CdS nanocrystals displays three PL bands the first one, within the range of 500 nm and the second band at 537 nm, and the third one around 713 nm is labelled red band emission due to attributed to a 4T1→6A1 transition within the 3d shell of divalent manganese. XRD analysis showed that the material was in cubic crystalline state. A comparative study of surfaces of un-doped and metal doped CdS nanocrystals were investigated using X-ray Photoelectron Spectroscopy (XPS). The synthesized nanomaterial in combination with polymer, poly (3-hexyl thiophene) was operated in the construction of photovoltaic cells. The photovoltaic devices with CdS nanocrystals exhibited power conversion efficiency of 0.34% without annealing and 0.38% with annealing. However, the power conversion efficiency was enhanced by a factor of 0.35 without annealing and 0.42 with annealing with corporation of Mn impurity in CdS lattice. Atomic Force Microscopy was employed for morphology and packing behavior of blend of nanocrystals with organic polymer.

Effect of silver doping on the elastic properties of CdS nanoparticles

NASA Astrophysics Data System (ADS)

Dey, P. C.; Das, R.

2018-05-01

CdS and Ag doped CdS (CdS/Ag) nanoparticles have been prepared via chemical method from a Cadmium acetate precursor and Thiourea. The synthesized CdS and CdS/Ag nanoparticles have been characterized by the X-ray Diffraction and High Resolution Transmission Electron Microscope. Here, these nanoparticles have been synthesized at room temperature and all the characterization have also been done at room temperature only. The XRD results reveal that the products are crystalline with cubic zinc blende structure. HRTEM images show that the prepared nanoparticles are nearly spherical in shape. Williamson-Hall method and Size-Strain Plot (SSP) have been used to study the individual contribution of crystalline sizes and lattice strain on the peak broadening of the CdS and CdS/Ag nanoparticles. The different modified model of Williamson-Hall method such as, uniform deformation model, uniform stress deformation model and uniform energy density deformation model and SSP method have been used to calculate the different physical parameter such as lattice strain, stress and energy density for all diffraction peaks of the XRD, corresponding to the CdS and silver doped CdS (CdS/Ag). The obtained results reveal that the average particle size of the prepared CdS and CdS/Ag nanoparticles estimated from the HRTEM images, Williamson-Hall analysis and SSP method are highly correlated with each other. Further, all these result confirms that doping of Ag significantly affects the elastic properties of CdS.

Studies on linear, nonlinear optical and excited state dynamics of silicon nanoparticles prepared by picosecond laser ablation

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

Hamad, Syed; Nageswara Rao, S. V. S.; Pathak, A. P.

2015-12-15

We report results from our studies on the fabrication and characterization of silicon (Si) nanoparticles (NPs) and nanostructures (NSs) achieved through the ablation of Si target in four different liquids using ∼2 picosecond (ps) pulses. The consequence of using different liquid media on the ablation of Si target was investigated by studying the surface morphology along with material composition of Si based NPs. The recorded mean sizes of these NPs were ∼9.5 nm, ∼37 nm, ∼45 nm and ∼42 nm obtained in acetone, water, dichloromethane (DCM) and chloroform, respectively. The generated NPs were characterized by selected area electron diffraction (SAED),more » high resolution transmission microscopy (HRTEM), Raman spectroscopic techniques and Photoluminescence (PL) studies. SAED, HRTEM and Raman spectroscopy data confirmed that the material composition was Si NPs in acetone, Si/SiO{sub 2} NPs in water, Si-C NPs in DCM and Si-C NPs in chloroform and all of them were confirmed to be polycrystalline in nature. Surface morphological information of the fabricated Si substrates was obtained using the field emission scanning electron microscopic (FESEM) technique. FESEM data revealed the formation of laser induced periodic surface structures (LIPSS) for the case of ablation in acetone and water while random NSs were observed for the case of ablation in DCM and chloroform. Femtosecond (fs) nonlinear optical properties and excited state dynamics of these colloidal Si NPs were investigated using the Z-scan and pump-probe techniques with ∼150 fs (100 MHz) and ∼70 fs (1 kHz) laser pulses, respectively. The fs pump-probe data obtained at 600 nm consisted of single and double exponential decays which were tentatively assigned to electron-electron collisional relaxation (<1 ps) and non-radiative transitions (>1 ps). Large third order optical nonlinearities (∼10{sup −14} e.s.u.) for these colloids have been estimated from Z-scan data at an excitation wavelength of 680 nm suggesting that the colloidal Si NPs find potential applications in photonic devices.« less

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

PubMed

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

2012-02-01

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

One-pot synthesis of MoS2/In2S3 ultrathin nanoflakes with mesh-shaped structure on indium tin oxide as photocathode for enhanced photo-and electrochemical hydrogen evolution reaction

NASA Astrophysics Data System (ADS)

Sun, Baoliang; Shan, Fei; Jiang, Xinxin; Ji, Jing; Wang, Feng

2018-03-01

A bifunctional MoS2/In2S3 hybrid composite that has both photo- and electrocatalytic activity toward hydrogen evolution reaction (HER) is prepared by a facile one pot hydrothermal method. The characterizations by scanning electron microscope (SEM), high resolution transmission electron microscope (HRTEM) and Photoluminescence (PL) shows that the MoS2/In2S3 hybrid exhibits ultrathin nanoflakes with mesh-shaped structure on transparent conductive substrates, and the as prepared catalyst composite obviously improves the separation of electro-hole pairs. The as prepared hybrid nanosheets with Mo:In of 1/2 integrate In-doped MoS2 to reduce the stacking and increase the active surface area. The novel mesh-shaped nanostructure with a moderate degree of disorder provides not only simultaneously intrinsic conductivity and defects but also higher electrochemically active surface area (ECSA). By electrochemical measurements, such as linear sweep voltammetry (LSV), electrochemical impedance spectroscope (EIS) and cyclic voltammetry (CV), we find that the MoS2/In2S3 hybrid possesses much better photo/electrochemical activity than pristine MoS2 or In2S3. MoS2/In2S3 ultrathin nanoflaks are anticipated to be a superior photoelectrocatalyst for PEC cells, and the rational use of the MoS2/In2S3 cathode offers a new avenue toward achieving effective photo-assistant electrocatalytic activity.

A comparative study on omnidirectional anti-reflection SiO2 nanostructure films coating by glancing angle deposition

NASA Astrophysics Data System (ADS)

Prachachet, R.; Samransuksamer, B.; Horprathum, M.; Eiamchai, P.; Limwichean, S.; Chananonnawathorn, C.; Lertvanithphol, T.; Muthitamongkol, P.; Boonruang, S.; Buranasiri, P.

2018-02-01

Fabricated omnidirectional anti-reflection nanostructure films as a one of the promising alternative solar cell applications have attracted enormous scientific and industrial research benefits to their broadband, effective over a wide range of incident angles, lithography-free and high-throughput process. Recently, the nanostructure SiO2 film was the most inclusive study on anti-reflection with omnidirectional and broadband characteristics. In this work, the three-dimensional silicon dioxide (SiO2) nanostructured thin film with different morphologies including vertical align, slant, spiral and thin films were fabricated by electron beam evaporation with glancing angle deposition (GLAD) on the glass slide and silicon wafer substrate. The morphological of the prepared samples were characterized by field-emission scanning electron microscope (FE-SEM) and high-resolution transmission electron microscope (HRTEM). The transmission, omnidirectional and birefringence property of the nanostructure SiO2 films were investigated by UV-Vis-NIR spectrophotometer and variable angle spectroscopic ellipsometer (VASE). The spectrophotometer measurement was performed at normal incident angle and a full spectral range of 200 - 2000 nm. The angle dependent transmission measurements were investigated by rotating the specimen, with incidence angle defined relative to the surface normal of the prepared samples. This study demonstrates that the obtained SiO2 nanostructure film coated on glass slide substrate exhibits a higher transmission was 93% at normal incident angle. In addition, transmission measurement in visible wavelength and wide incident angles -80 to 80 were increased in comparison with the SiO2 thin film and glass slide substrate due to the transition in the refractive index profile from air to the nanostructure layer that improve the antireflection characteristics. The results clearly showed the enhanced omnidirectional and broadband characteristic of the three dimensional SiO2 nanostructure film coating.

Erbium doped aluminum nitride nanoparticles for nano-thermometer applications

NASA Astrophysics Data System (ADS)

Pandya, Sneha G.; Kordesch, Martin E.

2015-06-01

We have synthesized nanoparticles (NPs) of aluminum nitride (AlN) doped in situ with erbium (Er) using the inert gas condensation technique. These NPs have optical properties that make them good candidates for nanoscale temperature sensors. The photoluminescence (PL) spectrum of Er3+ in these NPs shows two emission peaks in the green region at around 540 and 560 nm. The ratio of the intensities of these luminescence peaks is related to temperature. Using Boltzmann’s distribution, the temperature of the NP and its surrounding can be calculated. The NPs were directly deposited on (111) p-type silicon wafers, transmission electron microscope grids and glass cover slips. XRD and HRTEM study indicates that most of the NPs have crystalline hexagonal AlN structure. An enhancement of the luminescence from these NPs was observed after heating in-air at 770 K for 3 h. The sample was then heated in air using a scanning optical microscope laser. The corresponding change in PL peak intensities of the NPs was recorded for laser powers ranging from 0.2 to 15.1 mW. Temperature calculated using the Boltzmann’s distribution was in the range of 300-470 K. This temperature range is of interest for semiconductor device heating and for thermal treatment of cancerous cells, for example.

Nano-Crystalline Diamond Films with Pineapple-Like Morphology Grown by the DC Arcjet vapor Deposition Method

NASA Astrophysics Data System (ADS)

Li, Bin; Zhang, Qin-Jian; Shi, Yan-Chao; Li, Jia-Jun; Li, Hong; Lu, Fan-Xiu; Chen, Guang-Chao

2014-08-01

A nano-crystlline diamond film is grown by the dc arcjet chemical vapor deposition method. The film is characterized by scanning electron microscopy, high-resolution transmission electron microscopy (HRTEM), x-ray diffraction (XRD) and Raman spectra, respectively. The nanocrystalline grains are averagely with 80 nm in the size measured by XRD, and further proven by Raman and HRTEM. The observed novel morphology of the growth surface, pineapple-like morphology, is constructed by cubo-octahedral growth zones with a smooth faceted top surface and coarse side surfaces. The as-grown film possesses (100) dominant surface containing a little amorphous sp2 component, which is far different from the nano-crystalline film with the usual cauliflower-like morphology.

High-resolution transmission electron microscopy studies of graphite materials prepared by high-temperature treatment of unburned carbon concentrates from combustion fly ashes

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

Miguel Cabielles; Jean-Nol Rouzaud; Ana B. Garcia

2009-01-15

High-resolution transmission electron microscopy (HRTEM) has been used in this work to study the microstructural (structure and microtexture) changes occurring during the high-temperature treatment of the unburned carbon concentrates from coal combustion fly ashes. Emphasis was placed on two aspects: (i) the development of graphitic carbon structures and (ii) the disordered carbon forms remaining in the graphitized samples. In addition, by coupling HRTEM with energy-dispersive spectroscopy, the transformations with the temperature of the inorganic matter (mainly iron- and silicon-based phases) of the unburned carbon concentrates were evidenced. The HRTEM results were compared to the averaged structural order of the materialsmore » as evaluated by X-ray diffraction (XRD) and Raman spectroscopy. As indicated by XRD and Raman parameters, more-ordered materials were obtained from the unburned carbon concentrates with higher mineral/inorganic matter, thus inferring the catalytic effect of some of their components. However, the average character of the information provided by these instrumental techniques seems to be inconclusive in discriminating between carbon structures with different degrees of order (stricto sensu graphite, graphitic, turbostratic, etc.) in a given graphitized unburned carbon. Unlike XRD and Raman, HRTEM is a useful tool for imaging directly the profile of the polyaromatic layers (graphene planes), thus allowing the sample heterogeneity to be looked at, specifically the presence of disordered carbon phases. 49 refs., 9 figs., 3 tabs.« less

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.

Structural and Magnetic Response in Bimetallic Core/Shell Magnetic Nanoparticles

PubMed Central

Nairan, Adeela; Khan, Usman; Iqbal, Munawar; Khan, Maaz; Javed, Khalid; Riaz, Saira; Naseem, Shahzad; Han, Xiufeng

2016-01-01

Bimagnetic monodisperse CoFe2O4/Fe3O4 core/shell nanoparticles have been prepared by solution evaporation route. To demonstrate preferential coating of iron oxide onto the surface of ferrite nanoparticles X-ray diffraction (XRD), High resolution transmission electron microscope (HR-TEM) and Raman spectroscopy have been performed. XRD analysis using Rietveld refinement technique confirms single phase nanoparticles with average seed size of about 18 nm and thickness of shell is 3 nm, which corroborates with transmission electron microscopy (TEM) analysis. Low temperature magnetic hysteresis loops showed interesting behavior. We have observed large coercivity 15.8 kOe at T = 5 K, whereas maximum saturation magnetization (125 emu/g) is attained at T = 100 K for CoFe2O4/Fe3O4 core/shell nanoparticles. Saturation magnetization decreases due to structural distortions at the surface of shell below 100 K. Zero field cooled (ZFC) and Field cooled (FC) plots show that synthesized nanoparticles are ferromagnetic till room temperature and it has been noticed that core/shell sample possess high blocking temperature than Cobalt Ferrite. Results indicate that presence of iron oxide shell significantly increases magnetic parameters as compared to the simple cobalt ferrite. PMID:28335200

Electrical, thermal and electrochemical properties of disordered carbon prepared from palygorskite and cane molasses

NASA Astrophysics Data System (ADS)

Alvarez, Edelio Danguillecourt; Laffita, Yodalgis Mosqueda; Montoro, Luciano Andrey; Della Santina Mohallem, Nelcy; Cabrera, Humberto; Pérez, Guillermo Mesa; Frutis, Miguel Aguilar; Cappe, Eduardo Pérez

2017-02-01

We have synthesized and electrochemically tested a carbon sample that was suitable as anode for lithium secondary battery. The synthesis was based on the use of the palygorskite clay as template and sugar cane molasses as carbon source. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Brunauer-Emmett-Teller (BET) measurements and High Resolution Transmission Electron Microscope (HRTEM) analysis showed that the nanometric carbon material has a highly disordered graphene-like wrinkled structure and large specific surface area (467 m2 g-1). The compositional characterization revealed a 14% of heteroatoms-containing groups (O, H, N, S) doping the as-prepared carbon. Thermophysical measurements revealed the good thermal stability and an acceptable thermal diffusivity (9·10-7 m2 s-1) and conductivity (1.1 W m-1 K-1) of this carbon. The electrical properties showed an electronic conductivity of hole-like carriers of approximately one S/cm in a 173-293 K range. The testing of this material as anodes in a secondary lithium battery displayed a high specific capacity and excellent performance in terms of number of cycles. A high reversible capacity of 356 mA h g-1 was reached.

On the approach to Mott's transition in glass-ceramic nanocomposite due to heat treatment

NASA Astrophysics Data System (ADS)

Mahdy, Iman A.; Heikal, Sh.; Abd-Rabo, A. S.; Abdel Ghany, A.; Bahgat, A. A.

2015-07-01

In the present work, the glass-ceramic nanocomposite (GCNC) of the composition 30[0.75 BaTiO3+0.25 PbTiO3]+70 V2O5 (mol. %) was prepared from the parent glass by isothermal heat treatment (HT) at 723 K for different time intervals 0.25, 0.5, 1.5, 2, and 2.5 h, respectively. The bulk density and some related parameters were calculated. X-ray diffraction and Hi-Resolution Transmission Electron Microscope (HRTEM) were used to identify different phases as well as particle size of the precipitated nanocrystals during the heat treatment process. The DC electrical conductivity was enhanced three orders of magnitudes (3×103) by increasing HT time. The resistivity measurements on the other hand as a function of time show an approach to nonmetallic-metallic transition for the prepared NCGC samples. Mott's VRH conduction mechanism was predicted as a result of the increase of the heat treatment time.

Silver nanoparticle-human hemoglobin interface: time evolution of the corona formation and interaction phenomenon

NASA Astrophysics Data System (ADS)

Bhunia, A. K.; Kamilya, T.; Saha, S.

2017-10-01

In this paper, we have used spectroscopic and electron microscopic analysis to monitor the time evolution of the silver nanoparticles (Ag NP)-human hemoglobin (Hb) corona formation and to characterize the interaction of the Ag NPs with Hb. The time constants for surface plasmon resonance binding and reorganization are found to be 9.51 and 118.48 min, respectively. The drop of surface charge and the increase of the hydrodynamic diameter indicated the corona of Hb on the Ag NP surface. The auto correlation function is found to broaden with the increasing time of the corona formation. Surface zeta potential revealed that positively charged Hb interact electrostatically with negatively charged Ag NP surfaces. The change in α helix and β sheet depends on the corona formation time. The visualization of the Hb corona from HRTEM showed large number of Hb domains aggregate containing essentially Ag NPs and without Ag NPs. Emission study showed the tertiary deformation, energy transfer, nature of interaction and quenching under three different temperatures.

Spectral investigations and DFT studies of 3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione (caffeine) interaction and recognition by single amino acid derived self-assembled nanostructures

NASA Astrophysics Data System (ADS)

Govindhan, R.; Karthikeyan, B.

2018-03-01

Recognition of xanthine alkaloid caffeine with 3,5-bis(trifluoromethyl)benzylamine derived peptide nanotubes (BTTPNTs) through chemical interaction have been achieved through the host-guest like interaction. DFT simulation is carried out for caffeine interacted with BTTPNTs system and also experimentally characterized by ultraviolet-visible (UV-vis) absorbance, confocal Raman spectra (CRS) with microscopic imaging (CRM), FT-Raman, surface enhanced Raman scattering (SERS), UV-diffuse reflectance spectra (UV-DRS), high resolution transmission electron microscopy (HR-TEM) and cyclic voltammetry (CV) studies. The results are used to examine the morphologies, size of the nanostructure and study of its interaction with the caffeine molecule. The results show that BTTPNTs is having potential for sensing the caffeine molecules through the binding occurred from the NH2 of tyrosine moiety of the BTTPNTs. This intermolecular association through face-to-face stacking of BTTPNTs is explained by detailed DFT calculations.

Silver nanoparticle-human hemoglobin interface: time evolution of the corona formation and interaction phenomenon.

PubMed

Bhunia, A K; Kamilya, T; Saha, S

2017-01-01

In this paper, we have used spectroscopic and electron microscopic analysis to monitor the time evolution of the silver nanoparticles (Ag NP)-human hemoglobin (Hb) corona formation and to characterize the interaction of the Ag NPs with Hb. The time constants for surface plasmon resonance binding and reorganization are found to be 9.51 and 118.48 min, respectively. The drop of surface charge and the increase of the hydrodynamic diameter indicated the corona of Hb on the Ag NP surface. The auto correlation function is found to broaden with the increasing time of the corona formation. Surface zeta potential revealed that positively charged Hb interact electrostatically with negatively charged Ag NP surfaces. The change in α helix and β sheet depends on the corona formation time. The visualization of the Hb corona from HRTEM showed large number of Hb domains aggregate containing essentially Ag NPs and without Ag NPs. Emission study showed the tertiary deformation, energy transfer, nature of interaction and quenching under three different temperatures.

Electrochemical Study and Applications of Selective Electrodeposition of Silver on Quantum Dots.

PubMed

Martín-Yerga, Daniel; Rama, Estefanía Costa; Costa-García, Agustín

2016-04-05

In this work, selective electrodeposition of silver on quantum dots is described. The particular characteristics of the nanostructured silver thus obtained are studied by electrochemical and microscopic techniques. On one hand, quantum dots were found to catalyze the silver electrodeposition, and on the other hand, a strong adsorption between electrodeposited silver and quantum dots was observed, indicated by two silver stripping processes. Nucleation of silver nanoparticles followed different mechanisms depending on the surface (carbon or quantum dots). Voltammetric and confocal microscopy studies showed the great influence of electrodeposition time on surface coating, and high-resolution transmission electron microscopy (HRTEM) imaging confirmed the initial formation of Janus-like Ag@QD nanoparticles in this process. By use of moderate electrodeposition conditions such as 50 μM silver, -0.1 V, and 60 s, the silver was deposited only on quantum dots, allowing the generation of localized nanostructured electrode surfaces. This methodology can also be employed for sensing applications, showing a promising ultrasensitive electrochemical method for quantum dot detection.

MWCNT-MnFe2O4 nanocomposite for efficient hyperthermia applications

NASA Astrophysics Data System (ADS)

Seal, Papori; Hazarika, Monalisa; Paul, Nibedita; Borah, J. P.

2018-04-01

In this work we present synthesis of multi-walled carbon nanotube (MWCNT)-Manganese ferrite (MnFe2O4) nanocomposite and its probable application in hyperthermia. MnFe2O4 nanoparticles were synthesized by co-precipitation method. X ray diffractogram (XRD) confirms the formation of cubic phase of MnFe2O4 with preferred crystallographic orientation along (311) plane. High resolution electron microscope (HRTEM) image of the composites confirms the presence of MnFe2O4 spherical nanoparticles on the surface of CNT which are bound strongly to the surface. MWCNT-MnFe2O4 nanocomposite were prepared after acid functionalization of MWCNT. Vibrational features of the synthesized samples were confirmed through Fourier transformed infra-red spectroscopy (FTIR). FTIR spectra of acid functionalized MWCNT shows a peak positioned at ˜1620cm-1 which corresponds to C=O functional group of carboxylic acid. Prepared MnFe2O4 nanoparticles and MWCNT-MnFe2O4 nanocomposites were subjected to hyperthermia studies.

Electronic structure, magnetic and structural properties of Ni doped ZnO nanoparticles

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

Kumar, Shalendra, E-mail: shailuphy@gmail.com; Vats, Prashant; Gautam, S.

Highlights: • XRD, and HR-TEM results show the single phase nature of Ni doped ZnO nanoparticles. • dc magnetization results indicate the RT-FM in Ni doped ZnO nanoparticles. • Ni L{sub 3,2} edge NEXAFS spectra infer that Ni ions are in +2 valence state. • O K edge NEXAFS spectra show that O vacancy increases with Ni doping in ZnO. - Abstract: We report structural, magnetic and electronic structural properties of Ni doped ZnO nanoparticles prepared by auto-combustion method. The prepared nanoparticles were characterized by using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), near edge X-ray absorption finemore » structure (NEXAFS) spectroscopy, and dc magnetization measurements. The XRD and HR-TEM results indicate that Ni doped ZnO nanoparticles have single phase nature with wurtzite lattice and exclude the presence of secondary phase. NEXAFS measurements performed at Ni L{sub 3,2}-edges indicates that Ni ions are in +2 valence state and exclude the presence of Ni metal clusters. O K-edge NEXAFS spectra indicate an increase in oxygen vacancies with Ni-doping, while Zn L{sub 3,2}-edge show the absence of Zn-vacancies. The magnetization measurements performed at room temperature shows that pure and Ni doped ZnO exhibits ferromagnetic behavior.« less

Lattice distortion mechanism study of TiO2 nanoparticles during photocatalysis degradation and reactivation

NASA Astrophysics Data System (ADS)

Wu, Wenhui; Xue, Xudong; Jiang, Xudong; Zhang, Yupeng; Wu, Yichu; Pan, Chunxu

2015-05-01

In this paper, the photocatalytic process of TiO2 (P25) is directly characterized by using a positron annihilation lifetime spectroscopy (PALS), high-resolution transmission electron microscopy (HRTEM), Photoluminescence spectroscopy (PL) and UV Raman spectroscopy (Raman). The experimental results reveal that: 1) From PALS measurements, because τ1 and τ2 values and their intensity (I1 and I2) assigned to the different size and amounts of defects, respectively, their variations indicate the formation of different types and amounts of defects during the absorption and degradation. 2) HRTEM observations show that the lattice images become partly blurring when the methylene blue is fully degradated, and clear again after exposed in the air for 30 days. According to the results, we propose a mechanism that the lattice distortion induces the defects as electron capture sites and provides energy for improving photocatalytic process. Meanwhile, the lattice distortion relaxation after exposing in the air for 30 days perfectly explains the gradual deactivation of TiO2, because the smaller vacancy defects grow and agglomerate through the several photocatalytic processes. The instrumental PL and Raman are also used to analyze the samples and approved the results of PALS and HRTEM.

Omnidirectional anti-reflection properties of vertically align SiO2 nanorod films prepared by electron beam evaporation with glancing angle deposition

NASA Astrophysics Data System (ADS)

Prachachet, R.; Samransuksamer, B.; Horprathum, M.; Eiamchai, P.; Limwichean, S.; Chananonnawathorn, C.; Lertvanithphol, T.; Muthitamongkol, P.; Boonruang, S.; Buranasiri, P.

2018-03-01

Omnidirectional anti-reflection coating nanostructure film have attracted enormous attention for the developments of the optical coating, lenses, light emitting diode, display and photovoltaic. However, fabricated of the omnidirectional antireflection nanostructure film on glass substrate in large area was a challenge topic. In the past two decades, the invention of glancing angle deposition technique as a growth of well-controlled two and three-dimensional morphologies has gained significant attention because of it is simple, fast, cost-effective and high mass production capability. In this present work, the omnidirectional anti-reflection nanostructure coating namely silicon dioxide (SiO2) nanorods has been investigated for optimized high transparent layer at all light incident angle. The SiO2 nanorod films of an optimally low refractive index have been fabricated by electron beam evaporation with the glancing angle deposition technique. The morphological of the prepared sampled were characterized by field-emission scanning electron microscope (FE-SEM) and high-resolution transmission electron microscope (HRTEM). The optical transmission and omnidirectional property of the SiO2 nanorod films were investigated by UV-Vis-NIR spectrophotometer. The measurement were performed at normal incident angle and a full spectral range of 200 - 2000 nm. The angle dependent transmission measure were investigated by rotating the specimen, with incidence angle defined relative to the surface normal of the prepared samples. The morphological characterization results showed that when the glancing angle deposition technique was applied, the vertically align SiO2 nanorods with partially isolated columnar structure can be constructed due to the enhanced shadowing and limited addtom diffusion effect. The average transmission of the vertically align SiO2 nanorods were higher than the glass substrate reference sample over the visible wavelength range at all incident angle due to the transition in the refractive index profile from air to the nanostructure layer that improved the anti-reflection characteristics.

Nanoscale solely amorphous layer in silicon wafers induced by a newly developed diamond wheel

PubMed Central

Zhang, Zhenyu; Guo, Liangchao; Cui, Junfeng; Wang, Bo; Kang, Renke; Guo, Dongming

2016-01-01

Nanoscale solely amorphous layer is achieved in silicon (Si) wafers, using a developed diamond wheel with ceria, which is confirmed by high resolution transmission electron microscopy (HRTEM). This is different from previous reports of ultraprecision grinding, nanoindentation and nanoscratch, in which an amorphous layer at the top, followed by a crystalline damaged layer beneath. The thicknesses of amorphous layer are 43 and 48 nm at infeed rates of 8 and 15 μm/min, respectively, which is verified using HRTEM. Diamond-cubic Si-I phase is verified in Si wafers using selected area electron diffraction patterns, indicating the absence of high pressure phases. Ceria plays an important role in the diamond wheel for achieving ultrasmooth and bright surfaces using ultraprecision grinding. PMID:27734934

3D contour fluorescence spectroscopy with Brus model: Determination of size and band gap of double stranded DNA templated silver nanoclusters

NASA Astrophysics Data System (ADS)

Kamalraj, Devaraj; Yuvaraj, Selvaraj; Yoganand, Coimbatore Paramasivam; Jaffer, Syed S.

2018-01-01

Here, we propose a new synthetic methodology for silver nanocluster preparation by using a double stranded-DNA (ds-DNA) template which no one has reported yet. A new calculative method was formulated to determine the size of the nanocluster and their band gaps by using steady state 3D contour fluorescence technique with Brus model. Generally, the structure and size of the nanoclusters determine by using High Resolution Transmission Electron Microscopy (HR-TEM). Before imaging the samples by using HR-TEM, they are introduced to drying process which causes aggregation and forms bigger polycrystalline particles. It takes long time duration and expensive methodology. In this current methodology, we found out the size and band gap of the nanocluster in the liquid form without any polycrystalline aggregation for which 3D contour fluorescence technique was used as an alternative approach to the HR-TEM method.

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

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

Kumar, Shalendra, E-mail: shailuphy@gmail.com; School of Materials Science and Engineering, Changwon National University, Changwon, Gyeongnam 641-773; Song, T.K., E-mail: tksong@changwon.ac.kr

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

Multi-scale characterization by FIB-SEM/TEM/3DAP.

PubMed

Ohkubo, T; Sepehri-Amin, H; Sasaki, T T; Hono, K

2014-11-01

In order to improve properties of functional materials, it is important to understand the relation between the structure and the properties since the structure has large effect to the properties. This can be done by using multi-scale microstructure analysis from macro-scale to nano and atomic scale. Scanning electron microscope (SEM) equipped with focused ion beam (FIB), transmission electron microscope (TEM) and 3D atom probe (3DAP) are complementary analysis tools making it possible to know the structure and the chemistry from micron to atomic resolution. SEM gives us overall microstructural and chemical information by various kinds of detectors such as secondary electron, backscattered electron, EDS and EBSD detectors. Also, it is possible to analyze 3D structure and chemistry via FIB serial sectioning. In addition, using TEM we can focus on desired region to get more complementary information from HRTEM/STEM/Lorentz images, SAED/NBD patterns and EDS/EELS to see the detail micro or nano-structure and chemistry. Especially, combination of probe Cs corrector and split EDS detectors with large detector size enable us to analyze the atomic scale elemental distribution. Furthermore, if the specimen has a complicated 3D nanostructure, or we need to analyze light elements such as hydrogen, lithium or boron, 3DAP can be used as the only technique which can visualize and analyze distribution of all constituent atoms of our materials within a few hundreds nm area. Hence, site-specific sample preparation using FIB/SEM is necessary to get desired information from region of interest. Therefore, this complementary analysis combination works very well to understand the detail of materials.In this presentation, we will show the analysis results obtained from some of functional materials by Carl Zeiss CrossBeam 1540EsB FIB/SEM, FEI Tecnai G(2) F30, Titan G2 80-200 TEMs and locally build laser assisted 3DAP. As the one of the example, result of multi-scale characterization for ultra-fine grain Nd-Fe-B permanent magnet will be shown [1]. In order to improve the magnetic properties, especially to increase the coercivity (resistance against magnetization reversal) of the magnet, decreasing the grain size and isolating each grain by non-ferromagnetic grain boundary phase are quite important since the nucleation of magnetic reversal from grain boundary phase can be suppressed and pinning force of magnetic domain wall at the grain boundary phase can be strengthened. Therefore, micro and nano structure and chemistry analysis can shed a light do grain boundary engineering.Figure 1(a,b) shows SEM BSE images of ultrafine grain Nd-Fe-B sintered magnet and the reconstructed 3D tomography of Nd-rich phases obtained by FIB/SEM serial sectioning. This data can provide us information about the distribution of Nd-rich phase and its volume fraction. Moreover, the HRTEM image from the grain boundary phase, the 3DAP maps and the concentration depth profiles are shown in Fig. 1(c,d,e). This magnet shows high coercivity (1517kA/m), and by comparing these results with the microstructures of low coercivity specimen, importance of grain boundary formation was confirmed and it gives us hint to improve the coercivity further. We will show the detail and results from other materials.jmicro;63/suppl_1/i6/DFU046F1F1DFU046F1Fig. 1.(a) SEM BSE images of ultrafine grain Nd-Fe-B sintered magnet. (b) 3D FIB/SEM tomography of Nd-rich phases. (c) HRTEM image from the grain boundary phase. (d) 3DAP maps of Nd, Cu and Al. (e) Concentration depth profiles for Fe, Nd+Pr, B, Co, Cu and Al, determined from the selected box in (d)[1]. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

RBS/C, HRTEM and HRXRD study of damage accumulation in irradiated SrTiO3

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

Jagielski, Jacek; Jozwik, Przemyslaw A.; Jozwik Biala, Iwona

2013-05-14

Damage accumulation in argon-irradiated SrTiO3 single crystals has been studied by using combination of Rutherford Backscattering/Channeling (RBS/C), High Resolution Transmission Electron Microscopy (HRTEM) and High Resolution X-Ray Diffraction (HRXRD) techniques. The RBS/C spectra were fitted using McChasy, a Monte Carlo simulation code allowing the quantitative analysis of amorphous-like and dislocation-like types of defects. The results were interpreted by using a Multi-Step Damage Accumulation model which assumes, that the damage accumulation occurs in a series of structural transformations, the defect transformations are triggered by a stress caused by formation of a free volume in the irradiated crystal. This assumption has beenmore » confirmed by High Resolution Transmission Electron Microscopy and High Resolution X-Ray Diffraction analysis.« less

Microstructure of amorphous aluminum hydroxide in belite-calcium sulfoaluminate cement

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

Song, Fei; Yu, Zhenglei; Yang, Fengling

Belite-calcium sulfoaluminate (BCSA) cement is a promising low-CO{sub 2} alternative to ordinary Portland cement. Herein, aluminum hydroxide (AH{sub 3}), the main amorphous hydration product of BCSA cement, was investigated in detail. The microstructure of AH{sub 3} with various quantities of gypsum was investigated via scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). The AH{sub 3} with various morphologies were observed and confirmed in the resulting pastes. Particular attention was paid to the fact that AH{sub 3} always contained a small amount of Ca according to the results of EDS analysis. The AH{sub 3} was then characterized via highmore » resolution transmission electron microscopy (HRTEM). The results of HRTEM indicated that Ca arose from nanosized tricalcium aluminate hexahydrate which existed in the AH{sub 3}.« less

Electron radiation damage mechanisms in 2D MoSe2

NASA Astrophysics Data System (ADS)

Lehnert, T.; Lehtinen, O.; Algara-Siller, G.; Kaiser, U.

2017-01-01

The contributions of different damage mechanisms in single-layer MoSe2 were studied by investigating different MoSe2/graphene heterostructures by the aberration-corrected high-resolution transmission electron microscopy (AC-HRTEM) at 80 keV. The damage cross-sections were determined by direct counting of atoms in the AC-HRTEM images. The contributions of damage mechanisms such as knock-on damage or ionization effects were estimated by comparing the damage rates in different heterostructure configurations, similarly to what has been earlier done with MoS2. The behaviour of MoSe2 was found to be nearly identical to that of MoS2, which is an unexpected result, as the knock-on mechanism should be suppressed in MoSe2 due to the high mass of Se, as compared to S.

Growth and magnetoelectric properties of (00l)-oriented La{sub 0.67}Sr{sub 0.33}MnO{sub 3}/PbZr{sub 0.52}Ti{sub 0.48}O{sub 3} heterostructure films

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

Yan, Fuxue, E-mail: yanfuxue@126.com; Han, Kai, E-

2017-02-15

C-axis oriented La{sub 0.67}Sr{sub 0.33}MnO{sub 3}(LSMO)/PbZr{sub 0.52}Ti{sub 0.48}O{sub 3}(PZT) films are fabricated successfully by sol-gel method on LaAlO{sub 3} (00l) substrates. The structure, composition and morphology of the films are investigated by X-ray diffractometer (XRD, θ-2θ scan, ω-scan and ϕ-scan), X-ray photoelectron spectroscope (XPS), field emission scanning electron microscope (FESEM) and high resolution transmission electron microscope (HRTEM). The electric and magnetic properties of randomly and c-axis oriented LSMO/PZT films are studied comparably using ferroelectric testing apparatus and physical property measurement system (PPMS). It is found that the epitaxial LSMO/PZT composite films show well controlled growth along c-axis, and much bettermore » magnetoelectric properties than the randomly oriented ones. The ME voltage coefficient increases from 23 mV cm{sup −1} Oe{sup −1} for the randomly oriented LSMO/PZT composite films to 52 mV cm{sup −1} Oe{sup −1} for c-axis oriented ones prepared using the low cost sol-gel method presented in this study, which shows high potential in promising applications. - Highlights: •Epitaxial LSMO/PZT films were fabricated successfully by sol-gel method on LAO (00l) substrate. •The prepared films exhibit well-defined multiferroic properties for the epitaxial LSMO/PZT films. •Epitaxial LSMO/PZT films show superior magnetoelectric properties to the randomly oriented ones.« less

Efficient Photocatalytic Degradation of Norfloxacin in Aqueous Media by Hydrothermally Synthesized Immobilized TiO2/Ti Films with Exposed {001} Facets.

PubMed

Sayed, Murtaza; Shah, Luqman Ali; Khan, Javed Ali; Shah, Noor S; Nisar, Jan; Khan, Hasan M; Zhang, Pengyi; Khan, Abdur Rahman

2016-12-22

In this study, a novel immobilized TiO 2 /Ti film with exposed {001} facets was prepared via a facile one-pot hydrothermal route for the degradation of norfloxacin from aqueous media. The effects of various hydrothermal conditions (i.e., solution pH, hydrothermal time (H T ) and HF concentration) on the growth of {001} faceted TiO 2 /Ti film were investigated. The maximum photocatalytic performance of {001} faceted TiO 2 /Ti film was observed when prepared at pH 2.62, H T of 3 h and at HF concentration of 0.02 M. The as-prepared {001} faceted TiO 2 /Ti films were fully characterized by field-emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD), high resolution transmission electron microscope (HR-TEM), and X-ray photoelectron spectroscopy (XPS). More importantly, the as-prepared {001} faceted TiO 2 /Ti film exhibited excellent photocatalytic performance toward degradation of norfloxacin in various water matrices (Milli-Q water, tap water, river water and synthetic wastewater). The individual influence of various anions (SO 4 2- , HCO 3 - , NO 3 - , Cl - ) and cations (K + , Ca 2+ , Mg 2+ , Cu 2+ , Na + , Fe 3+ ) usually present in the real water samples on the photocatalytic performance of as-prepared TiO 2 /Ti film with exposed {001} facet was investigated. The mechanistic studies revealed that • OH is mainly involved in the photocatalytic degradation of norfloxacin by {001} faceted TiO 2 /Ti film. In addition, norfloxacin degradation byproducts were investigated, on the basis of which degradation schemes were proposed.

Synthesis, vibrational spectrometry and thermal characterizations of coordination polymers derived from divalent metal ions and hydroxyl terminated polyurethane as ligand

NASA Astrophysics Data System (ADS)

Laxmi; Khan, Shabnam; Kareem, Abdul; Zafar, Fahmina; Nishat, Nahid

2018-01-01

A series of novel coordination polyurethanes [HTPU-M, where M = Mn(II) 'd5', Ni(II) 'd8', and Zn(II) 'd10'] have been synthesized to investigate the effect of divalent metal ions coordination on structure, thermal and adsorption properties of low molecular weight hydroxyl terminated polyurethane (HTPU). HTPU-M have been synthesized in situ where, sbnd OH group of HTPU (synthesized by the condensation polymerization reaction of ethylene glycol (EG) and toluene diisocyanate (TDI) in presence of catalyst) on condensation polymerization with metal acetate in presence of acid catalyst synthesized HTPU-M followed by coordination of metal ions with hetero atoms. The structure, composition and geometry of HTPU-M have been confirmed by vibrational spectrometry (FTIR), 1H NMR, elemental analysis and UV-Visible spectroscopy. Morphological structures of HTPU-M were analyzed by X-Ray Diffraction analysis (XRD), Field Emission Scanning Electron Microscope (FE-SEM) with Energy Dispersive X-ray spectroscopy (EDX) and High Resolution Transmission Electron Microscope (HR-TEM) techniques. The thermal degradation pattern and thermal stability of HTPU-M in comparison to HTPU was investigated by thermal-gravimetric (TG)/differential thermal (DT), analyses along with Integral procedure decomposition temperature (IPDT) by Doyle method. The molecular weight of HTPU was determined by gel permeation chromatography (GPC). The preliminary adsorption/desorption studies of HTPU-M for Congo red (CR) was studied by batch adsorption techniques. The results indicated that HTPU-M have amorphous, layered morphology with higher number of nano-sized grooves in comparison to HTPU. Coordination of metal to HTPU plays a key role in enhancing the thermal stability [HTPU-Ni(II) > HTPU-Mn(II) > HTPU-Zn(II) > HTPU]. The HTPU-M can be utilized for industrial waste water treatment by removing environmental pollutants.

Effect of CoSi2 buffer layer on structure and magnetic properties of Co films grown on Si (001) substrate

NASA Astrophysics Data System (ADS)

Hu, Bo; He, Wei; Ye, Jun; Tang, Jin; Syed Sheraz, Ahmad; Zhang, Xiang-Qun; Cheng, Zhao-Hua

2015-01-01

Buffer layer provides an opportunity to enhance the quality of ultrathin magnetic films. In this paper, Co films with different thickness of CoSi2 buffer layers were grown on Si (001) substrates. In order to investigate morphology, structure, and magnetic properties of films, scanning tunneling microscope (STM), low energy electron diffraction (LEED), high resolution transmission electron microscopy (HRTEM), and surface magneto-optical Kerr effect (SMOKE) were used. The results show that the crystal quality and magnetic anisotropies of the Co films are strongly affected by the thickness of CoSi2 buffer layers. Few CoSi2 monolayers can prevent the interdiffusion of Si substrate and Co film and enhance the Co film quality. Furthermore, the in-plane magnetic anisotropy of Co film with optimal buffer layer shows four-fold symmetry and exhibits the two-jumps of magnetization reversal process, which is the typical phenomenon in cubic (001) films. Project supported by the National Basic Research Program of China (Grant Nos. 2011CB921801 and 2012CB933102), the National Natural Science Foundation of China (Grant Nos. 11374350, 11034004, 11274361, and 11274033), and the Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20131102130005).

Nanoscale modulations in (KLa)(CaW)O-6 and (NaLa)(CaW)O-6

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

Licurse, Mark; Borisevich, Albina Y; Davies, Peter

2012-01-01

Complex nanoscale modulations are identified in two new A-site ordered perovskites, (KLa)(CaW)O{sub 6} and (NaLa)(CaW)O{sub 6}. In (KLa)(CaW)O{sub 6}, selected-area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM) show an incommensurate nanocheckerboard modulation with {approx}9.4 x 9.4 a{sub p} periodicity (a{sub p} {approx} 4 {angstrom} for the cubic perovskite aristotype). For (NaLa)(CaW)O{sub 6} a one-dimensional modulation is observed with a {approx}16(1 1 0)a{sub p} repeat; the <1 1 0> orientation of the nanostripes is different from the <1 0 0> stripes observed in other mixed A-site systems. Studies using high temperature x-ray diffraction suggest the formation of the complexmore » modulations is associated with small deviations from the ideal 1:1:1:1 stoichiometry of the (A{sup +}La{sup 3+})(CaW)O{sub 6} phases. Z-contrast images acquired on an aberration-corrected microscope provide evidence for deviations from stoichiometry with a {approx}1:15 periodic arrangement of La{sub 4/3}(CaW)O{sub 6}:(NaLa)(CaW)O{sub 6} nano-phases.« less

Low-Temperature Synthesis of Anatase TiO2 Nanoparticles with Tunable Surface Charges for Enhancing Photocatalytic Activity

PubMed Central

Li, Ye; Qin, Zhenping; Guo, Hongxia; Yang, Hanxiao; Zhang, Guojun; Ji, Shulan; Zeng, Tingying

2014-01-01

In this work, the positively or negatively charged anatase TiO2 nanoparticles were synthesized via a low temperature precipitation-peptization process (LTPPP) in the presence of poly(ethyleneimine) (PEI) and poly(sodium4- styrenesulfonate) (PSS). X-ray diffraction (XRD) pattern and high-resolution transmission electron microscope (HRTEM) confirmed the anatase crystalline phase. The charges of the prepared TiO2, PEI-TiO2 and PSS-TiO2 nanoparticles were investigated by zeta potentials. The results showed that the zeta potentials of PEI-TiO2 nanoparticles can be tuned from +39.47 mV to +95.46 mV, and that of PSS-TiO2 nanoparticles can be adjusted from −56.63 mV to −119.32 mV. In comparison with TiO2, PSS-TiO2 exhibited dramatic adsorption and degradation of dye molecules, while the PEI modified TiO2 nanoparticles showed lower photocatalytic activity. The photocatalytic performances of these charged nanoparticles were elucidated by the results of UV-vis diffuse reflectance spectra (DRS) and the photoluminescence (PL) spectra, which indicated that the PSS-TiO2 nanoparticles showed a lower recombination rate of electron-hole pairs than TiO2 and PEI-TiO2. PMID:25506839

Tin-Platinum catalysts interactions on titania and silica

NASA Astrophysics Data System (ADS)

Nava, N.; Del Angel, P.; Salmones, J.; Baggio-Saitovitch, E.; Santiago, P.

2007-09-01

Pt-Sn was supported on titania and silica, and the resulting interactions between the components in prepared samples and the resulting interactions between the components before and after treatment with hydrogen were characterized by Mössbauer spectroscopy, X-ray diffraction, Rietveld refinement, high-resolution transmission electron microscopy (HRTEM) and catalytic tests data. Results show the presence of Pt and SnO 2 after calcinations, and Pt 3Sn, PtSn and PtSn 3 after reduction. Rietveld analysis shows that some Ti 4+ are replaced by Sn 4+ atoms in the titania structure. Finally, HRTEM and the practically absence of activity observed confirms that metallic platinum is encapsulated.

Motion of 1/3⟨111⟩ dislocations on Σ3 {112} twin boundaries in nanotwinned copper

NASA Astrophysics Data System (ADS)

Lu, N.; Du, K.; Lu, L.; Ye, H. Q.

2014-01-01

The atomic structure of Σ3 {112} ITBs in nanotwinned Cu is investigated by using aberration-corrected high resolution transmission electron microscopy (HRTEM) and in situ HRTEM observations. The Σ3 {112} ITBs are consisted of periodically repeated three partial dislocations. The in situ HRTEM results show that 1/3[111] partial dislocation moves on the Σ3 {112} incoherent twin boundary (ITB), which was accompanied by a migration of the ITB. A dislocation reaction mechanism is proposed for the motion of 1/3[111] Frank partial dislocation, in which the 1/3[111] partial dislocation exchanges its position with twin boundary dislocations in sequence. In this way, the 1/3[111] dislocation can move on the incoherent twin boundary in metals with low stacking fault energy. Meanwhile, the ITB will migrate in its normal direction accordingly. These results provide insight into the reaction mechanism of 1/3[111] dislocations and ITBs and the associated migration of ITBs.

Facile Synthesis and Optical Properties of Small Selenium Nanocrystals and Nanorods

NASA Astrophysics Data System (ADS)

Jiang, Fengrui; Cai, Weiquan; Tan, Guolong

2017-06-01

Selenium is an important element for human's health, small size is very helpful for Se nanoparticles to be absorbed by human's body. Here, we present a facile approach to fabrication of small selenium nanoparticles (Nano-Se) as well as nanorods by dissolving sodium selenite (Na2SeO3) in glycerin and using glucose as the reduction agent. The as-prepared selenium nanoparticles have been characterized by X-ray diffraction (XRD), UV-Vis absorption spectroscopy and high resolution transmission electron microscope (HRTEM). The morphology of small Se nanoparticles and nanorods have been demonstrated in the TEM images. A small amount of 3-mercaptoproprionic acid (MPA) and glycerin play a key role on controlling the particle size and stabilize the dispersion of Nano-Se in the glycerin solution. In this way, we obtained very small and uniform Se nanoparticles; whose size ranges from 2 to 6 nm. This dimension is much smaller than the best value (>20 nm) ever reported in the literatures. Strong quantum confinement effect has been observed upon the size-dependent optical spectrum of these Se nanoparticles.

Questing and the application for silicon based ternary compound within ultra-thin layer of SIS intermediate region

NASA Astrophysics Data System (ADS)

Chen, Shumin; Gao, Ming; Wan, Yazhou; Du, Huiwei; Li, Yong; Ma, Zhongquan

2016-12-01

A silicon based ternary compound was supposed to be solid synthesized with In, Si and O elements by magnetron sputtering of indium tin oxide target (ITO) onto crystal silicon substrate at 250 °C. To make clear the configuration of the intermediate region, a potential method to obtain the chemical bonding of Si with other existing elements was exploited by X-ray photoelectron spectroscopy (XPS) instrument combined with other assisted techniques. The phase composition and solid structure of the interfacial region between ITO and Si substrate were investigated by X-ray diffraction (XRD) and high resolution cross sectional transmission electron microscope (HR-TEM). A photovoltaic device with structure of Al/Ag/ITO/SiOx/p-Si/Al was assembled by depositing ITO films onto the p-Si substrate by using magnetron sputtering. The new matter has been assumed to be a buffer layer for semiconductor-insulator-semiconductor (SIS) photovoltaic device and plays critical role for the promotion of optoelectronic conversion performance from the view point of device physics.

Graphene oxide/MnO2 nanocomposite as destructive adsorbent of nerve-agent simulants in aqueous media

NASA Astrophysics Data System (ADS)

Šťastný, Martin; Tolasz, Jakub; Štengl, Václav; Henych, Jiří; Žižka, David

2017-08-01

Graphene oxide/MnO2 nanocomposite was prepared by thermal hydrolysis of potassium permanganate (KMnO4) and 2-chloroacetamide aqueous solutions with graphene oxide (GO) suspension. The synthesized samples were characterized by specific surface area (BET) and porosity determination (BJH), X-ray Diffraction (XRD) and high-resolution electron microscopes (HRSEM, HRTEM). These nanocomposites were used in an experimental evaluation of their adsorption activity with nerve agent simulants dimethyl methyl phosphonate (DMMP) and triethyl phosphate (TEP) in aqueous media. The nanocomposites exhibited enhanced adsorptive degradation ability compared to pure manganese oxide (MnO2) and GO. The GO amount in the nanocomposites affected their degradation activity substantially. The best adsorption efficiency was observed for samples with moderate GO amount. Three methods were used to observe the mechanism of the nerve-agent simulants deactivation: Gas chromatography with mass spectrometry (GC-MS), High-Performance Liquid Chromatography (HPLC) and in situ Infrared spectroscopy (FTIR). It was shown that the hydrolysis on the surface of prepared nanocomposites yields volatile primary alcohols (methanol and ethanol) as the main hydrolysis products.

Synthesis, Characterization, and Application of Gold Nanoparticles in Green Nanochemistry Dye-Sensitized Solar Cells

DTIC Science & Technology

2012-06-01

resolution tunneling electron microscopy (HR-TEM). 2.4 DSSC Assembly Annealed TiO2 nanoparticle photoanodes were placed into 10 mL each of the blackberry ...resolution tunneling electron microscopy, and ultraviolet-visible spectroscopy. After characterization, the NPs were found to vary in shape but had... Blackberry Anthocyanin Extraction Procedure ...............................................................3 2.3 Au Nanoparticle Synthesis

In-situ high resolution transmission electron microscopy observation of silicon nanocrystal nucleation in a SiO{sub 2} bilayered matrix

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

Yang, T. C.-J., E-mail: terry.yang@unsw.edu.au; Wu, L.; Lin, Z.

2014-08-04

Solid-state nucleation of Si nanocrystals in a SiO{sub 2} bilayered matrix was observed at temperatures as low as 450 °C. This was achieved by aberration corrected high-resolution transmission electron microscopy (HRTEM) with real-time in-situ heating up to 600 °C. This technique is a valuable characterization tool especially with the recent interest in Si nanostructures for light emitting devices, non-volatile memories, and third-generation photovoltaics which all typically require a heating step in their fabrication. The control of size, shape, and distribution of the Si nanocrystals are critical for these applications. This experimental study involves in-situ observation of the nucleation of Si nanocrystals inmore » a SiO{sub 2} bilayered matrix fabricated through radio frequency co-sputtering. The results show that the shapes of Si nanocrystals in amorphous SiO{sub 2} bilayered matrices are irregular and not spherical, in contrast to many claims in the literature. Furthermore, the Si nanocrystals are well confined within their layers by the amorphous SiO{sub 2}. This study demonstrates the potential of in-situ HRTEM as a tool to observe the real time nucleation of Si nanocrystals in a SiO{sub 2} bilayered matrix. Furthermore, ideas for improvements on this in-situ heating HRTEM technique are discussed.« less

Evidence for anisotropic dielectric properties of monoclinic hafnia using valence electron energy-loss spectroscopy in high-resolution transmission electron microscopy and ab initio time-dependent density-functional theory

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

Guedj, C.; CEA, LETI, MINATEC Campus, F-38054 Grenoble; Hung, L.

2014-12-01

The effect of nanocrystal orientation on the energy loss spectra of monoclinic hafnia (m-HfO{sub 2}) is measured by high resolution transmission electron microscopy (HRTEM) and valence energy loss spectroscopy (VEELS) on high quality samples. For the same momentum-transfer directions, the dielectric properties are also calculated ab initio by time-dependent density-functional theory (TDDFT). Experiments and simulations evidence anisotropy in the dielectric properties of m-HfO{sub 2}, most notably with the direction-dependent oscillator strength of the main bulk plasmon. The anisotropic nature of m-HfO{sub 2} may contribute to the differences among VEELS spectra reported in literature. The good agreement between the complex dielectricmore » permittivity extracted from VEELS with nanometer spatial resolution, TDDFT modeling, and past literature demonstrates that the present HRTEM-VEELS device-oriented methodology is a possible solution to the difficult nanocharacterization challenges given in the International Technology Roadmap for Semiconductors.« less

Quantitative strain and compositional studies of InxGa1-xAs Epilayer in a GaAs-based pHEMT device structure by TEM techniques.

PubMed

Sridhara Rao, Duggi V; Sankarasubramanian, Ramachandran; Muraleedharan, Kuttanellore; Mehrtens, Thorsten; Rosenauer, Andreas; Banerjee, Dipankar

2014-08-01

In GaAs-based pseudomorphic high-electron mobility transistor device structures, strain and composition of the In x Ga1-x As channel layer are very important as they influence the electronic properties of these devices. In this context, transmission electron microscopy techniques such as (002) dark-field imaging, high-resolution transmission electron microscopy (HRTEM) imaging, scanning transmission electron microscopy-high angle annular dark field (STEM-HAADF) imaging and selected area diffraction, are useful. A quantitative comparative study using these techniques is relevant for assessing the merits and limitations of the respective techniques. In this article, we have investigated strain and composition of the In x Ga1-x As layer with the mentioned techniques and compared the results. The HRTEM images were investigated with strain state analysis. The indium content in this layer was quantified by HAADF imaging and correlated with STEM simulations. The studies showed that the In x Ga1-x As channel layer was pseudomorphically grown leading to tetragonal strain along the [001] growth direction and that the average indium content (x) in the epilayer is ~0.12. We found consistency in the results obtained using various methods of analysis.

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

PubMed

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

2014-12-01

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

HR-TEM and FT-Raman dataset of the caffeine interacted Phe-Phe peptide nanotube for possible sensing applications.

PubMed

Narayanan, A Lakshmi; Dhamodaran, M; Solomon, J Samu; Karthikeyan, B; Govindhan, R

2018-02-01

Sensing ability of caffeine interaction with Phe-Phe annotates (PNTs), is presented (Govindhan et al., 2017; Karthikeyan et al., 2014; Tavagnacco et al., 2013; Kennedy et al., 2011; Wang et al., 2017) [1-5] in this data set. Investigation of synthesized caffeine carrying peptide nanotubes are carried out by FT-Raman spectral analysis and high resolution transmission electron microscopy (HR-TEM). Particle size of the caffeine loaded PNTs is < 40 nm. The FT-Raman spectrum signals are enhanced in the region of 400-1700 cm -1 . These data are ideal tool for the applications like biosensing and drug delivery research (DDS).

The electronic properties of SWNTs intercalated by electron acceptors

NASA Astrophysics Data System (ADS)

Chernysheva, M. V.; Kiseleva, E. A.; Verbitskii, N. I.; Eliseev, A. A.; Lukashin, A. V.; Tretyakov, Yu. D.; Savilov, S. V.; Kiselev, N. A.; Zhigalina, O. M.; Kumskov, A. S.; Krestinin, A. V.; Hutchison, J. L.

2008-05-01

Here we report synthesis of Chal@SWNT nanocomposites (where Chal=S, Se and Te) and the impact of the intercalated electron-acceptor compounds on the electronic properties of SWNTs. The chalcogens were introduced to the channels of single-walled carbon nanotubes by molten media technique via impregnation of pre-opened SWNTs with melted guest compounds in vacuum. HRTEM imaging confirms the filling of nanotube channels by continuous nanostructures of corresponding chalcogens. The strong influence of incorporated matter on the electronic properties of the SWNTs was detected by Raman spectroscopy.

Metal-free inactivation of E. coli O157:H7 by fullerene/C3N4 hybrid under visible light irradiation.

PubMed

Ouyang, Kai; Dai, Ke; Chen, Hao; Huang, Qiaoyun; Gao, Chunhui; Cai, Peng

2017-02-01

Interest has grown in developing safe and high-performance photocatalysts based on metal-free materials for disinfection of bacterial pathogens under visible light irradiation. In this paper, the C 60 /C 3 N 4 and C 70 /C 3 N 4 hybrids were synthesized by a hydrothermal method, and characterized by X-ray diffraction (XRD), UV-vis diffuse reflection spectroscopy (UV-vis DRS), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and high revolution transmission electron microscope (HRTEM). The performance of photocatalytic disinfection was investigated by the inactivation of Escherichia coli O157:H7. Both C 60 /C 3 N 4 and C 70 /C 3 N 4 hybrids showed similar crystalline structure and morphology with C 3 N 4 ; however, the two composites exhibited stronger bacterial inactivation than C 3 N 4 . In particular, C 70 /C 3 N 4 showed the highest bactericidal efficiency and was detrimental to all E. coli O157:H7 in 4h irradiation. Compared to C 3 N 4 , the enhancement of photocatalytic activity of composites could be attributed to the effective transfer of the photoinduced electrons under visible light irradiation. Owing to the excellent performance of fullerenes (C 60 , C 70 )/C 3 N 4 composites, a visible light response and environmental friendly photocatalysts for disinfection were achieved. Copyright © 2016. Published by Elsevier Inc.

Synthesis and electrical characterization of BaZr0.9Ho0.1O3-δ electrolyte ceramic for IT - SOFCs

NASA Astrophysics Data System (ADS)

Saini, Deepash S.; Singh, Lalit K.; Bhattacharya, D.

2018-04-01

A cost-effective modified combustion method using citric acid and glycine has recently been developed to synthesize high quality, and nanosized BaZr0.9Ho0.1O3 ceramic powder. BaZr0.9Ho0.1O3-δ ceramic powder was characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and field emission scanning electron microscopy (FESEM). XRD pattern of BaZr0.9Ho0.1O3-δ ceramic sintered at 1600 °C has shown that pure phase of BaZr0.9Ho0.1O3-δ with cubic Pm3¯m space group symmetry. The transmission electron microscopic investigation has shown that the particle size of the powder calcined at 1100 °C was in the range 30-80 nm. The FESEM image of sintered pellet at 1600 °C for 4 h reveals porous nature of BaZr0.9Ho0.1O3-δ with 83.7 relative density. Impedance analysis reveal three type relaxations in the temperature range 250 °C to 500 °C as studied at different frequencies over 100 Hz to 1 MHz in air. The grain boundary conductivity of BaZr0.9Ho0.1O3-δ ceramic is found lower then grain (bulk) conductivity due to core-space charge layer behavior in grain boundary.

Gas Sensing Properties of ZnO-SnO2 Nanostructures.

PubMed

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

2015-02-01

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

Synthesis and characterization of RuS2 nanostructures.

PubMed

Díaz, David; Castillo-Blum, Silvia E; Alvarez-Fregoso, Octavio; Rodríguez-Gattorno, Geonel; Santiago-Jacinto, Patricia; Rendon, Luis; Ortiz-Frade, Luis; León-Paredes, Yolia-Judith

2005-12-08

Small naked ruthenium sulfide nanoparticles (NPs) with narrow size distribution (2.5 +/- 0.4 nm of diameter) were synthesized in DMSO colloidal dispersions, under mild reaction conditions and using commercial RuCl3 as precursor. To test the chemical reactivity with soft and hard bases, fresh presynthesized RuS2 colloids were mixed with triethylamine (N(Et)3) and ammonium tetrathiomolybdate ((NH4)2MoS4) dimethyl sulfoxide solutions. Naked N(Et)3 and [MoS4](2-)-capped RuS2 nanoparticle colloids were characterized using UV-visible electronic absorption and emission spectroscopies and high-resolution transmission electron microscopy (HR-TEM). It has also been shown that capped RuS2-[MoS4]2- nanoparticles yield MoO3 crystalline matrix by means of HR-TEM experiments. The emission spectra of RuS2 and N(Et)3-RuS2 dispersions show that both nanosized materials have strong fluorescence. The existence of the ruthenium precursor species in solution was established by cyclic voltammetry. Moreover, naked RuS2 NPs were mixed with a chemical mixture with composition similar to gasoline (dibenzothiophene (Bz2S, 400 ppm), hexane, and toluene (55:45% v/v)). The reaction mixture consisted of two phases; in the polar phase, we found evidences of a strong interaction of Bz2S and toluene with the naked RuS2 NPs. We have also obtained self-organized thin films of capped N(Et)3- and RuS2-[MoS4]2- nanoparticles. In both cases, the shape and thickness of the resulting thin films were controlled by a dynamic vacuum procedure. The thin films have been characterized by atomic force microscopy, scanning electron microscopy, HR-TEM, energy dispersion spectroscopy, X-ray diffraction, and absorbance and fluorescence spectroscopies.

Surface Nanocrystallization and Amorphization of Dual-Phase TC11 Titanium Alloys under Laser Induced Ultrahigh Strain-Rate Plastic Deformation

PubMed Central

Luo, Sihai; Zhou, Liucheng; Wang, Xuede; Cao, Xin; Nie, Xiangfan

2018-01-01

As an innovative surface technology for ultrahigh strain-rate plastic deformation, laser shock peening (LSP) was applied to the dual-phase TC11 titanium alloy to fabricate an amorphous and nanocrystalline surface layer at room temperature. X-ray diffraction, transmission electron microscopy, and high-resolution transmission electron microscopy (HRTEM) were used to investigate the microstructural evolution, and the deformation mechanism was discussed. The results showed that a surface nanostructured surface layer was synthesized after LSP treatment with adequate laser parameters. Simultaneously, the behavior of dislocations was also studied for different laser parameters. The rapid slipping, accumulation, annihilation, and rearrangement of dislocations under the laser-induced shock waves contributed greatly to the surface nanocrystallization. In addition, a 10 nm-thick amorphous structure layer was found through HRTEM in the top surface and the formation mechanism was attributed to the local temperature rising to the melting point, followed by its subsequent fast cooling. PMID:29642379

Surface Nanocrystallization and Amorphization of Dual-Phase TC11 Titanium Alloys under Laser Induced Ultrahigh Strain-Rate Plastic Deformation.

PubMed

Luo, Sihai; Zhou, Liucheng; Wang, Xuede; Cao, Xin; Nie, Xiangfan; He, Weifeng

2018-04-06

As an innovative surface technology for ultrahigh strain-rate plastic deformation, laser shock peening (LSP) was applied to the dual-phase TC11 titanium alloy to fabricate an amorphous and nanocrystalline surface layer at room temperature. X-ray diffraction, transmission electron microscopy, and high-resolution transmission electron microscopy (HRTEM) were used to investigate the microstructural evolution, and the deformation mechanism was discussed. The results showed that a surface nanostructured surface layer was synthesized after LSP treatment with adequate laser parameters. Simultaneously, the behavior of dislocations was also studied for different laser parameters. The rapid slipping, accumulation, annihilation, and rearrangement of dislocations under the laser-induced shock waves contributed greatly to the surface nanocrystallization. In addition, a 10 nm-thick amorphous structure layer was found through HRTEM in the top surface and the formation mechanism was attributed to the local temperature rising to the melting point, followed by its subsequent fast cooling.

Effect of cobalt doping on structural and optical properties of ZnO nanoparticles

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

Singh, J.; Chanda, A., E-mail: anupamamatsc@gmail.com; Gupta, S.

Cobalt doped ZnO nanoparticles of uniform sizes were prepared by a chemical method using ZnCl{sub 2} and NaOH as the source materials. The formation of Co-doped ZnO nanoparticles was confirmed by transmission electron microscopy (TEM), high resolution TEM (HR-TEM) and selected area electron diffraction (SAED) studies. The optical properties of obtained products were examined using room temperature UV-visible and FTIR spectroscopy. SAED of cobalt doped ZnO nanoparticles shows homogeneous distribution of nanoparticles with hexagonal structure. The HRTEM image of the Co-doped ZnO nanoparticles reveals a clear lattice spacing of 0.52 nm corresponding to the interplanar spacing of wurtzite ZnO (002) plane.more » The absorption band at 857 cm{sup −1} in FTIR spectra confirmed the tetrahedral coordination of Zn and a shift of absorption peak to shorter wavelength region and decrease in absorbance with Co doping.is observed in UV-Visible spectra.« less

Fullerenes, PAH, Carbon Nanostructures, and Soot in Low Pressure Diffusion Flames

NASA Technical Reports Server (NTRS)

Grieco, William J.; Lafleur, Arthur L.; Rainey, Lenore C.; Taghizadeh, Koli; VanderSande, John B.; Howard, Jack B.

1997-01-01

The formation of fullerenes C60 and C7O is known to occur in premixed laminar benzene/oxygen/argon flames operated at reduced pressures. High resolution transmission electron microscopy (HRTEM) images of material collected from these flames has identified a variety of multishelled nanotubes and fullerene 'onions' as well as some trigonous structures. These fullerenes and nanostructures resemble the material that results from commercial fullerene production systems using graphite vaporization. As a result, combustion is an interesting method for fullerenes synthesis. If commercial scale operation is to be considered, the use of diffusion flames might be safer and less cumbersome than premixed flames. However, it is not known whether diffusion flames produce the types and yields of fullerenes obtained from premixed benzene/oxygen flames. Therefore, the formation of fullerenes and carbon nanostructures, as well as polycyclic aromatic hydrocarbons (PAH) and soot, in acetylene and benzene diffusion flames is being studied using high performance liquid chromatography (HPLC) and high resolution transmission electron microscopy (HRTEM).

Crystal Structure Variations of Sn Nanoparticles upon Heating

NASA Astrophysics Data System (ADS)

Mittal, Jagjiwan; Lin, Kwang-Lung

2018-04-01

Structural changes in Sn nanoparticles during heating below the melting point have been investigated using differential scanning calorimetry (DSC), x-ray diffraction (XRD) analysis, electron diffraction (ED), and high-resolution transmission electron microscopy (HRTEM). DSC revealed that the heat required to melt the nanoparticles (28.43 J/g) was about half compared with Sn metal (52.80 J/g), which was attributed to the large surface energy contribution for the nanoparticles. ED and XRD analyses of the Sn nanoparticles revealed increased intensity for crystal planes having large interplaner distances compared with regular crystal planes with increasing heat treatment temperature (HTT). HRTEM revealed an increase in interlayer spacing at the surface and near joints between nanoparticles with the HTT, leading to an amorphous structure of nanoparticles at the surface at 220°C. These results highlight the changes that occur in the morphology and crystal structure of Sn nanoparticles at the surface and in the interior with increase of the heat treatment temperature.

Transmission Electron Microscopy of Single Wall Carbon Nanotube/Polymer Nanocomposites: A First-Principles Study

NASA Technical Reports Server (NTRS)

Sola, Francisco; Xia, Zhenhai; Lebrion-Colon, Marisabel; Meador, Michael A.

2012-01-01

The physics of HRTEM image formation and electron diffraction of SWCNT in a polymer matrix were investigated theoretically on the basis of the multislice method, and the optics of a FEG Super TWIN Philips CM 200 TEM operated at 80 kV. The effect of nanocomposite thickness on both image contrast and typical electron diffraction reflections of nanofillers were explored. The implications of the results on the experimental applicability to study dispersion, chirality and diameter of nanofillers are discussed.

Preparation and physicochemical characterization of cellulose nanocrystals from industrial waste cotton

NASA Astrophysics Data System (ADS)

Thambiraj, S.; Ravi Shankaran, D.

2017-08-01

We aimed to develop a simple and low-cost method for the production of high-performance cellulose nanomaterials from renewable and sustainable resources. Here, cellulose microcrystals (CMCs) were prepared by controlled acidic and basic hydrolysis of cotton from textile industry wastes. The resulted CMCs were further converted into cellulose nanocrystals (CNCs) with high crystallinity by acidic hydrolysis. The physicochemical characteristics and morphological feature of CMCs and CNCs were studied by various analytical techniques such as UV-vis spectroscopy, Fourier-transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Fluorescence spectroscopy, Atomic force microscopy (AFM), High-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The isolated CNCs possess a needle-like morphological structure with the longitudinal and lateral dimensions of 180 ± 60 nm, 10 ± 1 nm, respectively. The AFM result reveals that the CNCs have a high aspect ratio of 40 ± 14 nm and the average thickness of 6.5 nm. The XRD and TEM analysis indicate that the synthesized CNCs possess face-centered cubic crystal structure. Preliminary experiments were carried out to fabricate CNCs incorporated poly (vinyl alcohol) (PVA) film. The results suggest that the concept of waste to wealth could be well executed from the prepared CNCs, which have great potential for various applications including bio-sensors, food packaging and drug delivery applications.

Catalytic reduction of hexavalent chromium by a novel nitrogen-functionalized magnetic ordered mesoporous carbon doped with Pd nanoparticles.

PubMed

Li, Sisi; Tang, Lin; Zeng, Guangming; Wang, Jiajia; Deng, Yaocheng; Wang, Jingjing; Xie, Zhihong; Zhou, Yaoyu

2016-11-01

Hexavalent chromium Cr(VI) is a toxic water pollutant which can cause serious influence to the health of the human and animals. Therefore, developing new methods to remove hexavalent chromium in water attracts great attention of scholars. In our research, we successfully synthesized a new type of magnetic mesoporous carbon hybrid nitrogen (Fe-NMC) loaded with catalyst Pd nanoparticles (NPs), which performed excellent catalytic reduction efficiency toward Cr(VI). The characterization of Pd/Fe-NMC composite was investigated in detail using scanning electron microscope (SEM), high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR), and nitrogen adsorption-desorption measurements. According to the experimental results, we dealt with in-depth discussion and studied on the mechanism of hexavalent chromium removed by Pd/Fe-NMC composite. Furthermore, the batch experiments were conducted to investigate the catalytic reduction ability of composite. It was found that the chromium reduction process conforms to pseudo-first-order reaction kinetics model when the concentrations of chromium and sodium formate were low. It took only 20 min for the Pd/Fe-NMC composite to reach 99.8 % reduction of Cr(VI) (50 mg/L). The results suggested that the Pd/Fe-NMC composite may exhibit significantly improved catalytic activity for the hexavalent chromium reduction at industrial wastewater.

Synthesis of new liquid crystals embedded gold nanoparticles for photoswitching properties.

PubMed

Rahman, Md Lutfor; Biswas, Tapan Kumar; Sarkar, Shaheen M; Yusoff, Mashitah Mohd; Yuvaraj, A R; Kumar, Sandeep

2016-09-15

A new series of liquid crystals decorated gold nanoparticles is synthesized whose molecular architecture has azobenzenes moieties as the peripheral units connected to gold nanoparticles (Au NPs) via alkyl groups. The morphology and mesomorphic properties were investigated by field emission scanning electron microscope, high-resolution transmission electron microscopy, differential scanning calorimetry and polarizing optical microscopy. The thiolated ligand molecules (3a-c) showed enantiotropic smectic A phase, whereas gold nanoparticles (5a-c) exhibit nematic and smectic A phase with monotropic nature. HR-TEM measurement showed that the functionalized Au NPs are of the average size of 2nm and they are well dispersed without any aggregation. The trans-form of azo compounds showed a strong band in the UV region at ∼378nm for the π-π(∗) transition, and a weak band in the visible region at ∼472nm due to the n-π(∗) transition. These molecules exhibit attractive photoisomerization behaviour in which trans-cis transition takes about 15s whereas the cis-trans transition requires about 45min for compound 5c. The extent of reversible isomerization did not decay after 10 cycles, which proved that the photo-responsive properties of 5c were stable and repeatable. Therefore, these materials may be suitably exploited in the field of molecular switches and the optical storage devices. Copyright © 2016 Elsevier Inc. All rights reserved.

Enhanced magneto-optical and photo-catalytic properties of transition metal cobalt (Co2+ ions) doped spinel MgFe2O4 ferrite nanocomposites

NASA Astrophysics Data System (ADS)

Abraham, A. Godlyn; Manikandan, A.; Manikandan, E.; Vadivel, S.; Jaganathan, S. K.; Baykal, A.; Renganathan, P. Sri

2018-04-01

In this study, spinel magnesium cobalt ferrite (CoxMg1-xFe2O4: x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0) nanocomposites were synthesized successfully by modified sol-gel combustion method. Magnesium nitrate, cobalt nitrate and iron nitrate were used as the source of divalent (Mg2+ and Co2+) and trivalent (Fe3+) cations, respectively and urea were used as the reducing (fuel) agent. The effects of cobalt ions on morphology, structural, optical, magnetic and photo-catalytic properties of spinel CoxMg1-xFe2O4 nanocomposites were investigated. Various characterization methods, including X-ray powder diffraction (XRD), high resolution scanning electron microscope (HR-SEM), transmission electron microscopy (HR-TEM), energy-dispersive X-ray spectroscopy (EDX), Fourier transforms infrared (FT-IR) spectroscopy, vibrating sample magnetometer (VSM) and photo-catalytic degradation (PCD) activity were used to study the phase purity, microstructure, particle size, elemental composition, functional group determination, band gap calculation, magnetic properties and degradation efficiency of nanoparticles, respectively. The observed results showed that the final products consists cubic spinel phase with sphere-like nanoparticles morphologies. Furthermore, spinel Co0.6Mg0.4Fe2O4 nanocomposite showed highest PCD efficiency (98.55%) than other composition of ferrite nanoparticles.

Micro-structural characterization of precipitation-synthesized fluorapatite nano-material by transmission electron microscopy using different sample preparation techniques.

PubMed

Chinthaka Silva, G W; Ma, Longzhou; Hemmers, Oliver; Lindle, Dennis

2008-01-01

Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.

Covalent modification and exfoliation of graphene oxide using ferrocene

NASA Astrophysics Data System (ADS)

Avinash, M. B.; Subrahmanyam, K. S.; Sundarayya, Y.; Govindaraju, T.

2010-09-01

Large scale preparation of single-layer graphene and graphene oxide is of great importance due to their potential applications. We report a simple room temperature method for the exfoliation of graphene oxide using covalent modification of graphene oxide with ferrocene to obtain single-layer graphene oxide sheets. The samples were characterized by FESEM, HRTEM, AFM, EDAX, FT-IR, Raman and Mössbauer spectroscopic studies. HRTEM micrograph of the covalently modified graphene oxide showed increased interlayer spacing of ~2.4 nm due to ferrocene intercalation. The presence of single-layer graphene oxide sheets were confirmed by AFM studies. The covalently modified ferrocene-graphene oxide composite showed interesting magnetic behavior.Large scale preparation of single-layer graphene and graphene oxide is of great importance due to their potential applications. We report a simple room temperature method for the exfoliation of graphene oxide using covalent modification of graphene oxide with ferrocene to obtain single-layer graphene oxide sheets. The samples were characterized by FESEM, HRTEM, AFM, EDAX, FT-IR, Raman and Mössbauer spectroscopic studies. HRTEM micrograph of the covalently modified graphene oxide showed increased interlayer spacing of ~2.4 nm due to ferrocene intercalation. The presence of single-layer graphene oxide sheets were confirmed by AFM studies. The covalently modified ferrocene-graphene oxide composite showed interesting magnetic behavior. Electronic supplementary information (ESI) available: Magnetic data; AFM images; TEM micrographs; and Mössbauer spectroscopic data. See DOI: 10.1039/c0nr00024h

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

PubMed

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

2014-11-07

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

Low temperature deposition of nanocrystalline silicon carbide films by plasma enhanced chemical vapor deposition and their structural and optical characterization

NASA Astrophysics Data System (ADS)

Rajagopalan, T.; Wang, X.; Lahlouh, B.; Ramkumar, C.; Dutta, Partha; Gangopadhyay, S.

2003-10-01

Nanocrystalline silicon carbide (SiC) thin films were deposited by plasma enhanced chemical vapor deposition technique at different deposition temperatures (Td) ranging from 80 to 575 °C and different gas flow ratios (GFRs). While diethylsilane was used as the source for the preparation of SiC films, hydrogen, argon and helium were used as dilution gases in different concentrations. The effects of Td, GFR and dilution gases on the structural and optical properties of these films were investigated using high resolution transmission electron microscope (HRTEM), micro-Raman, Fourier transform infrared (FTIR) and ultraviolet-visible optical absorption techniques. Detailed analysis of the FTIR spectra indicates the onset of formation of SiC nanocrystals embedded in the amorphous matrix of the films deposited at a temperature of 300 °C. The degree of crystallization increases with increasing Td and the crystalline fraction (fc) is 65%±2.2% at 575 °C. The fc is the highest for the films deposited with hydrogen dilution in comparison with the films deposited with argon and helium at the same Td. The Raman spectra also confirm the occurrence of crystallization in these films. The HRTEM measurements confirm the existence of nanocrystallites in the amorphous matrix with a wide variation in the crystallite size from 2 to 10 nm. These results are in reasonable agreement with the FTIR and the micro-Raman analysis. The variation of refractive index (n) with Td is found to be quite consistent with the structural evolution of these films. The films deposited with high dilution of H2 have large band gap (Eg) and these values vary from 2.6 to 4.47 eV as Td is increased from 80 to 575 °C. The size dependent shift in the Eg value has also been investigated using effective mass approximation. Thus, the observed large band gap is attributed to the presence of nanocrystallites in the films.

One Dimensional Coordination Polymer of Zn(II) for Developing Multifunctional Nanoparticles.

PubMed

Agarwal, Rashmi A

2017-10-16

A variety of nanoparticles (NPs) including Ag, Au, Pd, Cr and mixed Cu/Fe have been synthesized in a non-activated (without solvent removal) one dimensional coordination polymer (CP) of Zn(II) via two different mechanisms, acid formation and redox activity of the framework. Main driving force to grow these NPs within the cavities of CP is the presence of free oxygens of one of the monodentate carboxylate groups of BDC ligand. These free oxygens act as anchoring sites for the metal ions of the metal precursors. Chemical and physical characteristics of the NPs within the framework have been evaluated by the high resolution transmission electron microscopic (HRTEM) images. Excluding Ag(0) and Pd(0) other NPs are present as combinations of their elemental as well as oxide forms (Au/Au 2 O 3 , Cr/Cr 2 O 3 /CrO 2 and Cu/Cu 2 O, Fe/FeO). Synthesized Ag NPs within the framework show remarkable antibacterial efficacy at extremely low concentrations. Ag, Au and Cu/Fe NPs show ferromagnetic properties within the framework at room temperature. This polymer has potential to sequester highly toxic Cr(VI) to non toxic Cr(0), Cr(III) and Cr(IV) species.

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

Krumeich, F., E-mail: krumeich@inorg.chem.ethz.ch; Mueller, E.; Wepf, R.A.

While HRTEM is the well-established method to characterize the structure of dodecagonal tantalum (vanadium) telluride quasicrystals and their periodic approximants, phase-contrast imaging performed on an aberration-corrected scanning transmission electron microscope (STEM) represents a favorable alternative. The (Ta,V){sub 151}Te{sub 74} clusters, the basic structural unit in all these phases, can be visualized with high resolution. A dependence of the image contrast on defocus and specimen thickness has been observed. In thin areas, the projected crystal potential is basically imaged with either dark or bright contrast at two defocus values close to Scherzer defocus as confirmed by image simulations utilizing the principlemore » of reciprocity. Models for square-triangle tilings describing the arrangement of the basic clusters can be derived from such images. - Graphical abstract: PC-STEM image of a (Ta,V){sub 151}Te{sub 74} cluster. Highlights: Black-Right-Pointing-Pointer C{sub s}-corrected STEM is applied for the characterization of dodecagonal quasicrystals. Black-Right-Pointing-Pointer The projected potential of the structure is mirrored in the images. Black-Right-Pointing-Pointer Phase-contrast STEM imaging depends on defocus and thickness. Black-Right-Pointing-Pointer For simulations of phase-contrast STEM images, the reciprocity theorem is applicable.« less

Soybean peroxidase immobilized onto silica-coated superparamagnetic iron oxide nanoparticles: Effect of silica layer on the enzymatic activity.

PubMed

Donadelli, Jorge A; García Einschlag, Fernando S; Laurenti, Enzo; Magnacca, Giuliana; Carlos, Luciano

2018-01-01

Peroxidase immobilization onto magnetic supports is considered an innovative strategy for the development of technologies that involves enzymes in wastewater treatment. In this work, magnetic biocatalysts were prepared by immobilization of soybean peroxidase (SBP) onto different silica-coated superparamagnetic iron oxide nanoparticles. The obtained magnetic biocatalysts were tested for the degradation of malachite green (MG), a pollutant often found in industrial wastewaters and with significant drawbacks for the human and environmental health. A deep physicochemical characterization of the materials was performed by means of X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), High Resolution-Transmission Electron Microscope (HR-TEM) and magnetization measurements among others techniques. Results showed high immobilization yield of SBP onto nanomaterials with excellent properties for magnetic recoverability. A partial loss of activity with respect to free SBP was observed, compatible with the modification of the conformational structure of the enzyme after immobilization. The structural modification depended on the amount (and thickness) of silica present in the hybrid materials and the activity yield of 43% was obtained for the best biocatalyst. Thermal stability and reusability capacity were also evaluated. Copyright © 2017 Elsevier B.V. All rights reserved.

Multifunctional gold coated iron oxide core-shell nanoparticles stabilized using thiolated sodium alginate for biomedical applications.

PubMed

Sood, Ankur; Arora, Varun; Shah, Jyoti; Kotnala, R K; Jain, Tapan K

2017-11-01

In this paper we report synthesis of aqueous based gold coated iron oxide nanoparticles to integrate the localized surface plasma resonance (SPR) properties of gold and magnetic properties of iron oxide in a single system. Iron oxide-gold core shell nanoparticles were stabilized by attachment of thiolated sodium alginate to the surface of nanoparticles. Transmission electron microscope (TEM) micrograph presents an average elementary particle size of 8.1±2.1nm. High resolution TEM (HR-TEM) and X-ray photon spectroscopy further confirms the presence of gold shell around iron oxide core. Gold coating is responsible for reducing saturation magnetization (M s ) value from ~41emu/g to ~24emu/g - in thiolated sodium alginate stabilized gold coated iron oxide core-shell nanoparticles. The drug (curcumin) loading efficiency for the prepared nanocomposites was estimated to be around 7.2wt% (72μgdrug/mg nanoparticles) with encapsulation efficiency of 72.8%. Gold-coated iron oxide core-shell nanoparticles could be of immense importance in the field of targeted drug delivery along with capability to be used as contrast agent for MRI & CT. Copyright © 2017 Elsevier B.V. All rights reserved.

Anomalous Epitaxial Growth in Thermally Sprayed YSZ and LZ Splats

NASA Astrophysics Data System (ADS)

Chen, Lin; Yang, Guan-Jun

2017-08-01

Thermally sprayed coatings are essentially layered materials, and lamellar interfaces are of great importance to coatings' performances. In the present study, to investigate the microstructures and defect features at thermally sprayed coating interfaces, homoepitaxial 8 mol.% yttria-stabilized zirconia (YSZ) and heteroepitaxial lanthanum zirconia (LZ) films were fabricated. The epitaxial interfaces were examined by high-resolution transmission electron microscope (HR-TEM) in detail. As a result, we report, for the first time, an anomalous incommensurate homoepitaxial growth with mismatch-induced dislocations in thermally sprayed YSZ splats to create a homointerface. We also find the anomalous heteroepitaxial growth in thermally sprayed LZ splats. The mechanism of the anomalous incommensurate growth was analyzed in detail. Essentially, it is a pseudo-heteroepitaxy because of the lattice mismatch between the film and the locally heated substrate, as the locally heated substrate is significantly strained by its cold surroundings. Moreover, the super-high-density dislocations were found in the interfacial region, which resulted from sufficient thermal fluctuations and extremely rapid cooling rates. Both the anomalous lattice mismatch and super-high-density dislocations lead to weak interfaces and violent cracking in thermally sprayed coatings. These were also the essential differences between the conventional and the present epitaxy by thermal spray technique.

Room temperature magnetic ordering, enhanced magnetization and exchange bias of GdMnO3 nanoparticles in (GdMnO3)0.70(CoFe2O4)0.30

NASA Astrophysics Data System (ADS)

Mitra, A.; Mahapatra, A. S.; Mallick, A.; Chakrabarti, P. K.

2017-02-01

Nanoparticles of GdMnO3 (GMO) are prepared by sol-gel method. To enhance the magnetic property and also to obtain the magnetic ordering at room temperature (RT), nanoparticles of GMO are incorporated in the matrix of CoFe2O4 (CFO). Desired crystallographic phases of CFO, GMO and GMO-CFO are confirmed by analyzing X-ray diffractrograms (XRD) using Rietveld method. The average size of nanoparticles and their distribution, crystallographic phase, nanocrystallinity etc. are studied by high-resolution transmission electron microscope (HRTEM). Magnetic hysteresis loops (M-H) of GMO-CFO under zero field cooled (ZFC) and field cooled (FC) conditions are observed at different temperatures down to 5 K. Magnetization vs. temperature (M-T) under ZFC and FC conditions are also recorded. Interestingly, exchange bias (EB) is found at low temperature which suggests the encapsulation of the ferromagnetic (FM) nanoparticles of GMO by the ferrimagnetic nanoparticles of CFO below 100 K. Enhanced magnetization, EB effect and RT magnetic ordering of GMO-CFO would be interesting for both theoretical and experimental investigations.

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Competitive-type displacement reaction for direct potentiometric detection of low-abundance protein.

PubMed

Zhang, Bing; Liu, Bingqian; Chen, Guonan; Tang, Dianping

2014-03-15

Prostate-specific antigen (PSA), one of the indications of possible prostate malignancy, is used as a biomarker for the diagnosis and prognosis of prostate cancer. Herein, we develop a new homogeneous potentiometric immunoassay for sensitive detection of low-concentration PSA without the need of sample separation and washing step. Two nanostructures including positively charged polyethyleneimine-poly(styrene-co-acrylic acid) (PEI-PSAA) nanospheres and negatively charged gold nanoparticles conjugated with anti-PSA antibody (Ab-AuNP) were first synthesized by using mulsifier-free emulsion copolymerization and wet chemistry method, respectively. Thereafter, the as-prepared PEI-PSAA was used as a pseudo hapten for the construction of immunosensing probe based on an electrostatic interaction between PEI-PSAA and Ab-AuNP. Upon target introduction, the added PSA competed with PEI-PASS for Ab-AuNP based on a specific antigen-antibody interaction, and displaced Ab-AuNP from PEI-PASS. The dissociated PEI-PASS was captured through the negatively charged Nafion- modified electrode, thereby resulting in the change of membrane potential. The fabrication process was characterized by using high-resolution transmission electron microscope (HRTEM), scanning electron microscope with energy-dispersive X-ray spectroscopy (SEM-EDX), surface plasmon resonance (SPR) and dynamic laser scattering (DLS) technique. Under optimal conditions, the output signal was indirectly proportional to the concentration of target PSA in the sample and exhibited a dynamic range from 0.1 to 50 ng/mL with a detection limit (LOD) of 0.04 ng/mL. Intra- and inter-assay coefficients of variation (CVs) were 6.8 and 7.5%, respectively. In addition, the methodology was evaluated for analysis of 12 clinical serum samples and showed good accordance between the results obtained by the developed immunosensing protocol and a commercialized enzyme-linked immunosorbent assay (ELISA) method. © 2013 Published by Elsevier B.V.

Enhanced photocatalytic efficiency of NiS/TiO{sub 2} composite catalysts using sunset yellow, an azo dye under day light illumination

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

Rajamanickam, D.; Dhatshanamurthi, P.; Shanthi, M., E-mail: shanthimsm@gmail.com

2015-01-15

Highlights: • NiS/TiO{sub 2} was successfully synthesized by sol–gel method. • This new method of preparation gives a homogeneous dispersion of NiS on TiO{sub 2}. • Degradation activity of NiS/TiO{sub 2} is found to be more efficient than other catalysts. • Addition of oxidants enhances the degradation efficiency significantly. • COD measurements reveal the complete mineralization of dye molecules. • The catalyst is found to be reusable. - Abstract: To improve the solar light induced photocatalytic application performances of TiO{sub 2}, in this study, the NiS modified TiO{sub 2} composite photocatalysts with various ratios of NiS to TiO{sub 2} weremore » prepared by sol–gel method. The catalyst was characterized by X-ray diffraction (XRD), high resolution scanning electron microscope (HR-SEM), high resolution transmission electron microscope (HR-TEM), energy dispersive spectra (EDS), diffuse reflectance spectra (DRS), photoluminescence spectra (PL), X-ray photoelectron spectroscopy (XPS), and Brunauer–Emmett–Teller (B–E–T) surface area measurement methods. The photocatalytic activity of NiS/TiO{sub 2} was investigated for the degradation of sunset yellow (SY) in aqueous solution using solar light. The NiS/TiO{sub 2} is found to be more efficient than prepared TiO{sub 2} and TiO{sub 2}–P25 at pH 7 for the mineralization of SY. The effects of operational parameters such as the amount of photocatalyst, dye concentration and initial pH on photo mineralization of SY have been analyzed. The degradation was strongly enhanced in the presence of oxidants such as H{sub 3}K{sub 5}O{sub 18}S{sub 4} (Oxone), KIO{sub 4}, and KBrO{sub 3}. The mineralization of SY has been identified by COD measurements. The catalyst is found to be reusable.« less

TEM investigations on twin boundary structures of feathery crystals in aluminum alloys during Bridgman solidification

NASA Astrophysics Data System (ADS)

Yang, Luyan; Li, Shuangming; Fan, Kai; Li, Yang; Zhong, Hong; Fu, Hengzhi

2018-06-01

Feathery crystals are an ensemble of twinned dendrites, and are characterized by a unique twin boundary (TB) structure in the solidification pattern of aluminum alloys. In this work, the high-density twinned dendrites of Al-4.5 wt% Cu alloys, produced during the Bridgman solidification, have been studied using electron backscattered diffraction (EBSD) and high-resolution transmission electron microscopy (HRTEM). The experimental results showed that, after systematically decreasing the growth rate from 3000 μm/s to 1 μm/s, the TBs remained stable, while the solute field around the TBs changed significantly. According to the HRTEM results, successive stacking faults were occurred near the TBs at 1 μm/s, while slight distortion was observed around the TBs at 3000 μm/s. The composition analysis revealed an obvious solute enrichment near the TBs. Furthermore, the solute gradient profile within the TBs became smoother with the decrease in the growth speed. This is due to the more sufficient solid-state back diffusion occurring perpendicular to the twin plane after the solidification.

Highly crystalline zinc incorporated hydroxyapatite nanorods' synthesis, characterization, thermal, biocompatibility, and antibacterial study

NASA Astrophysics Data System (ADS)

Udhayakumar, Gayathri; Muthukumarasamy, N.; Velauthapillai, Dhayalan; Santhosh, Shanthi Bhupathi

2017-10-01

Highly crystalline zinc incorporated hydroxyapatite (Zn-HAp) nanorods have been synthesized using microwave irradiation method. To improve bioactivity and crystallinity of pure HAp, zinc was incorporated into it. As-synthesized samples were characterized by Fourier transform-infrared spectroscopy (FT-IR), X-ray diffraction, field-emission scanning electron microscopy (FESEM), energy dispersive X-ray analysis (EDAX), high-resolution transmission electron microscopy (HRTEM), and the thermal and crystallinity behavior of Zn-HAp nanoparticle were studied by thermogravimetry (TGA) and differential scanning calorimetry (DSC). Antibacterial activity of the as-synthesized nanorods was evaluated against two prokaryotic strains ( Escherichia coli and Staphylococcus aureus). The FT-IR studies show the presence of hydroxide and phosphate functional groups. HRTEM and FESEM images showed highly crystalline rod-shaped nanoparticles with the diameter of about 50-60 nm. EDAX revealed the presence of Ca, Zn, P, and O in the prepared samples. The crystallinity and thermal stability were further confirmed by TGA-DSC analysis. The biocompatibility evaluation results promoted that the Zn-HAp nanorods are biologically active apatites and potentially promising bone-substitute biomaterials for orthopaedic application.

Direct observation of antisite defects in LiCoPO4 cathode materials by annular dark- and bright-field electron microscopy.

PubMed

Truong, Quang Duc; Devaraju, Murukanahally Kempaiah; Tomai, Takaaki; Honma, Itaru

2013-10-23

LiCoPO4 cathode materials have been synthesized by a sol-gel route. X-ray diffraction analysis confirmed that LiCoPO4 was well-crystallized in an orthorhombic structure in the Pmna space group. From the high-resolution transmission electron microscopy (HR-TEM) image, the lattice fringes of {001} and {100} are well-resolved. The HR-TEM image and selected area electron diffraction pattern reveal the highly crystalline nature of LiCoPO4 having an ordered olivine structure. The atom-by-atom structure of LiCoPO4 olivine has been observed, for the first time, using high-angle annular dark-field (HAADF) and annual bright-field scanning transmission electron microscopy. We observed the bright contrast in Li columns in the HAADF images and strong contrast in the ABF images, directly indicating the antisite exchange defects in which Co atoms partly occupy the Li sites. The LiCoPO4 cathode materials delivered an initial discharge capacity of 117 mAh/g at a C/10 rate with moderate cyclic performance. The discharge profile of LiCoPO4 shows a plateau at 4.75 V, revealing its importance as a potentially high-voltage cathode. The direct visualization of atom-by-atom structure in this work represents important information for the understanding of the structure of the active cathode materials for Li-ion batteries.

Modified Graphene with SnO2 Nanocomposites Using Thermal Decomposition Method and Sensing Behavior Towards NO2 Gas

NASA Astrophysics Data System (ADS)

Sharma, Vikram

2017-11-01

This is the first time the graphene sample has been functionalized with metal oxide nanoparticles by thermal decomposition process. In this paper, graphene has been synthesized from natural resources using flower petals as carbon feedstock by thermal exfoliation technique at temperatures 1300 °C and the synthesis of graphene-tin oxide (SnO2) nanocomposites has been done using chemical treatment followed by thermal decomposition method. The response versus time condition has been investigated for the fabricated sample. The electrical resistance w.r.t. temperature could be explained by the thermal generation of electron-hole pairs and carrier scattering by acoustic phonons. The structural, morphological and chemical composition studies of the nanocomposites were carried out by the Raman spectroscopy, x-ray diffraction spectroscopy, scanning electron microscopy (SEM), x-ray photoelectron spectroscopy and high-resolution transmission electron microscopy (HRTEM). The evidence of good-quality graphene is obtained from Raman spectroscopy studies. The SEM and HRTEM images have shown that SnO2 nanoparticles are well distributed in the multilayer electron transparent graphene films. The sensor response was found to lie between 8.25 and 9.36% at 500 ppm of nitrogen dioxide, and also resistance recovered quickly without any application of heat. We believe such chemical treatment of graphene could potentially be used to manufacture a new generation of low-power nano-NO2 sensors.

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

PubMed

Eibl, O

1995-02-15

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

Atom by atom: HRTEM insights into inorganic nanotubes and fullerene-like structures

PubMed Central

Sadan, Maya Bar; Houben, Lothar; Enyashin, Andrey N.; Seifert, Gotthard; Tenne, Reshef

2008-01-01

The characterization of nanostructures down to the atomic scale is essential to understand some physical properties. Such a characterization is possible today using direct imaging methods such as aberration-corrected high-resolution transmission electron microscopy (HRTEM), when iteratively backed by advanced modeling produced by theoretical structure calculations and image calculations. Aberration-corrected HRTEM is therefore extremely useful for investigating low-dimensional structures, such as inorganic fullerene-like particles and inorganic nanotubes. The atomic arrangement in these nanostructures can lead to new insights into the growth mechanism or physical properties, where imminent commercial applications are unfolding. This article will focus on two structures that are symmetric and reproducible. The first structure that will be dealt with is the smallest stable symmetric closed-cage structure in the inorganic system, a MoS2 nanooctahedron. It is investigated by means of aberration-corrected microscopy which allowed validating the suggested DFTB-MD model. It will be shown that structures diverging from the energetically most stable structures are present in the laser ablated soot and that the alignment of the different shells is parallel, unlike the bulk material where the alignment is antiparallel. These findings correspond well with the high-energy synthetic route and they provide more insight into the growth mechanism. The second structure studied is WS2 nanotubes, which have already been shown to have a unique structure with very desirable mechanical properties. The joint HRTEM study combined with modeling reveals new information regarding the chirality of the different shells and provides a better understanding of their growth mechanism. PMID:18838681

Atom by atom: HRTEM insights into inorganic nanotubes and fullerene-like structures.

PubMed

Bar Sadan, Maya; Houben, Lothar; Enyashin, Andrey N; Seifert, Gotthard; Tenne, Reshef

2008-10-14

The characterization of nanostructures down to the atomic scale is essential to understand some physical properties. Such a characterization is possible today using direct imaging methods such as aberration-corrected high-resolution transmission electron microscopy (HRTEM), when iteratively backed by advanced modeling produced by theoretical structure calculations and image calculations. Aberration-corrected HRTEM is therefore extremely useful for investigating low-dimensional structures, such as inorganic fullerene-like particles and inorganic nanotubes. The atomic arrangement in these nanostructures can lead to new insights into the growth mechanism or physical properties, where imminent commercial applications are unfolding. This article will focus on two structures that are symmetric and reproducible. The first structure that will be dealt with is the smallest stable symmetric closed-cage structure in the inorganic system, a MoS(2) nanooctahedron. It is investigated by means of aberration-corrected microscopy which allowed validating the suggested DFTB-MD model. It will be shown that structures diverging from the energetically most stable structures are present in the laser ablated soot and that the alignment of the different shells is parallel, unlike the bulk material where the alignment is antiparallel. These findings correspond well with the high-energy synthetic route and they provide more insight into the growth mechanism. The second structure studied is WS(2) nanotubes, which have already been shown to have a unique structure with very desirable mechanical properties. The joint HRTEM study combined with modeling reveals new information regarding the chirality of the different shells and provides a better understanding of their growth mechanism.

Structural stability of coplanar 1T-2H superlattice MoS2 under high energy electron beam.

PubMed

Reshmi, S; Akshaya, M V; Satpati, Biswarup; Basu, Palash Kumar; Bhattacharjee, K

2018-05-18

Coplanar heterojunctions composed of van der Waals layered materials with different structural polymorphs have drawn immense interest recently due to low contact resistance and high carrier injection rate owing to low Schottky barrier height. Present research has largely focused on efficient exfoliation of these layered materials and their restacking to achieve better performances. We present here a microwave assisted easy, fast and efficient route to induce high concentration of metallic 1T phase in the original 2H matrix of exfoliated MoS 2 layers and thus facilitating the formation of a 1T-2H coplanar superlattice phase. High resolution transmission electron microscopy (HRTEM) investigations reveal formation of highly crystalline 1T-2H hybridized structure with sharp interface and disclose the evidence of surface ripplocations within the same exfoliated layer of MoS 2 . In this work, the structural stability of 1T-2H superlattice phase during HRTEM measurements under an electron beam of energy 300 keV is reported. This structural stability could be either associated to the change in electronic configuration due to induction of the restacked hybridized phase with 1T- and 2H-regions or to the formation of the surface ripplocations. Surface ripplocations can act as an additional source of scattering centers to the electron beam and also it is possible that a pulse train of propagating ripplocations can sweep out the defects via interaction from specific areas of MoS 2 sheets.

Structural stability of coplanar 1T-2H superlattice MoS2 under high energy electron beam

NASA Astrophysics Data System (ADS)

Reshmi, S.; Akshaya, M. V.; Satpati, Biswarup; Basu, Palash Kumar; Bhattacharjee, K.

2018-05-01

Coplanar heterojunctions composed of van der Waals layered materials with different structural polymorphs have drawn immense interest recently due to low contact resistance and high carrier injection rate owing to low Schottky barrier height. Present research has largely focused on efficient exfoliation of these layered materials and their restacking to achieve better performances. We present here a microwave assisted easy, fast and efficient route to induce high concentration of metallic 1T phase in the original 2H matrix of exfoliated MoS2 layers and thus facilitating the formation of a 1T-2H coplanar superlattice phase. High resolution transmission electron microscopy (HRTEM) investigations reveal formation of highly crystalline 1T-2H hybridized structure with sharp interface and disclose the evidence of surface ripplocations within the same exfoliated layer of MoS2. In this work, the structural stability of 1T-2H superlattice phase during HRTEM measurements under an electron beam of energy 300 keV is reported. This structural stability could be either associated to the change in electronic configuration due to induction of the restacked hybridized phase with 1T- and 2H-regions or to the formation of the surface ripplocations. Surface ripplocations can act as an additional source of scattering centers to the electron beam and also it is possible that a pulse train of propagating ripplocations can sweep out the defects via interaction from specific areas of MoS2 sheets.

Application of high-angle annular dark field scanning transmission electron microscopy, scanning transmission electron microscopy-energy dispersive X-ray spectrometry, and energy-filtered transmission electron microscopy to the characterization of nanoparticles in the environment.

PubMed

Utsunomiya, Satoshi; Ewing, Rodney C

2003-02-15

A major challenge to the development of a fundamental understanding of transport and retardation mechanisms of trace metal contaminants (<10 ppm) is their identification and characterization at the nanoscale. Atomic-scale techniques, such as conventional transmission electron microscopy, although powerful, are limited by the extremely small amounts of material that are examined. However, recent advances in electron microscopy provide a number of new analytical techniques that expand its application in environmental studies, particularly those concerning heavy metals on airborne particulates or water-borne colloids. High-angle annular dark field scanning transmission electron microscopy (HAADF-STEM), STEM-energy-dispersive X-ray spectrometry (EDX), and energy-filtered TEM (EFTEM) can be effectively used to identify and characterize nanoparticles. The image contrast in HAADF-STEM is strongly correlated to the atomic mass: heavier elements contribute to brighter contrast. Gold nanocrystals in pyrite and uranium nanocrystals in atmospheric aerosols have been identified by HAADF-STEM and STEM-EDX mapping and subsequently characterized by high-resolution TEM (HRTEM). EFTEM was used to identify U and Fe nanocrystals embedded in an aluminosilicate. A rare, As-bearing nanophase, westerveldite (FeAs), was identified by STEM-EDX and HRTEM. The combined use of these techniques greatly expands the effective application of electron microscopy in environmental studies, especially when applied to metals of very low concentrations. This paper describes examples of how these electron microbeam techniques can be used in combination to characterize a low concentration of heavy metals (a few ppm) on nanoscale particles.

Pronounced effects of the nominal concentrations of WO3 and Ag: WO3 nano-plates (obtained by a co-precipitation method) on their structural, morphological and optical properties

NASA Astrophysics Data System (ADS)

Rajendran, V.; Deepa, B.

2018-03-01

Tungsten oxide and different concentration of silver (Ag)-doped tungsten oxide nano material were synthesized by co-precipitation technique. The functional vibrations, structure, and morphology of as-prepared nano material were studied by Fourier transmission infrared spectroscopy, X-ray diffraction, scanning electron microscopy (SEM) and High-resolution transmission electron microscopy (HR-TEM) techniques. The SEM and HR-TEM analysis revealed the formation of nano-plate/nano rods with an average diameter of 40-80 nm diameter and 1-1.5 mm length. Fluorescence (PL) and UV-visible absorption techniques have been used to study the optical properties of the prepared nanoparticles. The observed red shift in the visible absorption spectra confirmed the promoted electron-phonon interaction in WO3 and Ag: WO3 nanoparticles compared to bulk structures. The photoluminescence of nanocrystalline Ag2+ doped WO3 exhibited a strong violet-blue, blue-green emission. Concentration dependence of the emission intensity of Ag2+ in WO3 was studied, and the significant concentration was found to be 0.5% of Ag: WO3. The effluent dye degradation executed for the 0.5% of Ag: WO3 sample under the visible light which reveals the highest degradation efficiency in appropriate time.

Nanoscale monoclinic domains in epitaxial SrRuO{sub 3} thin films deposited by pulsed laser deposition

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

Ghica, C., E-mail: cghica@infim.ro; Negrea, R. F.; Nistor, L. C.

2014-07-14

In this paper, we analyze the structural distortions observed by transmission electron microscopy in thin epitaxial SrRuO{sub 3} layers used as bottom electrodes in multiferroic coatings onto SrTiO{sub 3} substrates for future multiferroic devices. Regardless of the nature and architecture of the multilayer oxides deposited on the top of the SrRuO{sub 3} thin films, selected area electron diffraction patterns systematically revealed the presence of faint diffraction spots appearing in forbidden positions for the SrRuO{sub 3} orthorhombic structure. High-resolution transmission electron microscopy (HRTEM) combined with Geometric Phase Analysis (GPA) evidenced the origin of these forbidden diffraction spots in the presence ofmore » structurally disordered nanometric domains in the SrRuO{sub 3} bottom layers, resulting from a strain-driven phase transformation. The local high compressive strain (−4% ÷ −5%) measured by GPA in the HRTEM images induces a local orthorhombic to monoclinic phase transition by a cooperative rotation of the RuO{sub 6} octahedra. A further confirmation of the origin of the forbidden diffraction spots comes from the simulated diffraction patterns obtained from a monoclinic disordered SrRuO{sub 3} structure.« less

Spinel NixZn1-xFe2O4 (0.0 ≤ x ≤ 1.0) nano-photocatalysts: Synthesis, characterization and photocatalytic degradation of methylene blue dye

NASA Astrophysics Data System (ADS)

Padmapriya, G.; Manikandan, A.; Krishnasamy, V.; Jaganathan, Saravana Kumar; Antony, S. Arul

2016-09-01

Spinel NixZn1-xFe2O4 (x = 0.0 to 1.0) nanoparticles were successfully synthesized by a simple microwave combustion method (MCM) using metal nitrates as raw materials and glycine as the fuel. The structural, morphological and opto-magnetic properties of the spinel NixZn1-xFe2O4 ferrites were determined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray (EDX) spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED) pattern, UV-Visible diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). Powder XRD, and EDX analysis was confirmed the formation of pure phase of spinel ferrites. HR-SEM and HR-TEM analysis was confirmed the formation of sphere like-particle morphology of the samples with smaller agglomeration. VSM analysis clearly showed the superparamagnetic and ferromagnetic nature of the samples. The Ms value is 3.851 emu/g for undoped ZnFe2O4 sample and it increased with increase in Ni content. Photo-catalytic degradation (PCD) of methylene blue (MB) dye using the samples were carried out and observed good PCD results.

Nano silver decorated polyacrylamide/dextran nanohydrogels hybrid composites for drug delivery applications.

PubMed

Prusty, Kalyani; Swain, Sarat K

2018-04-01

Herein, novel biodegradable, stimuli responsive, chemically cross-linked and porous polyacrylamide/dextran (PAM/D) nanohydrogels hybrid composites are synthesized by in situ polymerization technique with incorporation of reduced nano silver. The interaction of nano silver with PAM in presence of dextran is investigated by Fourier transforms infrared spectroscopy (FTIR) and X-ray diffraction (XRD) studies. The elemental composition of the hybrid nanohydrogels is studied by X-ray photoelectron spectroscopy (XPS) whereas; the surface morphology of nanohydrogels hybrid composites is studied by field emission scanning electron microscope (FESEM) by which, it is observed that, the silver nanoparticles are homogeneously dispersed throughout the nanohydrogel network. From high resolution transmission electron microscopy (HRTEM), the average size of silver nanoparticles is found to be 20nm. The swelling, deswelling and water retention properties of nanohydrogels hybrid composites are measured in order to investigate the release rate of the ornidazole drugs. The in vitro release rate of ornidazole drugs is found to be 98.5% in 6h. The antibacterial activities and the cytotoxicity tests along with positive and negative control of hybrid nanohydrogels are investigated. The loss modulus, gain modulus and complex viscosities are determined from rheological behaviour of the nanohydrogels. It is found that, the value of tanδ varies from 0.1 to 0.8. Nano silver decorated PAM/D nanohydrogels are stable, nontoxic with antibacterial behaviour may be suitable for drugs delivery vehicle. Copyright © 2017 Elsevier B.V. All rights reserved.

Atomic Scale Imaging of Nucleation and Growth Trajectories of an Interfacial Bismuth Nanodroplet.

PubMed

Li, Yingxuan; Bunes, Benjamin R; Zang, Ling; Zhao, Jie; Li, Yan; Zhu, Yunqing; Wang, Chuanyi

2016-02-23

Because of the lack of experimental evidence, much confusion still exists on the nucleation and growth dynamics of a nanostructure, particularly of metal. The situation is even worse for nanodroplets because it is more difficult to induce the formation of a nanodroplet while imaging the dynamic process with atomic resolution. Here, taking advantage of an electron beam to induce the growth of Bi nanodroplets on a SrBi2Ta2O9 platelet under a high resolution transmission electron microscope (HRTEM), we directly observed the detailed growth pathways of Bi nanodroplets from the earliest stage of nucleation that were previously inaccessible. Atomic scale imaging reveals that the dynamics of nucleation involves a much more complex trajectory than previously predicted based on classical nucleation theory (CNT). The monatomic Bi layer was first formed in the nucleation process, which induced the formation of the prenucleated clusters. Following that, critical nuclei for the nanodroplets formed both directly from the addition of atoms to the prenucleated clusters by the classical growth process and indirectly through transformation of an intermediate liquid film based on the Stranski-Krastanov growth mode, in which the liquid film was induced by the self-assembly of the prenucleated clusters. Finally, the growth of the Bi nanodroplets advanced through the classical pathway and sudden droplet coalescence. This study allows us to visualize the critical steps in the nucleation process of an interfacial nanodroplet, which suggests a revision of the perspective of CNT.

Fabrication of mesoporous cerium dioxide films by cathodic electrodeposition.

PubMed

Kim, Young-Soo; Lee, Jin-Kyu; Ahn, Jae-Hoon; Park, Eun-Kyung; Kim, Gil-Pyo; Baeck, Sung-Hyeon

2007-11-01

Mesoporous cerium dioxide (Ceria, CeO2) thin films have been successfully electrodeposited onto ITO-coated glass substrates from an aqueous solution of cerium nitrate using CTAB (Cetyltrimethylammonium Bromide) as a templating agent. The synthesized films underwent detailed characterizations. The crystallinity of synthesized CeO2 film was confirmed by XRD analysis and HR-TEM analysis, and surface morphology was investigated by SEM analysis. The presence of mesoporosity in fabricated films was confirmed by TEM and small angle X-ray analysis. As-synthesized film was observed from XRD analysis and HR-TEM image to have well-crystallized structure of cubic phase CeO2. Transmission electron microscopy and small angle X-ray analysis revealed the presence of uniform mesoporosity with a well-ordered lamellar phase in the CeO2 films electrodeposited with CTAB templating.

Electrical conductivity and morphology of electrochemical synthesized polyaniline/CuO nano composites

NASA Astrophysics Data System (ADS)

Ashokkumar, S. P.; Yesappa, L.; Vijeth, H.; Niranjana, M.; Devendrappa, H.

2018-05-01

Polyaniline (PANI) and Polyaniline/CuO nanocomposite have been synthesized by using electrochemical deposition method. The composite was characterized using Fourier transform infra-red spectroscopy (FT-IR) to confirm the chemical interaction changes, micro structural morphology was done by Field Emission Scanning Electronic Microscopy (FESEM) and High Resolution Transmission Electron Microscopy (HRTEM). The dielectric constant and AC conductivity are found to increases with increase in temperature range (303 to 393K), these results shows enhancement in electrical conductivity due to effect of nanocomposite.

Novel Crystalline SiO2 Nanoparticles via Annelids Bioprocessing of Agro-Industrial Wastes

PubMed Central

2010-01-01

The synthesis of nanoparticles silica oxide from rice husk, sugar cane bagasse and coffee husk, by employing vermicompost with annelids (Eisenia foetida) is reported. The product (humus) is calcinated and extracted to recover the crystalline nanoparticles. X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and dynamic light scattering (DLS) show that the biotransformation allows creating specific crystalline phases, since equivalent particles synthesized without biotransformation are bigger and with different crystalline structure. PMID:20802789

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

NASA Astrophysics Data System (ADS)

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

2006-11-01

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

Investigation of the nanoscale two-component ZnS-ZnO heterostructures by means of HR-TEM and X-ray based analysis

NASA Astrophysics Data System (ADS)

Pankin, I. A.; Polozhentsev, O. E.; Soldatov, M. A.; Bugaev, A. L.; Tsaturyan, A.; Lomachenko, K. A.; Guda, A. A.; Budnyk, A. P.; Lamberti, C.; Soldatov, A. V.

2018-06-01

This article is devoted to the spectroscopic characterization of ZnS-ZnO nanoscale heterostructures synthesized by the microwave-assisted solvothermal method. The synthesized samples were investigated by means of X-ray powder diffraction (XRPD), high energy resolution fluorescence detected X-ray absorption near-edge-structure (HERFD-XANES) spectroscopy, valence-to-core X-ray emission spectroscopy (VtC-XES) and high resolution transmission electron microscopy (HR-TEM) as well as energy dispersive X-ray spectroscopy (EDX). The average crystallite size estimated by the broadening of XRPD peaks increases from 2.7 nm to 3.7 nm in the temperature range from 100 °C to 150 °C. HR-TEM images show that nanoparticles are arranged in aggregates with the 60-200 nm size. Theoretical estimation shows that the systems synthesized at higher temperatures more prone to the agglomeration. The full profile Reitveld analysis of XRPD data reveals the formation of hexagonal zinc sulfide structure, whereas electron diffraction data reveal also the formation of cubic zinc sulfide and claim the polymorphous character of the system. High energy resolution Zn K-edge XANES data unambiguously demonstrate the presence of a certain amount of the zinc oxide which is likely to have an amorphous structure and could not be detected by XRPD. Qualitative analysis of XANES data allows deriving ZnS/ZnO ratio as a function of synthesis temperature. EDX analysis depicts homogeneous distribution of ZnS and amorphous ZnO phases across the conglomerates. A complementary element-selective valence to core X-ray emission spectroscopy evidences formation of two-component system and confirms estimations of ZnS/ZnO fractions obtained by linear combination fit of XANES data.

Neutron irradiation damage of nuclear graphite studied by high-resolution transmission electron microscopy and Raman spectroscopy

NASA Astrophysics Data System (ADS)

Krishna, R.; Jones, A. N.; McDermott, L.; Marsden, B. J.

2015-12-01

Nuclear graphite components are produced from polycrystalline artificial graphite manufacture from a binder and filler coke with approximately 20% porosity. During the operational lifetime, nuclear graphite moderator components are subjected to fast neutron irradiation which contributes to the change of material and physical properties such as thermal expansion co-efficient, young's modulus and dimensional change. These changes are directly driven by irradiation-induced changes to the crystal structure as reflected through the bulk microstructure. It is therefore of critical importance that these irradiation changes and there implication on component property changes are fully understood. This work examines a range of irradiated graphite samples removed from the British Experimental Pile Zero (BEPO) reactor; a low temperature, low fluence, air-cooled Materials Test Reactor which operated in the UK. Raman spectroscopy and high-resolution transmission electron microscopy (HRTEM) have been employed to characterise the effect of increased irradiation fluence on graphite microstructure and understand low temperature irradiation damage processes. HRTEM confirms the structural damage of the crystal lattice caused by irradiation attributed to a high number of defects generation with the accumulation of dislocation interactions at nano-scale range. Irradiation-induced crystal defects, lattice parameters and crystallite size compared to virgin nuclear graphite are characterised using selected area diffraction (SAD) patterns in TEM and Raman Spectroscopy. The consolidated 'D'peak in the Raman spectra confirms the formation of in-plane point defects and reflected as disordered regions in the lattice. The reduced intensity and broadened peaks of 'G' and 'D' in the Raman and HRTEM results confirm the appearance of turbulence and disordering of the basal planes whilst maintaining their coherent layered graphite structure.

Improvement of the piezoelectric properties in (K,Na)NbO3-based lead-free piezoelectric ceramic with two-phase co-existing state

NASA Astrophysics Data System (ADS)

Yamada, H.; Matsuoka, T.; Kozuka, H.; Yamazaki, M.; Ohbayashi, K.; Ida, T.

2015-06-01

Two phases of (K,Na)NbO3 (KNN) co-exist in a KNN-based composite lead-free piezoelectric ceramic 0.910(K1-xNax)0.86Ca0.04Li0.02Nb0.85O3-δ-0.042K0.85Ti0.85Nb1.15O5-0.036BaZrO3-0.0016Co3O4- 0.0025Fe2O3-0.0069ZnO system, over a wide range of Na fractions, where 0.56 ≤ x ≤ 0.75. The crystal systems of the two KNN phases are identified to tetragonal and orthorhombic by analyzing the synchrotron powder X-ray diffraction (XRD) data, high-resolution transmission electron microscopy (HR-TEM), and selected-area electron diffraction (SAD). In the range 0.33 ≤ x ≤ 0.50, the main component of the composite system is found to be single-phase KNN with a tetragonal structure. Granular nanodomains of the orthorhombic phase dispersed in the tetragonal matrix have been identified by HR-TEM and SAD for 0.56 ≤ x ≤ 0.75. Only a trace amount of the orthorhombic phase has been found in the SAD patterns at the composition x = 0.56. However, the number of orthorhombic nanodomains gradually increases with increasing Na content up to x < 0.75, as observed from the HR-TEM images. An abrupt increase and agglomeration of the nanodomains are observed at x = 0.75, where weak diffraction peaks of the orthorhombic phase have also become detectable from the XRD data. The maximum value of the electromechanical coupling coefficient, kp = 0.56, has been observed at the composition x = 0.56.

Science 101: How Does an Electron Microscope Work?

ERIC Educational Resources Information Center

Robertson, Bill

2013-01-01

Contrary to popular opinion, electron microscopes are not used to look at electrons. They are used to look for structure in things that are too small to observe with an optical microscope, or to obtain images that are magnified much more than is obtainable with an optical microscope. To understand how electron microscopes work, it will help to go…

HRTEM of microcrystalline opal in chert and porcelanite from the Monterey Formation, California

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

Cady, S.L.; Wenk, H.R.; Downing, K.H.

Microcrystalline opal was investigated using low-dose transmission electron microscopy (TEM) methods to identify microstructural characteristics and possible phase-transformation mechanisms that accommodate silica diagenesis. High-resolution TEM (HRTEM) revealed that microcrystalline opal in opal-CT chert (>90 wt% silica) and opal-CT porcelanite (50-90 wt% silica) from the Miocene Monterey Formation of California displays various amounts of structural disorder and coherent and incoherent lamellar intergrowths. Species of microfibrous opal identified by HRTEM in early-formed opal-CT chert include length-slow opal-C and unidimensionally disordered length-slow opal-CT ({open_quotes}lussatite{close_quotes}). These fibers often display a microstructure characterized by an aperiodic distribution of highly strained domains that separate ordered domainsmore » located at discrete positions along the direction of the fiber axes. Microfibrous opal occurs as several types of fiber-aggregation forms. TEM revealed that the siliceous matrix in later-formed opal-CT porcelanite consists of equidimensional, nanometer-size opal-CT crystallites and lussatite fibers. Pseudo-orthorhombic tridymite (PO-2) was identified by HRTEM in one sample of opal-CT porcelanite. Burial diagenesis of chert and porcelanite results in the precipitation of opal-C and the epitaxial growth of opal-C domains on opal-CT substrates. Diagenetic maturation of lussatite was identified by TEM in banded opal-CT-quartz chert to occur as a result of solid-state ordering. The primary diagenetic silica phase transformations between noncrystalline opal, microcrystalline opal, and quartz occur predominantly by a series of dissolution-precipitation reactions. However, TEM showed that in banded opal-CT-quartz chert, the epitaxial growth of quartz on microfibrous opal enhances the rate of silica diagenesis.« less

Structural and physical properties of InAlAs quantum dots grown on GaAs

NASA Astrophysics Data System (ADS)

Vasile, B. S.; Daly, A. Ben; Craciun, D.; Alexandrou, I.; Lazar, S.; Lemaître, A.; Maaref, M. A.; Iacomi, F.; Craciun, V.

2018-04-01

Quantum dots (QDs), which have particular physical properties due to the three dimensions confinement effect, could be used in many advanced optoelectronic applications. We investigated the properties of InAlAs/AlGaAs QDs grown by molecular beam epitaxy on GaAs/Al0.5Ga0.5As layers. The optical properties of QDs were studied by low-temperature photoluminescence (PL). Two bandgap transitions corresponding to the X-Sh and X-Ph energy structure were observed. The QDs structure was investigated using high-resolution X-ray diffraction (HRXRD) and high-resolution transmission electron microscopy (HRTEM). HRXRD investigations showed that the layers grew epitaxially on the substrate, with no relaxation. HRTEM investigations confirmed the epitaxial nature of the grown structures. In addition, it was revealed that the In atoms aggregated in some prismatic regions, forming areas of high In concentration, that were still in perfect registry with the substrate.

Crystal-phase intergradation in InAs nanostructures grown by van der Waals heteroepitaxy on graphene

NASA Astrophysics Data System (ADS)

Choi, Ji Eun; Yoo, Jinkyoung; Lee, Donghwa; Hong, Young Joon; Fukui, Takashi

2018-04-01

This study demonstrates the crystal-phase intergradation of InAs nanostructures grown on graphene via van der Waals epitaxy. InAs nanostructures with diverse diameters are yielded on graphene. High-resolution transmission electron microscopy (HR-TEM) reveals two crystallographic features of (i) wurtzite (WZ)-to-zinc blende (ZB) intergradation along the growth direction of InAs nanostructures and (ii) an increased mean fraction of ZB according to diameter increment. Based on the HR-TEM observations, a crystal-phase intergradation diagram is depicted. We discuss how the formation of a WZ-rich phase during the initial growth stage is an effective way of releasing heterointerfacial stress endowed by the lattice mismatch of InAs/graphene for energy minimization in terms of less in-plane lattice mismatching between WZ-InAs and graphene. The WZ-to-ZB evolution is responsible for the attenuation of the bottom-to-top surface charge interaction as growth proceeds.

Influence of reaction time and synthesis temperature on the physical properties of ZnO nanoparticles synthesized by the hydrothermal method

NASA Astrophysics Data System (ADS)

Wasly, H. S.; El-Sadek, M. S. Abd; Henini, Mohamed

2018-01-01

Influence of synthesis temperature and reaction time on the structural and optical properties of ZnO nanoparticles synthesized by the hydrothermal method was investigated using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), energy-dispersive X-ray, Fourier transform infra-red spectroscopy, and UV-visible and fluorescence spectroscopy. The XRD pattern and HR-TEM images confirmed the presence of crystalline hexagonal wurtzite ZnO nanoparticles with average crystallite size in the range 30-40 nm. Their energy gap determined by fluorescence was found to depend on the synthesis temperature and reaction time with values in the range 2.90-3.78 eV. Thermal analysis, thermogravimetric and the differential scanning calorimetry were used to study the thermal reactions and weight loss with heat of the prepared ZnO nanoparticles.

Thin film assembly of nanosized cobalt(II) bis(5-phenyl-azo-8-hydroxyquinolate) using static step-by-step soft surface reaction technique: Structural characterization and optical properties.

PubMed

Seleim, S M; Hamdalla, Taymour A; Mahmoud, Mohamed E

2017-09-05

Nanosized (NS) cobalt (II) bis(5-phenyl-azo-8-hydroxyquinolate) (NS Co(II)-(5PA-8HQ) 2 ) thin films have been synthesized using static step-by-step soft surface reaction (SS-b-SSR) technique. Structural and optical characterizations of these thin films have been carried out using thermal gravimetric analysis (TGA), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD). The HR-TEM results revealed that the assembled Co(II)-complex exhibited a uniformly NS structure particles in the form of nanorods with width and length up to 16.90nm and 506.38nm, respectively. The linear and nonlinear optical properties have been investigated. The identified energy gap of the designed thin film materials was found 4.01eV. The refractive index of deposited Co(II)-complex thin film was identified by thickness-dependence and found as 1.9 at wavelength 1100nm. In addition, the refractive index was varied by about 0.15 due to an increase in the thickness by 19nm. Copyright © 2017 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

Structural and morphological peculiarities of hybrid Au/nanodiamond engineered nanostructures

NASA Astrophysics Data System (ADS)

Matassa, Roberto; Orlanducci, Silvia; Reina, Giacomo; Cassani, Maria Cristina; Passeri, Daniele; Terranova, Maria Letizia; Rossi, Marco

2016-08-01

Nanostructured Au nano-platelets have been synthesized from an Au(III) complex by growth process triggered by nanodiamond (ND). An electroless synthetic route has been used to obtain 2D Au/ND architectures, where individual nanodiamond particles are intimately embedded into face-centered cubic Au platelets. The combined use of high resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), was able to reveal the unusual organization of these hybrid nanoparticles, ascertaining the existence of preferential crystallographic orientations for both nanocrystalline species and highlighting their mutual locations. Detailed information on the sample microstructure have been gathered by fast Fourier transform (FFT) and inverse fast Fourier transform (IFFT) of HR-TEM images, allowing us to figure out the role of Au defects, able to anchor ND crystallites and to provide specific sites for heteroepitaxial Au growth. Aggregates constituted by coupled ND and Au, represent interesting systems conjugating the best optoelectronics and plasmonics properties of the two different materials. In order to promote realistically the applications of such outstanding Au/ND materials, the cooperative mechanisms at the basis of material synthesis and their influence on the details of the hybrid nanostructures have to be deeply understood.

Ion-induced crystal damage during plasma-assisted MBE growth of GaN layers

NASA Astrophysics Data System (ADS)

Kirchner, V.; Heinke, H.; Birkle, U.; Einfeldt, S.; Hommel, D.; Selke, H.; Ryder, P. L.

1998-12-01

Gallium nitride layers were grown by plasma-assisted molecular-beam epitaxy on (0001)-oriented sapphire substrates using an electron cyclotron resonance (ECR) and a radio frequency (rf) plasma source. An applied substrate bias was varied from -200 to +250 V, resulting in a change of the density and energy of nitrogen ions impinging the growth surface. The layers were investigated by high-resolution x-ray diffractometry and high-resolution transmission electron microscopy (HRTEM). Applying a negative bias during growth has a marked detrimental effect on the crystal perfection of the layers grown with an ECR plasma source. This is indicated by a change in shape and width of (0002) and (202¯5) reciprocal lattice points as monitored by triple axis x-ray measurements. In HRTEM images, isolated basal plane stacking faults were found, which probably result from precipitation of interstitial atoms. The crystal damage in layers grown with a highly negative substrate bias is comparable to that observed for ion implantation processes at orders of magnitude larger ion energies. This is attributed to the impact of ions on the growing surface. None of the described phenomena was observed for the samples grown with the rf plasma source.

Structural and morphological peculiarities of hybrid Au/nanodiamond engineered nanostructures

PubMed Central

Matassa, Roberto; Orlanducci, Silvia; Reina, Giacomo; Cassani, Maria Cristina; Passeri, Daniele; Terranova, Maria Letizia; Rossi, Marco

2016-01-01

Nanostructured Au nano-platelets have been synthesized from an Au(III) complex by growth process triggered by nanodiamond (ND). An electroless synthetic route has been used to obtain 2D Au/ND architectures, where individual nanodiamond particles are intimately embedded into face-centered cubic Au platelets. The combined use of high resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), was able to reveal the unusual organization of these hybrid nanoparticles, ascertaining the existence of preferential crystallographic orientations for both nanocrystalline species and highlighting their mutual locations. Detailed information on the sample microstructure have been gathered by fast Fourier transform (FFT) and inverse fast Fourier transform (IFFT) of HR-TEM images, allowing us to figure out the role of Au defects, able to anchor ND crystallites and to provide specific sites for heteroepitaxial Au growth. Aggregates constituted by coupled ND and Au, represent interesting systems conjugating the best optoelectronics and plasmonics properties of the two different materials. In order to promote realistically the applications of such outstanding Au/ND materials, the cooperative mechanisms at the basis of material synthesis and their influence on the details of the hybrid nanostructures have to be deeply understood. PMID:27514638

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

PubMed

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

2017-08-29

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

The Effect of Eu Doping on Microstructure, Morphology and Methanal-Sensing Performance of Highly Ordered SnO2 Nanorods Array

PubMed Central

Zhao, Yanping; Li, Yuehua; Ren, Xingping; Gao, Fan; Zhao, Heyun

2017-01-01

Layered Eu-doped SnO2 ordered nanoarrays constructed by nanorods with 10 nm diameters and several hundred nanometers length were synthesized by a substrate-free hydrothermal route using alcohol and water mixed solvent of sodium stannate and sodium hydroxide at 200 °C. The Eu dopant acted as a crystal growth inhibitor to prevent the SnO2 nanorods growth up, resulting in tenuous SnO2 nanorods ordered arrays. The X-ray diffraction (XRD) revealed the tetragonal rutile-type structure with a systematic average size reduction and unit cell volume tumescence, while enhancing the residual strain as the Eu-doped content increases. The surface defects that were caused by the incorporation of Eu ions within the surface oxide matrix were observed by high-resolution transmission electron microscope (HRTEM). The results of the response properties of sensors based on the different levels of Eu-doped SnO2 layered nanoarrays demonstrated that the 0.5 at % Eu-doped SnO2 layered nanorods arrays exhibited an excellent sensing response to methanal at 278 °C. The reasons of the enhanced sensing performance were discussed from the complicated defect surface structure, the large specific surface area, and the excellent catalytic properties of Eu dopant. PMID:29168796

Microstructure and Dry Sliding Wear Resistance of Laser Cladding Ti-Al-Si Composite Coating

NASA Astrophysics Data System (ADS)

Zhang, H. X.; Yu, H. J.; Chen, C. Z.; Dai, J. J.

In order to improve the wear resistance of Ti alloys, different mass ratios of Ti-Si-Al powders were designed to fabricate hard phases reinforced intermetallic matrix composite coatings on the Ti-6Al-4V substrate by laser cladding. The corresponding coatings were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive spectrometer (EDS) and high resolution transmission microscopy (HRTEM). The HV-1000 hardness tester and MM200 wear test machine were employed to test the hardness and the wear resistance of the composite coatings, respectively. The composite coatings mainly consisted of the reinforcements of Ti5Si3, Ti3AlC2 and Ti7Al5Si12 and the matrix of Ti3Al, TiAl, TiAl3 and α-Ti. The micro-hardness of the Ti-35Al-15Si coating was from 956 HV0.2 to 1130 HV0.2, which was approximately 3-4 times of the substrate and the highest in the three samples. The wear rate of the Ti-35Al-15Si coating was 0.023cm3ṡmin-1, which was about 1/4 of the Ti-6Al-4V substrate. It was the lowest in the three samples.

Spinel and orthopyroxene exsolved from clinopyroxene in the Haladala pluton in the middle Tianshan (Xinjiang, China)

NASA Astrophysics Data System (ADS)

Zhu, Yongfeng; Chen, Jing; Xue, Yunxin; Feng, Wanyi; Jiang, Jiuyang

2017-12-01

The Haladala pluton, consisting of troctolite, olivine gabbro and gabbro with zircon SHRIMP U-Pb age of 309 ± 2 Ma (MSWD = 0.72), intruded the Devonian-Carboniferous arc segments in the middle Tianshan. Amphibole, coexisting with magnetite, amphibole, and phlogopite, crystallized in a magma chamber at depth of 20 km (6.9-7.4 kbar, 934-943 °C) based on various thermobaramoters. Two kinds of exsolution textures (spinel rods in clinopyroxene, orthopyroxene lamellae in clinopyroxene) occur in troctolite and olivine gabbro. We describe oriented spinel rods and orthopyroxene lamellae exsolved from the host clinopyroxene based on optical and high-resolution transmission electron microscope (HRTEM) observations. The spinel rods (100) are parallel to their host clinopyroxene (010). Orthopyroxene lamellae (010) are coherent and strictly parallel to their host clinopyroxene (010). Exsolution of spinel rods from the host clinopyroxene is controlled by the reaction of (Ca0.5M2+ 0.5)Fe3+[AlSiO6]in clinopyroxene → (Ca0.86-0.17M2+ 0.14-0.17)(M2 + 1.00-0.96Al0-0.04)[Al0.17-0.10Si1.83-1.90O6] + Fe3O4 + O2.

Facile hydrothermal method for synthesizing nitrogen-doped graphene nanoplatelets using aqueous ammonia: dispersion, stability in solvents and thermophysical performances

NASA Astrophysics Data System (ADS)

Shafiah Shazali, Siti; Amiri, Ahmad; Zubir, Mohd. Nashrul Mohd; Rozali, Shaifulazuar; Zakuan Zabri, Mohd; Sabri, Mohd Faizul Mohd

2018-03-01

A simple and green approach has been developed to synthesize nitrogen-doped graphene nanoplatelets (N-doped GNPs) for mass production with a very high stability in different solvents e.g. water, ethylene glycol, methanol, ethanol, and 1-hexanol. The strategy is based on mild oxidation of GNPs using hydrogen peroxide and doping with nitrogen using hydrothermal process. The modification of N-doped GNPs was demonstrated by FTIR, TGA, XPS, Raman spectroscopy and high resolution-transmission electron microscope (HRTEM). Further study was carried out by using N-doped GNPs as an additive to prepare different colloidal dispersions. Water-based N-doped GNPs, methanol-based N-doped GNPs, ethanol-based N-doped GNPs, ethylene-glycol based N-doped GNPs and 1-hexanol-based N-doped GNPs dispersions at 0.01 wt.% shown great colloidal stabilities, indicating 17%, 29%, 33%, 18%, and 43% sedimentations after a 15-days period, respectively. The thermophysical properties e.g., viscosity and thermal conductivity of water-based N-doped GNP nanofluids were also evaluated for different weight concentrations of 0.100, 0.075, 0.050, and 0.025 wt.%. Through this, it is found that the obtained dispersions have great potential to be used as working fluids for industrial thermal systems.

Direct Correlation of Excitonics with Efficiency in a Core-Shell Quantum Dot Solar Cell.

PubMed

Dana, Jayanta; Maiti, Sourav; Tripathi, Vaidehi S; Ghosh, Hirendra N

2018-02-16

Shell thickness dependent band-gap engineering of quasi type II core-shell material with higher carrier cooling time, lower interfacial defect states, and longer charge carrier recombination time can be a promising candidate for both photocatalysis and solar cell. In the present investigation, colloidal CdSe@CdS core-shells with different shell thickness (2, 4 and 6 monolayer CdS) were synthesized through hot injection method and have been characterized by high resolution transmission electron microscope (HRTEM) followed by steady state absorption and luminescence techniques. Ultrafast transient absorption (TA) studies suggest longer carrier cooling, lower interfacial surface states, and slower carrier recombination time in CdSe@CdS core-shell with increasing shell thickness. By TA spectroscopy, the role of CdS shell in power conversion efficiency (PCE) has been explained in detail. The measured PCE was found to initially increase and then decrease with increasing shell thickness. Shell thickness has been optimized to maximize the efficiency after correlating the shell controlled carrier cooling and recombination with PCE values and a maximum PCE of 3.88 % was obtained with 4 monolayers of CdS shell, which is found to be 57 % higher than compared to bare CdSe QDs. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ag nanoparticles-decorated ZnO nanorod array on a mechanical flexible substrate with enhanced optical and antimicrobial properties

NASA Astrophysics Data System (ADS)

Chen, Yi; Tse, Wai Hei; Chen, Longyan; Zhang, Jin

2015-03-01

Heteronanostructured zinc oxide nanorod (ZnO NR) array are vertically grown on polydimethylsiloxane (PDMS) through a hydrothermal method followed by an in situ deposition of silver nanoparticles (Ag NPs) through a photoreduction process. The Ag-ZnO heterostructured nanorods on PDMS are measured with an average diameter of 160 nm and an average length of 2 μm. ZnO NRs measured by high-resolution transmission electron microscope (HRTEM) shows highly crystalline with a lattice fringe of 0.255 nm, which corresponds to the (0002) planes in ZnO crystal lattice. The average diameter of the Ag NPs in situ deposited on the ZnO NRs is estimated at 22 ± 2 nm. As compared to the bare ZnO NRs, the heterostructured Ag-ZnO nanorod array shows enhanced ultraviolet (UV) absorption at 440 nm, and significant emission in the visible region (λem = 542 nm). In addition, the antimicrobial efficiency of Ag-ZnO heterostructured nanorod array shows obvious improvement as compared to bare ZnO nanorod array. The cytotoxicity of ZnO nanorod array with and without Ag NPs was studied by using 3 T3 mouse fibroblast cell line. No significant toxic effect is imposed on the cells.

Ag nanoparticles-decorated ZnO nanorod array on a mechanical flexible substrate with enhanced optical and antimicrobial properties.

PubMed

Chen, Yi; Tse, Wai Hei; Chen, Longyan; Zhang, Jin

2015-01-01

Heteronanostructured zinc oxide nanorod (ZnO NR) array are vertically grown on polydimethylsiloxane (PDMS) through a hydrothermal method followed by an in situ deposition of silver nanoparticles (Ag NPs) through a photoreduction process. The Ag-ZnO heterostructured nanorods on PDMS are measured with an average diameter of 160 nm and an average length of 2 μm. ZnO NRs measured by high-resolution transmission electron microscope (HRTEM) shows highly crystalline with a lattice fringe of 0.255 nm, which corresponds to the (0002) planes in ZnO crystal lattice. The average diameter of the Ag NPs in situ deposited on the ZnO NRs is estimated at 22 ± 2 nm. As compared to the bare ZnO NRs, the heterostructured Ag-ZnO nanorod array shows enhanced ultraviolet (UV) absorption at 440 nm, and significant emission in the visible region (λem = 542 nm). In addition, the antimicrobial efficiency of Ag-ZnO heterostructured nanorod array shows obvious improvement as compared to bare ZnO nanorod array. The cytotoxicity of ZnO nanorod array with and without Ag NPs was studied by using 3 T3 mouse fibroblast cell line. No significant toxic effect is imposed on the cells.

Effect of temperature on magnetic and impedance properties of Fe3BO6 of nanotubular structure with a bonded B2O3 surface layer

NASA Astrophysics Data System (ADS)

Kumari, Kalpana; Ram, S.; Kotnala, R. K.

2018-03-01

In this investigation, we explore a facile synthesis of Fe3BO6 in the form of small crystallites in the specific shape of nanotubes crystallized from a supercooled liquid Fe2O3-B2O3 precursor. This study includes high resolution transmission electron microscopy (HRTEM) images, magnetic, optical, and impedance properties of the sample. HRTEM images reveal small tubes of Fe3BO6 of 20 nm diameter. A well resolved hysteresis loop appears at 5 K in which the magnetization does not saturate even up to as high field as 50 kOe. It means that the Fe3BO6 nanotubes behave as highly antiferromagnetic in nature in which the surface spins do not align along the field so easily. The temperature dependent impedance describes an ionic Fe3BO6 conductor with a reasonably small activation energy Ea ˜ 0.33 eV. Impedance formalism in terms of a Cole-Cole plot shows a deviation from an ideal Debye-like behavior. We have also reported that electronic absorption spectra are over a spectral range 200-800 nm of wavelengths in order to find out how a bonded surface layer present on the Fe3BO6 crystallites tunes the 3d → 3d electronic transitions in Fe3+ ions.

Association of the sites of heavy metals with nanoscale carbon in a Kentucky electrostatic precipitator fly ash

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

James C. Hower; Uschi M. Graham; Alan Dozier

2008-11-15

A combination of high-resolution transmission electron microscopy, scanning transmission electron microscopy, and electron energy-loss spectroscopy (HRTEM-STEM-EELS) was used to study fly ashes produced from the combustion of an eastern Kentucky coal at a southeastern-Kentucky wall-fired pulverized coal utility boiler retrofitted for low-NOx combustion. Fly ash was collected from individual hoppers in each row of the electrostatic precipitators (ESP) pollution-control system, with multiple hoppers sampled within each of the three rows. Temperatures within the ESP array range from about 200 {degree}C at the entry to the first row to <150{degree}C at the exit of the third row. HRTEM-STEM-EELS study demonstrated themore » presence of nanoscale (10 s nm) C agglomerates with typical soot-like appearance and others with graphitic fullerene-like nanocarbon structures. The minute carbon agglomerates are typically juxtaposed and intergrown with slightly larger aluminosilicate spheres and often form an ultrathin halo or deposit on the fly ash particles. The STEM-EELS analyses revealed that the nanocarbon agglomerates host even finer (<3 nm) metal and metal oxide particles. Elemental analysis indicated an association of Hg with the nanocarbon. Arsenic, Se, Pb, Co, and traces of Ti and Ba are often associated with Fe-rich particles within the nanocarbon deposits. 57 refs., 5 figs.« less

Iron silicide formation at different layers of (Fe/Si)3 multilayered structures determined by conversion electron Mössbauer spectroscopy

NASA Astrophysics Data System (ADS)

Badía-Romano, L.; Rubín, J.; Magén, C.; Bürgler, D. E.; Bartolomé, J.

2014-07-01

The morphology and the quantitative composition of the Fe-Si interface layer forming at each Fe layer of a (Fe/Si)3 multilayer have been determined by means of conversion electron Mössbauer spectroscopy (CEMS) and high-resolution transmission electron microscopy (HRTEM). For the CEMS measurements, each layer was selected by depositing the Mössbauer active 57Fe isotope with 95% enrichment. Samples with Fe layers of nominal thickness dFe = 2.6 nm and Si spacers of dSi = 1.5 nm were prepared by thermal evaporation onto a GaAs(001) substrate with an intermediate Ag(001) buffer layer. HRTEM images showed that Si layers grow amorphous and the epitaxial growth of the Fe is good only for the first deposited layer. The CEMS spectra show that at all Fe/Si and Si/Fe interfaces a paramagnetic c-Fe1-xSi phase is formed, which contains 16% of the nominal Fe deposited in the Fe layer. The bottom Fe layer, which is in contact with the Ag buffer, also contains α-Fe and an Fe1-xSix alloy that cannot be attributed to a single phase. In contrast, the other two layers only comprise an Fe1-xSix alloy with a Si concentration of ≃0.15, but no α-Fe.

Comparative study of image contrast in scanning electron microscope and helium ion microscope.

PubMed

O'Connell, R; Chen, Y; Zhang, H; Zhou, Y; Fox, D; Maguire, P; Wang, J J; Rodenburg, C

2017-12-01

Images of Ga + -implanted amorphous silicon layers in a 110 n-type silicon substrate have been collected by a range of detectors in a scanning electron microscope and a helium ion microscope. The effects of the implantation dose and imaging parameters (beam energy, dwell time, etc.) on the image contrast were investigated. We demonstrate a similar relationship for both the helium ion microscope Everhart-Thornley and scanning electron microscope Inlens detectors between the contrast of the images and the Ga + density and imaging parameters. These results also show that dynamic charging effects have a significant impact on the quantification of the helium ion microscope and scanning electron microscope contrast. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Ti, Ni and TiNi nanoparticles physically synthesized by Ar+ beam milling.

PubMed

Torres Castro, A; López Cuéllar, E; José Yacamán, M; Ortiz Méndez, U

2008-12-01

When the size of a particle decreases around 100 nm or less, there is a change in properties from those shown in the bulk material. In this work approximately 3 nm nanoparticles of Ni, Ti and TiNi bimetallic are produced using physical vapor deposition (PVD). Nanoparticles are characterized by High Resolution Transmission Electron Microscopy (HRTEM), High Angle Annular Dark Field (HAADF), Electron Diffraction (ED). The results show that all nanoparticles maintain the same crystal structure of bulk material but a change in their lattice parameter is produced.

Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies

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

Miehe, Gerhard; Lauterbach, Stefan; Kleebe, Hans-Joachim

The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH){sub 3}) to bixbyite-type indium oxide (c-In{sub 2}O{sub 3}). The electron beam is focused onto a single cube-shaped In(OH){sub 3} crystal of {l_brace}100{r_brace} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turnmore » enables the evaluation of the kinetics of c-In{sub 2}O{sub 3} crystallization. Supplementary material (video of the transformation) related to this article can be found online at (10.1016/j.jssc.2012.09.022). After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH){sub 3} is transformed to a diffuse strongly textured ring-like pattern of c-In{sub 2}O{sub 3} that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In{sub 2}O{sub 3} domains with the size of about 5-10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In{sub 2}O{sub 3}), calculated from the shrinkage of the parent c-In(OH){sub 3} crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In{sub 2}O{sub 3} crystallization within the framework of Avrami-Erofeev formalism. The Avrami exponent of {approx}3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive decomposition of c-In(OH){sub 3} to c-In{sub 2}O{sub 3} is discussed in terms of (i) the displacement of hydrogen atoms that lead to breaking the hydrogen bond between OH groups of [In(OH){sub 6}] octahedra and finally to their destabilization and (ii) transformation of the vertices-shared indium-oxygen octahedra in c-In(OH){sub 3} to vertices- and edge-shared octahedra in c-In{sub 2}O{sub 3}. - Graphical abstract: Frame-by-frame analysis of video sequences recorded of HR-TEM images reveals that a single cube-shaped In(OH){sub 3} nanocrystal with {l_brace}100{r_brace} morphology decomposes into bixbyite-type In{sub 2}O{sub 3} domains while being imaged. The mechanism of this decomposition is evaluated through the analysis of the structural relationship between initial (c-In(OH){sub 3}) and transformed (c-In{sub 2}O{sub 3}) phases and though the kinetics of the decomposition followed via the time-resolved shrinkage of the initial crystal of indium hydroxide. Highlights: Black-Right-Pointing-Pointer In-situ time-resolved High Resolution Transmission Electron Microscopy. Black-Right-Pointing-Pointer Crystallographic transformation path. Black-Right-Pointing-Pointer Kinetics of the decomposition in one nanocrystal.« less

Large area fabrication of plasmonic nanoparticle grating structure by conventional scanning electron microscope

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

Sudheer,, E-mail: sudheer@rrcat.gov.in; Tiwari, P.; Rai, V. N.

Plasmonic nanoparticle grating (PNG) structure of different periods has been fabricated by electron beam lithography using silver halide based transmission electron microscope film as a substrate. Conventional scanning electron microscope is used as a fabrication tool for electron beam lithography. Optical microscope and energy dispersive spectroscopy (EDS) have been used for its morphological and elemental characterization. Optical characterization is performed by UV-Vis absorption spectroscopic technique.

Direct evidence for organic carbon preservation as clay-organic nanocomposites in a Devonian black shale; from deposition to diagenesis

NASA Astrophysics Data System (ADS)

Kennedy, Martin John; Löhr, Stefan Carlos; Fraser, Samuel Alex; Baruch, Elizabeth Teresa

2014-02-01

The burial of marine sourced organic carbon (OC) in continental margin sediments is most commonly linked to oceanographic regulation of bottom-water oxygenation (anoxia) and/or biological productivity. Here we show an additional influence in the Devonian Woodford Shale, in which OC occurs as nanometer intercalations with specific phyllosilicate minerals (mixed-layer illite/smectite) that we term organo-mineral nanocomposites. High resolution transmission electron microscopic (HRTEM) images provide direct evidence of this nano-scale relationship. While discrete micron-scale organic particles, such as Tasmanites algal cysts, are present in some lamina, a strong relation between total organic carbon (TOC) and mineral surface area (MSA) over a range of 15% TOC indicate that the dominant association of organic carbon is with mineral surfaces and not as discrete pelagic grains, consistent with HRTEM images of nanocomposites. Where periods of oxygenation are indicated by bioturbation, this relationship is modified by a shift to lower OC loading on mineral surfaces and reduced MSA variability likely resulting from biological mixing and homogenization of the sediment, oxidative burn down of OC and/or stripping of OC from minerals in animal guts. The TOC-MSA relationship extends across a range of burial depths and thermal maturities into the oil window and persists through partial illitization. Where illitization occurs, the loss of mineral surface area associated with the collapse of smectite interlayer space results in a systematic increase in TOC:MSA and reorganization of organic carbon and clays into nano-scale aggregates. While the Woodford Shale is representative of black shale deposits commonly thought to record heightened marine productivity and/or anoxia, our results point to the importance of high surface area clay minerals for OC enrichment. Given that the vast majority of these clay minerals are formed in soils before being transported to continental margin settings, their mineralogy and attendant preservative potential is primarily a function of continental climate and provenance making these deposits a sensitive recorder of land as well as oceanographic change.

The effect of local atomic structure on the optical properties of GeSi self-assembled islands buried in silicon matrix

NASA Astrophysics Data System (ADS)

Demchenko, I. N.; Lawniczak-Jablonska, K.; Kret, S.; Novikov, A. V.; Laval, J.-Y.; Zak, M.; Szczepanska, A.; Yablonskiy, A. N.; Krasilnik, Z. F.

2007-03-01

The local atomic structure of GeSi self-assembled islands buried in a silicon matrix strongly influences the optical properties of such systems. In the present paper this structure was determined by x-ray absorption fine-structure (XAFS) spectroscopy and high resolution transmission electron microscopy (HRTEM) and used to build a schematic description of the band structure model. Quantitative analysis of the extended XAFS (EXAFS) spectrum was performed for three coordination shells around the Ge absorbing atom with multiple scattering taken into account. It was proved that the coordination number of elements in an alloy resulting from EXAFS analysis for all three coordination spheres (i.e. 'mixing degree' parameters) cannot be taken as the concentration of alloy but can be used together with a proper model of the alloy unit cell to calculate a realistic concentration. The fraction of Ge calculated in this way is consistent with HRTEM results. The found model of the unit cell was used to generate a x-ray absorption near edge structure spectrum by ab initio calculations. This approach yielded a spectrum in good agreement with the experimental one. The information gained from XAFS and HRTEM was then used for calculation of the band structure diagram. Results of the calculation are discussed and compared with the experimental photoluminescence spectrum.

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

Basak, Sushovan, E-mail: sushovanbasak@gmail.com; Das, Hrishikesh, E-mail: hrishichem@gmail.com; Pal, Tapan Kumar, E-mail: tkpal.ju@gmail.com

In order to meet the demand for lighter and more fuel efficient vehicles, a significant attempt is currently being focused toward the substitution of aluminum for steel in the car body structure. It generates vital challenge with respect to the methods of joining to be used for fabrication. However, the conventional fusion joining has its own difficulty owing to formation of the brittle intermetallic phases. In this present study AA6061-T6 of 2 mm and HIF-GA steel sheet of 1 mm thick are metal inert gas (MIG) brazed with 0.8 mm Al–5Si filler wire under three different heat inputs. The effectmore » of the heat inputs on bead geometry, microstructure and joint properties of MIG brazed Al-steel joints were exclusively studied and characterized by X-ray diffraction, field emission scanning electron microscopy (FESEM), electron probe micro analyzer (EPMA) and high resolution transmission electron microscopy (HRTEM) assisted X-ray spectroscopy (EDS) and selective area diffraction pattern. Finally microstructures were correlated with the performance of the joint. Diffusion induced intermetallic thickness measured by FESEM image and concentration profile agreed well with the numerically calculated one. HRTEM assisted EDS study was used to identify the large size FeAl{sub 3} and small size Fe{sub 2}Al{sub 5} type intermetallic compounds at the interface. The growth of these two phases in A2 (heat input: 182 J mm{sup −1}) is attributed to the slower cooling rate with higher diffusion time (~ 61 s) along the interface in comparison to the same for A1 (heat input: 155 J mm{sup −1}) with faster cooling rate and shorter diffusion time (~ 24 s). The joint efficiency as high as 65% of steel base metal is achieved for A2 which is the optimized parameter in the present study. - Highlights: • AA 6061 and HIF-GA could be successfully joined by MIG brazing. • Intermetallics are exclusively studied and characterized by XRD, FESEM and EPMA. • Intermetallic formation by diffusion is worth considering or not. • HRTEM-EDS, SAD pattern identifies the morphologies and size of intermetallics. • A compromise concerning formation of IMC is necessary.« less

Mechanical ball-milling preparation of fullerene/cobalt core/shell nanocomposites with high electrochemical hydrogen storage ability.

PubMed

Bao, Di; Gao, Peng; Shen, Xiande; Chang, Cheng; Wang, Longqiang; Wang, Ying; Chen, Yujin; Zhou, Xiaoming; Sun, Shuchao; Li, Guobao; Yang, Piaoping

2014-02-26

The design and synthesis of new hydrogen storage nanomaterials with high capacity at low cost is extremely desirable but remains challenging for today's development of hydrogen economy. Because of the special honeycomb structures and excellent physical and chemical characters, fullerenes have been extensively considered as ideal materials for hydrogen storage materials. To take the most advantage of its distinctive symmetrical carbon cage structure, we have uniformly coated C60's surface with metal cobalt in nanoscale to form a core/shell structure through a simple ball-milling process in this work. The X-ray diffraction (XRD), scanning electron microscope (SEM), Raman spectra, high-solution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectrometry (EDX) elemental mappings, and X-ray photoelectron spectroscopy (XPS) measurements have been conducted to evaluate the size and the composition of the composites. In addition, the blue shift of C60 pentagonal pinch mode demonstrates the formation of Co-C chemical bond, and which enhances the stability of the as-obtained nanocomposites. And their electrochemical experimental results demonstrate that the as-obtained C60/Co composites have excellent electrochemical hydrogen storage cycle reversibility and considerably high hydrogen storage capacities of 907 mAh/g (3.32 wt % hydrogen) under room temperature and ambient pressure, which is very close to the theoretical hydrogen storage capacities of individual metal Co (3.33 wt % hydrogen). Furthermore, their hydrogen storage processes and the mechanism have also been investigated, in which the quasi-reversible C60/Co↔C60/Co-Hx reaction is the dominant cycle process.

Morphology and magnetic characterisation of aluminium substituted yttrium-iron garnet nanoparticles prepared using sol gel technique.

PubMed

Yahya, Noorhana; Al Habashi, Ramadan Masoud; Koziol, Krzysztof; Borkowski, Rafal Dunin; Akhtar, Majid Niaz; Kashif, Muhammad; Hashim, Mansor

2011-03-01

Aluminum substituted yttrium iron garnet nano particles with compositional variation of Y(3.0-x) A1(x)Fe5O12, where x = 0.0, 0.5, 1.0, 1.5, 2.0, 2.5 and 3.0 were prepared using sol gel technique. The X-ray diffraction results showed that the best garnet phase appeared when the sintering temperature was 800 degrees C. Nano-crystalline particles with high purity and sizes ranging from 20 to 100 nm were obtained. It was found that the aluminum substitution had resulted in a sharp fall of the d-spacing when x = 2, which we speculated is due to the preference of the aluminum atoms to the smaller tetrahedron and octahedron sites instead of the much larger dodecahedron site. High resolution transmission electron microscope (HRTEM) and electron diffraction (ED) patterns showed single crystal nanoparticles were obtained from this method. The magnetic measurement gave moderate values of initial permeability; the highest value of 5.3 was shown by sample Y3Fe5O12 at more than 100 MHz which was attributed to the morphology of the microstructure which appeared to be homogeneous. This had resulted in an easy movement of domain walls. The substitution of aluminum for yttrium is speculated to cause a cubic to rhombodedral structural change and had weakened the super-exchange interactions thus a fall of real permeability was observed. This might have created a strain in the sub-lattices and had subsequently caused a shift of resonance frequencies to more than 1.8 GHz when x > 0.5.

Study on the Visible-Light Photocatalytic Performance and Degradation Mechanism of Diclofenac Sodium under the System of Hetero-Structural CuBi₂O₄/Ag₃PO₄ with H₂O₂.

PubMed

Chen, Xiaojuan; Li, Ning; Xu, Song; Wang, Hailong; Cai, Yumin

2018-03-28

Two kinds of CuBi₂O₄/Ag₃PO₄ with different heterojunction structures were prepared based on the combination of hydrothermal and in-situ precipitation methods with surfactant additives (sodium citrate and sodium stearate), and their characteristics were systematically resolved by X-ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), X-ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscope (SEM)/ High-resolution Transmission Electron Microscopy (HRTEM), UV-vis Diffuse Reflectance Spectra (DRS) and Photoluminescence (PL). Meanwhile, the photocatalytic properties of the catalysts were determined for diclofenac sodium (DS) degradation and the photocatalytic mechanism was also explored. The results indicate that both of the two kinds of CuBi₂O₄/Ag₃PO₄ exhibit higher photocatalytic efficiency, mineralization rate, and stability than that of pure CuBi₂O₄ or Ag₃PO₄. Moreover, the catalytic activity of CuBi₂O₄/Ag₃PO₄ can be further enhanced by adding H₂O₂. The free radical capture experiments show that in the pure CuBi₂O₄/Ag₃PO₄ photocatalytic system, the OH • and O₂ •- are the main species participating in DS degradation; however, in the CuBi₂O₄/Ag₃PO₄ photocatalytic system with H₂O₂, all OH • , h ⁺, and O₂ •- take part in the DS degradation, and the contribution order is OH • > h ⁺ > O₂ •- . Accordingly, the photocatalytic mechanism of CuBi₂O₄/Ag₃PO₄ could be explained by the Z-Scheme theory, while the catalysis of CuBi₂O₄/Ag₃PO₄ with H₂O₂ follows the heterojunction energy band theory.

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

Song, Bohang; Li, Wangda; Yan, Pengfei

A facile synthesis method was developed to prepare xLi 2MnO 3·(1-x)LiNi 0.7Co 0.15Mn 0.15O 2 (x = 0, 0.03, 0.07, 0.10, 0.20, and 0.30 as molar ratio) cathode materials, combining the advantages of high specific capacity from Ni-rich layered phase and surface chemical stability from Li-rich layered phase. X-ray diffraction (XRD), high resolution transmission electron microscope (HRTEM) and electrochemical charge/discharge performance confirm the formation of a Li-rich layered phase with C2/m symmetry. Most importantly, high-angle annular dark-field (HAADF) scanning transmission electron microscopy (STEM) reveals a spatial relationship that Li-rich nano-domain islands are integrated into a conventional Ni-rich layered matrix (Rmore » $$\\bar{3}$$m). This is the first time that Li-rich phase has been directly observed inside a particle at the nano-scale, when the overall composition of layered compounds (Li 1+δNi xMn yM 1-x-y-δO 2, M refers to transition metal elements) is Ni-rich (x > 0.5) rather than Mn-rich (y > 0.5). Remarkably, xLi 2MnO 3·(1-x)LiNi 0.7Co 0.15Mn 0.15O 2 cathode with optimized x value shows superior electrochemical performance at C/3, i.e., 170 mA h g -1 with 90.3 % of capacity retention after 400 cycles at 25 °C and 164 mA h g -1 with 81.3 % capacity retention after 200 cycles at 55 °C.« less

Structural and Kinetic Hydrogen Sorption Properties of Zr0.8Ti0.2Co Alloy Prepared by Ball Milling

PubMed Central

He, Hui; Tang, Tao; Huang, Zhiyong; Sang, Ge; Zhang, Guanghui; Ba, Jingwen; Liu, Meng

2018-01-01

The effects of ball milling on the hydrogen sorption kinetics and microstructure of Zr0.8Ti0.2Co have been systematically studied. Kinetic measurements show that the hydrogenation rate and amount of Zr0.8Ti0.2Co decrease with increasing the ball milling time. However, the dehydrogenation rate accelerates as the ball milling time increases. Meanwhile, the disproportionation of Zr0.8Ti0.2Co speeds up after ball milling and the disproportionation kinetics is clearly inclined to be linear with time at 500°C. It is found from X-ray powder diffraction (XRD) results that the lattice parameter of Zr0.8Ti0.2Co gradually decreases from 3.164 Å to 3.153 Å when the ball milling time extends from 0 h to 8 h, which is mainly responsible for the hydrogen absorption/desorption behaviors. In addition, scanning electron microscope (SEM) images demonstrate that the morphology of Zr0.8Ti0.2Co has obviously changed after ball milling, which is closely related to the hydrogen absorption kinetics. Besides, high-resolution transmission electron microscopy (HRTEM) images show that a large number of disordered microstructures including amorphous regions and defects exist after ball milling, which also play an important role in hydrogen sorption performances. This work will provide some insights into the principles of how to further improve the hydrogen sorption kinetics and disproportionation property of Zr0.8Ti0.2Co. PMID:29721128

Transmission electron microscope CCD camera

DOEpatents

Downing, Kenneth H.

1999-01-01

In order to improve the performance of a CCD camera on a high voltage electron microscope, an electron decelerator is inserted between the microscope column and the CCD. This arrangement optimizes the interaction of the electron beam with the scintillator of the CCD camera while retaining optimization of the microscope optics and of the interaction of the beam with the specimen. Changing the electron beam energy between the specimen and camera allows both to be optimized.

Controlling the size and optical properties of ZnO nanoparticles by capping with SiO{sub 2}

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

Babu, K. Sowri, E-mail: sowribabuk@gmail.com; Reddy, A. Ramachandra; Reddy, K. Venugopal

Graphical abstract: - Highlights: • Small and uniform sized ZnO nanoparticles were obtained with SiO{sub 2} coating. • ZnO and ZnO–SiO{sub 2} nanocomposite exhibited excitation wavelength dependent PL. • Maximum UV emission intensity was obtained with 353 nm excitation wavelength. • Excitation processes in SiO{sub 2} were also contributed to the UV intensity. • It was found that oxygen vacancies and interstitials enhanced with SiO{sub 2} coating. - Abstract: The size and shape of the ZnO nanoparticles synthesized through sol–gel method were controlled by capping with SiO{sub 2}. X-ray diffraction (XRD) and field emission scanning electron microscope (FE-SEM) and Highmore » Resolution Transmission Electron Microscope (HR-TEM) results demonstrated that the particle growth of the ZnO nanoparticles has been restricted to 5 nm with SiO{sub 2} capping. As a result, the absorption spectra of ZnO nanoparticles capped with SiO{sub 2} got blue shifted (toward lower wavelength side) due to strong quantum confinement effects. BET (Brunauer–Emmet–Teller) surface area pore size analyzer results showed that surface area of samples increased monotonously with increase of SiO{sub 2} concentration. It was observed that the absorption spectra of ZnO capped with SiO{sub 2} broadened with increase of SiO{sub 2} concentration. Absorption and photoluminescence excitation results (PLE) confirmed that this broadening is due to the absorption of non-bridging oxygen hole centers (NBOHC) of SiO{sub 2}. These results also indicated that ZnO nanoparticles capped with SiO{sub 2} are insensitive to Raman scattering. Maximum UV emission intensity was achieved with 353 nm excitation wavelength compared to 320 nm in ZnO as well as in SiO{sub 2} capped ZnO nanoparticles. Furthermore, there is an enhancement in the intensities of emission peaks related to oxygen vacancies and interstitials with SiO{sub 2} capping. The enhancement in the UV intensity is attributed to the surface passivation of ZnO nanoparticles and excitation processes in SiO{sub 2}.« less

76 FR 65696 - Battelle Energy Alliance, et al.;

Federal Register 2010, 2011, 2012, 2013, 2014

2011-10-24

... of Texas at Austin, Austin, TX 78712. Instrument: Electron Microscope. Manufacturer: FEI Company, the... research or scientific educational uses requiring an electron microscope. We know of no electron microscope...

Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies

NASA Astrophysics Data System (ADS)

Miehe, Gerhard; Lauterbach, Stefan; Kleebe, Hans-Joachim; Gurlo, Aleksander

2013-02-01

The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH)3) to bixbyite-type indium oxide (c-In2O3). The electron beam is focused onto a single cube-shaped In(OH)3 crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In2O3 crystallization. Supplementary material (video of the transformation) related to this article can be found online at 10.1016/j.jssc.2012.09.022. After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH)3 is transformed to a diffuse strongly textured ring-like pattern of c-In2O3 that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In2O3 domains with the size of about 5-10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In2O3), calculated from the shrinkage of the parent c-In(OH)3 crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In2O3 crystallization within the framework of Avrami-Erofeev formalism. The Avrami exponent of ˜3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive decomposition of c-In(OH)3 to c-In2O3 is discussed in terms of (i) the displacement of hydrogen atoms that lead to breaking the hydrogen bond between OH groups of [In(OH)6] octahedra and finally to their destabilization and (ii) transformation of the vertices-shared indium-oxygen octahedra in c-In(OH)3 to vertices- and edge-shared octahedra in c-In2O3.

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

Banfield, Jillian; Comolli, Luis R.; Singer, Steve

Of central interest in this study were microbial communities attached to sediment particles and in associated groundwater. Are the communities similar? What do the organisms look like and how do they associated with each other? Research was conducted on samples collected from the Department of Energy's (DOE) Rifle Integrated Field Research Challenge (IFRC) site in Rifle, Colorado, USA. This site served first as a test case for in situ bioremediation via biostimulation, and more recently as a location for studying the role of microbial communities in the carbon and other linked biogeochemical cycles. We addressed the question of the naturemore » of planktonic to sediment-attached microbial communities using field and laboratory experimental studies with a range of methods that provide 2- and 3-dimensional topological information coupled to information about chemical speciation, organism type, and activity levels. The research leveraged data from metagenomics and proteomics analyses that obtained through parallel work at the Rifle site in the context of the IFRC. In this project we integrated characterization methods with extensive genomic sequence information and associated environmental data to better understand the processes that occur within groundwater and sediment-attached communities. Notable is the range of characterization methods, including scanning transmission x-ray microscopy (STXM), micro-EXAFS/XANES and microdiffraction and 2D and 3D cryo-electron tomographic analysis, and high-resolutino transmission electron microscope (HRTEM) analysis to characterize these natural microbial communities. A cryo-TEM work was unique because samples for electron microscopic characterization were cryo-plunged directly on site immediately after sampling. This step minimizes post-collection alterations, including cell damages and change of redox state. Among many achievements documented in publications listed at the end of this report, we highlight the following: 1) The development of a platform for routine correlative cryogenic microscopy and spectroscopy with samples prepared on-site. 2) The determination of which organisms dominate planktonic and biofilm communities in the subsurface. 3) Identification of microorganism-mineral associations and discovery of a novel mechanism that sustains activity of iron-reducing bacteria. 4) The detection of bacteria from the OP11-OD1-WWE3 (etc.) radiation and elucidation of their remarkable structural organization by cryog-TEM cryo-electron tomograhpy (cryo-ET). 5) Extensive analysis of biofilms and documentation of the association of cells and Se minerals. 6) The comparison of expressed c-type cytochromes between pure cultures of G. bemidjiensis and related field populations, provided insight into possible molecular mechanisms for U(VI) reduction in the aquifer. At least sixteen publications will result from this project (partial support), which provide both graduate student and post doctoral training.« less

Characterization of crystal structure features of a SIMOX substrate

NASA Astrophysics Data System (ADS)

Eidelman, K. B.; Shcherbachev, K. D.; Tabachkova, N. Yu.; Podgornii, D. A.; Mordkovich, V. N.

2015-12-01

The SIMOX commercial sample (Ibis corp.) was investigated by a high-resolution X-ray diffraction (HRXRD), a high-resolution transmission electron microscopy (HRTEM) and an Auger electron spectroscopy (AES) to determine its actual parameters (the thickness of the top Si and a continuous buried oxide layer (BOX), the crystalline quality of the top Si layer). Under used implantation conditions, the thickness of the top Si and BOX layers was 200 nm and 400 nm correspondingly. XRD intensity distribution near Si(0 0 4) reciprocal lattice point was investigated. According to the oscillation period of the diffraction reflection curve defined thickness of the overtop silicon layer (220 ± 2) nm. HRTEM determined the thickness of the oxide layer (360 nm) and revealed the presence of Si islands with a thickness of 30-40 nm and a length from 30 to 100 nm in the BOX layer nearby "BOX-Si substrate" interface. The Si islands are faceted by (1 1 1) and (0 0 1) faces. No defects were revealed in these islands. The signal from Si, which corresponds to the particles in an amorphous BOX matrix, was revealed by AES in the depth profiles. Amount of Si single crystal phase at the depth, where the particles are deposited, is about 10-20%.

The microstructures of SCS-6 and SCS-8 SiC reinforcing fibers

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

Sattler, M.L.; Kinney, J.H.; Zywicz, E.

The microstructures of SCS-6 and SCS-8 SiC fibers have been examined and analyzed using high resolution transmission electron microscopy (HRTEM), microdiffraction, parallel electron energy loss spectroscopy (PEELS), x-ray diffraction and x-ray spectroscopy. The results of the study confirm findings from earlier studies wherein the microstructure of the fibers have been described as consisting of {beta}-SiC grown upon a monofilament turbostratic carbon core. The present study, however, provides much more detail regarding this microstructure. For example, PEELS spectroscopy and x-ray microscopy indicate that the composition of the SiC varies smoothly from SiC plus free C near the carbon core to SiCmore » at the midradial boundary. The SiC stoichiometry is roughly preserved from the midradial boundary to the exterior interface. HRTEM, microdiffraction, and dark field images provide evidence that the excess carbon is amorphous free carbon which is most likely situated at the grain boundaries of the SiC. The x-ray microscopy results are also consistent with the presence of two phases near the core which consist of SiC and free carbon having density less than graphite (2.25 g/cc). This complex microstructure may explain the recent observations of nonplanar failure in composites fabricated with SCS fibers.« less

Study on immobilization of yeast alcohol dehydrogenase on nanocrystalline Ni-Co ferrites as magnetic support.

PubMed

Shakir, Mohammad; Nasir, Zeba; Khan, Mohd Shoeb; Lutfullah; Alam, Md Fazle; Younus, Hina; Al-Resayes, Saud Ibrahim

2015-01-01

The covalent binding of yeast alcohol dehydrogenase (YADH) enzyme complex in a series of magnetic crystalline Ni-Co nanoferrites, synthesized via sol-gel auto combustion technique was investigated. The structural analysis, morphology and magnetic properties of Ni-Co nanoferrites were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), vibrating-sample magnetometer (VSM), high resolution transmission electron microscopy (HRTEM) and Fourier transform infrared spectroscopy (FTIR). The comparative analysis of the HRTEM micrographs of bare magnetic nanoferrite particles and particles immobilized with enzyme revealed an uniform distribution of the particles in both the cases without undergoing change in the size which was found to be in the range 20-30 nm. The binding of YADH to Ni-Co nanoferrites and the possible binding mechanism have been suggested by comparing the FTIR results. The binding properties of the immobilized YADH enzyme were also studied by kinetic parameters, optimum operational pH, temperature, thermal stability and reusability. The immobilized YADH exhibits enhanced thermal stability as compared to the free enzyme over a wide range of temperature and pH, and showed good durability after recovery by magnetic separation for repeated use. Copyright © 2014 Elsevier B.V. All rights reserved.

Optical and structural characterization of InAs/GaAs quantum wells

NASA Technical Reports Server (NTRS)

Ksendzov, A.; George, T.; Grunthaner, F. J.; Liu, J. K.; Rich, D. H.; Terhune, R. W.; Wilson, B. A.; Pollak, F. H.; Huang, Y.-S.

1991-01-01

Three InAs/GaAs single quantum wells of two-, three-, and four-monolayer thickness were characterized using optical and structural techniques. The results of high-resolution transmission electron (HRTEM) microscopy and optical studies which combine absorption, photoluminescence (PL), photoreflectance, and cathodoluminescence are presented. Using the polarization modulated absorptance technique, we observed two absorption features in our samples at 77 K. On the basis of their polarization properties and comparison with an envelope function calculation, these structures are assigned to transitions between the confined heavy-hole and confined and unconfined electron levels. Photoreflectance spectra of the three-monolayer sample in 77-300 K range show only the fundamental quantum well transition. The temperature dependence of this transition is approximately linear with a slope of 2.2 x 10 exp -4 eV/K, which is significantly lower than in both constituent materials. Comparison to the absorption data reveals that the PL spectra are affected by the carrier diffusion and therefore do not provide direct measure of the exciton density of states. The HRTEM images indicate that, while the interfaces of the two-monolayer sample are smooth and the well thickness is uniform, the four-monolayer sample has uneven interfaces and contains domains of two, three, and four monolayers.

As-pyrolyzed sugarcane bagasse possessing exotic field emission properties

NASA Astrophysics Data System (ADS)

Krishnia, Lucky; Yadav, Brajesh S.; Palnitkar, Umesh; Satyam, P. V.; Gupta, Bipin Kumar; Koratkar, Nikhil A.; Tyagi, Pawan K.

2018-06-01

The present study aims to demonstrate the application of sugarcane bagasse as an excellent field emitter. Field emission property of as-pyrolyzed sugarcane bagasse (p-SBg) before and after the plasma treatment has been investigated. It has been observed that electronic nature of p-SBg transformed from semiconducting to metallic after plasma treatment. Maximum current and turn-on field defined at 10 μA/cm2 was found to be 800 μA/cm2 and 2.2 V/μm for as-pyrolyzed sugarcane bagasse (p-SBg) and 25 μA/cm2 and 8.4 V/μm for H2-plasma treated p-SBg. These values are found to be better than the reported values for graphene and activated carbon. In this report, pyrolysis of bagasse has been carried in a thermal chemical vapor deposition (Th-CVD) system in inert argon atmosphere. Scanning electron microscopy (SEM), X-ray Diffraction (XRD), High-resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS) have been used to study the structure of both pre and post plasma-treated p-SBg bagasse's sample. HRTEM study reveals that carbonaceous structures such as 3D-nanographene oxide (3D-NGO), graphite nanodots (GNDs), carbon nanotubes (CNTs), and carbon onions are present in both pre-treated and plasma-treated p-SBg. Hence, we envision that the performed study will be a forwarding step to facilitate the application of p-SBg in display devices.

Comparison of the morphology, chemical composition and microstructure of cryptocrystalline graphite and carbon black

NASA Astrophysics Data System (ADS)

Quan, Ying; Liu, Qinfu; Zhang, Shilong; Zhang, Shuai

2018-07-01

The structures of cryptocrystalline graphite (CG) and carbon black (CB) have been analyzed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), organic elemental analysis (OEA), X-ray diffraction (XRD), RAMAN and high-resolution transmission electron microscopy (HRTEM). These results indicate that CG has the same elemental composition as CB, with carbon being the major element present. SL sample (CG with low graphitization degree) and CB exhibit similar microcrystalline structures. CG was shown to contain a layered graphitic structure that was significantly different to the primary spherical particles present in CB. It is proposed that these CG sheets may potentially be reduced and delaminated to afford multilayer graphene structures with improved material properties.

Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires

PubMed Central

Ibupoto, Zafar Hussain; Khun, Kimleang; Liu, Xianjie; Willander, Magnus

2013-01-01

Cetyltrimethyl ammonium bromide cationic (CTAB) surfactant was used as template for the synthesis of nanoclusters of ZnS composed of nanowires, by hydrothermal method. The structural and morphological studies were performed by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) techniques. The synthesized ZnS nanoclusters are composed of nanowires and high yield on the substrate was observed. The ZnS nanocrystalline consists of hexagonal phase and polycrystalline in nature. The chemical composition of ZnS nanoclusters composed of nanowires was studied by X-ray photo electron microscopy (XPS). This investigation has shown that the ZnS nanoclusters are composed of Zn and S atoms. PMID:28348350

Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires.

PubMed

Ibupoto, Zafar Hussain; Khun, Kimleang; Liu, Xianjie; Willander, Magnus

2013-09-09

Cetyltrimethyl ammonium bromide cationic (CTAB) surfactant was used as template for the synthesis of nanoclusters of ZnS composed of nanowires, by hydrothermal method. The structural and morphological studies were performed by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) techniques. The synthesized ZnS nanoclusters are composed of nanowires and high yield on the substrate was observed. The ZnS nanocrystalline consists of hexagonal phase and polycrystalline in nature. The chemical composition of ZnS nanoclusters composed of nanowires was studied by X-ray photo electron microscopy (XPS). This investigation has shown that the ZnS nanoclusters are composed of Zn and S atoms.

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

I. J. van Rooyen; E. Olivier; J. H Neethlin

Electron microscopy examinations of selected coated particles from the first advanced gas reactor experiment (AGR-1) at Idaho National Laboratory (INL) provided important information on fission product distribution and chemical composition. Furthermore, recent research using STEM analysis led to the discovery of Ag at SiC grain boundaries and triple junctions. As these Ag precipitates were nano-sized, high resolution transmission electron microscopy (HRTEM) examination was used to provide more information at the atomic level. This paper describes some of the first HRTEM results obtained by examining a particle from Compact 4-1-1, which was irradiated to an average burnup of 19.26% fissions permore » initial metal atom (FIMA), a time average, volume-averaged temperature of 1072°C; a time average, peak temperature of 1182°C and an average fast fluence of 4.13 x 1021 n/cm2. Based on gamma analysis, it is estimated that this particle may have released as much as 10% of its available Ag-110m inventory during irradiation. The HRTEM investigation focused on Ag, Pd, Cd and U due to the interest in Ag transport mechanisms and possible correlation with Pd, Ag and U previously found. Additionally, Compact 4-1-1 contains fuel particles fabricated with a different fuel carrier gas composition and lower deposition temperatures for the SiC layer relative to the Baseline fabrication conditions, which are expected to reduce the concentration of SiC defects resulting from uranium dispersion. Pd, Ag, and Cd were found to co-exist in some of the SiC grain boundaries and triple junctions whilst U was found to be present in the micron-sized precipitates as well as separately in selected areas at grain boundaries. This study confirmed the presence of Pd both at inter- and intragranular positions; in the latter case specifically at stacking faults. Small Pd nodules were observed at a distance of about 6.5 micron from the inner PyC/SiC interface.« less

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.

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

Yamada, H., E-mail: hide-yamada@mg.ngkntk.co.jp; Matsuoka, T.; Kozuka, H.

Two phases of (K,Na)NbO{sub 3} (KNN) co-exist in a KNN-based composite lead-free piezoelectric ceramic 0.910(K{sub 1−x}Na{sub x}){sub 0.86}Ca{sub 0.04}Li{sub 0.02}Nb{sub 0.85}O{sub 3−δ}–0.042K{sub 0.85}Ti{sub 0.85}Nb{sub 1.15}O{sub 5} –0.036BaZrO{sub 3}–0.0016Co{sub 3}O{sub 4}– 0.0025Fe{sub 2}O{sub 3}–0.0069ZnO system, over a wide range of Na fractions, where 0.56 ≤ x ≤ 0.75. The crystal systems of the two KNN phases are identified to tetragonal and orthorhombic by analyzing the synchrotron powder X-ray diffraction (XRD) data, high-resolution transmission electron microscopy (HR-TEM), and selected-area electron diffraction (SAD). In the range 0.33 ≤ x ≤ 0.50, the main component of the composite system is found to be single-phase KNN with a tetragonal structure. Granular nanodomains ofmore » the orthorhombic phase dispersed in the tetragonal matrix have been identified by HR-TEM and SAD for 0.56 ≤ x ≤ 0.75. Only a trace amount of the orthorhombic phase has been found in the SAD patterns at the composition x = 0.56. However, the number of orthorhombic nanodomains gradually increases with increasing Na content up to x < 0.75, as observed from the HR-TEM images. An abrupt increase and agglomeration of the nanodomains are observed at x = 0.75, where weak diffraction peaks of the orthorhombic phase have also become detectable from the XRD data. The maximum value of the electromechanical coupling coefficient, k{sub p} = 0.56, has been observed at the composition x = 0.56.« less

Imaging active topological defects in carbon nanotubes

NASA Astrophysics Data System (ADS)

Suenaga, Kazu; Wakabayashi, Hideaki; Koshino, Masanori; Sato, Yuta; Urita, Koki; Iijima, Sumio

2007-06-01

A single-walled carbon nanotube (SWNT) is a wrapped single graphene layer, and its plastic deformation should require active topological defects-non-hexagonal carbon rings that can migrate along the nanotube wall. Although in situ transmission electron microscopy (TEM) has been used to examine the deformation of SWNTs, these studies deal only with diameter changes and no atomistic mechanism has been elucidated experimentally. Theory predicts that some topological defects can form through the Stone-Wales transformation in SWNTs under tension at 2,000 K, and could act as a dislocation core. We demonstrate here, by means of high-resolution (HR)-TEM with atomic sensitivity, the first direct imaging of pentagon-heptagon pair defects found in an SWNT that was heated at 2,273 K. Moreover, our in situ HR-TEM observation reveals an accumulation of topological defects near the kink of a deformed nanotube. This result suggests that dislocation motions or active topological defects are indeed responsible for the plastic deformation of SWNTs.

Structural characterization of nano-oxide layers in PtMn based specular spin valves

NASA Astrophysics Data System (ADS)

Zhou, Min; Chen, Lifan; Diao, Zhitao; Park, Chang-Man; Huai, Yiming

2005-05-01

A systematic structure characterization of nano-oxide layers (NOLs) and specular spin valves using x-ray diffraction and high-resolution transmission electron microscopy (HRTEM) has been studied. High-angle x-ray diffraction data show almost identical fcc textures for both natural and plasma NOL spin-valves. Low-angle x-ray reflectivity spectrum shows more deteriorated Kiessig fringes at high incident angles for natural oxide sample, indicating rougher interfaces in natural oxidation than in plasma oxidation. Oxygen exposure plays an important role in NOLs process. Fabricating NOLs without any crystal structure degradation is critical to obtain high MR ratio. HRTEM reveals that oxide clusters mixing with insufficiently oxidized CoFe layers prevailed in natural NOL, and the natural oxidation was inhomogeneous. In contrast, plasma NOL has a thinner, more homogeneously oxidized CoFe layers with sharp interfaces. In plasma NOLs, the structures still maintain CoFe crystal structure. The structures and magnetic correlation of the NOL specular spin valves are discussed.

Detection of quantum well induced single degenerate-transition-dipoles in ZnO nanorods.

PubMed

Ghosh, Siddharth; Ghosh, Moumita; Seibt, Michael; Rao, G Mohan

2016-02-07

Quantifying and characterising atomic defects in nanocrystals is difficult and low-throughput using the existing methods such as high resolution transmission electron microscopy (HRTEM). In this article, using a defocused wide-field optical imaging technique, we demonstrate that a single ultrahigh-piezoelectric ZnO nanorod contains a single defect site. We model the observed dipole-emission patterns from optical imaging with a multi-dimensional dipole and find that the experimentally observed dipole pattern and model-calculated patterns are in excellent agreement. This agreement suggests the presence of vertically oriented degenerate-transition-dipoles in vertically aligned ZnO nanorods. The HRTEM of the ZnO nanorod shows the presence of a stacking fault, which generates a localised quantum well induced degenerate-transition-dipole. Finally, we elucidate that defocused wide-field imaging can be widely used to characterise defects in nanomaterials to answer many difficult questions concerning the performance of low-dimensional devices, such as in energy harvesting, advanced metal-oxide-semiconductor storage, and nanoelectromechanical and nanophotonic devices.

Towards single crystalline, highly monodisperse and catalytically active gold nanoparticles capped with probiotic Lactobacillus plantarum derived lipase

NASA Astrophysics Data System (ADS)

Khan, Imran; Nagarjuna, Ravikiran; Ray Dutta, Jayati; Ganesan, Ramakrishnan

2018-03-01

Owing to the eco-friendly nature of biomolecules, there lies a huge interest in exploring them as capping agents for nanoparticles to achieve stability and biocompatibility. Lipase extracted from the probiotic Lactobacillus plantarum is utilized for the first time to study its efficacy in capping gold nanoparticles (GNPs) in the room temperature synthesis using HAuCl4. The synthesized lipase-capped GNPs are characterized using UV-visible spectroscopy, FT-IR, HR-TEM, DLS and zeta potential measurements. Importantly, selected area electron diffraction (SAED) studies with HR-TEM have revealed the effect of lipase capping in tuning the polycrystallinity of the GNPs. The lipase-capped GNPs are explored for their catalytic efficiency towards an environmentally and industrially important conversion of 4-nitrophenol to 4-aminophenol. Exploiting the amine functional groups in the protein, the recoverability and reusability of the GNPs have been demonstrated through immobilization over amine-functionalized Fe3O4 nanoparticles.

Computer Simulations to Study Diffraction Effects of Stacking Faults in Beta-SiC: II. Experimental Verification. 2; Experimental Verification

NASA Technical Reports Server (NTRS)

Pujar, Vijay V.; Cawley, James D.; Levine, S. (Technical Monitor)

2000-01-01

Earlier results from computer simulation studies suggest a correlation between the spatial distribution of stacking errors in the Beta-SiC structure and features observed in X-ray diffraction patterns of the material. Reported here are experimental results obtained from two types of nominally Beta-SiC specimens, which yield distinct XRD data. These samples were analyzed using high resolution transmission electron microscopy (HRTEM) and the stacking error distribution was directly determined. The HRTEM results compare well to those deduced by matching the XRD data with simulated spectra, confirming the hypothesis that the XRD data is indicative not only of the presence and density of stacking errors, but also that it can yield information regarding their distribution. In addition, the stacking error population in both specimens is related to their synthesis conditions and it appears that it is similar to the relation developed by others to explain the formation of the corresponding polytypes.

Automatic software correction of residual aberrations in reconstructed HRTEM exit waves of crystalline samples

DOE PAGES

Ophus, Colin; Rasool, Haider I.; Linck, Martin; ...

2016-11-30

We develop an automatic and objective method to measure and correct residual aberrations in atomic-resolution HRTEM complex exit waves for crystalline samples aligned along a low-index zone axis. Our method uses the approximate rotational point symmetry of a column of atoms or single atom to iteratively calculate a best-fit numerical phase plate for this symmetry condition, and does not require information about the sample thickness or precise structure. We apply our method to two experimental focal series reconstructions, imaging a β-Si 3N 4 wedge with O and N doping, and a single-layer graphene grain boundary. We use peak and latticemore » fitting to evaluate the precision of the corrected exit waves. We also apply our method to the exit wave of a Si wedge retrieved by off-axis electron holography. In all cases, the software correction of the residual aberration function improves the accuracy of the measured exit waves.« less

Strain field mapping of dislocations in a Ge/Si heterostructure.

PubMed

Liu, Quanlong; Zhao, Chunwang; Su, Shaojian; Li, Jijun; Xing, Yongming; Cheng, Buwen

2013-01-01

Ge/Si heterostructure with fully strain-relaxed Ge film was grown on a Si (001) substrate by using a two-step process by ultra-high vacuum chemical vapor deposition. The dislocations in the Ge/Si heterostructure were experimentally investigated by high-resolution transmission electron microscopy (HRTEM). The dislocations at the Ge/Si interface were identified to be 90° full-edge dislocations, which are the most efficient way for obtaining a fully relaxed Ge film. The only defect found in the Ge epitaxial film was a 60° dislocation. The nanoscale strain field of the dislocations was mapped by geometric phase analysis technique from the HRTEM image. The strain field around the edge component of the 60° dislocation core was compared with those of the Peierls-Nabarro and Foreman dislocation models. Comparison results show that the Foreman model with a = 1.5 can describe appropriately the strain field around the edge component of a 60° dislocation core in a relaxed Ge film on a Si substrate.

Automatic software correction of residual aberrations in reconstructed HRTEM exit waves of crystalline samples

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

Ophus, Colin; Rasool, Haider I.; Linck, Martin

We develop an automatic and objective method to measure and correct residual aberrations in atomic-resolution HRTEM complex exit waves for crystalline samples aligned along a low-index zone axis. Our method uses the approximate rotational point symmetry of a column of atoms or single atom to iteratively calculate a best-fit numerical phase plate for this symmetry condition, and does not require information about the sample thickness or precise structure. We apply our method to two experimental focal series reconstructions, imaging a β-Si 3N 4 wedge with O and N doping, and a single-layer graphene grain boundary. We use peak and latticemore » fitting to evaluate the precision of the corrected exit waves. We also apply our method to the exit wave of a Si wedge retrieved by off-axis electron holography. In all cases, the software correction of the residual aberration function improves the accuracy of the measured exit waves.« less

Spectroscopic investigations on the orientation of 1,4-dibromonaphthalene on silver nanoparticles.

PubMed

Geetha, K; Umadevi, M; Sathe, G V; Erenler, R

2013-12-01

Silver nanoparticles (Ag NPs) have been prepared by solution combustion method with glycine as fuel. Silver nanoparticles were characterized by X-Ray Diffraction (XRD), High Resolution Transmission Electron Microscopy (HRTEM) and UV-visible spectroscopy. The prepared silver nanoparticles exhibit cubic crystalline structure with grain size of 59 nm. HRTEM image shows that the silver nanoparticles have strain and four-fold symmetry formed by twinning in the crystal structure. The optical adsorption spectrum shows that the surface plasmon resonance peak of silver is observed at 380 nm. The orientation of 1,4-dibromonaphthlaene (1,4-DBrN) on silver nanoparticles has been inferred from nRs and SERS spectral features. The absence of a C-H stretching vibrations, the observed high intense C-H out-of-plane bending modes and high intense C-Br stretching vibration suggest that the 1,4-DBrN molecule may be adsorbed in a 'stand-on' orientation to the surface. Copyright © 2013 Elsevier B.V. All rights reserved.

Orientation and phase mapping in the transmission electron microscope using precession-assisted diffraction spot recognition: state-of-the-art results.

PubMed

Viladot, D; Véron, M; Gemmi, M; Peiró, F; Portillo, J; Estradé, S; Mendoza, J; Llorca-Isern, N; Nicolopoulos, S

2013-10-01

A recently developed technique based on the transmission electron microscope, which makes use of electron beam precession together with spot diffraction pattern recognition now offers the possibility to acquire reliable orientation/phase maps with a spatial resolution down to 2 nm on a field emission gun transmission electron microscope. The technique may be described as precession-assisted crystal orientation mapping in the transmission electron microscope, precession-assisted crystal orientation mapping technique-transmission electron microscope, also known by its product name, ASTAR, and consists in scanning the precessed electron beam in nanoprobe mode over the specimen area, thus producing a collection of precession electron diffraction spot patterns, to be thereafter indexed automatically through template matching. We present a review on several application examples relative to the characterization of microstructure/microtexture of nanocrystalline metals, ceramics, nanoparticles, minerals and organics. The strengths and limitations of the technique are also discussed using several application examples. ©2013 The Authors. Journal of Microscopy published by John Wiley & Sons Ltd on behalf of Royal Microscopical Society.

Two-phase nc-TiN/a-(C,CN{sub x}) nanocomposite films: A HRTEM and MC simulation study

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

Guo, J.; Lu, Y. H.; Hu, X. J.

2013-06-18

The grain growth in two-phase nanocomposite Ti-C{sub x}-N{sub y} thin films grown by reactive close-field unbalanced magnetron sputtering in an Ar-N{sub 2} gas mixture with microstructures comprising of nanocrystalline (nc-) Ti(N,C) phase surrounded by amorphous (a-) (C,CN{sub x}) phase was investigated by a combination of high-resolution transmission electron microscopy (HRTEM) and Monte Carlo (MC) simulations. The HRTEM results revealed that amorphous-free solid solution Ti(C,N) thin films exhibited polycrystallites with different sizes, orientations and irregular shapes. The grain size varied in the range between several nanometers and several decade nanometers. Further increase of C content (up to {approx}19 at.% C) mademore » the amorphous phase wet nanocrystallites, which strongly hindered the growth of nanocrystallites. As a result, more regular Ti(C,N) nanocrystallites with an average size of {approx}5 nm were found to be separated by {approx}0.5-nm amorphous phases. When C content was further increased (up to {approx}48 at.% in this study), thicker amorphous matrices were produced and followed by the formation of smaller sized grains with lognormal distribution. Our MC analysis indicated that with increasing amorphous volume fraction (i.e. increasing C content), the transformation from nc/nc grain boundary (GB)-curvature-driven growth to a/nc GB-curvature-driven growth is directly responsible for the observed grain growth from great inhomogeneity to homogeneity process.« less

Green synthesis of novel zinc iron oxide (ZnFe2O4) nanocomposite via Moringa Oleifera natural extract for electrochemical applications

NASA Astrophysics Data System (ADS)

Matinise, N.; Kaviyarasu, K.; Mongwaketsi, N.; Khamlich, S.; Kotsedi, L.; Mayedwa, N.; Maaza, M.

2018-07-01

The main motivation of the research study involves development of reliable, accurate, inexpensive and environmental friendly method for the synthesis of zinc ferrite (ZnFe2O4) nanocomposites. It was thought of interest to synthesized zinc ferrite via green synthetic method using Moringa Oleifera extract. For the first time, we used green synthetic route via Moringa Oleifera extract acted as both chelating and reducing agents to synthesis spinel ZnFe2O4 nanocomposites. The physical and electrochemical properties were characterized using different techniques such as High Resolve Transmission Electron Microscope (HRTEM) Energy Dispersive X-ray Spectroscopy (EDS) X-ray diffraction (XRD) Fourier transform-infrared (FT-IR) Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The XRD pattern thus clearly illustrated that the ZnFe2O4 nanocmposites synthesized by the green method were good crystalline in nature. The time constant and exchange current of ZnFe2O4 nanocomposites from EIS analysis were calculated and found to be 5.2001 × 10-4 s/rad and 6.59432 × 10-4 A, respectively. Based on the electrochemical results, GCE/ZnFe2O4 electrode exhibited a good voltametric response, high electro-activity, and excellent electrochemical performance making it a highly suitable/promising electrode for electrochemical applications.

High-resolution, high-throughput imaging with a multibeam scanning electron microscope.

PubMed

Eberle, A L; Mikula, S; Schalek, R; Lichtman, J; Knothe Tate, M L; Zeidler, D

2015-08-01

Electron-electron interactions and detector bandwidth limit the maximal imaging speed of single-beam scanning electron microscopes. We use multiple electron beams in a single column and detect secondary electrons in parallel to increase the imaging speed by close to two orders of magnitude and demonstrate imaging for a variety of samples ranging from biological brain tissue to semiconductor wafers. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Non-enzymatic U(VI) interactions with biogenic mackinawite

NASA Astrophysics Data System (ADS)

Veeramani, H.; Qafoku, N. P.; Kukkadapu, R. K.; Murayama, M.; Hochella, M. F.

2011-12-01

Reductive immobilization of hexavalent uranium [U(VI)] by stimulation of dissimilatory metal and/or sulfate reducing bacteria (DMRB or DSRB) has been extensively researched as a remediation strategy for subsurface U(VI) contamination. These bacteria derive energy by reducing oxidized metals as terminal electron acceptors, often utilizing organic substrates as electron donors. Thus, when evaluating the potential for in-situ uranium remediation in heterogeneous subsurface media, it is important to understand how the presence of alternative electron acceptors such as Fe(III) and sulfate affect U(VI) remediation and the long term behavior and reactivity of reduced uranium. Iron, an abundant subsurface element, represents a substantial sink for electrons from DMRB, and the reduction of Fe(III) leads to the formation of dissolved Fe(II) or to reactive biogenic Fe(II)- and mixed Fe(II)/Fe(III)- mineral phases. Consequently, abiotic U(VI) reduction by reactive forms of biogenic Fe(II) minerals could be a potentially important process for uranium immobilization. In our study, the DMRB Shewanella putrefaciens CN32 was used to synthesize a biogenic Fe(II)-bearing sulfide mineral: mackinawite, that has been characterized by XRD, SEM, HRTEM and Mössbauer spectroscopy. Batch experiments involving treated biogenic mackinawite and uranium (50:1 molar ratio) were carried out at room temperature under strict anoxic conditions. Following complete removal of uranium from solution, the biogenic mackinawite was analyzed by a suite of analytical techniques including XAS, HRTEM and Mössbauer spectroscopy to determine the speciation of uranium and investigate concomitant Fe(II)-phase transformation. Determining the speciation of uranium is critical to success of a remediation strategy. The present work elucidates non-enzymatic/abiotic molecular scale redox interactions between biogenic mackinawite and uranium.

Designs for a quantum electron microscope.

PubMed

Kruit, P; Hobbs, R G; Kim, C-S; Yang, Y; Manfrinato, V R; Hammer, J; Thomas, S; Weber, P; Klopfer, B; Kohstall, C; Juffmann, T; Kasevich, M A; Hommelhoff, P; Berggren, K K

2016-05-01

One of the astounding consequences of quantum mechanics is that it allows the detection of a target using an incident probe, with only a low probability of interaction of the probe and the target. This 'quantum weirdness' could be applied in the field of electron microscopy to generate images of beam-sensitive specimens with substantially reduced damage to the specimen. A reduction of beam-induced damage to specimens is especially of great importance if it can enable imaging of biological specimens with atomic resolution. Following a recent suggestion that interaction-free measurements are possible with electrons, we now analyze the difficulties of actually building an atomic resolution interaction-free electron microscope, or "quantum electron microscope". A quantum electron microscope would require a number of unique components not found in conventional transmission electron microscopes. These components include a coherent electron beam-splitter or two-state-coupler, and a resonator structure to allow each electron to interrogate the specimen multiple times, thus supporting high success probabilities for interaction-free detection of the specimen. Different system designs are presented here, which are based on four different choices of two-state-couplers: a thin crystal, a grating mirror, a standing light wave and an electro-dynamical pseudopotential. Challenges for the detailed electron optical design are identified as future directions for development. While it is concluded that it should be possible to build an atomic resolution quantum electron microscope, we have also identified a number of hurdles to the development of such a microscope and further theoretical investigations that will be required to enable a complete interpretation of the images produced by such a microscope. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

75 FR 13486 - Application(s) for Duty-Free Entry of Scientific Instruments

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2010-03-22

... University, One Waterfront Place, PO Box 6024, Morgantown, WV 26506. Instrument: Electron Microscope.... Justification for Duty-Free Entry: There are no domestic manufacturers of this type of electron microscope.... Lawrence University, 23 Romoda Drive, Canton, NY 13617. Instrument: Electron Microscope. Manufacturer: FEI...

Optical properties of DNA induced starch capped PbS, CdS and PbS/CdS nanocomposites

NASA Astrophysics Data System (ADS)

Das, D.; Konwar, R.; Kalita, P. K.

2015-08-01

Starch capped PbS, CdS and PbS-CdS nanocomposites are conjugated with Calf-Thymus DNA. All the materials are characterized by X-ray diffraction, high-resolution transmission electron microscopy, UV-Vis spectroscopy and photoluminescence spectroscopy. The x-ray diffraction patterns of PbS and CdS show that the materials possess polycrystalline having both cubic and hexagonal phases. High resolution transmission electron microscopic results (HRTEM) shows PbS nanoparticles of size 3 nm and that of CdS nanoparticles having average size 4 nm which exhibit tendency of agglomeration. In case of PbS/CdS, it exhibits different types of nanosheets. The UV absorption spectra of all the samples exhibit clear blue-shift with the respective bulk absorption edges. This is attributed to the strong quantum confinement in the materials. The absorption spectra also exhibit increase of the band gaps from 2.25 to 4.35 eV for PbS; 2.25-4.2 eV for CdS with decrease of molarities from 0.1 to 0.001 M as well as conjugated with DNA. The photoluminescence spectra of all PbS, CdS and PbS/CdS composites synthesized at 0.1 M molar concentration show a further blue shift and an enhancement of intensity after conjugation with DNA, but the effect is reversed i.e. occurrence of red shift and reduction of intensity for those having 0.01 M. This is due to the two competing processes of surface passivation as well as stabilization of nanocomposites governed by bio-molecules and that of Dexter energy transfer with the effective charge separation. The result shows the applicability of the materials in development of biological labels and biosensors.

Electrical, thermal and electrochemical properties of disordered carbon prepared from palygorskite and cane molasses

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

Alvarez, Edelio Danguillecourt, E-mail: edelioalvarez42@gmail.com; Laffita, Yodalgis Mosqueda, E-mail: yodalgis@imre.uh.cu; Montoro, Luciano Andrey, E-mail: landrey.montoro@gmail.com

We have synthesized and electrochemically tested a carbon sample that was suitable as anode for lithium secondary battery. The synthesis was based on the use of the palygorskite clay as template and sugar cane molasses as carbon source. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Brunauer–Emmett–Teller (BET) measurements and High Resolution Transmission Electron Microscope (HRTEM) analysis showed that the nanometric carbon material has a highly disordered graphene-like wrinkled structure and large specific surface area (467 m{sup 2} g{sup −1}). The compositional characterization revealed a 14% of heteroatoms-containing groups (O, H, N, S) doping the as-prepared carbon. Thermophysicalmore » measurements revealed the good thermal stability and an acceptable thermal diffusivity (9·10{sup −7} m{sup 2} s{sup −1}) and conductivity (1.1 W m{sup −1} K{sup −1}) of this carbon. The electrical properties showed an electronic conductivity of hole-like carriers of approximately one S/cm in a 173–293 K range. The testing of this material as anodes in a secondary lithium battery displayed a high specific capacity and excellent performance in terms of number of cycles. A high reversible capacity of 356 mA h g{sup −1} was reached. - Graphical abstract: TEM image and electrochemistry behavior of a new graphene oxide-like carbon. - Highlights: • A high disordered graphene oxide-like conducting carbon is reported. • The synthesis was based on palygorskite and sugar cane molasses as precursors. • The disordered conducting carbon is composed of doped- graphene heterogeneous domains. • This material combines a large specific surface area and high electric conductivity. • The thermophysical and electrochemical properties of this material reveal adequate behavior.« less

Quantum Conductance in Metal Nanowires

NASA Astrophysics Data System (ADS)

Ugarte, Daniel

2004-03-01

Quantum Conductance in Metal Nanowires D. Ugarte Brazilian National Synchrotron Light Laboratory C.P. 6192, 13084-971 Campinas SP, Brazil. Electrical transport properties of metallic nanowires (NWs) have received great attention due to their quantum conductance behavior. Atomic scale wires can be generated by stretching metal contacts; during the elongation and just before rupture, the NW conductance shows flat plateaus and abrupt jumps of approximately a conductance quantum. In this experiments, both the NW atomic arrangement and conductance change simultaneously, making difficult to discriminate electronic and structural effects. In this work, the atomic structure of NWs was studied by time-resolved in situ experiments in a high resolution transmission electron microscope, while their electrical properties using an UHV mechanically controllable break junction (MCBJ). From the analysis of numerous HRTEM images and videos, we have deduced that metal (Au, Ag, Pt, etc.) junctions generated by tensile deformation are crystalline and free of defects. The neck structure is strongly dependent on the surface properties of the analyzed metal, this was verified by comparing different metal NWs (Au, Ag, Cu), which have similar atomic structure (FCC), but show very different faceting patterns. The correlation between the observed structural and transport properties of NW points out that the quantum conductance behavior is defined by preferred atomic arrangement at the narrowest constriction. In the case of magnetic (ex. Fe,Co,Ni) or quasi-magnetic (ex. Pd) wires, we have observed that one-atom-thick structures show a conductance of half the quantum as expected for a fully spin polarized current. This phenomenon seems to occur spontaneously for magnetic suspended atom-chains in zero magnetic field and at room temperature. These results open new opportunities for spin control in nanostructures. Funded by FAPESP, LNLS and CNPq.

Rapid Extracellular Biosynthesis of Silver Nanoparticles by Cunninghamella phaeospora Culture Supernatant

PubMed Central

Ghareib, Mohamed; Tahon, Medhat Abu; Saif, Mona Mostafa; El-Sayed Abdallah, Wafaa

2016-01-01

The development of green approaches for the biosynthesis of silver nanoparticles (AgNPs) is of prime significance in the field of nanotechnology research. A fast and eco-friendly protocol for the biosynthesis of extracellular AgNPs using culture supernatant (CS) from the fungus Cunninghamella phaeospora was studied in this work. This CS was proved as a potential new source for the extracellular biosynthesis of AgNPs. The AgNPs were formed at 100 oC and pH 9 within four min of contact between CS and 1mM silver nitrate (AgNO3) solution. Nitrate reductase (NR) was confirmed to play a pivotal role in the biosynthesis of AgNPs. The enzyme expressed its highest activity at 80 oC and pH 9. At 100 oC the enzyme retained 70% of its original activity for one hour. The half-life (T1/2) of the enzyme activity was calculated to be 1.55 h confirming its thermostability. The produced AgNPs were characterized by UV-Vis spectroscopy, high resolution-transmission electron microscope (HR-TEM) and x-ray diffraction (XRD). These NPs showed an absorption peak at 415 nm in UV-Vis spectrum corresponding to the plasmon resonance of AgNPs. Transmission electron micrographs revealed the production of monodispersed spherical NPs with average particle size 14 nm. XRD spectrum of the NPs confirmed the formation of metallic crystalline silver. It was also suggested that the aromatic amino acids play a role in the biosynthesis process. The current research provided an insight on the green biosynthesis of AgNPs including some mechanistic aspects using a new mycogenic source. PMID:28243290

77 FR 20009 - Howard Hughes Medical Institute, et al.; Notice of Consolidated Decision on Applications for Duty...

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2012-04-03

... decision consolidated pursuant to Section 6(c) of the Educational, Scientific, and Cultural Materials... 07470. Instrument: Electron Microscope. Manufacturer: Hitachi High Technologies America, Inc., Japan... educational uses requiring an electron microscope. We know of no electron microscope, or any other instrument...

The Design and Construction of a Simple Transmission Electron Microscope for Educational Purposes.

ERIC Educational Resources Information Center

Hearsey, Paul K.

This document presents a model for a simple transmission electron microscope for educational purposes. This microscope could demonstrate thermonic emission, particle acceleration, electron deflection, and flourescence. It is designed to be used in high school science courses, particularly physics, taking into account the size, weight, complexity…

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Secondary electron imaging of monolayer materials inside a transmission electron microscope

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

Cretu, Ovidiu, E-mail: cretu.ovidiu@nims.go.jp; Lin, Yung-Chang; Suenaga, Kazutomo

2015-08-10

A scanning transmission electron microscope equipped with a backscattered and secondary electron detector is shown capable to image graphene and hexagonal boron nitride monolayers. Secondary electron contrasts of the two lightest monolayer materials are clearly distinguished from the vacuum level. A signal difference between these two materials is attributed to electronic structure differences, which will influence the escape probabilities of the secondary electrons. Our results show that the secondary electron signal can be used to distinguish between the electronic structures of materials with atomic layer sensitivity, enhancing its applicability as a complementary signal in the analytical microscope.

Integration of a high-NA light microscope in a scanning electron microscope.

PubMed

Zonnevylle, A C; Van Tol, R F C; Liv, N; Narvaez, A C; Effting, A P J; Kruit, P; Hoogenboom, J P

2013-10-01

We present an integrated light-electron microscope in which an inverted high-NA objective lens is positioned inside a scanning electron microscope (SEM). The SEM objective lens and the light objective lens have a common axis and focal plane, allowing high-resolution optical microscopy and scanning electron microscopy on the same area of a sample simultaneously. Components for light illumination and detection can be mounted outside the vacuum, enabling flexibility in the construction of the light microscope. The light objective lens can be positioned underneath the SEM objective lens during operation for sub-10 μm alignment of the fields of view of the light and electron microscopes. We demonstrate in situ epifluorescence microscopy in the SEM with a numerical aperture of 1.4 using vacuum-compatible immersion oil. For a 40-nm-diameter fluorescent polymer nanoparticle, an intensity profile with a FWHM of 380 nm is measured whereas the SEM performance is uncompromised. The integrated instrument may offer new possibilities for correlative light and electron microscopy in the life sciences as well as in physics and chemistry. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Atmospheric scanning electron microscope observes cells and tissues in open medium through silicon nitride film.

PubMed

Nishiyama, Hidetoshi; Suga, Mitsuo; Ogura, Toshihiko; Maruyama, Yuusuke; Koizumi, Mitsuru; Mio, Kazuhiro; Kitamura, Shinichi; Sato, Chikara

2010-03-01

Direct observation of subcellular structures and their characterization is essential for understanding their physiological functions. To observe them in open environment, we have developed an inverted scanning electron microscope with a detachable, open-culture dish, capable of 8 nm resolution, and combined with a fluorescence microscope quasi-simultaneously observing the same area from the top. For scanning electron microscopy from the bottom, a silicon nitride film window in the base of the dish maintains a vacuum between electron gun and open sample dish while allowing electrons to pass through. Electrons are backscattered from the sample and captured by a detector under the dish. Cells cultured on the open dish can be externally manipulated under optical microscopy, fixed, and observed using scanning electron microscopy. Once fine structures have been revealed by scanning electron microscopy, their component proteins may be identified by comparison with separately prepared fluorescence-labeled optical microscopic images of the candidate proteins, with their heavy-metal-labeled or stained ASEM images. Furthermore, cell nuclei in a tissue block stained with platinum-blue were successfully observed without thin-sectioning, which suggests the applicability of this inverted scanning electron microscope to cancer diagnosis. This microscope visualizes mesoscopic-scale structures, and is also applicable to non-bioscience fields including polymer chemistry. (c) 2010 Elsevier Inc. All rights reserved.

Doping effect of polyaniline/MWCNT composites on capacitance and cyclic stability of supercapacitors.

PubMed

Karthikeyan, G; Sahoo, S; Nayak, G C; Das, C K

2012-03-01

Polyaniline doped by Zn2+ ions was synthesized as nanocomposites with multiwalled carbon nanotubes (MWCNT) by in-situ oxidative polymerization and investigated as electrode material for supercapacitors. The uniform coating of polyaniline on MWCNT was characterized by field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM). The effect of Zn2+ ions on nanocomposites were characterized by Fourier transform infrared (FTIR) spectroscopy. The electrochemical performances were investigated by cyclic voltammetry (CV), constant current charging/discharging cyclic test (CC) and electrochemical impedance spectroscopy (EIS) using a three-electrode system. The doped polyaniline composites show higher specific capacitance and better cyclic stability.

Synthesis and electrochemical performance of LiV3O8/polythiophene composite as cathode materials for lithium ion batteries

NASA Astrophysics Data System (ADS)

Guo, Haipeng; Liu, Li; Shu, Hongbo; Yang, Xiukang; Yang, Zhenhua; Zhou, Meng; Tan, Jinli; Yan, Zichao; Hu, Hai; Wang, Xianyou

2014-02-01

LiV3O8/polythiophene (LiV3O8/PTh) composite has been chemically synthesized via an in-situ oxidative polymerization method. The structure and morphology of the samples have been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM). LiV3O8/PTh composite shows a single phase in the XRD pattern, but the existence of PTh has been confirmed by FTIR spectra. HRTEM images show that an uniform PTh layer with a thickness of 3-5 nm covered on the surface of LiV3O8. Electrochemical performance of samples has been characterized by the charge/discharge test, cyclic voltammetry (CV), electrochemical impedance spectroscopic studies (EIS) and galvanostatic intermittent titration technique (GITT). The LiV3O8/PTh composite exhibits much better electrochemical performance than bare LiV3O8. The initial discharge capacities of 15 wt.% LiV3O8/PTh composite are 213.3 and 200.3 mAh g-1 with almost no capacity retention after 50 cycles at current densities of 300 and 900 mA g-1, respectively. PTh could enhance electronic conductivity, decrease the charge transfer resistance, increase the lithium diffusion coefficient, and thus improve cycling performance of LiV3O8. All these results demonstrate that the LiV3O8/PTh composite has a promising application as cathode material for lithium ion batteries.

Improved electrical properties of atomic layer deposited tin disulfide at low temperatures using ZrO2 layer

NASA Astrophysics Data System (ADS)

Lee, Juhyun; Lee, Jeongsu; Ham, Giyul; Shin, Seokyoon; Park, Joohyun; Choi, Hyeongsu; Lee, Seungjin; Kim, Juyoung; Sul, Onejae; Lee, Seungbeck; Jeon, Hyeongtag

2017-02-01

We report the effect of zirconium oxide (ZrO2) layers on the electrical characteristics of multilayered tin disulfide (SnS2) formed by atomic layer deposition (ALD) at low temperatures. SnS2 is a two-dimensional (2D) layered material which exhibits a promising electrical characteristics as a channel material for field-effect transistors (FETs) because of its high mobility, good on/off ratio and low temperature processability. In order to apply these 2D materials to large-scale and flexible electronics, it is essential to develop processes that are compatible with current electronic device manufacturing technology which should be conducted at low temperatures. Here, we deposited a crystalline SnS2 at 150 °C using ALD, and we then annealed at 300 °C. X-ray diffraction (XRD) and Raman spectroscopy measurements before and after the annealing showed that SnS2 had a hexagonal (001) peak at 14.9° and A1g mode at 313 cm-1. The annealed SnS2 exhibited clearly a layered structure confirmed by the high resolution transmission electron microscope (HRTEM) images. Back-gate FETs with SnS2 channel sandwiched by top and bottom ZrO2 on p++Si/SiO2 substrate were suggested to improve electrical characteristics. We used a bottom ZrO2 layer to increase adhesion between the channel and the substrate and a top ZrO2 layer to improve contact property, passivate surface, and protect from process-induced damages to the channel. ZTZ (ZrO2/SnS2/ZrO2) FETs showed improved electrical characteristics with an on/off ratio of from 0.39×103 to 6.39×103 and a mobility of from 0.0076 cm2/Vs to 0.06 cm2/Vs.

Substrate bias induced synthesis of flowered-like bunched carbon nanotube directly on bulk nickel

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

Bisht, Atul; Academy of Scientific and Innovative Research; Chockalingam, S.

2016-02-15

Highlights: • Flowered-like bunched MWCNTs have been synthesized by MW PECVD technique. • Effect of substrate bias on the properties of MWCNT has been studied. • Minimum E{sub T} = 1.9 V/μm with β = 4770 has been obtained in the film deposited at −350 V. - Abstract: This paper reports the effect of substrate bias on the multiwalled carbon nanotube (MWCNT) deposited on nickel foil by microwave plasma enhanced chemical vapor deposition technique. The MWCNTs have been characterized by the scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), Raman spectroscopy, field emission and current–voltage characteristic of themore » heterojunction diode. The SEM images exhibit unique hierarchical flowered-like bunched and conformally coated MWCNTs. Substrate bias induced ion bombardment helps in the enhancement of hydrocarbon dissociation and is responsible for flowered-like MWCNTs growth. The HRTEM micrographs show the base growth mechanism for MWCNTs. The value of turn on field for emission decreases from 5.5 to 1.9 V/μm and field enhancement factor increases from 927 to 4770, respectively, with the increase of substrate bias. The diode ideality factor of CNT/ n-Si heterojunction is evaluated as 2.4 and the on/off current ratio is found to be 7 at ±2 V, respectively.« less

The evolvement of pits and dislocations on TiO{sub 2}-B nanowires via oriented attachment growth

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

Zhao Bin; Chen Feng, E-mail: Fengchen@ecust.edu.c; Qu Wenwu

2009-08-15

TiO{sub 2}-B nanowires were synthesized by an ion exchanging-thermal treatment. The unique morphology of pits and dislocations interspersed on TiO{sub 2}-B nanowires were firstly characterized and studied by high-resolution transmission electron microscopy (HRTEM). Oriented attachment is suggested as an important growth mechanism in the evolvement of pits and dislocations on TiO{sub 2}-B nanowires. Lattice shears and fractures were originally formed during the ion exchanging process of the sodium titanate nanowires, which resulted in the formation of primary crystalline units and vacancies in the layered hydrogen titanate nanowires. Then the (110) lattice planes of TiO{sub 2}-B grown in [110] direction ismore » faster than the other lattice planes, which caused the exhibition of long dislocations on TiO{sub 2}-B nanowires. The enlargement of the vacancies, which was caused by the rearrangement of primary crystalline units, should be the reason of the formation of pits. Additionally, the transformation from TiO{sub 2}-B to anatase could be also elucidated by oriented attachment mechanism. - Graphical abstract: The unique morphology of pits and dislocations on TiO{sub 2}-B nanowires shown in high-resolution transmission electron microscopy (HRTEM) and a proposed evolvement mechanism of pits and dislocations on TiO{sub 2}-B nanowires.« less

Crystal Face Distributions and Surface Site Densities of Two Synthetic Goethites: Implications for Adsorption Capacities as a Function of Particle Size.

PubMed

Livi, Kenneth J T; Villalobos, Mario; Leary, Rowan; Varela, Maria; Barnard, Jon; Villacís-García, Milton; Zanella, Rodolfo; Goodridge, Anna; Midgley, Paul

2017-09-12

Two synthetic goethites of varying crystal size distributions were analyzed by BET, conventional TEM, cryo-TEM, atomic resolution STEM and HRTEM, and electron tomography in order to determine the effects of crystal size, shape, and atomic scale surface roughness on their adsorption capacities. The two samples were determined by BET to have very different site densities based on Cr VI adsorption experiments. Model specific surface areas generated from TEM observations showed that, based on size and shape, there should be little difference in their adsorption capacities. Electron tomography revealed that both samples crystallized with an asymmetric {101} tablet habit. STEM and HRTEM images showed a significant increase in atomic-scale surface roughness of the larger goethite. This difference in roughness was quantified based on measurements of relative abundances of crystal faces {101} and {201} for the two goethites, and a reactive surface site density was calculated for each goethite. Singly coordinated sites on face {210} are 2.5 more dense than on face {101}, and the larger goethite showed an average total of 36% {210} as compared to 14% for the smaller goethite. This difference explains the considerably larger adsorption capacitiy of the larger goethite vs the smaller sample and points toward the necessity of knowing the atomic scale surface structure in predicting mineral adsorption processes.

TEM and HRTEM study of oxide particles in an Al-alloyed high-Cr oxide dispersion strengthened ferritic steel with Hf addition

NASA Astrophysics Data System (ADS)

Dou, Peng; Kimura, Akihiko; Kasada, Ryuta; Okuda, Takanari; Inoue, Masaki; Ukai, Shigeharu; Ohnuki, Somei; Fujisawa, Toshiharu; Abe, Fujio; Jiang, Shan; Yang, Zhigang

2017-03-01

The nanoparticles in an Al-alloyed high-Cr oxide dispersion strengthened (ODS) ferritic steel with Hf addition, i.e., SOC-16 (Fe-15Cr-2W-0.1Ti-4Al-0.62Hf-0.35Y2O3), have been examined by transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). Relative to an Al-alloyed high-Cr ODS ferritic steel without Hf addition, i.e., SOC-9 (Fe-15.5Cr-2W-0.1Ti-4Al-0.35Y2O3), the dispersion morphology and coherency of the oxide nanoparticles in SOC-16 were significantly improved. Almost all the small nanoparticles (diameter <10 nm) in SOC-16 were found to be consistent with cubic Y2Hf2O7 oxides with the anion-deficient fluorite structure and coherent with the bcc steel matrix. The larger particles (diameter >10 nm) were also mainly identified as cubic Y2Hf2O7 oxides with the anion-deficient fluorite structure. The results presented here are compared with those of SOC-9 with a brief discussion of the underlying mechanisms of the unusual thermal and irradiation stabilities of the oxides as well as the superior strength, excellent irradiation tolerance and extraordinary corrosion resistance of SOC-16.

Correction of image drift and distortion in a scanning electron microscopy.

PubMed

Jin, P; Li, X

2015-12-01

Continuous research on small-scale mechanical structures and systems has attracted strong demand for ultrafine deformation and strain measurements. Conventional optical microscope cannot meet such requirements owing to its lower spatial resolution. Therefore, high-resolution scanning electron microscope has become the preferred system for high spatial resolution imaging and measurements. However, scanning electron microscope usually is contaminated by distortion and drift aberrations which cause serious errors to precise imaging and measurements of tiny structures. This paper develops a new method to correct drift and distortion aberrations of scanning electron microscope images, and evaluates the effect of correction by comparing corrected images with scanning electron microscope image of a standard sample. The drift correction is based on the interpolation scheme, where a series of images are captured at one location of the sample and perform image correlation between the first image and the consequent images to interpolate the drift-time relationship of scanning electron microscope images. The distortion correction employs the axial symmetry model of charged particle imaging theory to two images sharing with the same location of one object under different imaging fields of view. The difference apart from rigid displacement between the mentioned two images will give distortion parameters. Three-order precision is considered in the model and experiment shows that one pixel maximum correction is obtained for the employed high-resolution electron microscopic system. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

[Thirty years of the electron microscope investigation in zoology and parasitology in the Zoological Institute of the Russian Academy of Sciences].

PubMed

Shatrov, A B

2003-01-01

The history of the electron microscope investigations in zoology and parasitology in the Zoological Institute of the Russian Academy of Sciences and progress in scanning and transmission electron microscope investigations in this field of biology to the moment are briefly accounted.

75 FR 52928 - Emory University, et al., Notice of Consolidated Decision on Applications for Duty-Free Entry of...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-08-30

... Consolidated Decision on Applications for Duty-Free Entry of Electron Microscopes This is a decision... 30322. Instrument: Electron Microscope. Manufacturer: JEOL, Ltd., Japan. Intended Use: See notice at 75... Department of Health, Menands, NY 12204-2719. Instrument: Electron Microscope. Manufacturer: JEOL Ltd., Japan...

Imaging of Norway spruce early somatic embryos with the ESEM, Cryo-SEM and laser scanning microscope.

PubMed

Neděla, Vilém; Hřib, Jiří; Havel, Ladislav; Hudec, Jiří; Runštuk, Jiří

2016-05-01

This article describes the surface structure of Norway spruce early somatic embryos (ESEs) as a typical culture with asynchronous development. The microstructure of extracellular matrix covering ESEs were observed using the environmental scanning electron microscope as a primary tool and using the scanning electron microscope with cryo attachment and laser electron microscope as a complementary tool allowing our results to be proven independently. The fresh samples were observed in conditions of the air environment of the environmental scanning electron microscope (ESEM) with the pressure from 550Pa to 690Pa and the low temperature of the sample from -18°C to -22°C. The samples were studied using two different types of detector to allow studying either the thin surface structure or material composition. The scanning electron microscope with cryo attachment was used for imaging frozen extracellular matrix microstructure with higher resolution. The combination of both electron microscopy methods was suitable for observation of "native" plant samples, allowing correct evaluation of our results, free of error and artifacts. Copyright © 2016 Elsevier Ltd. All rights reserved.

The effect of high energy concentration source irradiation on structure and properties of Fe-based bulk metallic glass

NASA Astrophysics Data System (ADS)

Pilarczyk, Wirginia

2016-06-01

Metallic glasses exhibit metastable structure and maintain this relatively stable amorphous state within certain temperature range. High intensity laser beam was used for the surface irradiation of Fe-Co-B-Si-Nb bulk metallic glasses. The variable parameter was laser beam pulse energy. For the analysis of structure and properties of bulk metallic glasses and their surface after laser remelting the X-ray analysis, microscopic observation and test of mechanical properties were carried out. Examination of the nanostructure of amorphous materials obtained by high pressure copper mold casting method and the irradiated with the use of TITAN 80-300 HRTEM was carried out. Nanohardness and reduced Young's modulus of particular amorphous and amorphous-crystalline material zone of the laser beam were examined with the use of Hysitron TI950 Triboindenter nanoindenter and with the use of Berkovich's indenter. The XRD and microscopic analysis showed that the test material is amorphous in its structure before irradiation. Microstructure observation with electron transmission microscopy gave information about alloy crystallization in the irradiated process. Identification of given crystal phases allows to determine the kind of crystal phases created in the first place and also further changes of phase composition of alloy. The main value of the nanohardness of the surface prepared by laser beam has the order of magnitude similar to bulk metallic glasses formed by casting process irrespective of the laser beam energy used. Research results analysis showed that the area between parent material and fusion zone is characterized by extraordinarily interesting structure which is and will be the subject of further analysis in the scope of bulk metallic glasses amorphous structure and high energy concentration source. The main goal of this work is the results' presentation of structure and chosen properties of the selected bulk metallic glasses after casting process and after irradiation process employing the high energy concentration sources.

Grayscale inhomogeneity correction method for multiple mosaicked electron microscope images

NASA Astrophysics Data System (ADS)

Zhou, Fangxu; Chen, Xi; Sun, Rong; Han, Hua

2018-04-01

Electron microscope image stitching is highly desired to acquire microscopic resolution images of large target scenes in neuroscience. However, the result of multiple Mosaicked electron microscope images may exist severe gray scale inhomogeneity due to the instability of the electron microscope system and registration errors, which degrade the visual effect of the mosaicked EM images and aggravate the difficulty of follow-up treatment, such as automatic object recognition. Consequently, the grayscale correction method for multiple mosaicked electron microscope images is indispensable in these areas. Different from most previous grayscale correction methods, this paper designs a grayscale correction process for multiple EM images which tackles the difficulty of the multiple images monochrome correction and achieves the consistency of grayscale in the overlap regions. We adjust overall grayscale of the mosaicked images with the location and grayscale information of manual selected seed images, and then fuse local overlap regions between adjacent images using Poisson image editing. Experimental result demonstrates the effectiveness of our proposed method.

High-resolution, high-throughput imaging with a multibeam scanning electron microscope

PubMed Central

EBERLE, AL; MIKULA, S; SCHALEK, R; LICHTMAN, J; TATE, ML KNOTHE; ZEIDLER, D

2015-01-01

Electron–electron interactions and detector bandwidth limit the maximal imaging speed of single-beam scanning electron microscopes. We use multiple electron beams in a single column and detect secondary electrons in parallel to increase the imaging speed by close to two orders of magnitude and demonstrate imaging for a variety of samples ranging from biological brain tissue to semiconductor wafers. Lay Description The composition of our world and our bodies on the very small scale has always fascinated people, making them search for ways to make this visible to the human eye. Where light microscopes reach their resolution limit at a certain magnification, electron microscopes can go beyond. But their capability of visualizing extremely small features comes at the cost of a very small field of view. Some of the questions researchers seek to answer today deal with the ultrafine structure of brains, bones or computer chips. Capturing these objects with electron microscopes takes a lot of time – maybe even exceeding the time span of a human being – or new tools that do the job much faster. A new type of scanning electron microscope scans with 61 electron beams in parallel, acquiring 61 adjacent images of the sample at the same time a conventional scanning electron microscope captures one of these images. In principle, the multibeam scanning electron microscope’s field of view is 61 times larger and therefore coverage of the sample surface can be accomplished in less time. This enables researchers to think about large-scale projects, for example in the rather new field of connectomics. A very good introduction to imaging a brain at nanometre resolution can be found within course material from Harvard University on http://www.mcb80x.org/# as featured media entitled ‘connectomics’. PMID:25627873

Characterisation of phases in nanostructured, multilayered titanium alloys by analytical and high-resolution electron microscopy.

PubMed

Czyrska-Filemonowicz, A; Buffat, P A

2009-01-01

Surface processing of a Ti-6Al-4V alloy led to a complex multilayered microstructure containing several phases of the Ni-Ti-P-Al-O system, which improves the mechanical and tribological surface properties. The microstructure, chemical and phase compositions of the hard layer formed on the surface were investigated by LM, XRD, SEM as well as analytical/high-resolution TEM, STEM, EDS, electron diffraction and FIB. Phase identification based on electron diffraction, HRTEM and EDS microanalysis revealed the presence of several binary and ternary phases in the system Ti-Ni-P, sometimes with partial substitution of Ti by Al. However some phases, mainly nanoparticles, still remain not identified satisfactorily. Electron microscopy techniques used for identification of phases present in surface multilayers and some practical limits to their routine application are reminded here.

Analysis of improvement in performance and design parameters for enhancing resolution in an atmospheric scanning electron microscope.

PubMed

Yoon, Yeo Hun; Kim, Seung Jae; Kim, Dong Hwan

2015-12-01

The scanning electron microscope is used in various fields to go beyond diffraction limits of the optical microscope. However, the electron pathway should be conducted in a vacuum so as not to scatter electrons. The pretreatment of the sample is needed for use in the vacuum. To directly observe large and fully hydrophilic samples without pretreatment, the atmospheric scanning electron microscope (ASEM) is needed. We developed an electron filter unit and an electron detector unit for implementation of the ASEM. The key of the electron filter unit is that electrons are transmitted while air molecules remain untransmitted through the unit. The electron detector unit collected the backscattered electrons. We conducted experiments using the selected materials with Havar foil, carbon film and SiN film. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Structural properties of ultrafine Ba-hexaferrite nanoparticles

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

Makovec, Darko, E-mail: Darko.Makovec@ijs.si; Primc, Darinka; Sturm, Saso

2012-12-15

Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was studied using X-ray diffractometry (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDXS), X-ray absorption fine structure (XAFS), and Moessbauer spectroscopy (MS), to be compared to the structure of larger nanoparticles and the bulk. The nanoparticles were synthesized with hydrothermal treatment of an appropriate suspension of Ba and Fe hydroxides in the presence of a large excess of OH{sup -}. The ultrafine nanoparticles were formed in a discoid shape, {approx}10 nm wide and only {approx}3 nm thick, comparable to the size of the hexagonal unit cell in the c-direction.more » The HRTEM image analysis confirmed the hexaferrite structure, whereas EDXS showed the composition matching the BaFe{sub 12}O{sub 19} formula. XAFS and MS analyses showed considerable disorder of the structure, most probably responsible for the low magnetization. - Graphical abstract: Left: HREM image of an ultrafine Ba-hexaferrite nanoparticle (inset: TEM image of the nanoparticles); Right: the experimental HRTEM image is compared with calculated image and corresponding atomic model. Highlights: Black-Right-Pointing-Pointer Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was compared to the structure of the bulk. Black-Right-Pointing-Pointer Thickness the discoid nanoparticles was comparable to the size of the hexagonal unit cell in the c-direction. Black-Right-Pointing-Pointer Considerable disorder of the nanoparticles' structure is most probably responsible for their low magnetization.« less

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.

Reprint of: Atmospheric scanning electron microscope observes cells and tissues in open medium through silicon nitride film.

PubMed

Nishiyama, Hidetoshi; Suga, Mitsuo; Ogura, Toshihiko; Maruyama, Yuusuke; Koizumi, Mitsuru; Mio, Kazuhiro; Kitamura, Shinichi; Sato, Chikara

2010-11-01

Direct observation of subcellular structures and their characterization is essential for understanding their physiological functions. To observe them in open environment, we have developed an inverted scanning electron microscope with a detachable, open-culture dish, capable of 8 nm resolution, and combined with a fluorescence microscope quasi-simultaneously observing the same area from the top. For scanning electron microscopy from the bottom, a silicon nitride film window in the base of the dish maintains a vacuum between electron gun and open sample dish while allowing electrons to pass through. Electrons are backscattered from the sample and captured by a detector under the dish. Cells cultured on the open dish can be externally manipulated under optical microscopy, fixed, and observed using scanning electron microscopy. Once fine structures have been revealed by scanning electron microscopy, their component proteins may be identified by comparison with separately prepared fluorescence-labeled optical microscopic images of the candidate proteins, with their heavy-metal-labeled or stained ASEM images. Furthermore, cell nuclei in a tissue block stained with platinum-blue were successfully observed without thin-sectioning, which suggests the applicability of this inverted scanning electron microscope to cancer diagnosis. This microscope visualizes mesoscopic-scale structures, and is also applicable to non-bioscience fields including polymer chemistry. Copyright © 2010 Elsevier Inc. All rights reserved.

Electron microscopy study of gold nanoparticles deposited on transition metal oxides.

PubMed

Akita, Tomoki; Kohyama, Masanori; Haruta, Masatake

2013-08-20

Many researchers have investigated the catalytic performance of gold nanoparticles (GNPs) supported on metal oxides for various catalytic reactions of industrial importance. These studies have consistently shown that the catalytic activity and selectivity depend on the size of GNPs, the kind of metal oxide supports, and the gold/metal oxide interface structure. Although researchers have proposed several structural models for the catalytically active sites and have identified the specific electronic structures of GNPs induced by the quantum effect, recent experimental and theoretical studies indicate that the perimeter around GNPs in contact with the metal oxide supports acts as an active site in many reactions. Thus, it is of immense importance to investigate the detailed structures of the perimeters and the contact interfaces of gold/metal oxide systems by using electron microscopy at an atomic scale. This Account describes our investigation, at the atomic scale using electron microscopy, of GNPs deposited on metal oxides. In particular, high-resolution transmission electron microscopy (HRTEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) are valuable tools to observe local atomic structures, as has been successfully demonstrated for various nanoparticles, surfaces, and material interfaces. TEM can be applied to real powder catalysts as received without making special specimens, in contrast to what is typically necessary to observe bulk materials. For precise structure analyses at an atomic scale, model catalysts prepared by using well-defined single-crystalline substrates are also adopted for TEM observations. Moreover, aberration-corrected TEM, which has high spatial resolution under 0.1 nm, is a promising tool to observe the interface structure between GNPs and metal oxide supports including oxygen atoms at the interfaces. The oxygen atoms in particular play an important role in the behavior of gold/metal oxide interfaces, because they may participate in catalytic reaction steps. Detailed information about the interfacial structures between GNPs and metal oxides provides valuable structure models for theoretical calculations which can elucidate the local electronic structure effective for activating a reactant molecule. Based on our observations with HRTEM and HAADF-STEM, we report the detailed structure of gold/metal oxide interfaces.

An electron microscope for the aberration-corrected era.

PubMed

Krivanek, O L; Corbin, G J; Dellby, N; Elston, B F; Keyse, R J; Murfitt, M F; Own, C S; Szilagyi, Z S; Woodruff, J W

2008-02-01

Improved resolution made possible by aberration correction has greatly increased the demands on the performance of all parts of high-end electron microscopes. In order to meet these demands, we have designed and built an entirely new scanning transmission electron microscope (STEM). The microscope includes a flexible illumination system that allows the properties of its probe to be changed on-the-fly, a third-generation aberration corrector which corrects all geometric aberrations up to fifth order, an ultra-responsive yet stable five-axis sample stage, and a flexible configuration of optimized detectors. The microscope features many innovations, such as a modular column assembled from building blocks that can be stacked in almost any order, in situ storage and cleaning facilities for up to five samples, computer-controlled loading of samples into the column, and self-diagnosing electronics. The microscope construction is described, and examples of its capabilities are shown.

Hartmann characterization of the PEEM-3 aberration-corrected X-ray photoemission electron microscope.

PubMed

Scholl, A; Marcus, M A; Doran, A; Nasiatka, J R; Young, A T; MacDowell, A A; Streubel, R; Kent, N; Feng, J; Wan, W; Padmore, H A

2018-05-01

Aberration correction by an electron mirror dramatically improves the spatial resolution and transmission of photoemission electron microscopes. We will review the performance of the recently installed aberration corrector of the X-ray Photoemission Electron Microscope PEEM-3 and show a large improvement in the efficiency of the electron optics. Hartmann testing is introduced as a quantitative method to measure the geometrical aberrations of a cathode lens electron microscope. We find that aberration correction leads to an order of magnitude reduction of the spherical aberrations, suggesting that a spatial resolution of below 100 nm is possible at 100% transmission of the optics when using x-rays. We demonstrate this improved performance by imaging test patterns employing element and magnetic contrast. Published by Elsevier B.V.

A new apparatus for electron tomography in the scanning electron microscope

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

Morandi, V., E-mail: morandi@bo.imm.cnr.it; Maccagnani, P.; Masini, L.

2015-06-23

The three-dimensional reconstruction of a microscopic specimen has been obtained by applying the tomographic algorithm to a set of images acquired in a Scanning Electron Microscope. This result was achieved starting from a series of projections obtained by stepwise rotating the sample under the beam raster. The Scanning Electron Microscope was operated in the scanning-transmission imaging mode, where the intensity of the transmitted electron beam is a monotonic function of the local mass-density and thickness of the specimen. The detection strategy has been implemented and tailored in order to maintain the projection requirement over the large tilt range, as requiredmore » by the tomographic workflow. A Si-based electron detector and an eucentric-rotation specimen holder have been specifically developed for the purpose.« less

Magnetite and magnetite/silver core/shell nanoparticles with diluted magnet-like behavior

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

Garza-Navarro, Marco; Torres-Castro, Alejandro, E-mail: alejandro.torrescs@uanl.edu.m; Centro de Innovacion, Investigacion y Desarrollo en Ingenieria y Tecnologia, Universidad Autonoma de Nuevo Leon, Apodaca, Nuevo Leon 66600

2010-01-15

In the present work is reported the use of the biopolymer chitosan as template for the preparation of magnetite and magnetite/silver core/shell nanoparticles systems, following a two step procedure of magnetite nanoparticles in situ precipitation and subsequent silver ions reduction. The crystalline and morphological characteristics of both magnetite and magnetite/silver core/shell nanoparticles systems were analyzed by high resolution transmission electron microscopy (HRTEM) and nanobeam diffraction patterns (NBD). The results of these studies corroborate the core/shell morphology and the crystalline structure of the magnetite core and the silver shell. Moreover, magnetization temperature dependent, M(T), measurements show an unusual diluted magnetic behaviormore » attributed to the dilution of the magnetic ordering in the magnetite and magnetite/silver core/shell nanoparticles systems. - Graphical abstract: Biopolymer chitosan was used as stabilization media to synthesize both magnetite and magnetite/silver core/shell nanoparticles. Results of HRTEM and NBD patterns confirm core/shell morphology of the obtained nanoparticles. It was found that the composites show diluted magnet-like behavior.« less

Interfacial effect on the structural and optical properties of pure SnO2 and dual shells (ZnO; SiO2) coated SnO2 core-shell nanospheres for optoelectronic applications

NASA Astrophysics Data System (ADS)

Selvi, N.; Sankar, S.; Dinakaran, K.

2014-12-01

Nanocrystallites of SnO2 core and dual shells (ZnO, SiO2) coated SnO2 core-shell nanospheres were successfully synthesized by co-precipitation method. The as prepared and annealed samples were characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), High resolution transmission electron microscopy (HRTEM) and UV-Vis analysis. XRD pattern confirms the obtained SnO2 core with tetragonal rutile crystalline structure and the shell ZnO with hexagonal structure. FTIR result shows the functional groups present in the samples. The spherical morphology and the formation of the core-shell structures have been confirmed by HRTEM measurements. The UV-Vis showed that band gap is red shifted for as-prepared and the shells coated core-shell samples. From this investigation it can be concluded that the surface modification with different metal and insulating oxides strongly influences the optical properties of the core-shell materials which enhance their potential applications towards optical devices fabrication.

Platinum Electrodeposition at Unsupported Electrochemically Reduced Nanographene Oxide for Enhanced Ammonia Oxidation

PubMed Central

2015-01-01

The electrochemical reduction of highly oxidized unsupported graphene oxide nanosheets and its platinum electrodeposition was done by the rotating disk slurry electrode technique. Avoiding the use of a solid electrode, graphene oxide was electrochemically reduced in a slurry solution with a scalable process without the use of a reducing agent. Graphene oxide nanosheets were synthesized from carbon platelet nanofibers to obtain highly hydrophilic layers of less than 250 nm in width. The graphene oxide and electrochemically reduced graphene oxide/Pt (erGOx/Pt) hybrid materials were characterized through different spectroscopy and microscopy techniques. Pt nanoparticles with 100 facets, clusters, and atoms at erGOx were identified by high resolution transmission electron microscopy (HRTEM). Cyclic voltammetry was used to characterize the electrocatalytic activity of the highly dispersed erGOx/Pt hybrid material toward the oxidation of ammonia, which showed a 5-fold current density increase when compared with commercially available Vulcan/Pt 20%. This is in agreement with having Pt (100) facets present in the HRTEM images of the erGOx/Pt material. PMID:24417177

Effect of carbon coating on spontaneous C12A7 whisker formation

NASA Astrophysics Data System (ADS)

Zaikovskii, Vladimir I.; Volodin, Alexander M.; Stoyanovskii, Vladimir O.; Cherepanova, Svetlana V.; Vedyagin, Aleksey A.

2018-06-01

A carbon nanoreactor concept was applied to study the stabilization effect of carbon shell on phase composition and morphology of dodecacalcium hepta-aluminate Ca12Al14O33. The starting C12A7 powder was obtained using aluminum and calcium hydroxides as precursors. Carbon shell was formed by a chemical vapor deposition of divinyl at 550 °C. After the calcination at 1400 °C, the product was characterized by X-ray diffraction analysis (XRD) and high resolution transmission electron microscopy (HRTEM). It was observed for a first time that spontaneous formation of calcium aluminate whiskers take place under the conditions described. Each whisker consists of a 'head' (globular particle of 0.5 microns in diameter) and a 'tail' (prolonged whisker of few microns in length and 0.1-0.2 microns in diameter). According to HRTEM, the 'head' is characterized with microcrystal lattice of Ca12Al14O33 compound. XRD data show the presence of CaAl2O4 phase traces. The 'head' and 'tail' of the whisker are covered with structured graphene layers of 10 nm and 3 nm, correspondingly.

Kinetic mechanism of V-shaped twinning in 3C/4H-SiC heteroepitaxy

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

Xin, Bin; Zhang, Yu-Ming; Jia, Ren-Xu, E-mail: rxjia@mail.xidian.edu.cn

The authors investigated the kinetic mechanism of V-shaped twinning in 3C/4H-SiC heteroepitaxy. A fourfold V-shaped twinning complex was found, and its interface was measured with high-resolution transmission electron microscopy (HRTEM). Two linear coherent boundaries and a nonlinear incoherent boundary (also called the double-position boundary) were observed. On the basis of the HRTEM results, the authors proposed an adatom migration growth model, in which the activation barrier at the coherent boundary is much lower than that at the incoherent boundary. From a kinetic perspective, adatoms are prone to migrate to the side of the boundary with the lower potential energy ifmore » they have sufficient thermal energy to overcome the activation barrier. In the case of a coherent boundary, the growth rates of the domains either side of the boundary can be balanced through the intermigration of adatoms, leading to a linear boundary. Conversely, it is difficult for adatoms to migrate across an incoherent boundary, which results in asynchronous growth rates and a nonlinear boundary.« less

ultraLM and miniLM: Locator tools for smart tracking of fluorescent cells in correlative light and electron microscopy.

PubMed

Brama, Elisabeth; Peddie, Christopher J; Wilkes, Gary; Gu, Yan; Collinson, Lucy M; Jones, Martin L

2016-12-13

In-resin fluorescence (IRF) protocols preserve fluorescent proteins in resin-embedded cells and tissues for correlative light and electron microscopy, aiding interpretation of macromolecular function within the complex cellular landscape. Dual-contrast IRF samples can be imaged in separate fluorescence and electron microscopes, or in dual-modality integrated microscopes for high resolution correlation of fluorophore to organelle. IRF samples also offer a unique opportunity to automate correlative imaging workflows. Here we present two new locator tools for finding and following fluorescent cells in IRF blocks, enabling future automation of correlative imaging. The ultraLM is a fluorescence microscope that integrates with an ultramicrotome, which enables 'smart collection' of ultrathin sections containing fluorescent cells or tissues for subsequent transmission electron microscopy or array tomography. The miniLM is a fluorescence microscope that integrates with serial block face scanning electron microscopes, which enables 'smart tracking' of fluorescent structures during automated serial electron image acquisition from large cell and tissue volumes.

Spherical aberration correction in a scanning transmission electron microscope using a sculpted thin film.

PubMed

Shiloh, Roy; Remez, Roei; Lu, Peng-Han; Jin, Lei; Lereah, Yossi; Tavabi, Amir H; Dunin-Borkowski, Rafal E; Arie, Ady

2018-06-01

Nearly eighty years ago, Scherzer showed that rotationally symmetric, charge-free, static electron lenses are limited by an unavoidable, positive spherical aberration. Following a long struggle, a major breakthrough in the spatial resolution of electron microscopes was reached two decades ago by abandoning the first of these conditions, with the successful development of multipole aberration correctors. Here, we use a refractive silicon nitride thin film to tackle the second of Scherzer's constraints and demonstrate an alternative method for correcting spherical aberration in a scanning transmission electron microscope. We reveal features in Si and Cu samples that cannot be resolved in an uncorrected microscope. Our thin film corrector can be implemented as an immediate low cost upgrade to existing electron microscopes without re-engineering of the electron column or complicated operation protocols and can be extended to the correction of additional aberrations. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Diagenetic Microcrystalline Opal Varieties from the Monterey Formation, CA: HRTEM Study of Structures and Phase Transformation Mechanisms

NASA Technical Reports Server (NTRS)

Cady, Sherry L.; Wenk, H.-R.; DeVincenzi, Don (Technical Monitor)

1994-01-01

Microcrystalline opal varieties form as intermediary precipitates during the diagenetic transformation of biogenically precipitated non-crystalline opal (opal-A) to microquartz. With regard to the Monterey Formation of California, X-ray powder diffraction studies have shown that a decrease in the primary d-spacing of opal-CT toward that of cristobalite occurs with increasing diagenesis. The initial timing of opal-CT/quartz formation and the value of the primary opal-CT d-spacing, are influenced by the sediment. lithology. Transmission electron microscopy methods (CTEM/HRTEM) were used to investigate the structure of the diagenetic phases and establish transformation mechanisms between the varieties of microcrystalline opals in charts and porcelanites from the Monterey Formation. HRTEM images revealed that the most common fibrous varieties of microcrystalline opals contain varying amounts of structural disorder. Finite lamellar units of cristobalite-and tridymite-type. layer sequences were found to be randomly stacked in a direction perpendicular to the fiber axis. Disordered and ordered fibers were found to have coprecipitated within the same radial fiber bundles that formed within the matrix of the Most siliceous samples. HRTEM images, which reveal that the fibers within radial and lepispheric fiber bundles branch non-crystallographically, support an earlier proposal that microspheres in chert grow via a spherulitic growth mechanism. A less common variety of opal-CT was found to be characterized by non-parallel (low-angle) stacking sequences that often contain twinned lamellae. Tabular-shaped crystals of orthorhombic tridymite (PO-2) were also identified in the porcelanite samples. A shift in the primary d-spacing of opal-CT has been interpreted as an indication of solid-state ordering g toward a predominantly cristobalite structure, (opal-C). Domains of opal-C were identified as topotactically-oriented overgrowths on discrete Sections of opal-CT fibers and as lamellar domains within relict opal-CT fibers. These findings indicate that the type of transformation mechanism depends upon the primary structural characteristics of the authigenic opaline. varieties that are in turn influenced by the sediment lithology.

Fabrication and structure characterization of te butterfly nanostructures.

PubMed

Wong, Tailun; She, Guangwei; Cheng, Chun; Li, Wei; Shi, Wensheng; Zhang, Xiaohong; Wang, Ning

2011-12-01

Te nanowires and butterfly nanostructures have been fabricated by template-free electrodeposition (TFED) in aqueous solution. By high-resolution transmission electron microscopy (HRTEM) study, the favored growth directions of the nanowires and the wings of the butterfly nanostructures were determined to be along the [0001] direction of trigonal Te, and the twinning plane of the butterfly nanostructures was (11-22). The cathodoluminescence measurements carried out at different positions of the butterfly nanostructure indicated that the twin boundaries influenced the photoemission efficiency.

Scanning electron microscope observation of dislocations in semiconductor and metal materials.

PubMed

Kuwano, Noriyuki; Itakura, Masaru; Nagatomo, Yoshiyuki; Tachibana, Shigeaki

2010-08-01

Scanning electron microscope (SEM) image contrasts have been investigated for dislocations in semiconductor and metal materials. It is revealed that single dislocations can be observed in a high contrast in SEM images formed by backscattered electrons (BSE) under the condition of a normal configuration of SEM. The BSE images of dislocations were compared with those of the transmission electron microscope and scanning transmission electron microscope (STEM) and the dependence of BSE image contrast on the tilting of specimen was examined to discuss the origin of image contrast. From the experimental results, it is concluded that the BSE images of single dislocations are attributed to the diffraction effect and related with high-angle dark-field images of STEM.

Flexible high-voltage supply for experimental electron microscope

NASA Technical Reports Server (NTRS)

Chapman, G. L.; Jung, E. A.; Lewis, R. N.; Van Loon, L. S.; Welter, L. M.

1969-01-01

Scanning microscope uses a field-emission tip for the electron source, an electron gun that simultaneously accelerates and focuses electrons from the source, and one auxiliary lens to produce a final probe size at the specimen on the order of angstroms.

Infiltration of CdTe nano crystals into a ZnO wire vertical matrix by using the isothermal closed space technique

NASA Astrophysics Data System (ADS)

Larramendi, S.; Vaillant Roca, Lidice; Saint-Gregoire, Pierre; Ferraz Dias, Johnny; Behar, Moni

2017-10-01

A ZnO nanorod structure was grown by the hydrothermal method and interpenetrated with CdTe using the isothermal closed space sublimation technique. The obtained structure was studied by using the Rutherford backscattering spectrometry (RBS), Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HRTEM). The X-ray Diffraction (XRD) technique confirmed the presence of CdTe nanocrystals (NCs) of very small size formed on the surface and in the interspaces between the ZnO nanorods. The RBS observations together with the SEM observations give information on the obtained structure. Finally the photoluminescence studies show a strong energy confinement effect on the grown CdTe NCs.

A new method of functionalized multi walled carbon nanotubes by natural oil for microorganism cells detection

NASA Astrophysics Data System (ADS)

Haider, Adawiya J.; Marzoog, Thorria R.; Hadi, Iman H.; Jameel, Zainab N.

2018-05-01

In this work, new surfactants for Functionalization of Multi Walled Carbon Nanotubes (F-MWCNTs) with functional groups have been developed by using walnut oil, to improve their surface activity (solubility) and a create free reticules (functional groups) on it. MWCNTs were functionalized with walnut oil via ultra-sonication technique at 25°C for 1h with no drastic fragmentation of MWCNTs. Fourier Transformed Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HRTEM) and have been employed for the characterizations and analysis. In addition, the antibacterial activity of functionalized MWCNTs against Gram negative. Escherichia coli (E. coli) and Gram positive Staphylococcus aureus (S. aureus) bacteria are examined.

Formation of interconnections between carbon nanotubes and copper using tin solder

NASA Astrophysics Data System (ADS)

Mittal, Jagjiwan; Lina, Kwang-Lung

2013-06-01

A process is developed for connecting Multiwalled carbon nanotubes (MWCNTs) between Cu terminals using tin solder. Connections were made on the Cu grid after heating the Sn coated nanotubes above the melting point of tin. High resolution transmission electron microscopy (HRTEM) micrographs demonstrated the joining by CNTs either as straight between two sides or on the one side after bending in the middle. The connections were found to be stable in air and electron beam under TEM observations. Energy dispersive X-ray (EDX) study showed that the formation of intermetallic compound η-C6Sn5 was responsible for the formation and stability of joints between Cu and MWCNT.

Formation of MoS2 inorganic fullerenes (IFs) by the reaction of MoO3 nanobelts and S.

PubMed

Li, Xiao Lin; Li, Ya Dong

2003-06-16

The reaction of MoO3 and S at temperatures higher than 300 degrees C in an argon atmosphere provides a convenient and effective method for the synthesis of MoS2 nanocrystalline substances. MoS2 nanotubes and fullerene-like nanoparticles have been obtained by the reaction at 850 degrees C under well-controlled conditions. The influences of reaction temperature and duration were carefully investigated in this paper. All of the nanostructures were characterized by Xray powder diffraction (XRD), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). A stepwise reaction model and rolling mechanism were proposed based on the experimental results.

Scanning-electron-microscope used in real-time study of friction and wear

NASA Technical Reports Server (NTRS)

Brainard, W. A.; Buckley, D. H.

1975-01-01

Small friction and wear apparatus built directly into scanning-electron-microscope provides both dynamic observation and microscopic view of wear process. Friction and wear tests conducted using this system have indicated that considerable information can readily be gained.

Thermal-Wave Microscope

NASA Technical Reports Server (NTRS)

Jones, Robert E.; Kramarchuk, Ihor; Williams, Wallace D.; Pouch, John J.; Gilbert, Percy

1989-01-01

Computer-controlled thermal-wave microscope developed to investigate III-V compound semiconductor devices and materials. Is nondestructive technique providing information on subsurface thermal features of solid samples. Furthermore, because this is subsurface technique, three-dimensional imaging also possible. Microscope uses intensity-modulated electron beam of modified scanning electron microscope to generate thermal waves in sample. Acoustic waves generated by thermal waves received by transducer and processed in computer to form images displayed on video display of microscope or recorded on magnetic disk.

Morphology evolution of single-crystalline hematite nanocrystals: magnetically recoverable nanocatalysts for enhanced facet-driven photoredox activity

NASA Astrophysics Data System (ADS)

Patra, Astam K.; Kundu, Sudipta K.; Bhaumik, Asim; Kim, Dukjoon

2015-12-01

We have developed a new green chemical approach for the shape-controlled synthesis of single-crystalline hematite nanocrystals in aqueous medium. FESEM, HRTEM and SAED techniques were used to determine the morphology and crystallographic orientations of each nanocrystal and its exposed facets. PXRD and HRTEM techniques revealed that the nanocrystals are single crystalline in nature; twins and stacking faults were not detected in these nanocrystals. The structural, vibrational, and electronic spectra of these nanocrystals were highly dependent on their shape. Different shaped hematite nanocrystals with distinct crystallographic planes have been synthesized under similar reaction conditions, which can be desired as a model for the purpose of properties comparison with the nanocrystals prepared under different reaction conditions. Here we investigated the photocatalytic performance of these different shaped-nanocrystals for methyl orange degradation in the presence of white light (λ > 420 nm). In this study, we found that the density of surface Fe3+ ions in particular facets was the key factor for the photocatalytic activity and was higher on the bitruncated-dodecahedron shape nanocrystals by coexposed {104}, {100} and {001} facets, attributing to higher catalytic activity. The catalytic activity of different exposed facet nanocrystals were as follows: {104} + {100} + {001} (bitruncated-dodecahedron) > {101} + {001} (bitruncated-octahedron) > {001} + {110} (nanorods) > {012} (nanocuboid) which provided the direct evidence of exposed facet-driven photocatalytic activity. The nanocrystals were easily recoverable using an external magnet and reused at least six times without significant loss of its catalytic activity.We have developed a new green chemical approach for the shape-controlled synthesis of single-crystalline hematite nanocrystals in aqueous medium. FESEM, HRTEM and SAED techniques were used to determine the morphology and crystallographic orientations of each nanocrystal and its exposed facets. PXRD and HRTEM techniques revealed that the nanocrystals are single crystalline in nature; twins and stacking faults were not detected in these nanocrystals. The structural, vibrational, and electronic spectra of these nanocrystals were highly dependent on their shape. Different shaped hematite nanocrystals with distinct crystallographic planes have been synthesized under similar reaction conditions, which can be desired as a model for the purpose of properties comparison with the nanocrystals prepared under different reaction conditions. Here we investigated the photocatalytic performance of these different shaped-nanocrystals for methyl orange degradation in the presence of white light (λ > 420 nm). In this study, we found that the density of surface Fe3+ ions in particular facets was the key factor for the photocatalytic activity and was higher on the bitruncated-dodecahedron shape nanocrystals by coexposed {104}, {100} and {001} facets, attributing to higher catalytic activity. The catalytic activity of different exposed facet nanocrystals were as follows: {104} + {100} + {001} (bitruncated-dodecahedron) > {101} + {001} (bitruncated-octahedron) > {001} + {110} (nanorods) > {012} (nanocuboid) which provided the direct evidence of exposed facet-driven photocatalytic activity. The nanocrystals were easily recoverable using an external magnet and reused at least six times without significant loss of its catalytic activity. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr06509g

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

Phase diagram and structural evolution of tin/indium (Sn/In) nanosolder particles: from a non-equilibrium state to an equilibrium state.

PubMed

Shu, Yang; Ando, Teiichi; Yin, Qiyue; Zhou, Guangwen; Gu, Zhiyong

2017-08-31

A binary system of tin/indium (Sn/In) in the form of nanoparticles was investigated for phase transitions and structural evolution at different temperatures and compositions. The Sn/In nanosolder particles in the composition range of 24-72 wt% In were synthesized by a surfactant-assisted chemical reduction method under ambient conditions. The morphology and microstructure of the as-synthesized nanoparticles were analyzed by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED) and X-ray diffraction (XRD). HRTEM and SAED identified InSn 4 and In, with some Sn being detected by XRD, but no In 3 Sn was observed. The differential scanning calorimetry (DSC) thermographs of the as-synthesized nanoparticles exhibited an endothermic peak at around 116 °C, which is indicative of the metastable eutectic melting of InSn 4 and In. When the nanosolders were subjected to heat treatment at 50-225 °C, the equilibrium phase In 3 Sn appeared while Sn disappeared. The equilibrium state was effectively attained at 225 °C. A Tammann plot of the DSC data of the as-synthesized nanoparticles indicated that the metastable eutectic composition is about 62% In, while that of the DSC data of the 225 °C heat-treated nanoparticles yielded a eutectic composition of 54% In, which confirmed the attainment of the equilibrium state at 225 °C. The phase boundaries estimated from the DSC data of heat-treated Sn/In nanosolder particles matched well with those in the established Sn-In equilibrium phase diagram. The phase transition behavior of Sn/In nanosolders leads to a new understanding of binary alloy particles at the nanoscale, and provides important information for their low temperature soldering processing and applications.

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

PubMed

Brodusch, N; Demers, H; Gauvin, R

2013-04-01

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

Phytosynthesized gold nanoparticles from C. roxburghii DC. leaf and their toxic effects on normal and cancer cell lines.

PubMed

Balashanmugam, Pannerselvam; Durai, Prabhu; Balakumaran, Manickam Dakshinamoorthi; Kalaichelvan, Pudupalayam Thangavelu

2016-12-01

Gold nanoparticles are considered of great importance compared to other noble metal nanoparticles and its wide range of applications like pharmaceutics, therapeutics and diagnostics etc. During the past decade, phytosynthesized gold nanoparticles (AuNPs) are more focused in in vitro and in vivo study. The present study was focused on the gold chloride and phytosynthesized gold nanoparticles from aqueous leaf extract of Cassia roxburghii and their toxic effects on African green monkey normal kidney Vero cell line and three different cancer cell lines such as HepG2, MCF7 and HeLa. Phytosynthesized AuNPs were characterized by HRTEM, EDX, XRD and FTIR analysis. The particles size range of 25-35nm was confirmed by HRTEM. The elemental gold and the crystalline nature of AuNPs were confirmed by EDX and XRD, respectively. The reduction of functional groups was confirmed by FTIR. In in vitro study, the IC 50 of HepG2 cells was found to be 30μg/ml compared to other cell lines, HeLa and MCF7 cell line showing IC 50 of 50μg/ml and normal Vero cell line also nontoxic up to 75μg/ml confirmed by MTT assay. Further, apoptosis in HepG2 was analyzed by fluorescence microscope and DNA fragmentation was observed in HepG2 treated cells. These results suggested that phytosynthesized AuNPs of C. roxburghii extract clearly limited toxic on normal cells but toxic in cancer cells. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-10-28

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

Fabrication of highly active Melem/Zn0.25Cd0.75S composites for the degradation of bisphenol A and methyl orange under visible light irradiation

NASA Astrophysics Data System (ADS)

Wang, Xiaodong; Yan, Tao; Liu, Xiaohuan; Ji, Pengge; Sun, Meng; Wei, Dong; Yan, Liangguo; Du, Bin

2016-11-01

Metal-free polymeric catalyst hold great promise owing to their abundant sources, low-cost fabrication and easy processibility. Melem, an important intermediate during condensation of melamine rings to graphitic carbon nitride (g-C3N4), was synthesized by simple solid phase polymerization process. A novel Melem/Zn0.25Cd0.75S composite was fabricated through a facile one-step hydrothermal method. The as-products were characterized by X-ray diffraction (XRD), UV-vis DRS spectroscopy, fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM). The TEM and HRTEM results reveal that Zn0.25Cd0.75S nanoparticles and Melem closely contact with each other to form an intimate interface. The as-prepared composites exhibit significantly enhanced visible light photocatalytic performance for the degradation of Methyl orange (MO) and Bisphenol A (BPA), which could be attributed to the effective photo-induced charges transfer and separation in Melem/Zn0.25Cd0.75S composites. On the basis of radical scavenger experiments, superoxide radicals and holes are suggested to play a critical role in MO degradation over Melem/Zn0.25Cd0.75S heterojunctions. A possible mechanism for charge separation and transfer in the Melem/Zn0.25Cd0.75S composites was proposed to explain the enhanced photocatalytic performance.

Green synthesis, characterization and catalytic degradation studies of gold nanoparticles against congo red and methyl orange.

PubMed

Umamaheswari, C; Lakshmanan, A; Nagarajan, N S

2018-01-01

The present study reports, novel and greener method for synthesis of gold nanoparticles (AuNPs) using 5,7-dihydroxy-6-metoxy-3 ' ,4 ' methylenedioxyisoflavone (Dalspinin), isolated from the roots of Dalbergia coromandeliana was carried out for the first time. The synthesized gold nanoparticles were characterized by UV-Vis spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The observed surface plasmon resonance (SPR) at 532nm in the UV-Vis absorption spectrum indicates the formation of gold nanoparticles. The powder XRD and SAED pattern for synthesized gold nanoparticles confirms crystalline nature. The HR-TEM images showed that the AuNPs formed were small in size, highly monodispersed and spherical in shape. The average particle sizes of the AuNPs are found to be ~10.5nm. The prepared AuNPs were found to be stable for more than 5months without any aggregation. The catalytic degradation studies of the synthesized AuNPs towards degradation of congo red and methyl orange, showed good catalytic in the complete degradation of both the dyes. The reduction catalyzed by gold nanoparticles followed the pseudo-first order kinetics, with a rate constant of 4.5×10 -3 s -1 (R 2 =0.9959) and 1.7×10 -3 s -1 (R 2 =0.9918) for congo red (CR) and methyl orange (MO), respectively. Copyright © 2017. Published by Elsevier B.V.

Rapid synthesis and decoration of reduced graphene oxide with gold nanoparticles by thermostable peptides for memory device and photothermal applications.

PubMed

Otari, Sachin V; Kumar, Manoj; Anwar, Muhammad Zahid; Thorat, Nanasaheb D; Patel, Sanjay K S; Lee, Dongjin; Lee, Jai Hyo; Lee, Jung-Kul; Kang, Yun Chan; Zhang, Liaoyuan

2017-09-08

This article presents novel, rapid, and environmentally benign synthesis method for one-step reduction and decoration of graphene oxide with gold nanoparticles (NAuNPs) by using thermostable antimicrobial nisin peptides to form a gold-nanoparticles-reduced graphene oxide (NAu-rGO) nanocomposite. The formed composite material was characterized by UV/Vis spectroscopy, X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, field emission scanning electron microscopy, and high-resolution transmission electron microscopy (HR-TEM). HR-TEM analysis revealed the formation of spherical AuNPs of 5-30 nm in size on reduced graphene oxide (rGO) nanosheets. A non-volatile-memory device was prepared based on a solution-processed ZnO thin-film transistor fabricated by inserting the NAu-rGO nanocomposite in the gate dielectric stack as a charge trapping medium. The transfer characteristic of the ZnO thin-film transistor memory device showed large clockwise hysteresis behaviour because of charge carrier trapping in the NAu-rGO nanocomposite. Under positive and negative bias conditions, clear positive and negative threshold voltage shifts occurred, which were attributed to charge carrier trapping and de-trapping in the ZnO/NAu-rGO/SiO 2 structure. Also, the photothermal effect of the NAu-rGO nanocomposites on MCF7 breast cancer cells caused inhibition of ~80% cells after irradiation with infrared light (0.5 W cm -2 ) for 5 min.

Room Temperature Ferromagnetic Mn:Ge(001).

PubMed

Lungu, George Adrian; Stoflea, Laura Elena; Tanase, Liviu Cristian; Bucur, Ioana Cristina; Răduţoiu, Nicoleta; Vasiliu, Florin; Mercioniu, Ionel; Kuncser, Victor; Teodorescu, Cristian-Mihail

2013-12-27

We report the synthesis of a room temperature ferromagnetic Mn-Ge system obtained by simple deposition of manganese on Ge(001), heated at relatively high temperature (starting with 250 °C). The samples were characterized by low energy electron diffraction (LEED), scanning tunneling microscopy (STM), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), superconducting quantum interference device (SQUID), and magneto-optical Kerr effect (MOKE). Samples deposited at relatively elevated temperature (350 °C) exhibited the formation of ~5-8 nm diameter Mn₅Ge₃ and Mn 11 Ge₈ agglomerates by HRTEM, while XPS identified at least two Mn-containing phases: the agglomerates, together with a Ge-rich MnGe ~2.5 phase, or manganese diluted into the Ge(001) crystal. LEED revealed the persistence of long range order after a relatively high amount of Mn (100 nm) deposited on the single crystal substrate. STM probed the existence of dimer rows on the surface, slightly elongated as compared with Ge-Ge dimers on Ge(001). The films exhibited a clear ferromagnetism at room temperature, opening the possibility of forming a magnetic phase behind a nearly ideally terminated Ge surface, which could find applications in integration of magnetic functionalities on semiconductor bases. SQUID probed the co-existence of a superparamagnetic phase, with one phase which may be attributed to a diluted magnetic semiconductor. The hypothesis that the room temperature ferromagnetic phase might be the one with manganese diluted into the Ge crystal is formulated and discussed.

Room Temperature Ferromagnetic Mn:Ge(001)

PubMed Central

Lungu, George Adrian; Stoflea, Laura Elena; Tanase, Liviu Cristian; Bucur, Ioana Cristina; Răduţoiu, Nicoleta; Vasiliu, Florin; Mercioniu, Ionel; Kuncser, Victor; Teodorescu, Cristian-Mihail

2014-01-01

We report the synthesis of a room temperature ferromagnetic Mn-Ge system obtained by simple deposition of manganese on Ge(001), heated at relatively high temperature (starting with 250 °C). The samples were characterized by low energy electron diffraction (LEED), scanning tunneling microscopy (STM), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), superconducting quantum interference device (SQUID), and magneto-optical Kerr effect (MOKE). Samples deposited at relatively elevated temperature (350 °C) exhibited the formation of ~5–8 nm diameter Mn5Ge3 and Mn11Ge8 agglomerates by HRTEM, while XPS identified at least two Mn-containing phases: the agglomerates, together with a Ge-rich MnGe~2.5 phase, or manganese diluted into the Ge(001) crystal. LEED revealed the persistence of long range order after a relatively high amount of Mn (100 nm) deposited on the single crystal substrate. STM probed the existence of dimer rows on the surface, slightly elongated as compared with Ge–Ge dimers on Ge(001). The films exhibited a clear ferromagnetism at room temperature, opening the possibility of forming a magnetic phase behind a nearly ideally terminated Ge surface, which could find applications in integration of magnetic functionalities on semiconductor bases. SQUID probed the co-existence of a superparamagnetic phase, with one phase which may be attributed to a diluted magnetic semiconductor. The hypothesis that the room temperature ferromagnetic phase might be the one with manganese diluted into the Ge crystal is formulated and discussed. PMID:28788444

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

Li, X.J., E-mail: lixj@alum.imr.ac.cn

During the deposition of diamond films on Ti alloy substrates, titanium carbide is a common precipitated phase, preferentially formed at the interfacial region. However, in this case, the precipitation of an ordered structure of titanium carbide has not been reported. In our work, a long periodic ordered structure of TiC has been observed at the deposited diamond film/Ti alloy interface by high resolution transmission electron microscopy (HRTEM). The long periodic ordered structure is identified as 6H-type. The formation mechanism is revealed by comparative studies on the different structures of TiC precipitated under different diamond deposition conditions in terms of depositionmore » time, atmosphere and temperature. A large number of carbon vacancies in the interfacial precipitated TiC phase are verified through electron energy loss spectroscopy (EELS) quantification analysis. However, an ordered arrangement of these carbon vacancies occurs only when the interfacial stress is large enough to induce the precipitation of 6H-type TiC. The supplementary analysis by X-ray diffraction (XRD) further confirms that additional diffraction peaks presented in the XRD patterns are corresponding to the precipitation of 6H-type TiC. - Highlights: •Different structures of TiC are observed during deposited diamond on Ti alloy. •One is common NaCl structure, the other is periodic structure. •The periodic structure is identified as 6H-type by HRTEM. •Carbon vacancies are verified to always exist in the TiC phase. •The precipitation of 6H-type TiC is mainly affected by interfacial stress.« less

Characterization and formation of σ/γ interface in Ni-based single crystal superalloys

NASA Astrophysics Data System (ADS)

Ma, Shiyu; Zhang, Jianxin; Li, Xueqiao; Mao, Shengcheng

2017-11-01

High-resolution transmission electron microscopy was used to study interfacial characteristics between the plate-shaped σ phase and the γ phase in a Ni-based single crystal superalloy. The atomic structure of the σ/γ interface constituted by steps was presented. However, the HRTEM micrograph of σ phase is not almost identical with the veritable atomic arrangement of σ phase on the same zone axis. The image formation of HRTEM relies on phase contrast, instead of the amplification of the atomic arrangement. From the simulated HRTEM images, the approximate defocus and thickness of the sample can be got as  -3 nm and 6 nm. σ phase has the following crystallographic orientations relations with γ matrix: [0 0 1] γ //[1 1 2] σ , (1 1 0) γ //(1   -1 0) σ , (-1 1 0) γ //(1 1   -1) σ , which can be proved by the stereographic projection. The interfacial steps are made up by (1 1 0) γ and (-1 1 0) γ or (1   -1 0) σ and (1 1   -1) σ . In the interface steps, the length of (-1 1 0) γ //(1 1   -1) σ is longer than (1 1 0) γ //(1   -1 0) σ , which is caused by that distortion factor of (-1 1 0) γ //(1 1   -1)σ is much smaller than that of (1 1 0) γ //(1   -1 0) σ .

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

PubMed

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

2005-07-19

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

Morphological investigation of nanostructured CoMo catalysts

NASA Astrophysics Data System (ADS)

Pawelec, B.; Castaño, P.; Zepeda, T. A.

2008-04-01

This work reports the morphological investigation of nanostructured sulfided CoMo catalysts by means of high-resolution transmission electron microscopy (HRTEM). The catalysts were supported on Ti-modified hexagonal mesoporous silica (HMS-Ti) and P-modified HMS-Ti (P/HMS-Ti) materials. The oxide precursors were characterized by specific surface area (S BET), temperature-programmed reduction (TPR), diffuse reflectance infrared Fourier transform spectroscopy in the OH region (DRIFTS-OH) and X-ray photoelectron spectroscopy (XPS) in order to elucidate the influence of the impregnation sequence (successive vs. simultaneous) and the effect of P-incorporation into HMS-Ti material on the morphology of calcined CoMo catalysts. Both TPR and XPS measurements indicate that the catalysts prepared by successive impregnation possess well-dispersed MoO 3 and CoO phases, whereas their counterparts prepared by simultaneous impregnation additionally possess the CoMoO 4 phase. For all sulfided catalysts, the presence of MoS 2 phase with particle size in the range 3.3-4.4 nm was confirmed by HRTEM. Catalytic activity was evaluated in the reaction of hydrodesulfurization (HDS) of dibenzothiophene (DBT) carried out in a flow reactor at 593 K and hydrogen pressure of 5.5 MPa. P-incorporation into the HMS-Ti material led to an overall increase in HDS activity and the hydrogenation ability of the sulfided catalysts. All catalysts proved to be stable during 10 h time-on-stream (TOS) operation. The activity of sulfide catalysts in the target reaction depends linearly on the surface exposure of Co species in the oxide precursors, as determined by XPS, and on the morphology of the sulfide form of catalysts (surface density of MoS 2 particles and their sizes) as determined by HRTEM.

Scanning electron microscope fine tuning using four-bar piezoelectric actuated mechanism

NASA Astrophysics Data System (ADS)

Hatamleh, Khaled S.; Khasawneh, Qais A.; Al-Ghasem, Adnan; Jaradat, Mohammad A.; Sawaqed, Laith; Al-Shabi, Mohammad

2018-01-01

Scanning Electron Microscopes are extensively used for accurate micro/nano images exploring. Several strategies have been proposed to fine tune those microscopes in the past few years. This work presents a new fine tuning strategy of a scanning electron microscope sample table using four bar piezoelectric actuated mechanisms. The introduced paper presents an algorithm to find all possible inverse kinematics solutions of the proposed mechanism. In addition, another algorithm is presented to search for the optimal inverse kinematic solution. Both algorithms are used simultaneously by means of a simulation study to fine tune a scanning electron microscope sample table through a pre-specified circular or linear path of motion. Results of the study shows that, proposed algorithms were able to minimize the power required to drive the piezoelectric actuated mechanism by a ratio of 97.5% for all simulated paths of motion when compared to general non-optimized solution.

Towards native-state imaging in biological context in the electron microscope

PubMed Central

Weston, Anne E.; Armer, Hannah E. J.

2009-01-01

Modern cell biology is reliant on light and fluorescence microscopy for analysis of cells, tissues and protein localisation. However, these powerful techniques are ultimately limited in resolution by the wavelength of light. Electron microscopes offer much greater resolution due to the shorter effective wavelength of electrons, allowing direct imaging of sub-cellular architecture. The harsh environment of the electron microscope chamber and the properties of the electron beam have led to complex chemical and mechanical preparation techniques, which distance biological samples from their native state and complicate data interpretation. Here we describe recent advances in sample preparation and instrumentation, which push the boundaries of high-resolution imaging. Cryopreparation, cryoelectron microscopy and environmental scanning electron microscopy strive to image samples in near native state. Advances in correlative microscopy and markers enable high-resolution localisation of proteins. Innovation in microscope design has pushed the boundaries of resolution to atomic scale, whilst automatic acquisition of high-resolution electron microscopy data through large volumes is finally able to place ultrastructure in biological context. PMID:19916039

Purchase of a Transmission Electron Microscope for Xavier University of Louisiana

DTIC Science & Technology

2015-05-15

imaging facility on the second floor of the Pharmacy Addition at Xavier University that already includes two scanning electron microscopes. The new TEM...is now in use. Xavier University has formally pledged to provide funds for the 1. REPORT DATE (DD-MM-YYYY) 4. TITLE AND SUBTITLE 13. SUPPLEMENTARY...for Public Release; Distribution Unlimited Final Report: Purchase of a Transmission Electron Microscope for Xavier University of Louisiana The views

Scanning electron microscopy of hepatic ultrastructure: secondary, backscattered, and transmitted electron imaging.

PubMed

Miyai, K; Abraham, J L; Linthicum, D S; Wagner, R M

1976-10-01

Several methods of tissue preparation and different modes of operation of the scanning electron microscope were used to study the ultrastructure of rat liver. Rat livers were perfusion fixed with buffered 2 per cent paraformaldehyde or a mixture of 1.5 per cent paraformaldehyde and 1 per cent glutaraldehyde and processed as follows. Tissue blocks were postfixed in buffered 2 per cent osmium tetroxide followed sequentially by the ligand-mediated osmium binding technique, dehydration and cryofracture in ethanol, and critical point drying. They were then examined without metal coating in the scanning electron microscope operating in the secondary electron and backscattered electron modes. Fifty-micrometer sections were cut with a tissue sectioner, stained with lead citrate, postfixed with osmium, dehydrated, critical point dried, and examined in the secondary electron and back-scattered electron modes. Frozen sections (0.25 to 0.75 mum. thick) were cut by the method of Tokuyasu (Toluyasu KT: J Cell Biol 57:551, 1973) and their scanning transmission electron microscope images were examined either with a scanning transmission electron microscope detector or with a conversion stub using the secondary electron detector. Secondary electron images of the liver prepared by ligand-mediated osmium binding and subsequent cryofracture revealed such intracellular structures as cisternae of the endoplasmic reticulum, lysosomes, mitochondria, lipid droplets, nucleolus and nuclear chromatin, as well as the usual surface morphology, Lipocytes in the perisinusoidal space were readily identified. Backscattered electron images. Unembedded frozen sections had little drying artifact and were virtually free of freezing damage. The scanning transmission electron microscope image revealed those organelles visualized by the secondary electron mode in the ligand-mediated osmium binding-treated tissue.

Electron Microscope Center Opens at Berkeley.

ERIC Educational Resources Information Center

Robinson, Arthur L.

1981-01-01

A 1.5-MeV High Voltage Electron Microscope has been installed at the Lawrence Berkeley Laboratory which will help materials scientists and biologists study samples in more true-to-life situations. A 1-MeV Atomic Resolution Microscope will be installed at the same location in two years which will allow scientists to distinguish atoms. (DS)

Specimen Holder for Analytical Electron Microscopes

NASA Technical Reports Server (NTRS)

Clanton, U. S.; Isaacs, A. M.; Mackinnon, I.

1985-01-01

Reduces spectral contamination by spurious X-ray. Specimen holder made of compressed carbon, securely retains standard electron microscope grid (disk) 3 mm in diameter and absorbs backscattered electrons that otherwise generate spurious X-rays. Since holder inexpensive, dedicated to single specimen when numerous samples examined.

Microscope and method of use

DOEpatents

Bongianni, Wayne L.

1984-01-01

A method and apparatus for electronically focusing and electronically scanning microscopic specimens are given. In the invention, visual images of even moving, living, opaque specimens can be acoustically obtained and viewed with virtually no time needed for processing (i.e., real time processing is used). And planar samples are not required. The specimens (if planar) need not be moved during scanning, although it will be desirable and possible to move or rotate nonplanar specimens (e.g., laser fusion targets) against the lens of the apparatus. No coupling fluid is needed, so specimens need not be wetted. A phase acoustic microscope is also made from the basic microscope components together with electronic mixers.

Simultaneous specimen and stage cleaning device for analytical electron microscope

DOEpatents

Zaluzec, Nestor J.

1996-01-01

An improved method and apparatus are provided for cleaning both a specimen stage, a specimen and an interior of an analytical electron microscope (AEM). The apparatus for cleaning a specimen stage and specimen comprising a plasma chamber for containing a gas plasma and an air lock coupled to the plasma chamber for permitting passage of the specimen stage and specimen into the plasma chamber and maintaining an airtight chamber. The specimen stage and specimen are subjected to a reactive plasma gas that is either DC or RF excited. The apparatus can be mounted on the analytical electron microscope (AEM) for cleaning the interior of the microscope.

Microscope and method of use

DOEpatents

Bongianni, W.L.

1984-04-17

A method and apparatus for electronically focusing and electronically scanning microscopic specimens are given. In the invention, visual images of even moving, living, opaque specimens can be acoustically obtained and viewed with virtually no time needed for processing (i.e., real time processing is used). And planar samples are not required. The specimens (if planar) need not be moved during scanning, although it will be desirable and possible to move or rotate nonplanar specimens (e.g., laser fusion targets) against the lens of the apparatus. No coupling fluid is needed, so specimens need not be wetted. A phase acoustic microscope is also made from the basic microscope components together with electronic mixers. 7 figs.

NiCo2S4 nanorod embedded rGO sheets as electrodes for supercapacitor

NASA Astrophysics Data System (ADS)

Sarkar, Aatreyee; Bera, Supriya; Chakraborty, Amit Kumar

2018-04-01

We report the synthesis of a hybrid nanostructure based on NiCo2S4 and reduced graphene oxide (rGO) following a facile hydrothermal method. X-ray diffraction (XRD), and electron microscopy (FESEM and HRTEM) analyses showed rod-like NiCo2S4 nanostructures embedded in rGO sheets. The electrochemical analysis of the synthesized nanohybrid using cyclic voltammetry (CV) and galvanostatic charge discharge (GCD) revealed specific capacitance of 410 F/gm indicating its suitability as a good electrode material for supercapacitor.

RBS Depth Profiling Analysis of (Ti, Al)N/MoN and CrN/MoN Multilayers.

PubMed

Han, Bin; Wang, Zesong; Devi, Neena; Kondamareddy, K K; Wang, Zhenguo; Li, Na; Zuo, Wenbin; Fu, Dejun; Liu, Chuansheng

2017-12-01

(Ti, Al)N/MoN and CrN/MoN multilayered films were synthesized on Si (100) surface by multi-cathodic arc ion plating system with various bilayer periods. The elemental composition and depth profiling of the films were investigated by Rutherford backscattering spectroscopy (RBS) using 2.42 and 1.52 MeV Li 2+ ion beams and different incident angles (0°, 15°, 37°, and 53°). The microstructures of (Ti, Al)N/MoN multilayered films were evaluated by X-ray diffraction. The multilayer periods and thickness of the multilayered films were characterized by scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HR-TEM) and then compared with RBS results.

Band Gap Tuning in 2D Layered Materials by Angular Rotation.

PubMed

Polanco-Gonzalez, Javier; Carranco-Rodríguez, Jesús Alfredo; Enríquez-Carrejo, José L; Mani-Gonzalez, Pierre G; Domínguez-Esquivel, José Manuel; Ramos, Manuel

2017-02-08

We present a series of computer-assisted high-resolution transmission electron (HRTEM) simulations to determine Moiré patters by induced twisting effects between slabs at rotational angles of 3°, 5°, 8°, and 16°, for molybdenum disulfide, graphene, tungsten disulfide, and tungsten selenide layered materials. In order to investigate the electronic structure, a series of numerical simulations using density functional methods (DFT) methods was completed using Cambridge serial total energy package (CASTEP) with a generalized gradient approximation to determine both the band structure and density of states on honeycomb-like new superlattices. Our results indicated metallic transitions when the rotation approached 8° with respect to each other laminates for most of the two-dimensional systems that were analyzed.

Synthesis of TiO2 nanoparticles by hydrolysis and peptization of titanium isopropoxide solution

NASA Astrophysics Data System (ADS)

Mahata, S.; Mahato, S. S.; Nandi, M. M.; Mondal, B.

2012-07-01

Here we report the synthesis and characterization of a stable suspension of modified titania nanoparticles. Phase-pure TiO2 nanocrystallites with narrow particle-size distributions were selectively prepared by hydrolysis-peptization of modified alkoxide followed by hydrothermal treatment. Autoclaving modified TiO2 in the presence of HNO3 as cooperative catalysts led to the formation of crystalline TiO2 with narrow-sized distribution. Following the hydrothermal treatment at 150°C, X-ray diffraction shows the particles to be exclusively anatase. Synthesized powder is characterized by FT-IR, scanning electron microscopy (FESEM) and transmission electron microscopy (HRTEM). The photocatalytic activity in the degradation of orange-II is quite comparable to good anatase and rutile nanocrystallites.

Size controlled biogenic silver nanoparticles as antibacterial agent against isolates from HIV infected patients

NASA Astrophysics Data System (ADS)

Suganya, K. S. Uma; Govindaraju, K.; Kumar, V. Ganesh; Dhas, T. Stalin; Karthick, V.; Singaravelu, G.; Elanchezhiyan, M.

2015-06-01

Silver nanoparticles (AgNPs) are synthesized using biological sources due to its high specificity in biomedical applications. Herein, we report the size and shape controlled synthesis of AgNPs using the aqueous extract of blue green alga, Spirulina platensis. Size, shape and elemental composition of AgNPs were characterized using UV-vis spectroscopy, Fluorescence spectroscopy, FT-IR (Fourier Transform-Infrared Spectroscopy), FT-RS (Fourier Transform-Raman Spectroscopy), SEM-EDAX (Scanning Electron Microscopy-Energy Dispersive X-ray analysis) and HR-TEM (High Resolution Transmission Electron Microscopy). AgNPs were stable, well defined and monodispersed (spherical) with an average size of 6 nm. The synthesized AgNPs were tested for its antibacterial potency against isolates obtained from HIV patients.

Colloidal synthesis of monodispersed ZnS and CdS nanocrystals from novel zinc and cadmium complexes

NASA Astrophysics Data System (ADS)

Onwudiwe, Damian C.; Mohammed, Aliyu D.; Strydom, Christien A.; Young, Desmond A.; Jordaan, Anine

2014-06-01

Monodispersed spherical and hexagonal shaped ZnS and CdS nanocrystals respectively, have been synthesized using novel heteroleptic complexes of xanthate (S2CObu) and dithiocarbamate (S2CNMePh). The nanocrystals were prepared via colloidal route and stabilized in hexadecylamine (HDA). The morphology of the as-prepared nanocrystals was characterized using transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), and powdered X-ray diffraction (p-XRD) analysis. An average diameter of 7.2 nm and 8.6 nm were obtained for the ZnS and CdS respectively. The optical properties of the nanoparticles studied by UV-vis and photoluminescence (PL) spectroscopy showed a blue shift in the absorption spectra, and band edge emission respectively.

Band Gap Tuning in 2D Layered Materials by Angular Rotation

PubMed Central

Polanco-Gonzalez, Javier; Carranco-Rodríguez, Jesús Alfredo; Enríquez-Carrejo, José L.; Mani-Gonzalez, Pierre G.; Domínguez-Esquivel, José Manuel; Ramos, Manuel

2017-01-01

We present a series of computer-assisted high-resolution transmission electron (HRTEM) simulations to determine Moiré patters by induced twisting effects between slabs at rotational angles of 3°, 5°, 8°, and 16°, for molybdenum disulfide, graphene, tungsten disulfide, and tungsten selenide layered materials. In order to investigate the electronic structure, a series of numerical simulations using density functional methods (DFT) methods was completed using Cambridge serial total energy package (CASTEP) with a generalized gradient approximation to determine both the band structure and density of states on honeycomb-like new superlattices. Our results indicated metallic transitions when the rotation approached 8° with respect to each other laminates for most of the two-dimensional systems that were analyzed. PMID:28772507

Development of a SEM-based low-energy in-line electron holography microscope for individual particle imaging.

PubMed

Adaniya, Hidehito; Cheung, Martin; Cassidy, Cathal; Yamashita, Masao; Shintake, Tsumoru

2018-05-01

A new SEM-based in-line electron holography microscope has been under development. The microscope utilizes conventional SEM and BF-STEM functionality to allow for rapid searching of the specimen of interest, seamless interchange between SEM, BF-STEM and holographic imaging modes, and makes use of coherent low-energy in-line electron holography to obtain low-dose, high-contrast images of light element materials. We report here an overview of the instrumentation and first experimental results on gold nano-particles and carbon nano-fibers for system performance tests. Reconstructed images obtained from the holographic imaging mode of the new microscope show substantial image contrast and resolution compared to those acquired by SEM and BF-STEM modes, demonstrating the feasibility of high-contrast imaging via low-energy in-line electron holography. The prospect of utilizing the new microscope to image purified biological specimens at the individual particle level is discussed and electron optical issues and challenges to further improve resolution and contrast are considered. Copyright © 2018 Elsevier B.V. All rights reserved.

Development of Ternary and Quaternary Catalysts for the Electrooxidation of Glycerol

PubMed Central

Artem, L. M.; Santos, D. M.; De Andrade, A. R.; Kokoh, K. B.; Ribeiro, J.

2012-01-01

This work consisted in the preparation of platinum-based catalysts supported on carbon (Vulcan XC-72) and investigation of their physicochemical and electrochemical properties. Catalysts of the C/Pt-Ni-Sn-Me (Me = Ru or Ir) type were prepared by the Pechini method at temperature of 350°C. Four different compositions were homemade: C/Pt60Sn10Ni30, C/Pt60Sn10Ni20Ru10, C/Pt60Sn10Ni10Ru20, and C/Pt60Sn10Ni10Ir20. These catalysts were electrochemically and physically characterized by cyclic voltammetry (CV), chronoamperometry (CA) in the presence of glycerol 1.0 mol dm−3, X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HRTEM). XRD results showed the main peaks of face-centered cubic Pt. The particle sizes obtained from XRD and HRTEM experiments were close to values ranging from 3 to 8.5 nm. The CV results indicate behavior typical of Pt-based catalysts in acid medium. The CV and CA data reveal that quaternary catalysts present the highest current density for the electrooxidation of glycerol. PMID:22623905

Formic acid-assisted synthesis of palladium nanocrystals and their electrocatalytic properties.

PubMed

Wang, Qinchao; Wang, Yiqian; Guo, Peizhi; Li, Qun; Ding, Ruixue; Wang, Baoyan; Li, Hongliang; Liu, Jingquan; Zhao, X S

2014-01-14

Palladium (Pd) nanocrystals have been synthesized by using formic acid as the reducing agent at room temperature. When the concentration of formic acid was increased continuously, the size of Pd nanocrystals first decreased to a minimum and then increased slightly again. The products have been investigated by a series of techniques, including X-ray diffraction, high-resolution transmission electron microscopy (HRTEM), UV-vis absorption, and electrochemical measurements. The formation of Pd nanocrystals is proposed to be closely related to the dynamical imbalance of the growth and dissolution rate of Pd nanocrystals associated with the adsorption of formate ions onto the surface of the intermediates. It is found that small Pd nanocrystals showed blue-shifted adsorption peaks compared with large ones. Pd nanocrystals with the smallest size display the highest electrocatalytic activity for the electrooxidation of formic acid and ethanol on the basis of cyclic voltammetry and chronoamperometric data. It is suggested that both the electrochemical active surface area and the small size effect are the key roles in determining the electrocatalytic performances of Pd nanocrystals. A "dissolution-deposition-aggregation" process is proposed to explain the variation of the electrocatalytic activity during the electrocatalysis according to the HRTEM characterization.

75 FR 43918 - National Center for Toxicological Research, et al.; Notice of Consolidated Decision on...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-07-27

... Research, et al.; Notice of Consolidated Decision on Applications for Duty-Free Entry of Electron...: National Center for Toxicological Research, (USFDA), Jefferson, AK 72079. Instrument: Electron Microscope.... Applicant: University of Virginia, Charlottesville, VA 22903. Instrument: Electron Microscope. Manufacturer...

Scanning Electron Microscope Observations of Marine Microorganisms on Surfaces Coated with Antifouling Paints.

DTIC Science & Technology

1981-06-01

sessile marine inverte- brates in Monterey harbor. Veliger 17 (supplement): 1-35. 1977. The nature of primary organic films in the marine environment and...I A10A4h 605 NAVAL POSTGRADUATE SCHOOL MONTEREY CA F/S 11/3 SCANING ELECTRON MICROSCOPE OBSERVATIONS OF MARINE MICROORANI-E-C(U) UNLSSIFIED N*2...Scanning Electron Microscope Observations Master’s thesis; of Marine Microorganisms on Surfaces June 1981 Coated with Ant ifouling Paints 6.PERFORMING

Electron microscope aperture system

NASA Technical Reports Server (NTRS)

Heinemann, K. (Inventor)

1976-01-01

An electron microscope including an electron source, a condenser lens having either a circular aperture for focusing a solid cone of electrons onto a specimen or an annular aperture for focusing a hollow cone of electrons onto the specimen, and an objective lens having an annular objective aperture, for focusing electrons passing through the specimen onto an image plane are described. The invention also entails a method of making the annular objective aperture using electron imaging, electrolytic deposition and ion etching techniques.

Choice and maintenance of equipment for electron crystallography.

PubMed

Mills, Deryck J; Vonck, Janet

2013-01-01

The choice of equipment for an electron crystallography laboratory will ultimately be determined by the available budget; nevertheless, the ideal lab will have two electron microscopes: a dedicated 300 kV cryo-EM with a field emission gun and a smaller LaB(6) machine for screening. The high-end machine should be equipped with photographic film or a very large CCD or CMOS camera for 2D crystal data collection; the screening microscope needs a mid-size CCD for rapid evaluation of crystal samples. The microscope room installations should provide adequate space and a special environment that puts no restrictions on the collection of high-resolution data. Equipment for specimen preparation includes a carbon coater, glow discharge unit, light microscope, plunge freezer, and liquid nitrogen containers and storage dewars. When photographic film is to be used, additional requirements are a film desiccator, dark room, optical diffractometer, and a film scanner. Having the electron microscopes and ancillary equipment well maintained and always in optimum condition facilitates the production of high-quality data.

Vibrational spectroscopy in the electron microscope.

PubMed

Krivanek, Ondrej L; Lovejoy, Tracy C; Dellby, Niklas; Aoki, Toshihiro; Carpenter, R W; Rez, Peter; Soignard, Emmanuel; Zhu, Jiangtao; Batson, Philip E; Lagos, Maureen J; Egerton, Ray F; Crozier, Peter A

2014-10-09

Vibrational spectroscopies using infrared radiation, Raman scattering, neutrons, low-energy electrons and inelastic electron tunnelling are powerful techniques that can analyse bonding arrangements, identify chemical compounds and probe many other important properties of materials. The spatial resolution of these spectroscopies is typically one micrometre or more, although it can reach a few tens of nanometres or even a few ångströms when enhanced by the presence of a sharp metallic tip. If vibrational spectroscopy could be combined with the spatial resolution and flexibility of the transmission electron microscope, it would open up the study of vibrational modes in many different types of nanostructures. Unfortunately, the energy resolution of electron energy loss spectroscopy performed in the electron microscope has until now been too poor to allow such a combination. Recent developments that have improved the attainable energy resolution of electron energy loss spectroscopy in a scanning transmission electron microscope to around ten millielectronvolts now allow vibrational spectroscopy to be carried out in the electron microscope. Here we describe the innovations responsible for the progress, and present examples of applications in inorganic and organic materials, including the detection of hydrogen. We also demonstrate that the vibrational signal has both high- and low-spatial-resolution components, that the first component can be used to map vibrational features at nanometre-level resolution, and that the second component can be used for analysis carried out with the beam positioned just outside the sample--that is, for 'aloof' spectroscopy that largely avoids radiation damage.

Ultrastructural Study of Some Pollen Grains of Prairie Flowers

ERIC Educational Resources Information Center

Kozar, Frank

1973-01-01

Discusses the importance of the electron microscope, and in particular the scanning electron microscope, in studying the surface topography, sectional substructures, and patterns of development of pollen grains. The production, dispersal methods, and structure of pollen grains are described and illustrated with numerous electron micrographs. (JR)

Synthesis Properties and Electron Spin Resonance Properties of Titanic Materials (abstract)

NASA Astrophysics Data System (ADS)

Cho, Jung Min; Lee, Jun; Kim, Tak Hee; Sun, Min Ho; Jang, Young Bae; Cho, Sung June

2009-04-01

Titanic materials were synthesized by hydrothermal method of TiO2 anatase in 10M LiOH, 10M NaOH, and 14M KOH at 130° C for 30 hours. Alkaline media were removed from the synthesized products using 0.1N HCl aqueous solution. The as-prepared samples were characterized by scanning electron microscope, transmission electron microscope, X-ray diffraction, Brunauer-Emmett-Teller isotherm, and electron spin resonance. Different shapes of synthesized products were observed through the typical electron microscope and indicated that the formation of the different morphologies depends on the treatment conditions of highly alkaline media. Many micropores were observed in the cubic or octahedral type of TiO2 samples through the typical electron microscope and Langmuir adsorption-desorption isotherm of liquid nitrogen at 77° K. Electron spin resonance studies have also been carried out to verify the existence of paramagnetic sites such as oxygen vacancies on the titania samples. The effect of alkali metal ions on the morphologies and physicochemical properties of nanoscale titania are discussed.

Design and performance of a beetle-type double-tip scanning tunneling microscope

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

Jaschinsky, Philipp; Coenen, Peter; Pirug, Gerhard

2006-09-15

A combination of a double-tip scanning tunneling microscope with a scanning electron microscope in ultrahigh vacuum environment is presented. The compact beetle-type design made it possible to integrate two independently driven scanning tunneling microscopes in a small space. Moreover, an additional level for coarse movement allows the decoupling of the translation and approach of the tunneling tip. The position of the two tips can be controlled from the millimeter scale down to 50 nm with the help of an add-on electron microscope. The instrument is capable of atomic resolution imaging with each tip.

Development of Scanning Ultrafast Electron Microscope Capability.

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

Collins, Kimberlee Chiyoko; Talin, Albert Alec; Chandler, David W.

Modern semiconductor devices rely on the transport of minority charge carriers. Direct examination of minority carrier lifetimes in real devices with nanometer-scale features requires a measurement method with simultaneously high spatial and temporal resolutions. Achieving nanometer spatial resolutions at sub-nanosecond temporal resolution is possible with pump-probe methods that utilize electrons as probes. Recently, a stroboscopic scanning electron microscope was developed at Caltech, and used to study carrier transport across a Si p-n junction [ 1 , 2 , 3 ] . In this report, we detail our development of a prototype scanning ultrafast electron microscope system at Sandia National Laboratoriesmore » based on the original Caltech design. This effort represents Sandia's first exploration into ultrafast electron microscopy.« less

Ultrastructure of cholinergic neurons in the laterodorsal tegmental nucleus of the rat: interaction with catecholamine fibers.

PubMed

Kubota, Y; Leung, E; Vincent, S R

1992-01-01

The ultrastructure of choline acetyltransferase (ChAT)-immunoreactive neurons in the laterodorsal tegmental nucleus (TLD) of the rat was investigated by immunohistochemical techniques. The immunoreactive neurons were medium to large in size, with a few elongated dendrites, contained well-developed cytoplasm, and a nucleus with deep infoldings. They received many nonimmunoreactive, mostly asymmetric synaptic inputs on their soma and dendrites. ChAT-immunoreactive, usually myelinated, axons were occasionally seen in TLD. Only one immunoreactive axon terminal was observed within TLD, and it made synaptic contact with a nonimmunoreactive neuronal perikaryon. The synaptic interactions between ChAT-immunoreactive neurons and tyrosine hydroxylase (TH)-immunoreactive fibers in the TLD were investigated with a double immunohistochemical staining method. ChAT-immunoreactivity detected with a beta-galactosidase method was light blue-green in the light microscope and formed dot-like electron dense particles at the electron microscopic level. TH-immunoreactivity, visualized with a nickel-enhanced immunoperoxidase method, was dark blue-black in the light microscope and diffusely opaque in the electron microscope. Therefore, the difference between these two kinds of immunoreactivity could be quite easily distinguished at both light and electron microscopic levels. In the light microscope, TH-positive fibers were often closely apposed to ChAT-immunoreactive cell bodies and dendrites in TLD. In the electron microscope, the cell soma and proximal dendrites of ChAT-immunoreactive neurons received synaptic contacts from TH-immunoreactive axon terminals. These results provide a morphological basis for catecholaminergic regulation of the cholinergic reticular system.

77 FR 71776 - Ohio University, et al.; Notice of Consolidated Decision on Applications for Duty-Free Entry of...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-12-04

... Consolidated Decision on Applications for Duty-Free Entry of Electron Microscope This is a decision... Stocker Center, Athens, OH 45701. Instrument: Electron Microscope. Manufacturer: JEOL Ltd., Japan... North Carolina Wilmington, 601 South College Road, Wilmington, NC 28403-5915. Instrument: Electron...

Influence of mechanical noise inside a scanning electron microscope.

PubMed

de Faria, Marcelo Gaudenzi; Haddab, Yassine; Le Gorrec, Yann; Lutz, Philippe

2015-04-01

The scanning electron microscope is becoming a popular tool to perform tasks that require positioning, manipulation, characterization, and assembly of micro-components. However, some of these applications require a higher level of performance with respect to dynamics and precision of positioning. One limiting factor is the presence of unidentified noises and disturbances. This work aims to study the influence of mechanical disturbances generated by the environment and by the microscope, identifying how these can affect elements in the vacuum chamber. To achieve this objective, a dedicated setup, including a high-resolution vibrometer, was built inside the microscope. This work led to the identification and quantification of main disturbances and noise sources acting on a scanning electron microscope. Furthermore, the effects of external acoustic excitations were analysed. Potential applications of these results include noise compensation and real-time control for high accuracy tasks.

Microcircuit testing and fabrication, using scanning electron microscopes

NASA Technical Reports Server (NTRS)

Nicolas, D. P.

1975-01-01

Scanning electron microscopes are used to determine both user-induced damages and manufacturing defects subtle enough to be missed by conventional light microscopy. Method offers greater depth of field and increased working distances.

Method of forming aperture plate for electron microscope

NASA Technical Reports Server (NTRS)

Heinemann, K. (Inventor)

1974-01-01

An electron microscope is described with an electron source a condenser lens having either a circular aperture for focusing a solid cone of electrons onto a specimen or an annular aperture for focusing a hollow cone of electrons onto the specimen. It also has objective lens with an annular objective aperture, for focusing electrons passing through the specimen onto an image plane. A method of making the annular objective aperture using electron imaging, electrolytic deposition and ion etching techniques is included.

Development of scanning electron and x-ray microscope

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

Matsumura, Tomokazu, E-mail: tomokzau.matsumura@etd.hpk.co.jp; Hirano, Tomohiko, E-mail: tomohiko.hirano@etd.hpk.co.jp; Suyama, Motohiro, E-mail: suyama@etd.hpk.co.jp

We have developed a new type of microscope possessing a unique feature of observing both scanning electron and X-ray images under one unit. Unlike former X-ray microscopes using SEM [1, 2], this scanning electron and X-ray (SELX) microscope has a sample in vacuum, thus it enables one to observe a surface structure of a sample by SEM mode, to search the region of interest, and to observe an X-ray image which transmits the region. For the X-ray observation, we have been focusing on the soft X-ray region from 280 eV to 3 keV to observe some bio samples and softmore » materials. The resolutions of SEM and X-ray modes are 50 nm and 100 nm, respectively, at the electron energy of 7 keV.« less

Examination of Surveyor 3 parts with the scanning electron microscope and electron microprobe

NASA Technical Reports Server (NTRS)

Chodos, A. A.; Devaney, J. R.; Evens, K. C.

1972-01-01

Two screws and two washers, several small chips of tubing, and a fiber removed from a third screw were examined with the scanning electron microscope and the electron microprobe. The purpose of the examination was to determine the nature of the material on the surface of these samples and to search for the presence of meteoritic material.

The Antibacterial Polyamide 6-ZnO Hierarchical Nanofibers Fabricated by Atomic Layer Deposition and Hydrothermal Growth

NASA Astrophysics Data System (ADS)

Wang, Zhengduo; Zhang, Li; Liu, Zhongwei; Sang, Lijun; Yang, Lizhen; Chen, Qiang

2017-06-01

In this paper, we report the combination of atomic layer deposition (ALD) with hydrothermal techniques to deposit ZnO on electrospun polyamide 6 (PA 6) nanofiber (NF) surface in the purpose of antibacterial application. The micro- and nanostructures of the hierarchical fibers are characterized by field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), and scanning transmission electron microscopy (STEM). We find that NFs can grow into "water lily"- and "caterpillar"-like shapes, which depend on the number of ALD cycles and the hydrothermal reaction period. It is believed that the thickness of ZnO seed layer by ALD process and the period in hydrothermal reaction have the same importance in crystalline growth and hierarchical fiber formation. The tests of antibacterial activity demonstrate that the ZnO/PA 6 core-shell composite fabricated by the combination of ALD with hydrothermal are markedly efficient in suppressing bacteria survivorship.

Growth, characterization and device development in monocrystalline diamond films

NASA Astrophysics Data System (ADS)

Davis, R. F.; Glass, J. T.; Nemanich, R. J.; Bozeman, S. P.; Sowers, A. T.

1995-06-01

Experimental and theoretical studies concerned with interface interactions of diamond with Si, Ni, and Ni3Si substrates have been conducted. Oriented diamond films deposited on (100) Si were characterized by polar Raman, polar x-ray diffraction (XRD), and cross-sectional high resolution transmission electron microscopy (HRTEM). These sutides showed that the diamond(100)/Si(100) interface adopted the 3:2-match arrangement rather than a 45 deg rotation. Extended Hueckel tight-binding (EHTB) electronic structure calculations for a model system revealed that the interface interaction favors the 3:2-match arrangement. Growth on polycrystalline Ni3Si resulted in oriented diamond particles; under the same growth conditions, graphite was formed on the nickel substrate. Our EHTB electronic structure calculations showed that the (111) and (100) surfaces of Ni3Si have a strong preference for diamond nucleation over graphite nucleation, but this was not the case for the (111) and (100) surfaces of Ni.

High-resolution transmission electron microscopy of hexagonal and rhombohedral molybdenum disulfide crystals.

PubMed

Isshiki, T; Nishio, K; Saijo, H; Shiojiri, M; Yabuuchi, Y; Takahashi, N

1993-07-01

Natural (molybdenite) and synthesized molybdenum disulfide crystals have been studied by high-resolution transmission electron microscopy. The image simulation demonstrates that the [0001] and [0110] HRTEM images of hexagonal and rhombohedral MoS2 crystals hardly disclose their stacking sequences, and that the [2110] images can distinguish the Mo and S columns along the incident electron beam and enable one to determine not only the crystal structure but also the fault structure. Observed [0001] images of cleaved molybdenite and synthesized MoS2 crystals, however, reveal the strain field around partial dislocations limiting an extended dislocation. A cross-sectional image of a single molecular (S-Mo-S) layer cleaved from molybdenite has been observed. Synthesized MoS2 flakes which were prepared by grinding have been found to be rhombohedral crystals containing many stacking faults caused by glides between S/S layers.

A facile hydrothermal approach to synthesize rGO/BiVO4 photocatalysts for visible light induced degradation of RhB dye

NASA Astrophysics Data System (ADS)

Pal, Shreyasi; Dutta, Shibsankar; De, Sukanta

2018-05-01

RGO/BiVO4 composites were synthesized by a simple hydrothermal method. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HRTEM) and surface analysis (BET). The photocatalytic activity of the as-prepared samples was evaluated by studying the degradation of model dyes rhodamine B (RhB) under visible light. The prepared rGO/BiVO4 composites exhibited higher photocatalytic activity for the degradation of RhB with a maximum removal rate of 86% under visible light irradiation under visible-light irradiation than pure BiVO4 nanoparticles (63%). This behavior could be associated to their higher specific surface area (BET), increased light absorption intensity and the degradation of electron-hole pair recombination in BiVO4 with the introduction of the rGO.

Thin single-crystalline Bi2(Te1-xSex)3 ternary nanosheets synthesized by a solvothermal technique

NASA Astrophysics Data System (ADS)

Guo, Jing; Jian, Jikang; Zhang, Zhihua; Wu, Rong; Li, Jin; Sun, Yanfei

2016-01-01

Bi2(Te1-xSex)3 ternary nanosheets have been successfully synthesized through a facile solvothermal technique using diethylenetriamine as solvent, where x can vary from 0 to 1. X-ray diffraction (XRD) and Scanning electron microscopy (SEM) indicate that the as-synthesized Bi2(Te1-xSex)3 samples are nanosheets with rhombohedral structure, and the thickness of the nanosheets can be as thin as several nanometers. High resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) reveal that the nanosheets are single crystalline with a rhombohedral structure. Energy disperse spectroscopy (EDS) and XRD analysis by Vegard's law confirm that the ternary Bi2(Te1-xSex)3 nanosheets have been obtained here. The growth of the nanosheets is discussed based on an amine-based molecular template mechanism that has been employed to synthesize some other metal chalcogenides.

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

PubMed Central

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

2016-01-01

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

Heterojunction CuO-TiO2 nanocomposite synthesis for significant photocatalytic hydrogen production

NASA Astrophysics Data System (ADS)

Manjunath, K.; Souza, V. S.; Ramakrishnappa, T.; Nagaraju, G.; Scholten, J. D.; Dupont, J.

2016-11-01

Effective and low-cost photocatalysts have been synthesized by a simple hydrothermal process. In this process, the two CuO and TiO2 bound one over the other and formed a heterojunction CuO-TiO2 nanocomposite. CuO serves as electron reservoir by receiving electrons from TiO2, which suppresses the recombination of e-/h+ and transfers the received electron to split water, which results in enhanced H2 production. Heterojunction CuO-TiO2 nanocomposite material recorded a maximum of 9284 μmolg-1 H2 production for 2.5 h. The recorded result is 15 times higher than bare TiO2 and 16 times higher than bare CuO. The synthesized materials were characterized and analyzed using various analytical techniques such as XRD, FTIR, UV-vis spectra and the morphology was studied using SEM, TEM, and HRTEM images.

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

PubMed

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

2017-03-01

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

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

PubMed

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

1999-04-01

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

Multi-pass transmission electron microscopy

DOE PAGES

Juffmann, Thomas; Koppell, Stewart A.; Klopfer, Brannon B.; ...

2017-05-10

Feynman once asked physicists to build better electron microscopes to be able to watch biology at work. While electron microscopes can now provide atomic resolution, electron beam induced specimen damage precludes high resolution imaging of sensitive materials, such as single proteins or polymers. Here, we use simulations to show that an electron microscope based on a multi-pass measurement protocol enables imaging of single proteins, without averaging structures over multiple images. While we demonstrate the method for particular imaging targets, the approach is broadly applicable and is expected to improve resolution and sensitivity for a range of electron microscopy imaging modalities,more » including, for example, scanning and spectroscopic techniques. The approach implements a quantum mechanically optimal strategy which under idealized conditions can be considered interaction-free.« less

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.

Elucidating the electronic structure of supported gold nanoparticles and its relevance to catalysis by means of hard X-ray photoelectron spectroscopy

DOE PAGES

Reinecke, Benjamin N.; Kuhl, Kendra P.; Ogasawara, Hirohito; ...

2015-12-31

We report on the electronic structure of Au (gold) nanoparticles supported onto TiO 2 with a goal of elucidating the most important effects that contribute to their high catalytic activity. We synthesize and characterize with high resolution transmission electron microscopy (HRTEM) 3.4, 5.3, and 9.5 nm diameter TiO 2-supported Au nanoparticles with nearly spherical shape and measure their valence band using Au 5d subshell sensitive hard X-ray photoelectron spectroscopy (HAXPES) conducted at Spring-8. Based on density functional theory (DFT) calculations of various Au surface structures, we interpret the observed changes in the Au 5d valence band structure as a functionmore » of size in terms of an increasing percentage of Au atoms at corners/edges for decreasing particle size. Finally, this work elucidates how Au coordination number impacts the electronic structure of Au nanoparticles, ultimately giving rise to their well-known catalytic activity.« less

Functionalized Cobalt Triarylcorrole Covalently Bonded with Graphene Oxide: A Selective Catalyst for the Two- or Four-Electron Reduction of Oxygen.

PubMed

Tang, Jijun; Ou, Zhongping; Guo, Rui; Fang, Yuanyuan; Huang, Dong; Zhang, Jing; Zhang, Jiaoxia; Guo, Song; McFarland, Frederick M; Kadish, Karl M

2017-08-07

A cobalt triphenylcorrole (CorCo) was covalently bonded to graphene oxide (GO), and the resulting product, represented as GO-CorCo, was characterized by UV-vis, FT-IR, and micro-Raman spectroscopy as well as by HRTEM, TGA, XRD, XPS, and AFM. The electrocatalytic activity of GO-CorCo toward the oxygen reduction reaction (ORR) was then examined in air-saturated 0.1 M KOH and 0.5 M H 2 SO 4 solutions by cyclic voltammetry and linear sweep voltammetry using a rotating disk electrode and/or a rotating ring-disk electrode. An overall 4-electron reduction of O 2 is obtained in alkaline media while under acidic conditions a 2-electron process is seen. The ORR results thus indicate that covalently bonded GO-CoCor can be used as a selective catalyst for either the 2- or 4-electron reduction of oxygen, the prevailing reaction depending upon the acidity of the solution.

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

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

NASA Astrophysics Data System (ADS)

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

2015-11-01

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

Construction of a fluorescent nanostructured chitosan-hydroxyapatite scaffold by nanocrystallon induced biomimetic mineralization and its cell biocompatibility.

PubMed

Wang, Guancong; Zheng, Lin; Zhao, Hongshi; Miao, Junying; Sun, Chunhui; Liu, Hong; Huang, Zhen; Yu, Xiaoqiang; Wang, Jiyang; Tao, Xutang

2011-05-01

Biomaterial surfaces and their nanostructures can significantly influence cell growth and viability. Thus, manipulating surface characteristics of scaffolds can be a potential strategy to control cell functions for stem cell tissue engineering. In this study, in order to construct a hydroxyapatite (HAp) coated genipin-chitosan conjugation scaffold (HGCCS) with a well-defined HAp nanostructured surface, we have developed a simple and controllable approach that allows construction of a two-level, three-dimensional (3D) networked structure to provide sufficient calcium source and achieve desired mechanical function and mass transport (permeability and diffusion) properties. Using a nontoxic cross-linker (genipin) and a nanocrystallon induced biomimetic mineralization method, we first assembled a layer of HAp network-like nanostructure on a 3D porous chitosan-based framework. X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM) analysis confirm that the continuous network-like nanostructure on the channel surface of the HGCCS is composed of crystalline HAp. Compressive testing demonstrated that the strength of the HGCCS is apparently enhanced because of the strong cross-linking of genipin and the resulting reinforcement of the HAp nanonetwork. The fluorescence properties of genipin-chitosan conjugation for convenient monitoring of the 3D porous scaffold biodegradability and cell localization in the scaffold was specifically explored using confocal laser scanning microscopy (CLSM). Furthermore, through scanning electron microscope (SEM) observation and immunofluorescence measurements of F-actin, we found that the HAp network-like nanostructure on the surface of the HGCCS can influence the morphology and integrin-mediated cytoskeleton organization of rat bone marrow-derived mesenchymal stem cells (BMSCs). Based on cell proliferation assays, rat BMSCs tend to have higher viability on HGCCS in vitro. The results of this study suggest that the fluorescent two-level 3D nanostructured chitosan-HAp scaffold will be a promising scaffold for bone tissue engineering application.

Nonstoichiometry and phase stability of Al and Cr substituted Mg ferrite nanoparticles synthesized by citrate method

NASA Astrophysics Data System (ADS)

Ateia, Ebtesam. E.; Mohamed, Amira. T.

2017-03-01

The spinel ferrite Mg0.7Cr0.3Fe2O4, and Mg0.7Al0.3Fe2O4 were prepared by the citrate technique. All samples were characterized by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), High Resolution Transmission Electron Micrographs (HRTEM), Energy Dispersive X ray Spectroscopy (EDAX) and Atomic Force Microscope (AFM). XRD confirmed the formation of cubic spinel structure of the investigated samples. The average crystallite sizes were found to be between 24.7 and 27.5 nm for Al3+ and Mg2+ respectively. The substitution of Cr3+/Al3+ in place of Mg2+ ion initiates a crystalline anisotropy due to large size mismatch between Cr /Al and Mg2+, which creates strain inside the crystal volume. According to VSM results, by adding Al3+ or Cr3+ ions at the expense of Mg2+, the saturation magnetization increased. The narrow hysteresis loop of the samples indicates that the amount of dissipated energy is small, which is desirable for soft magnetic applications. Magnetic dynamics of the samples were studied by measuring magnetic susceptibility versus temperature at different magnetic fields. The band gap energy, which was calculated from near infrared (NIR) and visible (VIS) reflectance spectra using the Kubelka-Munk function, decreases with increasing the particle size. Furthermore, the band gaps were quite narrow (1.5-1.7 eV), hence the investigated samples could act as visible light driven photo catalysts. To sum up the addition of trivalent Al3+, and Cr3+ ions enhanced the optical, magnetic and structure properties of the samples. Mg0.7 Cr0.3Fe2O4 sample will be a better candidate for the optical applications and will also be a guaranteeing hopeful for technological applications.

Study on the Visible-Light Photocatalytic Performance and Degradation Mechanism of Diclofenac Sodium under the System of Hetero-Structural CuBi2O4/Ag3PO4 with H2O2

PubMed Central

Chen, Xiaojuan; Li, Ning; Xu, Song; Cai, Yumin

2018-01-01

Two kinds of CuBi2O4/Ag3PO4 with different heterojunction structures were prepared based on the combination of hydrothermal and in-situ precipitation methods with surfactant additives (sodium citrate and sodium stearate), and their characteristics were systematically resolved by X-ray Diffraction (XRD), Brunauer–Emmett–Teller (BET), X-ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscope (SEM)/ High-resolution Transmission Electron Microscopy (HRTEM), UV-vis Diffuse Reflectance Spectra (DRS) and Photoluminescence (PL). Meanwhile, the photocatalytic properties of the catalysts were determined for diclofenac sodium (DS) degradation and the photocatalytic mechanism was also explored. The results indicate that both of the two kinds of CuBi2O4/Ag3PO4 exhibit higher photocatalytic efficiency, mineralization rate, and stability than that of pure CuBi2O4 or Ag3PO4. Moreover, the catalytic activity of CuBi2O4/Ag3PO4 can be further enhanced by adding H2O2. The free radical capture experiments show that in the pure CuBi2O4/Ag3PO4 photocatalytic system, the OH• and O2•− are the main species participating in DS degradation; however, in the CuBi2O4/Ag3PO4 photocatalytic system with H2O2, all OH•, h+, and O2•− take part in the DS degradation, and the contribution order is OH• > h+ > O2•−. Accordingly, the photocatalytic mechanism of CuBi2O4/Ag3PO4 could be explained by the Z-Scheme theory, while the catalysis of CuBi2O4/Ag3PO4 with H2O2 follows the heterojunction energy band theory. PMID:29597267

Visualizing Morphological Changes of Abscission Zone Cells in Arabidopsis by Scanning Electron Microscope.

PubMed

Shi, Chun-Lin; Butenko, Melinka A

2018-01-01

Scanning electron microscope (SEM) is a type of electron microscope which produces detailed images of surface structures. It has been widely used in plants and animals to study cellular structures. Here, we describe a detailed protocol to prepare samples of floral abscission zones (AZs) for SEM, as well as further image analysis. We show that it is a powerful tool to detect morphologic changes at the cellular level during the course of abscission in wild-type plants and to establish the details of phenotypic alteration in abscission mutants.

Scanning electron microscopic appearance of rat otocyst of the twelfth postcoital day: elaboration of a method.

PubMed

Marovitz, W F; Khan, K M

1977-01-01

A method for removal, fixation, microdissection, and drying of early rat otocyst for examination by the scanning electron microscope is elaborated. Tissues were dissected, fixed as for conventional transmission electron microscopy and dried by critical point evaporation using amylacetate as the transitional fluid and carbon dioxide as the pressure head. Otocysts were either dissected at the time of initial fixation, or subsequent to drying. The otocyst of the 12th postcoital day was used as a model system in this preliminary report. Critical point drying retained the overall configuration and the fine ultrastructural detail of the otocyst. The interior otocystic surface was visualized and cilia bearing cells of the luminal surface were identified. Most if not all of these cells had a comspicuous, but short kinocillum which terminated in an ovoid bulb. The scanning electron microscopic appearance was correlated to the transmission electron microscopic image seen in the second paper in this Supplement.

Atmospheric scanning electron microscope for correlative microscopy.

PubMed

Morrison, Ian E G; Dennison, Clare L; Nishiyama, Hidetoshi; Suga, Mitsuo; Sato, Chikara; Yarwood, Andrew; O'Toole, Peter J

2012-01-01

The JEOL ClairScope is the first truly correlative scanning electron and optical microscope. An inverted scanning electron microscope (SEM) column allows electron images of wet samples to be obtained in ambient conditions in a biological culture dish, via a silicon nitride film window in the base. A standard inverted optical microscope positioned above the dish holder can be used to take reflected light and epifluorescence images of the same sample, under atmospheric conditions that permit biochemical modifications. For SEM, the open dish allows successive staining operations to be performed without moving the holder. The standard optical color camera used for fluorescence imaging can be exchanged for a high-sensitivity monochrome camera to detect low-intensity fluorescence signals, and also cathodoluminescence emission from nanophosphor particles. If these particles are applied to the sample at a suitable density, they can greatly assist the task of perfecting the correlation between the optical and electron images. Copyright © 2012 Elsevier Inc. All rights reserved.

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

Juffmann, Thomas; Koppell, Stewart A.; Klopfer, Brannon B.

Feynman once asked physicists to build better electron microscopes to be able to watch biology at work. While electron microscopes can now provide atomic resolution, electron beam induced specimen damage precludes high resolution imaging of sensitive materials, such as single proteins or polymers. Here, we use simulations to show that an electron microscope based on a multi-pass measurement protocol enables imaging of single proteins, without averaging structures over multiple images. While we demonstrate the method for particular imaging targets, the approach is broadly applicable and is expected to improve resolution and sensitivity for a range of electron microscopy imaging modalities,more » including, for example, scanning and spectroscopic techniques. The approach implements a quantum mechanically optimal strategy which under idealized conditions can be considered interaction-free.« less

Electron holography study of magnetization behavior in the writer pole of a perpendicular magnetic recording head by a 1 MV transmission electron microscope.

PubMed

Hirata, Kei; Ishida, Yoichi; Akashi, Tetsuya; Shindo, Daisuke; Tonomura, Akira

2012-01-01

The magnetic domain structure of the writer poles of perpendicular magnetic recording heads was studied using electron holography. Although the domain structure of a 100-nm-thick writer pole could be observed with a 300 kV transmission electron microscope, that of the 250-nm-thick writer pole could not be analyzed due to the limited transmission capability of the instrument. On the other hand, the detailed domain structure of the 250-nm-thick writer pole was successfully analyzed by a 1 MV electron microscope using its high transmission capability. The thickness and material dependency of the domain structure of a writer pole were discussed.

Attainment of 40.5 pm spatial resolution using 300 kV scanning transmission electron microscope equipped with fifth-order aberration corrector.

PubMed

Morishita, Shigeyuki; Ishikawa, Ryo; Kohno, Yuji; Sawada, Hidetaka; Shibata, Naoya; Ikuhara, Yuichi

2018-02-01

The achievement of a fine electron probe for high-resolution imaging in scanning transmission electron microscopy requires technological developments, especially in electron optics. For this purpose, we developed a microscope with a fifth-order aberration corrector that operates at 300 kV. The contrast flat region in an experimental Ronchigram, which indicates the aberration-free angle, was expanded to 70 mrad. By using a probe with convergence angle of 40 mrad in the scanning transmission electron microscope at 300 kV, we attained the spatial resolution of 40.5 pm, which is the projected interatomic distance between Ga-Ga atomic columns of GaN observed along [212] direction.

Optics of high-performance electron microscopes*

PubMed Central

Rose, H H

2008-01-01

During recent years, the theory of charged particle optics together with advances in fabrication tolerances and experimental techniques has lead to very significant advances in high-performance electron microscopes. Here, we will describe which theoretical tools, inventions and designs have driven this development. We cover the basic theory of higher-order electron optics and of image formation in electron microscopes. This leads to a description of different methods to correct aberrations by multipole fields and to a discussion of the most advanced design that take advantage of these techniques. The theory of electron mirrors is developed and it is shown how this can be used to correct aberrations and to design energy filters. Finally, different types of energy filters are described. PMID:27877933

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

Rau, E. I.; Orlikovskiy, N. A.; Ivanova, E. S.

A new highly efficient design for semiconductor detectors of intermediate-energy electrons (1-50 keV) for application in scanning electron microscopes is proposed. Calculations of the response function of advanced detectors and control experiments show that the efficiency of the developed devices increases on average twofold, which is a significant positive factor in the operation of modern electron microscopes in the mode of low currents and at low primary electron energies.

Synthesis of highly stable silver nanoparticles through a novel green method using Mirabillis jalapa for antibacterial, nonlinear optical applications

NASA Astrophysics Data System (ADS)

Pugazhendhi, S.; Palanisamy, P. K.; Jayavel, R.

2018-05-01

Green synthesis techniques are developing as more simplistic and eco-friendly approach for the synthesis of metal nanoparticles compared to chemical reduction methods. Herein we report Synthesis of highly stable silver nanoparticles using Mirabillis jalapa seed extract as a reducing and capping agent. The as-prepared silver nanoparticles were characterized by UV-vis spectroscopy (UV-vis) to confirm the formation of silver nanoparticles by its characteristic surface plasmon resonance peak observed at 420 nm. The Powder X-ray diffraction (P-XRD) revealed the structure and crystalline nature of synthesized silver nanoparticles, The Fourier transform infra-red spectroscopic (FT-IR) revealed the presence of the biomolecules in the extract that acted as reducing as well stabilizing agent. The high resolution transmission electron microscopic (HRTEM) images divulged that the synthesized silver nanoparticles were spherical in shape and poly dispersed. The energy dispersive X-ray diffraction (EDX) profile revealed the elements present in the as-synthesized colloidal silver nanoparticles and its percentages. The Zeta potential measured for silver nanoparticles evidenced that the prepared silver nanoparticles owned high stability in room temperature itself. The as-synthesized silver nanoparticles (AgNPs) in colloidal form were showed good antimicrobial effects and it's were found to exhibit third order optical nonlinearity as studied by Z-scan technique using 532 nm Nd:YAG (SHG) CW laser beam (COHERENT-Compass 215 M-50 diode pumped) output as source. The negative nonlinearity observed was well utilized for the study of optical limiting behavior of the silver nanoparticles.

Using the scanning electron microscope on the production line to assure quality semiconductors

NASA Technical Reports Server (NTRS)

Adolphsen, J. W.; Anstead, R. J.

1972-01-01

The use of the scanning electron microscope to detect metallization defects introduced during batch processing of semiconductor devices is discussed. A method of determining metallization integrity was developed which culminates in a procurement specification using the scanning microscope on the production line as a quality control tool. Batch process control of the metallization operation is monitored early in the manufacturing cycle.

Influence of mechanical noise inside a scanning electron microscope

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

Gaudenzi de Faria, Marcelo; Haddab, Yassine, E-mail: yassine.haddab@femto-st.fr; Le Gorrec, Yann

The scanning electron microscope is becoming a popular tool to perform tasks that require positioning, manipulation, characterization, and assembly of micro-components. However, some of these applications require a higher level of performance with respect to dynamics and precision of positioning. One limiting factor is the presence of unidentified noises and disturbances. This work aims to study the influence of mechanical disturbances generated by the environment and by the microscope, identifying how these can affect elements in the vacuum chamber. To achieve this objective, a dedicated setup, including a high-resolution vibrometer, was built inside the microscope. This work led to themore » identification and quantification of main disturbances and noise sources acting on a scanning electron microscope. Furthermore, the effects of external acoustic excitations were analysed. Potential applications of these results include noise compensation and real-time control for high accuracy tasks.« less

78 FR 5776 - Columbia University, et al.; Notice of Consolidated Decision on Applications for Duty-Free Entry...

Federal Register 2010, 2011, 2012, 2013, 2014

2013-01-28

... 94305. Instrument: Titan 80-300 Environmental Transmission Electron Microscope. Manufacturer: FEI Co.../Scanning Electron Microscope. Manufacturer: FEI Co., the Netherlands. Intended Use: See notice at 77 FR...

Fine needle aspiration (FNA) of synovial sarcoma--a comparative histological-cytological study of 15 cases, including immunohistochemical, electron microscopic and cytogenetic examination and DNA-ploidy analysis.

PubMed

Akerman, M; Willén, H; Carlén, B; Mandahl, N; Mertens, F

1996-06-01

A retrospective study of 25 FNAs (11 aspirates from primary tumours and 14 from recurrencies and metastases) from 15 synovial sarcomas was performed. The cytological findings were correlated with the histopathology and the value of immunohistochemical and electron microscopic examination as well as DNA-ploidy and cytogenetic analysis for diagnosis were assessed. A reproducible cellular pattern with a reliable diagnosis of spindle cell sarcoma was possible provided that the aspirates were cell rich. However, a true biphasic pattern indicative of synovial sarcoma was only seen in one of the 25 specimens. Electron microscopic examination of the aspirates was a valuable adjunctive diagnostic method, whereas immunocytochemistry and DNA-ploidy analysis were not. Immunohistochemical, electron microscopic and cytogenetic analysis were all valuable ancillary methods when performed on surgical specimens. Malignant haemangiopericytoma and fibrosarcoma were the most important differential diagnoses in the FNA specimens.

A two-dimensional Dirac fermion microscope

NASA Astrophysics Data System (ADS)

Bøggild, Peter; Caridad, José M.; Stampfer, Christoph; Calogero, Gaetano; Papior, Nick Rübner; Brandbyge, Mads

2017-06-01

The electron microscope has been a powerful, highly versatile workhorse in the fields of material and surface science, micro and nanotechnology, biology and geology, for nearly 80 years. The advent of two-dimensional materials opens new possibilities for realizing an analogy to electron microscopy in the solid state. Here we provide a perspective view on how a two-dimensional (2D) Dirac fermion-based microscope can be realistically implemented and operated, using graphene as a vacuum chamber for ballistic electrons. We use semiclassical simulations to propose concrete architectures and design rules of 2D electron guns, deflectors, tunable lenses and various detectors. The simulations show how simple objects can be imaged with well-controlled and collimated in-plane beams consisting of relativistic charge carriers. Finally, we discuss the potential of such microscopes for investigating edges, terminations and defects, as well as interfaces, including external nanoscale structures such as adsorbed molecules, nanoparticles or quantum dots.

A two-dimensional Dirac fermion microscope

PubMed Central

Bøggild, Peter; Caridad, José M.; Stampfer, Christoph; Calogero, Gaetano; Papior, Nick Rübner; Brandbyge, Mads

2017-01-01

The electron microscope has been a powerful, highly versatile workhorse in the fields of material and surface science, micro and nanotechnology, biology and geology, for nearly 80 years. The advent of two-dimensional materials opens new possibilities for realizing an analogy to electron microscopy in the solid state. Here we provide a perspective view on how a two-dimensional (2D) Dirac fermion-based microscope can be realistically implemented and operated, using graphene as a vacuum chamber for ballistic electrons. We use semiclassical simulations to propose concrete architectures and design rules of 2D electron guns, deflectors, tunable lenses and various detectors. The simulations show how simple objects can be imaged with well-controlled and collimated in-plane beams consisting of relativistic charge carriers. Finally, we discuss the potential of such microscopes for investigating edges, terminations and defects, as well as interfaces, including external nanoscale structures such as adsorbed molecules, nanoparticles or quantum dots. PMID:28598421

Synthesis of TiO{sub 2} nanoparticles by hydrolysis and peptization of titanium isopropoxide solution

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

Mahata, S.; Mahato, S. S.; Nandi, M. M.

2012-07-23

Here we report the synthesis and characterization of a stable suspension of modified titania nanoparticles. Phase-pure TiO{sub 2} nanocrystallites with narrow particle-size distributions were selectively prepared by hydrolysis-peptization of modified alkoxide followed by hydrothermal treatment. Autoclaving modified TiO{sub 2} in the presence of HNO3 as cooperative catalysts led to the formation of crystalline TiO{sub 2} with narrow-sized distribution. Following the hydrothermal treatment at 150 Degree-Sign C, X-ray diffraction shows the particles to be exclusively anatase. Synthesized powder is characterized by FT-IR, scanning electron microscopy (FESEM) and transmission electron microscopy (HRTEM). The photocatalytic activity in the degradation of orange-II is quitemore » comparable to good anatase and rutile nanocrystallites.« less

Morphological and phase evolution of TiO 2 nanocrystals prepared from peroxotitanate complex aqueous solution: Influence of acetic acid

NASA Astrophysics Data System (ADS)

Chang, Jeong Ah; Vithal, Muga; Baek, In Chan; Seok, Sang Il

2009-04-01

Nanosized anatase and rutile TiO 2 having different shape, phase and size have been prepared from aqueous solutions of peroxo titanium complex starting from titanium(IV) isopropoxide (TTIP), acetic acid and hydrogen peroxide (H 2O 2) in water/isopropanol media by a facile sol-gel process. The TiO 2 nanocrystals are characterized by powder X-ray diffraction (XRD), Raman spectroscopy, FT-IR spectroscopy, TEM, high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) techniques. The influence of pH and the sequence of addition of reaction contents on the phase and morphology of TiO 2 are studied. The reasons for the observation of only anatase and/or mixture of anatase and rutile are given.

Analysis of composition and microstructures of Ge grown on porous silicon using Raman spectroscopy and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Aouassa, Mansour; Jadli, Imen; Hassayoun, Latifa Slimen; Maaref, Hassen; Panczer, Gerard; Favre, Luc; Ronda, Antoine; Berbezier, Isabelle

2017-12-01

Composition and microstructure of Ge grown on porous silicon (PSi) by Molecular Beam Epitaxy (MBE) at different temperatures are examined using High Resolution Transmission Electron Microscopy (HRTEM) and Raman spectroscopy. Ge grown at 400 °C on PSi buffer produces a planar Ge film with high crystalline quality compared to Ge grown on bulk Si. This result is attributed to the compliant nature of PSi. Increasing growth temperature >600 °C, changes the PSi morphology, increase the Ge/Si intermixing in the pores during Ge growth and lead to obtain a composite SiGe/Si substrate. Ge content in the composite SiGe substrate can controlled via growth temperature. These substrates serve as low cost virtual substrate for high efficiency III-V/Si solar cells.

Superionic conductor PbSnF4 in the inner channel of SWNT

NASA Astrophysics Data System (ADS)

Zakalyukin, Ruslan Mikhalovich; Levkevich, Ekaterina Alexandrovna; Kumskov, Andrey Sergeevich; Orekhov, Andrey Sergeevich

2018-04-01

The nanocomposite PbSnF4@SWNT was obtained by capillary technique for the first time. This nanocomposite was investigated using X-ray diffraction phase analysis (XRD), high-resolution transmission electron microscopy (HRTEM) and scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDX). SWNT diameter is ˜2 nm. Lead tetrafluorostannate (PbSnF4) monoclinic modification (space group P2/n) was identified by XRD analysis. The periodicity of the crystal plane (201) along the tube axis is ˜3.2Å. The distortion of plane is 11° with respect to the nanotube axis. The model of PbSnF4 single crystal contains ˜168 atoms. The structure of 1D PbSnF4@SWNT nanocomposite and HREM image were modelled.

Scanning Microscopes Using X Rays and Microchannels

NASA Technical Reports Server (NTRS)

Wang, Yu

2003-01-01

Scanning microscopes that would be based on microchannel filters and advanced electronic image sensors and that utilize x-ray illumination have been proposed. Because the finest resolution attainable in a microscope is determined by the wavelength of the illumination, the xray illumination in the proposed microscopes would make it possible, in principle, to achieve resolutions of the order of nanometers about a thousand times as fine as the resolution of a visible-light microscope. Heretofore, it has been necessary to use scanning electron microscopes to obtain such fine resolution. In comparison with scanning electron microscopes, the proposed microscopes would likely be smaller, less massive, and less expensive. Moreover, unlike in scanning electron microscopes, it would not be necessary to place specimens under vacuum. The proposed microscopes are closely related to the ones described in several prior NASA Tech Briefs articles; namely, Miniature Microscope Without Lenses (NPO-20218), NASA Tech Briefs, Vol. 22, No. 8 (August 1998), page 43; and Reflective Variants of Miniature Microscope Without Lenses (NPO-20610), NASA Tech Briefs, Vol. 26, No. 9 (September 2002) page 6a. In all of these microscopes, the basic principle of design and operation is the same: The focusing optics of a conventional visible-light microscope are replaced by a combination of a microchannel filter and a charge-coupled-device (CCD) image detector. A microchannel plate containing parallel, microscopic-cross-section holes much longer than they are wide is placed between a specimen and an image sensor, which is typically the CCD. The microchannel plate must be made of a material that absorbs the illuminating radiation reflected or scattered from the specimen. The microchannels must be positioned and dimensioned so that each one is registered with a pixel on the image sensor. Because most of the radiation incident on the microchannel walls becomes absorbed, the radiation that reaches the image sensor consists predominantly of radiation that was launched along the longitudinal direction of the microchannels. Therefore, most of the radiation arriving at each pixel on the sensor must have traveled along a straight line from a corresponding location on the specimen. Thus, there is a one-to-one mapping from a point on a specimen to a pixel in the image sensor, so that the output of the image sensor contains image information equivalent to that from a microscope.

Development of the field of structural physiology

PubMed Central

FUJIYOSHI, Yoshinori

2015-01-01

Electron crystallography is especially useful for studying the structure and function of membrane proteins — key molecules with important functions in neural and other cells. Electron crystallography is now an established technique for analyzing the structures of membrane proteins in lipid bilayers that closely simulate their natural biological environment. Utilizing cryo-electron microscopes with helium-cooled specimen stages that were developed through a personal motivation to understand the functions of neural systems from a structural point of view, the structures of membrane proteins can be analyzed at a higher than 3 Å resolution. This review covers four objectives. First, I introduce the new research field of structural physiology. Second, I recount some of the struggles involved in developing cryo-electron microscopes. Third, I review the structural and functional analyses of membrane proteins mainly by electron crystallography using cryo-electron microscopes. Finally, I discuss multifunctional channels named “adhennels” based on structures analyzed using electron and X-ray crystallography. PMID:26560835

Development of an environmental high-voltage electron microscope for reaction science.

PubMed

Tanaka, Nobuo; Usukura, Jiro; Kusunoki, Michiko; Saito, Yahachi; Sasaki, Katuhiro; Tanji, Takayoshi; Muto, Shunsuke; Arai, Shigeo

2013-02-01

Environmental transmission electron microscopy and ultra-high resolution electron microscopic observation using aberration correctors have recently emerged as topics of great interest. The former method is an extension of the so-called in situ electron microscopy that has been performed since the 1970s. Current research in this area has been focusing on dynamic observation with atomic resolution under gaseous atmospheres and in liquids. Since 2007, Nagoya University has been developing a new 1-MV high voltage (scanning) transmission electron microscope that can be used to observe nanomaterials under conditions that include the presence of gases, liquids and illuminating lights, and it can be also used to perform mechanical operations to nanometre-sized areas as well as electron tomography and elemental analysis by electron energy loss spectroscopy. The new instrument has been used to image and analyse various types of samples including biological ones.

Nucleotide-Specific Contrast for DNA Sequencing by Electron Spectroscopy.

PubMed

Mankos, Marian; Persson, Henrik H J; N'Diaye, Alpha T; Shadman, Khashayar; Schmid, Andreas K; Davis, Ronald W

2016-01-01

DNA sequencing by imaging in an electron microscope is an approach that holds promise to deliver long reads with low error rates and without the need for amplification. Earlier work using transmission electron microscopes, which use high electron energies on the order of 100 keV, has shown that low contrast and radiation damage necessitates the use of heavy atom labeling of individual nucleotides, which increases the read error rates. Other prior work using scattering electrons with much lower energy has shown to suppress beam damage on DNA. Here we explore possibilities to increase contrast by employing two methods, X-ray photoelectron and Auger electron spectroscopy. Using bulk DNA samples with monomers of each base, both methods are shown to provide contrast mechanisms that can distinguish individual nucleotides without labels. Both spectroscopic techniques can be readily implemented in a low energy electron microscope, which may enable label-free DNA sequencing by direct imaging.

High-resolution electron microscope

NASA Technical Reports Server (NTRS)

Nathan, R.

1977-01-01

Employing scanning transmission electron microscope as interferometer, relative phases of diffraction maximums can be determined by analysis of dark field images. Synthetic aperture technique and Fourier-transform computer processing of amplitude and phase information provide high resolution images at approximately one angstrom.

75 FR 9867 - University of Pittsburgh, et al

Federal Register 2010, 2011, 2012, 2013, 2014

2010-03-04

... DEPARTMENT OF COMMERCE International Trade Administration University of Pittsburgh, et al.; Notice of Consolidated Decision on Applications for Duty-Free Entry of Electron Microscopes This is a...: University of Pittsburgh, Pittsburgh, PA 15260. Instrument: Electron Microscope. Manufacturer: JEOL, Ltd...

Development of a miniature scanning electron microscope for in-flight analysis of comet dust

NASA Technical Reports Server (NTRS)

Conley, J. M.; Bradley, J. G.; Giffin, C. E.; Albee, A. L.; Tomassian, A. D.

1983-01-01

A description is presented of an instrument which was developed with the original goal of being flown on the International Comet Mission, scheduled for a 1985 launch. The Scanning Electron Microscope and Particle Analyzer (SEMPA) electron miniprobe is a miniaturized electrostatically focused electron microscope and energy dispersive X-ray analyzer for in-flight analysis of comet dust particles. It was designed to be flown on board a comet rendezvous spacecraft. Other potential applications are related to asteroid rendezvous and planetary lander missions. According to the development objectives, SEMPA miniprobe is to have the capability for imaging and elemental analysis of particles in the size range of 0.25 microns and larger.

Ultrasonication-assisted synthesis of high aspect ratio gold nanowires on a graphene template and investigation of their growth mechanism.

PubMed

Xin, Wenbo; De Rosa, Igor M; Cao, Yang; Yin, Xunqian; Yu, Hang; Ye, Peiyi; Carlson, Larry; Yang, Jenn-Ming

2018-04-19

We report a facile synthesis of Au nanowires (AuNWs) with a high aspect ratio (l/D) of up to 5000 on a plasma activated graphene template with ultrasound assistance. We demonstrate that the ultrasonication induced symmetry breaking of Au clusters facilitates the growth of AuNWs from the embryonic stages. Furthermore, the growth mechanism of AuNWs is systematically investigated using high resolution electron transmission microscopy (HRTEM), which reveals the unique role of the defective graphene template in directing the growth of AuNWs.

Annealing effect and photovoltaic properties of nano-ZnS/textured p-Si heterojunction.

PubMed

Ji, Liang-Wen; Hsiao, Yu-Jen; Tang, I-Tseng; Meen, Teen-Hang; Liu, Chien-Hung; Tsai, Jenn-Kai; Wu, Tien-Chuan; Wu, Yue-Sian

2013-11-09

The preparation and characterization of heterojunction solar cell with ZnS nanocrystals synthesized by chemical bath deposition method were studied in this work. The ZnS nanocrystals were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Lower reflectance spectra were found as the annealing temperature of ZnS film increased on the textured p-Si substrate. It was found that the power conversion efficiency (PCE) of the AZO/ZnS/textured p-Si heterojunction solar cell with an annealing temperature of 250°C was η = 3.66%.

Annealing effect and photovoltaic properties of nano-ZnS/textured p-Si heterojunction

PubMed Central

2013-01-01

The preparation and characterization of heterojunction solar cell with ZnS nanocrystals synthesized by chemical bath deposition method were studied in this work. The ZnS nanocrystals were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Lower reflectance spectra were found as the annealing temperature of ZnS film increased on the textured p-Si substrate. It was found that the power conversion efficiency (PCE) of the AZO/ZnS/textured p-Si heterojunction solar cell with an annealing temperature of 250°C was η = 3.66%. PMID:24206942

Annealing effect and photovoltaic properties of nano-ZnS/textured p-Si heterojunction

NASA Astrophysics Data System (ADS)

Ji, Liang-Wen; Hsiao, Yu-Jen; Tang, I.-Tseng; Meen, Teen-Hang; Liu, Chien-Hung; Tsai, Jenn-Kai; Wu, Tien-Chuan; Wu, Yue-Sian

2013-11-01

The preparation and characterization of heterojunction solar cell with ZnS nanocrystals synthesized by chemical bath deposition method were studied in this work. The ZnS nanocrystals were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Lower reflectance spectra were found as the annealing temperature of ZnS film increased on the textured p-Si substrate. It was found that the power conversion efficiency (PCE) of the AZO/ZnS/textured p-Si heterojunction solar cell with an annealing temperature of 250°C was η = 3.66%.

Uranium migration in spark plasma sintered W/UO2 CERMETS

NASA Astrophysics Data System (ADS)

Tucker, Dennis S.; Wu, Yaqiao; Burns, Jatuporn

2018-03-01

W/UO2 CERMET samples were sintered in a Spark Plasma Sintering (SPS) furnace at various temperature under vacuum and pressure. High Resolution Transmission Electron Microscopy (HRTEM) with Energy Dispersive Spectroscopy (EDS) was performed on the samples to determine interface structures and uranium diffusion from the UO2 particles into the tungsten matrix. Local Electrode Atom Probe (LEAP) was also performed to determine stoichiometry of the UO2 particles. It was seen that uranium diffused approximately 10-15 nm into the tungsten matrix. This is explained in terms of production of oxygen vacancies and Fick's law of diffusion.

Profiling with the electron microscope.

NASA Technical Reports Server (NTRS)

Vedder, J. F.; Lem, H. Y.

1972-01-01

Discussion of a profiling technique using a scanning electron microscope for obtaining depth information on a single micrograph of a small specimen. A stationary electron beam is used to form a series of contamination spots in a line across the specimen. Micrographs obtained by this technique are useful as a means of projection and display where stereo viewers are not practical.

Atomic structure solution of the complex quasicrystal approximant Al77Rh15Ru8 from electron diffraction data.

PubMed

Samuha, Shmuel; Mugnaioli, Enrico; Grushko, Benjamin; Kolb, Ute; Meshi, Louisa

2014-12-01

The crystal structure of the novel Al77Rh15Ru8 phase (which is an approximant of decagonal quasicrystals) was determined using modern direct methods (MDM) applied to automated electron diffraction tomography (ADT) data. The Al77Rh15Ru8 E-phase is orthorhombic [Pbma, a = 23.40 (5), b = 16.20 (4) and c = 20.00 (5) Å] and has one of the most complicated intermetallic structures solved solely by electron diffraction methods. Its structural model consists of 78 unique atomic positions in the unit cell (19 Rh/Ru and 59 Al). Precession electron diffraction (PED) patterns and high-resolution electron microscopy (HRTEM) images were used for the validation of the proposed atomic model. The structure of the E-phase is described using hierarchical packing of polyhedra and a single type of tiling in the form of a parallelogram. Based on this description, the structure of the E-phase is compared with that of the ε6-phase formed in Al-Rh-Ru at close compositions.

Anti-bacteria activity of carbon nanotubes grown on trimetallic catalyst

NASA Astrophysics Data System (ADS)

Ibrahim, S. O.; Abdulkareem, A. S.; Isah, K. U.; Ahmadu, U.; Bankole, M. T.; Kariim, I.

2018-06-01

Trimetallic catalyst was prepared using wet impregnation method to produce carbon nanotubes (CNTs) through the method of catalytic chemical vapor deposition (CCVD). Characterization of the developed catalyst and CNTs were carried out using thermogravimetric analysis (TGA), x-ray diffraction (XRD), specific surface area Brunauer-Emmett-Teller (BET), Fourier-transform infrared spectroscopy (FTIR), high-resolution scanning electron microscopy (HRSEM)/energy dispersive x-ray spectroscopy (EDS) and high-resolution transmission electron microscopy (HRTEM)/selected area electron diffraction (SAED). The BET and TGA analysis indicated that the catalyst has a high surface area and is thermally stable. The FTIR of the developed catalyst shows notable functional group with presence of unbound water. The HRSEM of the catalyst revealed agglomerated, homogeneous and porous particles while the HRSEM/HRTEM of the produced CNTs gave the formation of long strand of multiwalled carbon nanotubes (MWCNTs), and homogeneous crystalline fringe like structure with irregular diameter. EDS revealed the dominance of carbon in the elemental composition. XRD/SAED patterns of the catalyst suggest high dispersion of the metallic particles in the catalyst mixture while that of the CNTs confirmed that the produced MWCNTs were highly graphitized and crystalline in nature with little structural defects. The anti-bacteria activity of the produced MWCNTs on Klebsiella pneumoneae, Escherichia coli, and Pseudomonas aeruginosa was also carried out. It was observed that the produced MWCNTs have an inhibitory property on bacteria; Escherichia coli and Klebsiella pneumoneae from zero day ( and ) through to twelfth day (Nil count) respectively. It has no effect on Pseudomonas aeruginosa with too numerous to count at zero-sixth day, but a breakdown in its growth at ninth-twelfth day (). This study implied that MWCNTs with varying diameter and well-ordered nano-structure can be produced from catalyst via CCVD method, and it can be recommended that the MWCNTs can be used to treat infected media contaminated with Klebsiella pneumoneae, Escherichia coli, and Pseudomonas aeruginosa.

In situ spectroscopic characterization of Ni 1-xZn x/ZnO catalysts and their selectivity for acetylene semihydrogenation in excess ethylene

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

Spanjers, Charles S.; Sim, Richard S.; Sturgis, Nicholas P.

2015-10-30

The structures of ZnO-supported Ni catalysts were explored with in situ X-ray absorption spectroscopy, temperature-programmed reduction, X-ray diffraction, high-resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy, and electron energy loss spectroscopy. Calcination of nickel nitrate on a nanoparticulate ZnO support at 450 °C results in the formation of Zn-doped NiO (ca. N₀̣̣₈₅ Zn₀̣̣₁₅O) nanoparticles with the rock salt crystal structure. Subsequent in situ reduction monitored by X-ray absorption near-edge structure (XANES) at the Ni K edge reveals a direct transformation of the Zn-doped NiO nanoparticles to a face-centered cubic alloy, Ni 1-xZn x, at ~400 °C with x increasingmore » with increasing temperature. Both in situ XANES and ex situ HRTEM provide evidence for intermetallic β₁-NiZn formation at ~550 °C. In comparison to a Ni/SiO₂ catalyst, Ni/ZnO necessitates a higher temperature for the reduction of Ni II to Ni⁰, which highlights the strong interaction between Ni and the ZnO support. The catalytic activity for acetylene removal from an ethylene feed stream is decreased by a factor of 20 on Ni/ZnO in comparison to Ni/SiO₂. The decrease in catalytic activity of Ni/ZnO is accompanied by a reduced absolute selectivity to ethylene. H–D exchange measurements demonstrate a reduced ability of Ni/ZnO to dissociate hydrogen in comparison to Ni/SiO₂.These results of the catalytic experiments suggest that the catalytic properties are controlled, in part, by the zinc oxide support and stress the importance of reporting absolute ethylene selectivity for the catalytic semihydrogenation of acetylene in excess ethylene.« less

Classification of Streptomyces Spore Surfaces into Five Groups

PubMed Central

Dietz, Alma; Mathews, John

1971-01-01

Streptomyces spores surfaces have been classified into five groups, smooth, warty, spiny, hairy, and rugose, by examination of carbon replicas of spores with the transmission electron microscope and by direct examination of spores with the scanning electron microscope. Images PMID:4928607

COLONIAL GROWTH OF MYCOPLASMA GALLISEPTICUM OBSERVED WITH THE ELECTRON MICROSCOPE

PubMed Central

Shifrine, Moshe; Pangborn, Jack; Adler, Henry E.

1962-01-01

Shifrine, Moshe (University of California, Davis), Jack Pangborn, and Henry E. Adler. Colonial growth of Mycoplasma gallisepticum observed with the electron microscope. J. Bacteriol. 83:187–192. 1962.—Mycoplasma gallisepticum strain S6 was grown on collodion film on solid medium. Samples were removed every few hours, fixed, washed, shadowed, and observed with the electron microscope. Three distinct forms of growth were observed: elementary cells (hexagonally shaped), platycytes, and exoblasts. A tentative mode of growth was postulated. The significance of the angular morphology to the relation between mycoplasmas and L-forms of bacteria is discussed. Images PMID:13911868

In situ electronic probing of semiconducting nanowires in an electron microscope.

PubMed

Fauske, V T; Erlbeck, M B; Huh, J; Kim, D C; Munshi, A M; Dheeraj, D L; Weman, H; Fimland, B O; Van Helvoort, A T J

2016-05-01

For the development of electronic nanoscale structures, feedback on its electronic properties is crucial, but challenging. Here, we present a comparison of various in situ methods for electronically probing single, p-doped GaAs nanowires inside a scanning electron microscope. The methods used include (i) directly probing individual as-grown nanowires with a sharp nano-manipulator, (ii) contacting dispersed nanowires with two metal contacts and (iii) contacting dispersed nanowires with four metal contacts. For the last two cases, we compare the results obtained using conventional ex situ litho-graphy contacting techniques and by in situ, direct-write electron beam induced deposition of a metal (Pt). The comparison shows that 2-probe measurements gives consistent results also with contacts made by electron beam induced deposition, but that for 4-probe, stray deposition can be a problem for shorter nanowires. This comparative study demonstrates that the preferred in situ method depends on the required throughput and reliability. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Transmission electron microscope studies of extraterrestrial materials

NASA Technical Reports Server (NTRS)

Keller, Lindsay P.

1995-01-01

Transmission Electron Microscopy, X-Ray spectrometry and electron-energy-loss spectroscopy are used to analyse carbon in interplanetary dust particles. Optical micrographs are shown depicting cross sections of the dust particles embedded in sulphur. Selected-area electron diffraction patterns are shown. Transmission Electron Microscope specimens of lunar soil were prepared using two methods: ion-milling and ultramicrotomy. A combination of high resolution TEM imaging and electron diffraction is used to characterize the opaque assemblages. The opaque assemblages analyzed in this study are dominated by ilmenite with lesser rutile and spinel exsolutions, and traces of Fe metal.

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

Salili, S.M.; School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran; Ataie, A., E-mail: aataie@ut.ac.ir

This research aimed to synthesize nanostructured strontium-doped lanthanum manganite, La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LSMO), with its Curie temperature (T{sub c}) adjusted to the therapeutic range, through a mechanothermal route. In order to investigate the effect of heat treatment temperature and duration on the resulting crystallite size, morphology, magnetic behavior and Curie temperature, the starting powder mixture was milled in a planetary ball mill before being subsequently heat treated at distinct temperatures for different time lengths. The composition, morphology, and magnetic behavior were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopymore » (HRTEM), selected area electron diffraction (SAED) and vibrating sample magnetometer (VSM). In addition, magnetic properties were further investigated using an alternating current (AC) susceptometer and thermo-magnetic analyzer. 20 h of milling produced a crystallite size reduction leading to a decrease in the heat treatment temperature of LSMO synthesis to 800 °C. Moreover, SEM analysis has shown the morphology of a strong agglomeration of fine nanoparticles. HRTEM showed clear lattice fringes of high crystallinity. The mean crystallite and particle size of 20-hour milled sample heat treated at 1100 °C for 10 h are relatively 69 and 100 nm, respectively. The VSM data at room temperature, indicated a paramagnetic behavior for samples heat treated at 800 °C. However, by increasing heat treatment temperature to 1100 °C, LSMO indicates a ferromagnetic behavior with well-adjusted Curie temperature of 320 K, suitable for hyperthermia applications. Also, reentrant spin glass (RSG) behavior has been found in heat treated samples. The particles are coated with (3-aminopropyl) triethoxysilane (APTES) for biocompatibility purposes; Fourier transform infrared spectroscopy (FTIR) and thermo-gravimetric analysis (TGA) are used for further confirmation of APTES coating. - Highlights: • La{sub 0.8}Sr{sub 0.2}MnO{sub 3} nanoparticles were synthesized via a mechanothermal route. • We report a significant reduction in the heat treatment temperature. • The Curie temperature was tuned within the therapeutic range. • The particles were coated with (3-aminopropyl) triethoxysilane for biocompatibility purposes.« less

Carbon-encapsulated cobalt nanoparticles: synthesis, properties, and magnetic particle hyperthermia efficiency

NASA Astrophysics Data System (ADS)

Kotoulas, A.; Dendrinou-Samara, C.; Sarafidis, C.; Kehagias, Th.; Arvanitidis, J.; Vourlias, G.; Angelakeris, M.; Kalogirou, Orestis

2017-12-01

A facile and low-cost method for structuring carbon-encapsulated cobalt nanoparticles (Co@C) is presented. Three samples were solvothermally prepared in one step at 220 °C and one in two steps at 200 °C. Three different polyols such as propylene glycol, triethylene glycol, and tetraethylene glycol were used as carbon sources, solvents, and reducing agents. The samples were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. Concerning the crystal structure of the particles, a mixture of hcp/ fcc Co phases was obtained in three of the samples, independently of the polyol used. The coexistence of cubic and hexagonal phases was revealed both from XRD and high-resolution TEM (HRTEM). The formation of the cubic fcc structure, despite the relatively low reaction temperature, is attributed to the role of the interface between carbon coating and metallic core. The presence of carbon coating was demonstrated by Raman spectrometry, exhibiting the characteristic D and G graphitic bands, and by HRTEM observations. All samples showed ferromagnetic behavior with saturation magnetization up to 158 emu/g and coercivity up to 206 Oe. From the magnetic particle hyperthermia measurements recorded at a frequency of 765 kHz, a maximum SLP value of 241 W/g was obtained.

Filling double-walled carbon nanotubes with WO3 and W nanowires via confined chemical reactions.

PubMed

Zhao, Keke; Wang, Zhiyong; Shi, Zujin; Gu, Zhennan; Jinj, Zhaoxia

2011-03-01

Carbon nanotubes filled with metals and semiconductors have been regarded as one of the most promising materials for nanodevices. Here, we demonstrate a simple and effective method to produce tungsten trioxide (WO3) and tungsten (W) nanowires with diameters of below 4 nm inside double-walled carbon nanotubes (DWCNTs). First, the precursors, i.e., phosphotungstic acid (HPW, H3PW12O40) molecules, are successfully introduced into DWCNTs. Subsequent decomposition and reduction lead to the formation of WO3 and W nanowires inside DWCNTs. The products were carefully characterized by high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. FTIR spectra provide a direct proof that the HPW molecules enter the DWCNTs as an ionic state, i.e., PW12O40(3-) and H+, instead of the molecular state. HRTEM analysis shows that the diameter of the WO3 nanowires inside DWCNTs is 1.1-2.4 nm with the average length of 16-18 nm, and that for W nanowires is 1.2-3.4 nm with the average length of 15-17 nm. Meanwhile, DWCNTs are doped by the encapsulated WO3 and W nanowires. Tangential band shift in Raman spectra revealed the charge transfer between the nanowires and carbon nanotubes.

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

Zehtab Yazdi, Alireza; Roberts, Edward P.L.; Sundararaj, Uttandaraman, E-mail: u.sundararaj@ucalgary.ca

Highlights: • MWCNTs synthesized and electrochemically oxidized to study the formation of GNR • HRTEM, Raman and XPS confirmed no successful unzipping occurred after oxidation • Electrochemical oxidation very unlikely facilitate formation of intercalated MWCNTs - Abstract: Multiwalled carbon nanotubes (MWCNTs) with different geometrical characteristics and chemical doping have been synthesized and electrochemically oxidized to study the possibility of unzipping, and creating graphene nanoribbon (GNR) nanostructures. Modified glassy carbon electrodes of the MWCNTs have been tested in an aqueous electrolyte via anodic scans in a wide range of potentials, followed by keeping at the maximum potential for different times. Themore » microstructural features, structural defects, and functional groups and their elements have been then studied using high resolution transmission electron microscopy (HRTEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS), respectively. All results have confirmed that no successful unzipping occurs in the MWCNTs after electrochemical oxidation, even for the nitrogen-doped MWCNTs (CN{sub x}-MWCNTs) with reactive nitrogen groups and defective bamboo structures. In contrast to the report by Shinde et al. (J. Am. Chem. Soc. 2011, 133, 4168–4171), it has been concluded that the electrochemical oxidation in aqueous electrolytes is very unlikely to facilitate sufficient incorporation of the intercalated molecules among the walls of the MWCNTs. These molecules are, however, responsible for unzipping of MWCNTs.« less

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

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

Ferric hydroxide supported gold subnano clusters or quantum dots: enhanced catalytic performance in chemoselective hydrogenation.

PubMed

Liu, Lequan; Qiao, Botao; Ma, Yubo; Zhang, Juan; Deng, Youquan

2008-05-21

An attempt to prepare ferric hydroxide supported Au subnano clusters via modified co-precipitation without any calcination was made. High resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) have been employed to study the structure and chemical states of these catalysts. No Au species could be observed in the HRTEM image nor from the XRD pattern, suggesting that the sizes of the Au species in and on the ferric hydroxide support were less than or around 1 nm. Chemoselective hydrogenation of aromatic nitro compounds and alpha,beta-unsaturated aldehydes was selected as a probe reaction to examine the catalytic properties of this catalyst. Under the same reaction conditions, such as 100 degrees C and 1 MPa H2 in the hydrogenation of aromatic nitro compounds, a 96-99% conversion (except for 4-nitrobenzonitrile) with 99% selectivity was obtained over the ferric hydroxide supported Au catalyst, and the TOF values were 2-6 times higher than that of the corresponding ferric oxide supported catalyst with 3-5 nm size Au particles. For further evaluation of this Au catalyst in the hydrogenation of citral and cinnamaldehyde, selectivity towards unsaturated alcohols was 2-20 times higher than that of the corresponding ferric oxide Au catalyst.

Isolation and characterisation of nanoparticles from tef and maize starch modified with stearic acid.

PubMed

Cuthbert, Wokadala O; Ray, Suprakas S; Emmambux, Naushad M

2017-07-15

Nanoparticles were isolated from tef and maize starch modified with added stearic acid after pasting at 90°C for 130min. This was followed by thermo-stable alpha-amylase hydrolysis of the paste. The resultant residues were then characterized using X-ray diffraction (XRD), differential scanning calorimetry (DSC), dynamic laser scattering particle size distribution (DLPSD), atomic force microscopy (AFM) and high-resolution transmission electron microscopy (HRTEM). XRD and DSC showed that the isolated residues consisted of amylose-lipid complexes. These complexes were type II with melting temperature above 104°C. DLPSD, AFM and HRTEM showed that the isolated tef and maize starch residues consisted of nanoparticles which became more distinct with increased hydrolysis time. The isolated tef and maize nanoparticles had distinct particles of about 3-10nm and 2.4-6.7nm, respectively and the yield was about 24-30%. The results demonstrated that distinct (physically separate) nanoparticles of less than 10nm can be isolated after formation during pasting of tef and maize starch with stearic acid. The production and isolation of the nanoparticles uses green chemistry principles and these nanoparticles can be used in food and non-food systems as nanofillers. Copyright © 2017 Elsevier Ltd. All rights reserved.

Role of the Short Distance Order in Glass Reactivity

PubMed Central

2018-01-01

In 2005, our group described for the first time the structural characterization at the atomic scale of bioactive glasses and the influence of the glasses’ nanostructure in their reactivity in simulated body fluids. In that study, two bioactive sol-gel glasses with composition 80%SiO2–20%CaO and 80%SiO2–17%CaO–3%P2O5 (in mol-%) were characterized by High-Resolution Transmission Electron Microscopy (HRTEM). Such characterization revealed unknown features of the glasses’ structure at the local scale that allowed the understanding of their different in vitro behaviors as a consequence of the presence or absence of P2O5. Since then, the nanostructure of numerous bioactive glasses, including melt-prepared, sol-gel derived, and mesoporous glasses, was investigated by HRTEM, Nuclear Magnetic Resonance (NMR) spectroscopy, Molecular Dynamics (MD) simulations, and other experimental techniques. These studies have shown that although glasses are amorphous solids, a certain type of short distance order, which greatly influences the in vitro and in vivo reactivity, is always present. This paper reviews the most significant advances in the understanding of bioactive glasses that took place in the last years as a result of the growing knowledge of the glasses’ nanostructure. PMID:29534481

Revisiting the relevance of using a constant voltage step to improve electrochemical performances of Li-rich lamellar oxides

NASA Astrophysics Data System (ADS)

Pradon, A.; Caldes, M. T.; Petit, P.-E.; La Fontaine, C.; Elkaim, E.; Tessier, C.; Ouvrard, G.; Dumont, E.

2018-03-01

A Li-rich lamellar oxide was cycled at high potential and the relevance of using a constant voltage step (CVS) at the end of the charge, needed for industrial application, was investigated by electrochemical performance, X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). Electrochemical studies at 4.7 and 4.5 V with and without CVS showed that capacity and voltage fading occurred mostly when cells operated at high potential. After cycling, 3D-type defects involving transition metals trapped in lithium layer were observed by HRTEM into the electrode bulk. These defects are responsible for the voltage fading. XRD microstrain parameter was used to evaluate defects rate in aged materials subjected to a CVS, showing more 3D-type defects when cycled at 4.7 V than at 4.5 V. The time spent at high potential at the end of the charge as well as the value of the upper potential limit, are both relevant parameters to voltage decay. The use of a CVS at the end of the charge needs at the same time, a reduced upper potential window in order to minimize 3D-type defects occurrence. Unfortunately, this approach is still not sufficient to prevent voltage fading.

Epitaxial CuInSe2 thin films grown by molecular beam epitaxy and migration enhanced epitaxy

NASA Astrophysics Data System (ADS)

Abderrafi, K.; Ribeiro-Andrade, R.; Nicoara, N.; Cerqueira, M. F.; Gonzalez Debs, M.; Limborço, H.; Salomé, P. M. P.; Gonzalez, J. C.; Briones, F.; Garcia, J. M.; Sadewasser, S.

2017-10-01

While CuInSe2 chalcopyrite materials are mainly used in their polycrystalline form to prepare thin film solar cells, epitaxial layers have been used for the characterization of defects. Typically, epitaxial layers are grown by metal-organic vapor phase epitaxy or molecular beam epitaxy (MBE). Here we present epitaxial layers grown by migration enhanced epitaxy (MEE) and compare the materials quality to MBE grown layers. CuInSe2 layers were grown on GaAs (0 0 1) substrates by co-evaporation of Cu, In, and Se using substrate temperatures of 450 °C, 530 °C, and 620 °C. The layers were characterized by high resolution X-ray diffraction (HR-XRD), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, and atomic force microscopy (AFM). HR-XRD and HR-TEM show a better crystalline quality of the MEE grown layers, and Raman scattering measurements confirm single phase CuInSe2. AFM shows the previously observed faceting of the (0 0 1) surface into {1 1 2} facets with trenches formed along the [1 1 0] direction. The surface of MEE-grown samples appears smoother compared to MBE-grown samples, a similar trend is observed with increasing growth temperature.

Accurate Virus Quantitation Using a Scanning Transmission Electron Microscopy (STEM) Detector in a Scanning Electron Microscope

DTIC Science & Technology

2017-06-29

Accurate Virus Quantitation Using a Scanning Transmission Electron Microscopy (STEM) Detector in a Scanning Electron Microscope Candace D Blancett1...L Norris2, Cynthia A Rossi4 , Pamela J Glass3, Mei G Sun1,* 1 Pathology Division, United States Army Medical Research Institute of Infectious...Diseases (USAMRIID), 1425 Porter Street, Fort Detrick, Maryland, 21702 2Biostatistics Division, United States Army Medical Research Institute of

Damage-free vibrational spectroscopy of biological materials in the electron microscope

PubMed Central

Rez, Peter; Aoki, Toshihiro; March, Katia; Gur, Dvir; Krivanek, Ondrej L.; Dellby, Niklas; Lovejoy, Tracy C.; Wolf, Sharon G.; Cohen, Hagai

2016-01-01

Vibrational spectroscopy in the electron microscope would be transformative in the study of biological samples, provided that radiation damage could be prevented. However, electron beams typically create high-energy excitations that severely accelerate sample degradation. Here this major difficulty is overcome using an ‘aloof' electron beam, positioned tens of nanometres away from the sample: high-energy excitations are suppressed, while vibrational modes of energies <1 eV can be ‘safely' investigated. To demonstrate the potential of aloof spectroscopy, we record electron energy loss spectra from biogenic guanine crystals in their native state, resolving their characteristic C–H, N–H and C=O vibrational signatures with no observable radiation damage. The technique opens up the possibility of non-damaging compositional analyses of organic functional groups, including non-crystalline biological materials, at a spatial resolution of ∼10 nm, simultaneously combined with imaging in the electron microscope. PMID:26961578

Damage-free vibrational spectroscopy of biological materials in the electron microscope.

PubMed

Rez, Peter; Aoki, Toshihiro; March, Katia; Gur, Dvir; Krivanek, Ondrej L; Dellby, Niklas; Lovejoy, Tracy C; Wolf, Sharon G; Cohen, Hagai

2016-03-10

Vibrational spectroscopy in the electron microscope would be transformative in the study of biological samples, provided that radiation damage could be prevented. However, electron beams typically create high-energy excitations that severely accelerate sample degradation. Here this major difficulty is overcome using an 'aloof' electron beam, positioned tens of nanometres away from the sample: high-energy excitations are suppressed, while vibrational modes of energies <1 eV can be 'safely' investigated. To demonstrate the potential of aloof spectroscopy, we record electron energy loss spectra from biogenic guanine crystals in their native state, resolving their characteristic C-H, N-H and C=O vibrational signatures with no observable radiation damage. The technique opens up the possibility of non-damaging compositional analyses of organic functional groups, including non-crystalline biological materials, at a spatial resolution of ∼10 nm, simultaneously combined with imaging in the electron microscope.

Damage-free vibrational spectroscopy of biological materials in the electron microscope

DOE PAGES

Rez, Peter; Aoki, Toshihiro; March, Katia; ...

2016-03-10

Vibrational spectroscopy in the electron microscope would be transformative in the study of biological samples, provided that radiation damage could be prevented. However, electron beams typically create high-energy excitations that severely accelerate sample degradation. Here this major difficulty is overcome using an ‘aloof’ electron beam, positioned tens of nanometres away from the sample: high-energy excitations are suppressed, while vibrational modes of energies o1 eV can be ‘safely’ investigated. To demonstrate the potential of aloof spectroscopy, we record electron energy loss spectra from biogenic guanine crystals in their native state, resolving their characteristic C–H, N–H and C=O vibrational signatures with nomore » observable radiation damage. Furthermore, the technique opens up the possibility of non-damaging compositional analyses of organic functional groups, including non-crystalline biological materials, at a spatial resolution of ~10nm, simultaneously combined with imaging in the electron microscope.« less

Damage-free vibrational spectroscopy of biological materials in the electron microscope

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

Rez, Peter; Aoki, Toshihiro; March, Katia

Vibrational spectroscopy in the electron microscope would be transformative in the study of biological samples, provided that radiation damage could be prevented. However, electron beams typically create high-energy excitations that severely accelerate sample degradation. Here this major difficulty is overcome using an ‘aloof’ electron beam, positioned tens of nanometres away from the sample: high-energy excitations are suppressed, while vibrational modes of energies o1 eV can be ‘safely’ investigated. To demonstrate the potential of aloof spectroscopy, we record electron energy loss spectra from biogenic guanine crystals in their native state, resolving their characteristic C–H, N–H and C=O vibrational signatures with nomore » observable radiation damage. Furthermore, the technique opens up the possibility of non-damaging compositional analyses of organic functional groups, including non-crystalline biological materials, at a spatial resolution of ~10nm, simultaneously combined with imaging in the electron microscope.« less

Structure and properties of electrodeposited nanocrystalline Ni and Ni-Fe alloy continuous foils

NASA Astrophysics Data System (ADS)

Giallonardo, Jason Derek

This research work presents the first comprehensive study on nanocrystalline materials produced in bulk quantities using a novel continuous electrodeposition process. A series of nanocrystalline Ni and Ni-Fe alloy continuous foils were produced and an intensive investigation into their structure and various properties was carried out. High-resolution transmission electron microscopy (HR-TEM) revealed the presence of local strain at high and low angle, and twin boundaries. The cause for these local strains was explained based on the interpretation of non-equilibrium grain boundary structures that result when conditions of compatibility are not satisfied. HR-TEM also revealed the presence of twin faults of the growth type, or "growth faults", which increased in density with the addition of Fe. This observation was found to be consistent with a corresponding increase in the growth fault probabilities determined quantitatively using X-ray diffraction (XRD) pattern analysis. Hardness and Young's modulus were measured by nanoindentation. Hardness followed the regular Hall-Petch behaviour down to a grain size of 20 nm after which an inverse trend was observed. Young's modulus was slightly reduced at grain sizes less than 20 nm and found to be affected by texture. Microstrain based on XRD line broadening was measured for these materials and found to increase primarily with a decrease in grain size or an increase in intercrystal defect density (i.e., grain boundaries and triple junctions). This microstrain is associated with the local strains observed at grain boundaries in the HR-TEM image analysis. A contribution to microstrain from the presence of growth faults in the nanocrystalline Ni-Fe alloys was also noted. The macrostresses for these materials were determined from strain measurements using a two-dimensional XRD technique. At grain sizes less than 20 nm, there was a sharp increase in compressive macrostresses which was also owed to the corresponding increase in intercrystal defects or interfaces in the solid.

U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

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

Prabhakaran, Ramprashad; Joshi, Vineet V.; Rhodes, Mark A.

2016-10-01

The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

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

Prabhakaran, Ramprashad; Joshi, Vineet V.; Rhodes, Mark A.

2016-03-30

The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

A Student-Built Scanning Tunneling Microscope

ERIC Educational Resources Information Center

Ekkens, Tom

2015-01-01

Many introductory and nanotechnology textbooks discuss the operation of various microscopes including atomic force (AFM), scanning tunneling (STM), and scanning electron microscopes (SEM). In a nanotechnology laboratory class, students frequently utilize microscopes to obtain data without a thought about the detailed operation of the tool itself.…

78 FR 2659 - Application(s) for Duty-Free Entry of Scientific Instruments

Federal Register 2010, 2011, 2012, 2013, 2014

2013-01-14

..., 2201 West End Ave., Nashville, TN 37235. Instrument: Electron Microscope. Manufacturer: FEI Company... St., West Lafayette, IN 47907-2024. Instrument: Electron Microscope. Manufacturer: FEI Company, the..., microorganisms, nanomaterials, and chemical compounds. Justification for Duty-Free Entry: There are no...

Tunneling rates in electron transport through double-barrier molecular junctions in a scanning tunneling microscope

PubMed Central

Nazin, G. V.; Wu, S. W.; Ho, W.

2005-01-01

The scanning tunneling microscope enables atomic-scale measurements of electron transport through individual molecules. Copper phthalocyanine and magnesium porphine molecules adsorbed on a thin oxide film grown on the NiAl(110) surface were probed. The single-molecule junctions contained two tunneling barriers, vacuum gap, and oxide film. Differential conductance spectroscopy shows that electron transport occurs via vibronic states of the molecules. The intensity of spectral peaks corresponding to the individual vibronic states depends on the relative electron tunneling rates through the two barriers of the junction, as found by varying the vacuum gap tunneling rate by changing the height of the scanning tunneling microscope tip above the molecule. A simple, sequential tunneling model explains the observed trends. PMID:15956189

Tunneling rates in electron transport through double-barrier molecular junctions in a scanning tunneling microscope.

PubMed

Nazin, G V; Wu, S W; Ho, W

2005-06-21

The scanning tunneling microscope enables atomic-scale measurements of electron transport through individual molecules. Copper phthalocyanine and magnesium porphine molecules adsorbed on a thin oxide film grown on the NiAl(110) surface were probed. The single-molecule junctions contained two tunneling barriers, vacuum gap, and oxide film. Differential conductance spectroscopy shows that electron transport occurs via vibronic states of the molecules. The intensity of spectral peaks corresponding to the individual vibronic states depends on the relative electron tunneling rates through the two barriers of the junction, as found by varying the vacuum gap tunneling rate by changing the height of the scanning tunneling microscope tip above the molecule. A simple, sequential tunneling model explains the observed trends.

Microcellular nanocomposite injection molding process

Treesearch

Mingjun Yuan; Lih-Sheng Turng; Rick Spindler; Daniel Caulfield; Chris Hunt

2003-01-01

This study aims to explore the processing benefits and property improvements of combining nanocomposites with microcellular injection molding. The molded parts produced based on the Design of Experiments (DOE) matrices were subjected to tensile testing, impact testing, and Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Dynamic Mechanical...

The microscopic world: A demonstration of electron microscopy for younger students

NASA Technical Reports Server (NTRS)

Horton, Linda L.

1992-01-01

The purpose is to excite students about the importance of scientific investigation and demonstrate why they should look at things in greater detail, extending beyond superficial examination. The topics covered include: microscopy, scanning electron microscopes, high magnification, and the scientific method.

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

Örnek, Ahmet, E-mail: ahmetornek@kafkas.edu.tr; Can, Mustafa; Yeşildağ, Ali

Nanostructured LiCo{sub 1−x}Mn{sub x}PO{sub 4}/C (x = 0 and 0.05) materials were successfully produced as superior quality cathodes by combined sol-gel and carbothermal reduction methods. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma (ICP), cyclic voltammetry (CV) and galvanostatic measurements were applied to determine the phase purity, morphology and electrochemical qualifications. HR-TEM analysis reveals that the thickness of the surface carbon layer of 5 to 10 nm range with the uniform distribution. LiCo{sub 0·95}Mn{sub 0·05}PO{sub 4}/C particles were betweenmore » 40 and 80 nm and the same material exhibits a higher and stable reversible capacity (140 mA h g{sup −1}) with the long voltage plateau (4.76 V). Substitution of Co{sup 2+} with Mn{sup 2+} in LiCoPO{sub 4}/C has an influence on the initial discharge capacity and excellent cycling behaviour. The obtained results have attributed that production dynamics in nano-synthesis, the coating process with proper carbon source and an effective doping represent three parameters to prepare favorable cathode materials. - Highlights: • Structural, morphological and electrochemical effects of Mn doped LiCo{sub 1−x}Mn{sub x}PO{sub 4}–C electrodes are investigated. • Cheap, effective and simple sol-gel assisted carbothermal reduction approach is used. • After 60th cycle, capacity retention is almost 92% for LiCo{sub 0·95}Mn{sub 0.05}PO{sub 4}–C electrode. • Mn-doped sample exhibits distinctive oxidation (4.76 V and 4.12 V) peaks.« less

Silver nanoparticles embedded mesoporous SiO2 nanosphere: an effective anticandidal agent against Candida albicans 077

NASA Astrophysics Data System (ADS)

Qasim, M.; Singh, Braj R.; Naqvi, A. H.; Paik, P.; Das, D.

2015-07-01

Candida albicans is a diploid fungus that causes common infections such as denture stomatitis, thrush, urinary tract infections, etc. Immunocompromised patients can become severely infected by this fungus. Development of an effective anticandidal agent against this pathogenic fungus, therefore, will be very useful for practical application. In this work, Ag-embedded mesoporous silica nanoparticles (mSiO2@AgNPs) have successfully been synthesized and their anticandidal activities against C. albicans have been studied. The mSiO2@AgNPs nanoparticles (d ˜ 400 nm) were designed using pre-synthesized Ag nanoparticles and tetraethyl orthosilicate (TEOS) as a precursor for SiO2 in the presence of cetyltrimethyl ammonium bromide (CTAB) as an easily removable soft template. A simple, cost-effective, and environmentally friendly approach has been adopted to synthesize silver (Ag) nanoparticles using silver nitrate and leaf extract of Azadirachta indica. The mesopores, with size-equivalent diameter of the micelles (d = 4-6 nm), were generated on the SiO2 surface by calcination after removal of the CTAB template. The morphology and surface structure of mSiO2@AgNPs were characterized through x-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), particle size analysis (PSA), atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM), Brunauer-Emmett-Teller (BET) and high-resolution transmission electron microscopy (HRTEM). The HRTEM micrograph reveals the well-ordered mesoporous structure of the SiO2 sphere. The antifungal activities of mSiO2@AgNPs on the C. albicans cell have been studied through microscopy and are seen to increase with increasing dose of mSiO2@AgNPs, suggesting mSiO2@AgNPs to be a potential antifungal agent for C. albicans 077.

An eco-benign synthesis of AgNPs using aqueous extract of Longan fruit peel: Antiproliferative response against human breast cancer cell line MCF-7, antioxidant and photocatalytic deprivation of methylene blue.

PubMed

Khan, Arif Ullah; Yuan, Qipeng; Khan, Zia Ul Haq; Ahmad, Aftab; Khan, Faheem Ullah; Tahir, Kamran; Shakeel, Muhammad; Ullah, Sadeeq

2018-05-07

Plants mediated synthesis of noble metal nanoparticles is encountered as a clean, environment friendly, lucrative and benign loom. The current study consists of clean and green synthesis of Silver nanoparticles (AgNPs). Phytoconstituents from Longan (Euphorbia longana Lam.) fruit peel were used to reduce Ag + into AgNPs. Different analytical techniques i.e. UV-vis Spectroscopy, X-ray diffraction spectroscopy (XRD), electron dispersive X-ray (EDX), High-resolution transmission electron microscopy (HRTEM) and Fourier transform infrared spectroscopy (FTIR) were used to analyze the synthesized AgNPs. AgNPs have localized surface plasmon resonance (LSPR) peak at 445 nm which is confirmed by UV-vis spectroscopy. HRTEM showed that the prepared AgNPs are spheroid in shape and well dispersed while XRD results showed that the AgNPs are face centered cubic crystalline. EDX confirmed the elemental composition of AgNPs. The antiproliferative response of AgNPs was assayed by an exhaustive MTT assay. AgNPs showed potent anticancer activity (88%) against breast cancer cells MCF-7. Moreover, the green produced AgNPs effectively scavenged 91% of the stable and harmful 2, 2-diphenyl-1-picrylhydrazyl (DPPH) free radical which confirms its' efficient antioxidant nature. AgNPs have profound photocatalytic degradation (99%) of methylene blue in a short period of time (7 min). The noteworthy biological and photocatalytic responses of the green and cleanly produced AgNPs are encountered to their well dispersion, petite volume and round shaped structure. Copyright © 2018 Elsevier B.V. All rights reserved.

Alignment control and atomically-scaled heteroepitaxial interface study of GaN nanowires.

PubMed

Liu, Qingyun; Liu, Baodan; Yang, Wenjin; Yang, Bing; Zhang, Xinglai; Labbé, Christophe; Portier, Xavier; An, Vladimir; Jiang, Xin

2017-04-20

Well-aligned GaN nanowires are promising candidates for building high-performance optoelectronic nanodevices. In this work, we demonstrate the epitaxial growth of well-aligned GaN nanowires on a [0001]-oriented sapphire substrate in a simple catalyst-assisted chemical vapor deposition process and their alignment control. It is found that the ammonia flux plays a key role in dominating the initial nucleation of GaN nanocrystals and their orientation. Typically, significant improvement of the GaN nanowire alignment can be realized at a low NH 3 flow rate. X-ray diffraction and cross-sectional scanning electron microscopy studies further verified the preferential orientation of GaN nanowires along the [0001] direction. The growth mechanism of GaN nanowire arrays is also well studied based on cross-sectional high-resolution transmission electron microscopy (HRTEM) characterization and it is observed that GaN nanowires have good epitaxial growth on the sapphire substrate following the crystallographic relationship between (0001) GaN ∥(0001) sapphire and (101[combining macron]0) GaN ∥(112[combining macron]0) sapphire . Most importantly, periodic misfit dislocations are also experimentally observed in the interface region due to the large lattice mismatch between the GaN nanowire and the sapphire substrate, and the formation of such dislocations will favor the release of structural strain in GaN nanowires. HRTEM analysis also finds the existence of "type I" stacking faults and voids inside the GaN nanowires. Optical investigation suggests that the GaN nanowire arrays have strong emission in the UV range, suggesting their crystalline nature and chemical purity. The achievement of aligned GaN nanowires will further promote the wide applications of GaN nanostructures toward diverse high-performance optoelectronic nanodevices including nano-LEDs, photovoltaic cells, photodetectors etc.

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.

Effect of chitosan coating on the structural and magnetic properties of MnFe2O4 and Mn0.5Co0.5Fe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Mdlalose, W. B.; Mokhosi, S. R.; Dlamini, S.; Moyo, T.; Singh, M.

2018-05-01

We report the influence of polymer coatings on structural and magnetic properties of MnFe2O4 and Mn0.5Co0.5Fe2O4 nanoferrites synthesized by glycol thermal technique and then coated with chitosan viz. CHI-MnFe2O4 and CHI-Mn0.5Co0.5Fe2O4. The compounds were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), high-resolution scanning electron microscopy (HRSEM), Mössbauer spectroscopy and magnetization measurements. The powder XRD patterns of naked nanoferrites confirmed single-phase spinel cubic structure with an average crystallite size of 13 nm, while the coated samples exhibited an average particle size of 15 nm. We observed a reduction in lattice parameters with coating. HRTEM results correlated well with XRD results. 57Fe Mössbauer spectra showed ordered magnetic spin states in both nanoferrites. This study shows that coatings have significant effects on the structural and magnetic properties of Mn-nanoferrites. Magnetization studies performed at room temperature in fields up to 14 kOe revealed the superparamagnetic nature of both naked and coated nanoparticles with spontaneous magnetizations at room temperature of 49.2 emu/g for MnFe2O4, 23.6 emu/g for coated CHI-MnFe2O4 nanoparticles, 63.2 emu/g for Mn0.5Co0.5Fe2O4 and 33.2 emu/g for coated CHI-Mn0.5Co0.5Fe2O4 nanoparticles. We observed reduction in coercive fields due to coating. Overall, chitosan-coated manganese and manganese-cobalt nanoferrites present as suitable candidates for biomedical applications owing to physicochemical, and magnetic properties exhibited.

Clay mineralogy and its palaeoclimatic significance in the Luochuan loess-palaeosols over ˜1.3 Ma, Shaanxi, northwestern China

NASA Astrophysics Data System (ADS)

Won, Changdok; Hong, Hanlie; Cheng, Feng; Fang, Qian; Wang, Chaowen; Zhao, Lulu; Churchman, Gordon Jock

2018-03-01

To understand climate changes recorded in the Luochuan loess-palaeosols, Shaanxi province, northwestern China, clay mineralogy was studied using X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), and scanning electron microscopy (SEM) methods. XRD results show that clay mineral compositions in the Luochuan loess-palaeosols are dominantly illite, with minor chlorite, kaolinite, smectite, and illite-smectite mixed-layer clays (I/S). Illite is the most abundant species in the sediments, with a content of 61%-83%. The content of chlorite ranges from 5%-22%, and the content of kaolinite ranges from 5%-19%. Smectite (or I/S) occurs discontinuously along the loess profile, with a content of 0-8%. The Kübler index of illite (IC) ranges from 0.255°-0.491°, and the illite chemical index (ICI) ranges from 0.294-0.394. The CIA values of the loesspalaeosols are 61.9-69.02, and the R3+/(R3+ + R2+ + M+) values are 0.508-0.589. HRTEM observations show that transformation of illite to illite-smectite has occurred in both the loess and palaeosol, suggesting that the Luochuan loess-palaeosols have experienced a certain degree of chemical weathering. The Luochuan loess-palaeosols have the same clay mineral assemblage along the profile. However, the relative contents of clay mineral species, CIA, ICI, and IC values fluctuate frequently along the profile, and all these parameters display a similar trend. Moreover, climate changes suggested by the clay index are consistent with variations in the deep-sea δ18O records and the magnetic susceptibility value, and thus, climate changes in the Luochuan region have been controlled by global climate change.

Melamine dependent fluorescence of glutathione protected gold nanoclusters and ratiometric quantification of melamine in commercial cow milk and infant formula

NASA Astrophysics Data System (ADS)

Kalaiyarasan, Gopi; K, Anusuya; Joseph, James

2017-10-01

Companies processing the milk for the further production of powdered infant formulation normally check the protein level through a test measuring nitrogen content. The addition of melamine which is a nitrogen-rich organic chemical in milk increases the nitrogen content and therefore enhances its apparent protein content. However, the melamine causes kidney failure and death owing to the formation of kidney stone. Thus the determination of melamine in humans and milk products have gained great significance in recent years. The gold nanoclusters (AuNCs) have attracting features due to its unique electronic and optical properties like fluorescence nature. Therefore one can use AuNCs in the field of biosensor, bio-imaging, nanobiotechnology, drug delivery, diagnosis etc. We report, a new ratiometric nanosensor established for the selective and sensitive detection of melamine based optical sensing using glutathione stabilized AuNCs. The AuNCs were characterized by high-resolution transmission electron microscopy (HR-TEM), UV-visible and Photoluminescence (PL) spectroscopic techniques. In the presence of melamine, the PL intensity at 430 nm increases owing to the (turn-on) enhancement in fluorescence, whereas PL intensity at 610 nm decreases due to the melamine-induced aggregation and subsequent aggregation-enhanced emission quenching. The observed changes were ascribed to the hydrogen bonding interaction between melamine and AuNCs, which led to the aggregation of the nanoclusters. This was confirmed by dynamic light scattering and HR-TEM measurements. The present probe showed an extreme selectivity towards the determination of 28.2 μM melamine in the presence of 100-fold excess of common interfering molecules such as Alanine, Glycine, Glucose, Cystine etc. The proposed method was successfully applied to determine melamine in cow milk.

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.

Nucleotide-Specific Contrast for DNA Sequencing by Electron Spectroscopy

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

Mankos, Marian; Persson, Henrik H. J.; N’Diaye, Alpha T.

DNA sequencing by imaging in an electron microscope is an approach that holds promise to deliver long reads with low error rates and without the need for amplification. Earlier work using transmission electron microscopes, which use high electron energies on the order of 100 keV, has shown that low contrast and radiation damage necessitates the use of heavy atom labeling of individual nucleotides, which increases the read error rates. Other prior work using scattering electrons with much lower energy has shown to suppress beam damage on DNA. Here we explore possibilities to increase contrast by employing two methods, X-ray photoelectronmore » and Auger electron spectroscopy. Using bulk DNA samples with monomers of each base, both methods are shown to provide contrast mechanisms that can distinguish individual nucleotides without labels. In conclusion, both spectroscopic techniques can be readily implemented in a low energy electron microscope, which may enable label-free DNA sequencing by direct imaging.« less

Nucleotide-Specific Contrast for DNA Sequencing by Electron Spectroscopy

DOE PAGES

Mankos, Marian; Persson, Henrik H. J.; N’Diaye, Alpha T.; ...

2016-05-05

DNA sequencing by imaging in an electron microscope is an approach that holds promise to deliver long reads with low error rates and without the need for amplification. Earlier work using transmission electron microscopes, which use high electron energies on the order of 100 keV, has shown that low contrast and radiation damage necessitates the use of heavy atom labeling of individual nucleotides, which increases the read error rates. Other prior work using scattering electrons with much lower energy has shown to suppress beam damage on DNA. Here we explore possibilities to increase contrast by employing two methods, X-ray photoelectronmore » and Auger electron spectroscopy. Using bulk DNA samples with monomers of each base, both methods are shown to provide contrast mechanisms that can distinguish individual nucleotides without labels. In conclusion, both spectroscopic techniques can be readily implemented in a low energy electron microscope, which may enable label-free DNA sequencing by direct imaging.« less

A next generation positron microscope and a survey of candidate samples for future positron studies

NASA Astrophysics Data System (ADS)

Dull, Terry Lou

A positron microscope has been constructed and is nearing the conclusion of its assembly and testing. The instrument is designed to perform positron and electron microscopy in both scanning and magnifying modes. In scanning mode, a small beam of particles is rastered across the target and the amplitude of a positron or electron related signal is recorded as a function of position. For positrons this signal may come from Doppler Broadening Spectroscopy, Reemitted Positron Spectroscopy or Positron Annihilation Lifetime Spectroscopy. For electrons this signal may come from the number of secondary electrons or Auger Electron Spectroscopy. In magnifying mode an incident beam of particles is directed onto the target and emitted particles, either secondary electrons or reemitted positrons, are magnified to form an image. As a positron microscope the instrument will primarily operate in magnifying mode, as a positron reemission microscope. As an electron microscope the instrument will be able to operate in both magnifying and scanning modes. Depth-profiled Doppler Broadening Spectroscopy studies using a non-microscopic low-energy positron beam have also been performed on a series of samples to ascertain the applicability of positron spectroscopies and/or microscopy to their study. All samples have sub-micron film and/or feature size and thus are only susceptible to positron study with low-energy beams. Several stoichiometries and crystallinities of chalcogenide thin films (which can be optically reversibly switched between crystalline states) were studied and a correlation was found to exist between the amorphous/FCC S-parameter difference and the amorphous/FCC switching time. Amorphous silicon films were studied in an attempt to observe the well-established Staebler-Wronski effect as well as the more controversial photodilatation effect. However, DBS was not able to detect either effect. The passive oxide films on titanium and aluminum were studied in an attempt to verify the Point Defect Model, a detailed, but as yet microscopically unconfirmed, theory of the corrosive breakdown of passive films. DBS results supportive of the PDM were observed. Graphitic carbon fibers were also studied and DBS indicated the presence of a 200 nm thick outer fiber skin possibly characterized by a high degree of graphitic crystallite alignment.

Microscopic Electron Variations Measured Simultaneously By The Cluster Spacecraft

NASA Astrophysics Data System (ADS)

Buckley, A. M.; Carozzi, T. D.; Gough, M. P.; Beloff, N.

Data is used from the Particle Correlator experiments running on each of the four Cluster spacecraft so as to determine common microscopic behaviour in the elec- tron population observed over the macroscopic Cluster separations. The Cluster par- ticle correlator experiments operate by forming on board Auto Correlation Functions (ACFs) generated from short time series of electron counts obtained, as a function of electron energy, from the PEACE HEEA sensor. The information on the microscopic variation of the electron flux covers the frequency range DC up to 41 kHz (encom- passing typical electron plasma frequencies and electron gyro frequencies and their harmonics), the electron energy range is that covered by the PEACE HEEA sensor (within the range 1 eV to 26 keV). Results are presented of coherent electron struc- tures observed simultaneously by the four spacecraft in the differing plasma interac- tion regions and boundaries encountered by Cluster. As an aid to understanding the plasma interactions, use is made of numerical simulations which model both the un- derlying statistical properties of the electrons and also the manner in which particle correlator experiments operate.

Interference experiment with asymmetric double slit by using 1.2-MV field emission transmission electron microscope.

PubMed

Harada, Ken; Akashi, Tetsuya; Niitsu, Kodai; Shimada, Keiko; Ono, Yoshimasa A; Shindo, Daisuke; Shinada, Hiroyuki; Mori, Shigeo

2018-01-17

Advanced electron microscopy technologies have made it possible to perform precise double-slit interference experiments. We used a 1.2-MV field emission electron microscope providing coherent electron waves and a direct detection camera system enabling single-electron detections at a sub-second exposure time. We developed a method to perform the interference experiment by using an asymmetric double-slit fabricated by a focused ion beam instrument and by operating the microscope under a "pre-Fraunhofer" condition, different from the Fraunhofer condition of conventional double-slit experiments. Here, pre-Fraunhofer condition means that each single-slit observation was performed under the Fraunhofer condition, while the double-slit observations were performed under the Fresnel condition. The interference experiments with each single slit and with the asymmetric double slit were carried out under two different electron dose conditions: high-dose for calculation of electron probability distribution and low-dose for each single electron distribution. Finally, we exemplified the distribution of single electrons by color-coding according to the above three types of experiments as a composite image.

Pre-microscope tunnelling — Inspiration or constraint?

NASA Astrophysics Data System (ADS)

Walmsley, D. G.

1987-03-01

Before the microscope burst upon the scene, tunnelling had established for itself a substantial niche in the repertoire of the solid state physicist. Over a period of 20 years it has contributed importantly to our understanding of many systems. It elucidated the superconducting state, first by a direct display of the energy gap then by providing detailed information on the phonon spectra and electron-phonon coupling strength in junction electrodes. Its use as a phonon spectrometer was subsequently extended to semiconductors and to the oxides of insulating barriers. Eventually the vibrational spectra of monolayer organic and inorganic adsorbates became amenable with rich scientific rewards. In a few cases electronic transitions have been observed. Plasmon excitation by tunnelling electrons led to insights on the electron loss function in metals at visible frequencies and provided along the way an intriguing light emitting device. With the advent of the microscope it is now appropriate to enquire how much of this experience can profitably be carried over to the new environment. Are we constrained just to repeat the experiments in a new configuration? Happily no. The microscope offers us topographical and spectroscopic information of a new order. One might next ask how great is the contact between the two disciplines? We explore this question and seek to establish where the pre-microscope experience can be helpful in inspiring our use of this marvellous new facility that we know as the scanning tunnelling microscope.

Electronic structure and microscopic model of V(2)GeO(4)F(2)-a quantum spin system with S = 1.

PubMed

Rahaman, Badiur; Saha-Dasgupta, T

2007-07-25

We present first-principles density functional calculations and downfolding studies of the electronic and magnetic properties of the oxide-fluoride quantum spin system V(2)GeO(4)F(2). We discuss explicitly the nature of the exchange paths and provide quantitative estimates of magnetic exchange couplings. A microscopic modelling based on analysis of the electronic structure of this systems puts it in the interesting class of weakly coupled alternating chain S = 1 systems. Based on the microscopic model, we make inferrences about its spin excitation spectra, which needs to be tested by rigorous experimental study.

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

Guetaz, Laure; Lopez-Haro, M.; Escribano, S.

Investigation of membrane/electrode assembly (MEA) microstructure has become an essential step to optimize the MEA components and manufacturing processes or to study the MEA degradation. For these investigations, transmission electron microscopy (TEM) is a tool of choice as it provides direct imaging of the different components. TEM is then widely used for analyzing the catalyst nanoparticles and their carbon support. However, the ionomer inside the electrode is more difficult to be imaged. The difficulties come from the fact that the ionomer forms an ultrathin layer surrounding the carbon particles and in addition, these two components, having similar density, present nomore » difference in contrast. In this paper, we show how the recent progresses in TEM techniques as spherical aberration (Cs) corrected HRTEM, electron tomography and X-EDS elemental mapping provide new possibilities for imaging this ionomer network and consequently to study its degradation.« less

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Ultrasound with low intensity assisted the synthesis of nanocrystalline TiO2 without calcination.

PubMed

Ghows, Narjes; Entezari, Mohamad H

2010-06-01

A novel method has been developed for the preparation of nano-sized TiO(2) with anatase phase. Nanoparticles with diameter about 6 nm were prepared at a relatively low temperature (75 degrees C) and short time. The synthesis was carried out by the hydrolysis of titanium tetra-isopropoxide (TTIP) in the presence of water, ethanol, and dispersant under ultrasonic irradiation (500 kHz) at low intensity. The results show that variables such as water/ethanol ratio, irradiation time, and temperature have a great influence on the particle size and crystalline phases of TiO(2) nanoparticles. Characterization of the product was carried out by different techniques such as powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and UV-vis spectroscopy. (c) 2010 Elsevier B.V. All rights reserved.

Hybrid magnetic materials formed by ferritin intercalated into a layered double hydroxide

NASA Astrophysics Data System (ADS)

Clemente-León, Miguel; Coronado, Eugenio; Primo, Vicent; Ribera, Antonio; Soriano-Portillo, Alejandra

2008-12-01

A hybrid magnetic material formed by ferritin intercalated into a layered double hydroxide (LDH) of Mg and Al (Mg/Al molar ratio 2) is prepared and characterized through powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared (FT-IR) spectroscopy, electron probe microanalysis (EPMA) and high resolution transmission electron microscopy (HRTEM). One observes an enhancement in the thermal stability of the ferritin molecules when they are inserted in the layered material. Magnetic measurements of the hybrid material exhibit the typical superparamagnetic behaviour of the ferritin molecule. On the other hand, the intercalation of ferritin into the LDH guarantees a homogeneous dispersion of the ferritin molecules, which do not aggregate even after calcination of the sample. This feature allows obtaining well-dispersed magnetic metal oxide nanoparticles upon calcination of the hybrid material.

The adsorption of L-phenylalanine on oxidized single-walled carbon nanotubes.

PubMed

Piao, Lingyu; Liu, Quanrun; Li, Yongdan; Wang, Chen

2009-02-01

A simple and green approach was proceeded to obtain a stable single-walled carbon nanotubes (SWNTs)/L-phenylalanine (Phe) solution. The oxidized SWNTs (OSWNT) were used in this work. The scanning electron microscopy (SEM), High-resolution transmission electron microscopy (HRTEM), Raman spectrometer, Fourier transform-infrared resonance (FT-IR), Ultraviolet-visible (UV-vis) spectroscopy, Thermogravimetric analysis (TGA) and High performance liquid chromatography (HPLC) were joined together to investigate the interaction between OSWNT and Phe. The OSWNT became soluble in the water and formed a stable solution since the Phe was adsorbed. The absorbed amount of Phe on the OSWNT is around 33 wt%. Adsorption of the Phe was mainly carried out on the OSWNT with smaller diameters. The Phe molecules were absorbed on the OSWNT by conjunct interaction of the pi-pi stacking, hydrogen bond and part of covalent bond.

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

PubMed

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

2018-05-15

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

Localized surface plasmon and exciton interaction in silver-coated cadmium sulphide quantum dots

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

Ghosh, P.; Rustagi, K. C.; Vasa, P.

2015-05-15

Localized surface plasmon and exciton coupling has been investigated on colloidal solutions of silver-coated CdS nanoparticles (NPs), synthesized by gamma irradiation. Two broad photoluminescence (PL) bands (blue/red) corresponding to band to band and defect state transitions have been observed for the bare and coated samples. In case of bare CdS NPs, the intensity of the red PL peak is about ten times higher than the blue PL peak intensity. However, on coating the CdS NPs with silver, the peak intensity of the blue PL band gets enhanced and becomes equal to that of the red PL band. High-resolution transmission electronmore » microscopic (HRTEM) images adequately demonstrate size distribution of these metal/semiconductor nanocomposites. UV-Vis absorption studies show quantum confinement effect in these semiconductor quantum dot (SQD) systems. Absorption spectrum of silver-coated SQDs shows signature of surface plasmon-exciton coupling which has been theoretically verified.« less

Miniature self-contained vacuum compatible electronic imaging microscope

DOEpatents

Naulleau, Patrick P.; Batson, Phillip J.; Denham, Paul E.; Jones, Michael S.

2001-01-01

A vacuum compatible CCD-based microscopic camera with an integrated illuminator. The camera can provide video or still feed from the microscope contained within a vacuum chamber. Activation of an optional integral illuminator can provide light to illuminate the microscope subject. The microscope camera comprises a housing with a objective port, modified objective, beam-splitter, CCD camera, and LED illuminator.

Electron Source Brightness and Illumination Semi-Angle Distribution Measurement in a Transmission Electron Microscope.

PubMed

Börrnert, Felix; Renner, Julian; Kaiser, Ute

2018-05-21

The electron source brightness is an important parameter in an electron microscope. Reliable and easy brightness measurement routes are not easily found. A determination method for the illumination semi-angle distribution in transmission electron microscopy is even less well documented. Herein, we report a simple measurement route for both entities and demonstrate it on a state-of-the-art instrument. The reduced axial brightness of the FEI X-FEG with a monochromator was determined to be larger than 108 A/(m2 sr V).

An ultrafast electron microscope gun driven by two-photon photoemission from a nanotip cathode

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

Bormann, Reiner; Strauch, Stefanie; Schäfer, Sascha, E-mail: schaefer@ph4.physik.uni-goettingen.de

We experimentally and numerically investigate the performance of an advanced ultrafast electron source, based on two-photon photoemission from a tungsten needle cathode incorporated in an electron microscope gun geometry. Emission properties are characterized as a function of the electrostatic gun settings, and operating conditions leading to laser-triggered electron beams of very low emittance (below 20 nm mrad) are identified. The results highlight the excellent suitability of optically driven nano-cathodes for the further development of ultrafast transmission electron microscopy.

A scanning electron microscopy study of the macro-crystalline structure of 2-(2,4-dinitrobenzyl) pyridine

NASA Technical Reports Server (NTRS)

Ware, Jacqueline; Hammond, Ernest C., Jr.

1989-01-01

The compound, 2-(2,4-dinitrobenzyl) pyridine, was synthesized in the laboratory; an introductory level electron microscopy study of the macro-crystalline structure was conducted using the scanning electron microscope (SEM). The structure of these crystals was compared with the macrostructure of the crystal of 2-(2,4-dinitrobenzyl) pyridinium bromide, the hydrobromic salt of the compound which was also synthesized in the laboratory. A scanning electron microscopy crystal study was combined with a study of the principle of the electron microscope.

Electron beam assisted field evaporation of insulating nanowires/tubes

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

Blanchard, N. P., E-mail: nicholas.blanchard@univ-lyon1.fr; Niguès, A.; Choueib, M.

2015-05-11

We demonstrate field evaporation of insulating materials, specifically BN nanotubes and undoped Si nanowires, assisted by a convergent electron beam. Electron irradiation leads to positive charging at the nano-object's apex and to an important increase of the local electric field thus inducing field evaporation. Experiments performed both in a transmission electron microscope and in a scanning electron microscope are presented. This technique permits the selective evaporation of individual nanowires in complex materials. Electron assisted field evaporation could be an interesting alternative or complementary to laser induced field desorption used in atom probe tomography of insulating materials.

The contributions of Otto Scherzer (1909-1982) to the development of the electron microscope.

PubMed

Marko, Michael; Rose, Harald

2010-08-01

Otto Scherzer was one of the pioneers of theoretical electron optics. He was coauthor of the first comprehensive book on electron optics and was the first to understand that round electron lenses could not be combined to correct aberrations, as is the case in light optics. He subsequently was the first to describe several alternative means to correct spherical and chromatic aberration of electron lenses. These ideas were put into practice by his laboratory and students at Darmstadt and their successors, leading to the fully corrected electron microscopes now in operation.

Application of automatic image analysis for morphometric studies of peroxisomes stained cytochemically for catalase. II. Light-microscopic application.

PubMed

Beier, K; Fahimi, H D

1987-01-01

The feasibility of the application of a television-based image analyzer, the Texture Analysis System (TAS, Leitz Wetzlar, FRG) in conjunction with a light microscope for morphometric studies of hepatic peroxisomes has been investigated. Rat liver peroxisomes were stained with the alkaline-DAB method for localization of catalase and semithin (0.25 and 1 micron) sections of plastic-embedded material were examined under an oil immersion objective. The TAS detected the peroxisomal profiles selectively and determined their morphometric parameters automatically. The same parameters were obtained also by morphometric analysis of electron micrographs from the same material. The volume density of peroxisomes determined by TAS in semithin sections of normal liver, after correction for section thickness, is quite close to the corresponding value obtained by morphometry of electron micrographs. The difference is approximately 20%. In animals treated with the hypolipidemic drug bezafibrate, which causes proliferation of peroxisomes, TAS detected readily the increase in volume density of peroxisomes in semithin sections. In comparison with electron microscopy, however, the light-microscopic approach seems to underestimate the proliferation. The lower resolution of the light microscope and overlapping of neighbouring particles in relatively thick sections used for light-microscopic analysis may account for the differences. The present study has demonstrated the usefulness of automatic image analysis in conjunction with selective cytochemical staining of peroxisomes for morphometry of this organelle in rat liver. The light-microscopic approach is not only faster but is also extremely economical by obviating the use of an electron microscope.

Electron beam induced deposition of silicon nanostructures from a liquid phase precursor.

PubMed

Liu, Yin; Chen, Xin; Noh, Kyong Wook; Dillon, Shen J

2012-09-28

This work demonstrates electron beam induced deposition of silicon from a SiCl(4) liquid precursor in a transmission electron microscope and a scanning electron microscope. Silicon nanodots of tunable size are reproducibly grown in controlled geometries. The volume of these features increases linearly with deposition time. The results indicate that secondary electrons generated at the substrate surface serve as the primary source of silicon reduction. However, at high current densities the influence of the primary electrons is observed to retard growth. The results demonstrate a new approach to fabricating silicon nanostructures and provide fundamental insights into the mechanism for liquid phase electron beam induced deposition.

Electron beam induced deposition of silicon nanostructures from a liquid phase precursor

NASA Astrophysics Data System (ADS)

Liu, Yin; Chen, Xin; Noh, Kyong Wook; Dillon, Shen J.

2012-09-01

This work demonstrates electron beam induced deposition of silicon from a SiCl4 liquid precursor in a transmission electron microscope and a scanning electron microscope. Silicon nanodots of tunable size are reproducibly grown in controlled geometries. The volume of these features increases linearly with deposition time. The results indicate that secondary electrons generated at the substrate surface serve as the primary source of silicon reduction. However, at high current densities the influence of the primary electrons is observed to retard growth. The results demonstrate a new approach to fabricating silicon nanostructures and provide fundamental insights into the mechanism for liquid phase electron beam induced deposition.

Transmission Electron Microscope Measures Lattice Parameters

NASA Technical Reports Server (NTRS)

Pike, William T.

1996-01-01

Convergent-beam microdiffraction (CBM) in thermionic-emission transmission electron microscope (TEM) is technique for measuring lattice parameters of nanometer-sized specimens of crystalline materials. Lattice parameters determined by use of CBM accurate to within few parts in thousand. Technique developed especially for use in quantifying lattice parameters, and thus strains, in epitaxial mismatched-crystal-lattice multilayer structures in multiple-quantum-well and other advanced semiconductor electronic devices. Ability to determine strains in indivdual layers contributes to understanding of novel electronic behaviors of devices.

Ponderomotive phase plate for transmission electron microscopes

DOEpatents

Reed, Bryan W [Livermore, CA

2012-07-10

A ponderomotive phase plate system and method for controllably producing highly tunable phase contrast transfer functions in a transmission electron microscope (TEM) for high resolution and biological phase contrast imaging. The system and method includes a laser source and a beam transport system to produce a focused laser crossover as a phase plate, so that a ponderomotive potential of the focused laser crossover produces a scattering-angle-dependent phase shift in the electrons of the post-sample electron beam corresponding to a desired phase contrast transfer function.

In situ flat embedding of monolayers and cell relocation in the acrylic resin LR white for comparative light and electron microscopy studies.

PubMed

Steiner, M; Schöfer, C; Mosgoeller, W

1994-12-01

A simple and reliable method has been developed for the in situ LR White embedding of cell monolayers grown on glass cover-slips. Combined with cytochemical or immunological procedures, this technique allows light and/or electron microscopy investigations of a large number of cells in the same horizontal plane within a relatively short period of time. It can be applied to cells grown on microgrid finder cover-slips which allows a distinct site of even an individual cell of a monolayer to be studied at first at the light microscope level and subsequently at the electron microscope level. Hence, it is also suitable for controlling manipulation of single cells, followed by their serial sectioning after relocation in the electron microscope.

Diffusion and phase transformation behavior in poly-synthetically-twinned (PST) titanium-aluminum/titanium diffusion couple

NASA Astrophysics Data System (ADS)

Pan, Ling

Motivated by the great potential applications of gamma titanium aluminide based alloys and the important effect of diffusion on the properties of gamma-TiAl/alpha2-Ti3Al two-phase lamellar structure, we conduct this thesis research to explore the microstructural evolution and interdiffusion behavior, and their correlations in multi-phase solid state diffusion couples made up of pure titanium and polysynthetically-twinned (PST) Ti-49.3 at.% Al "single" crystal, in the temperature range of 973--1173 K. The diffusion couples are prepared by high vacuum hot-pressing, with the diffusion direction parallel to the lamellar planes. Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) are employed to observe the microstructure at various interfaces/interphases. A reaction zone (RZ) of polycrystalline alpha 2-Ti3Al phase forms along the PST Ti-Al/Ti bonding interface having a wavy interface with the PST crystal and exhibits deeper penetration in alpha2 lamellae, consisting of many fine alpha2 and secondary gamma laths, than in primary gamma lamellae. Direct measurement of the RZ thickness on SEM back-scattered electron images reveals a parabolic growth of the RZ, indicating a macroscopically diffusion-controlled growth. Concentration profiles from Ti, through the RZ, into the alpha2 lamellae of the PST crystal are measured by quantitative energy-dispersive x-ray spectroscopy (EDS) in a scanning transmission electron microscope (STEM). A plateau of composition adjacent to the RZ/(mixed alpha2 lath in PST) interface forms in the deeply penetrated RZ grains, implying a diffusion barrier crossing the interface and some extent of interface control in the RZ grain growth. The interdiffusion coefficient is evaluated both independent of composition and as a function of composition. No significant concentration dependence of the interdiffusion coefficients is observed using Boltzmann-Matano analysis. The temperature dependence of the interdiffusion coefficients obeys the Arrhenius relationship with a pre-exponential factor of D 0 = (7.56 +/- 7.14) x 10-5 m2/s and an activation enthalpy of Q = 255.6+8.9-8.3 kJ/mol = (2.65 +/- 0.09) eV/atom. The initial nucleation stage of the RZ grains plays an important role in the later microstructural evolution as does the local mass balance. The interfacial energy and the strain energy in the deeply penetrated RZ grains are possible reasons for the plateau.

Mars Life? - Microscopic Tubular Structures

NASA Image and Video Library

1996-08-09

This electron microscope image shows extremely tiny tubular structures that are possible microscopic fossils of bacteria-like organisms that may have lived on Mars more than 3.6 billion years ago. http://photojournal.jpl.nasa.gov/catalog/PIA00285

Mars Life? - Microscopic Egg-shaped Structures

NASA Image and Video Library

1996-08-09

This electron microscope image shows egg-shaped structures, some of which may be possible microscopic fossils of Martian origin as discussed by NASA research published in the Aug. 16, 1996. http://photojournal.jpl.nasa.gov/catalog/PIA00286

CHARACTERISTICS OF INDIVIDUAL PARTICLES AT A RURAL SITE IN THE EASTERN UNITED STATES

EPA Science Inventory

To determine the nature of aerosol particles in a rural area of the eastern United States, aerosol samples were collected at Deep Creek Lake, Maryland, on various substrates and analyzed by a scanning electron microscope (SEM) and a transmission electron microscope (TEM). SEM ana...

Characterization of calcium crystals in Abelia using x-ray diffraction and electron microscopes

USDA-ARS?s Scientific Manuscript database

Localization, chemical composition, and morphology of calcium crystals in leaves and stems of Abelia mosanensis and A. ×grandiflora were analyzed with a variable pressure scanning electron microscope (VP-SEM) equipped with an X-ray diffraction system, low temperature SEM (LT-SEM) and a transmission ...

77 FR 33422 - The Regents of the University of California, et al.; Notice of Consolidated Decision on...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-06-06

... DEPARTMENT OF COMMERCE International Trade Administration The Regents of the University of...: Washington University in St. Louis, Saint Louis, MO 63130. Instrument: Electron Microscope. Manufacturer: FEI.... Applicant: The Regents of the University of California, Berkeley, CA 94720. Instrument: Electron Microscope...

Neuroanatomy from Mesoscopic to Nanoscopic Scales: An Improved Method for the Observation of Semithin Sections by High-Resolution Scanning Electron Microscopy

PubMed Central

Rodríguez, José-Rodrigo; Turégano-López, Marta; DeFelipe, Javier; Merchán-Pérez, Angel

2018-01-01

Semithin sections are commonly used to examine large areas of tissue with an optical microscope, in order to locate and trim the regions that will later be studied with the electron microscope. Ideally, the observation of semithin sections would be from mesoscopic to nanoscopic scales directly, instead of using light microscopy and then electron microscopy (EM). Here we propose a method that makes it possible to obtain high-resolution scanning EM images of large areas of the brain in the millimeter to nanometer range. Since our method is compatible with light microscopy, it is also feasible to generate hybrid light and electron microscopic maps. Additionally, the same tissue blocks that have been used to obtain semithin sections can later be used, if necessary, for transmission EM, or for focused ion beam milling and scanning electron microscopy (FIB-SEM). PMID:29568263

Neuroanatomy from Mesoscopic to Nanoscopic Scales: An Improved Method for the Observation of Semithin Sections by High-Resolution Scanning Electron Microscopy.

PubMed

Rodríguez, José-Rodrigo; Turégano-López, Marta; DeFelipe, Javier; Merchán-Pérez, Angel

2018-01-01

Semithin sections are commonly used to examine large areas of tissue with an optical microscope, in order to locate and trim the regions that will later be studied with the electron microscope. Ideally, the observation of semithin sections would be from mesoscopic to nanoscopic scales directly, instead of using light microscopy and then electron microscopy (EM). Here we propose a method that makes it possible to obtain high-resolution scanning EM images of large areas of the brain in the millimeter to nanometer range. Since our method is compatible with light microscopy, it is also feasible to generate hybrid light and electron microscopic maps. Additionally, the same tissue blocks that have been used to obtain semithin sections can later be used, if necessary, for transmission EM, or for focused ion beam milling and scanning electron microscopy (FIB-SEM).

Variations in contrast of scanning electron microscope images for microstructure analysis of Si-based semiconductor materials.

PubMed

Itakura, Masaru; Kuwano, Noriyuki; Sato, Kaoru; Tachibana, Shigeaki

2010-08-01

Image contrasts of Si-based semiconducting materials have been investigated by using the latest scanning electron microscope with various detectors under a range of experimental conditions. Under a very low accelerating voltage (500 V), we obtained a good image contrast between crystalline SiGe whiskers and the amorphous matrix using an in-lens secondary electron (SE) detector, while the conventional topographic SE image and the compositional backscattered electron (BSE) image gave no distinct contrast. By using an angular-selective BSE (AsB) detector for wide-angle scattered BSE, on the other hand, the crystal grains in amorphous matrix can be clearly visualized as 'channelling contrast'. The image contrast is very similar to that of their transmission electron microscope image. The in-lens SE (true SE falling dots SE1) and the AsB (channelling) contrasts are quite useful to distinguish crystalline parts from amorphous ones.

Dynamic imaging with electron microscopy

ScienceCinema

Campbell, Geoffrey; McKeown, Joe; Santala, Melissa

2018-02-13

Livermore researchers have perfected an electron microscope to study fast-evolving material processes and chemical reactions. By applying engineering, microscopy, and laser expertise to the decades-old technology of electron microscopy, the dynamic transmission electron microscope (DTEM) team has developed a technique that can capture images of phenomena that are both very small and very fast. DTEM uses a precisely timed laser pulse to achieve a short but intense electron beam for imaging. When synchronized with a dynamic event in the microscope's field of view, DTEM allows scientists to record and measure material changes in action. A new movie-mode capability, which earned a 2013 R&D 100 Award from R&D Magazine, uses up to nine laser pulses to sequentially capture fast, irreversible, even one-of-a-kind material changes at the nanometer scale. DTEM projects are advancing basic and applied materials research, including such areas as nanostructure growth, phase transformations, and chemical reactions.

Energy-filtered real- and k-space secondary and energy-loss electron imaging with Dual Emission Electron spectro-Microscope: Cs/Mo(110).

PubMed

Grzelakowski, Krzysztof P

2016-05-01

Since its introduction the importance of complementary k||-space (LEED) and real space (LEEM) information in the investigation of surface science phenomena has been widely demonstrated over the last five decades. In this paper we report the application of a novel kind of electron spectromicroscope Dual Emission Electron spectroMicroscope (DEEM) with two independent electron optical channels for reciprocal and real space quasi-simultaneous imaging in investigation of a Cs covered Mo(110) single crystal by using the 800eV electron beam from an "in-lens" electron gun system developed for the sample illumination. With the DEEM spectromicroscope it is possible to observe dynamic, irreversible processes at surfaces in the energy-filtered real space and in the corresponding energy-filtered kǁ-space quasi-simultaneously in two independent imaging columns. The novel concept of the high energy electron beam sample illumination in the cathode lens based microscopes allows chemically selective imaging and analysis under laboratory conditions. Copyright © 2015 Elsevier B.V. All rights reserved.

Tem Observation of Precipitates in Ag-Added Al-Mg-Si Alloys

NASA Astrophysics Data System (ADS)

Nagai, Takeshi; Matsuda, Kenji; Nakamura, Junya; Kawabata, Tokimasa; Marioara, Calin; Andersen, Sigmund J.; Holmestad, Randi; Hirosawa, Shoichi; Horita, Zenji; Terada, Daisuke; Ikeno, Susumu

The influence of addition of the small amount of transition metals to Al-Mg-Si alloy had reported by many researchers. In the previous our work, β' phase in alloys Al — 1.0 mass% Mg2Si -0.5 mass% Ag (Ag-addition) and Al -1.0 mass% Mg2Si (base) were investigated by high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), in order to understand the effect of Ag. In addition, the distribution of Ag was investigated by energy filtered mapping and high annular angular dark field scanning transmission electron microscopy (HAADF-STEM). One Ag-containing atomic column was observed per β' unit cell, and the unit cell symmetry is slightly changed as compared with the Ag-free β'. In this work, the microstructure of G.P. zone and β'' phase was investigated by TEM observation, which were formed before β' phase. The deformed sample by high pressure torsion (HPT) technique before aging was also investigated to understand its effect for aging in this alloy.

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).

Synthesis of MoS2/rGO nanosheets hybrid materials for enhanced visible light assisted photocatalytic activity

NASA Astrophysics Data System (ADS)

Pal, Shreyasi; Dutta, Shibsankar; De, Sukanta

2018-04-01

A facile hydrothermal method has been adopted to synthesize pure MoS2 nanosheets and MoS2/rGO nanosheets hybrid. The samples were characterized using field emission scanning electron microscopy (FESEM), transmission electron microscopy (HRTEM), X-ray diffraction spectroscopy (XRD), Brunauer-Emmett-Teller (BET). The photocatalytic performance and reusability of MoS2 nanosheets and MoS2/rGO hybrids was evaluated by discoloring of RhB under visible light irradiation. Results indicated that MoS2/rGO photocatalysts with large surface area of 69.5 m2 g-1 could completely degrade 50 mL of 8 mg L-1 RhB aqueous solution in 90 min with excellent recycling and structural stability as compared with pure MoS2 nanosheets (53%). Such enhanced performance could be explained due to the high surface area, enhanced light absorption and the increased dye adsorptivity and reduced electron-hole pair recombination with the presence of rGO.

Synthesis, Characterization, and Mechanism of Formation of Janus-Like Nanoparticles of Tantalum Silicide-Silicon (TaSi2/Si)

PubMed Central

Nomoev, Andrey V.; Bardakhanov, Sergey P.; Schreiber, Makoto; Bazarova, Dashima Zh.; Baldanov, Boris B.; Romanov, Nikolai A.

2014-01-01

Metal-semiconductor Janus-like nanoparticles with the composition tantalum silicide-silicon (TaSi2/Si) were synthesized for the first time by means of an evaporation method utilizing a high-power electron beam. The composition of the synthesized particles were characterized using high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), selective area electron diffraction (SAED), and energy dispersive X-ray fluorescence (EDX) analysis. The system is compared to previously synthesized core-shell type particles in order to show possible differences responsible for the Janus-like structure forming instead of a core-shell architecture. It is proposed that the production of Janus-like as opposed to core-shell or monophase particles occurs due to the ability of Ta and Si to form compounds and the relative content of Ta and Si atoms in the produced vapour. Based on the results, a potential mechanism of formation for the TaSi2/Si nanoparticles is discussed. PMID:28346996

Synthesis, Characterization, and Mechanism of Formation of Janus-Like Nanoparticles of Tantalum Silicide-Silicon (TaSi₂/Si).

PubMed

Nomoev, Andrey V; Bardakhanov, Sergey P; Schreiber, Makoto; Bazarova, Dashima Zh; Baldanov, Boris B; Romanov, Nikolai A

2014-12-25

Metal-semiconductor Janus-like nanoparticles with the composition tantalum silicide-silicon (TaSi₂/Si) were synthesized for the first time by means of an evaporation method utilizing a high-power electron beam. The composition of the synthesized particles were characterized using high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), selective area electron diffraction (SAED), and energy dispersive X-ray fluorescence (EDX) analysis. The system is compared to previously synthesized core-shell type particles in order to show possible differences responsible for the Janus-like structure forming instead of a core-shell architecture. It is proposed that the production of Janus-like as opposed to core-shell or monophase particles occurs due to the ability of Ta and Si to form compounds and the relative content of Ta and Si atoms in the produced vapour. Based on the results, a potential mechanism of formation for the TaSi₂/Si nanoparticles is discussed.

Green synthesis of gold nanoparticles using aqueous extract of Dillenia indica

NASA Astrophysics Data System (ADS)

Sett, Arghya; Gadewar, Manoj; Sharma, Pragya; Deka, Manab; Bora, Utpal

2016-06-01

In this study, we report a novel method of gold nanoparticle (AuNP) synthesis using aqueous fruit extract of Dillenia indica. The phytochemicals present in the fruit extract act as an effective reducing and capping agent to synthesize AuNPs. The synthesized AuNPs were characterized by spectrophotometry, transmission electron microscopy (TEM), x-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. TEM studies revealed the particles of various sizes and mainly spherical in shape. Selected-area electron diffraction (SAED) patterns and high-resolution transmission electron microscopy (HRTEM) images confirmed the crystallinity of the particles. The XRD patterns showed peaks at (111), (200), (220) which exhibited preferential orientation of the AuNPs as face-centered cubic crystal. FTIR measurements confirmed the coating of phenolic compounds on the AuNPs indicating a possible role of biomolecules for the capping and efficient stabilization of the AuNPs. The synthesized AuNPs did not show any form of cytotoxicity in the normal fibroblast cell line L929.

TEM-EELS Investigation of Boron and Phosphorus Passivated 4H-SiC/SiO2 Interface Structures

NASA Astrophysics Data System (ADS)

Klingshirn, Christopher; Taillon, Joshua; Liu, Gang; Dhar, Sarit; Feldman, Leonard; Zheleva, Tsvetanka; Lelis, Aivars; Salamanca-Riba, Lourdes

A high density of electronic defects at the SiC/SiO2 interface adversely affects SiC-based metal oxide semiconductor devices. Various treatments are known to improve device performance. Annealing in a nitric oxide (NO) environment, for example, passivates electronic defects at the interface and raises the carrier mobility in the active region to 35-40 cm2/Vs, but the effect saturates after about 60 minutes of annealing. Passivation with phosphorus or boron improves upon NO by a factor of 2, increasing the mobility to over 90 cm2/Vs.2 We investigate the chemical and structural effects of these treatments on the SiC/SiO2 transition layer using high-resolution transmission electron microscopy (HRTEM) and high angle annular dark field (HAADF). Electron energy loss spectroscopy Spectrum Imaging (EELS SI) collected across the transition region allow identification of the width, composition and types of bonding at the transition layer. Advanced machine learning techniques applied to the EELS data reveal intermediate bonding states within this region. Supported by ARL under Grant No. W911NF1420110.

Development of a secondary electron energy analyzer for a transmission electron microscope.

PubMed

Magara, Hideyuki; Tomita, Takeshi; Kondo, Yukihito; Sato, Takafumi; Akase, Zentaro; Shindo, Daisuke

2018-04-01

A secondary electron (SE) energy analyzer was developed for a transmission electron microscope. The analyzer comprises a microchannel plate (MCP) for detecting electrons, a coil for collecting SEs emitted from the specimen, a tube for reducing the number of backscattered electrons incident on the MCP, and a retarding mesh for selecting the energy of SEs incident on the MCP. The detection of the SEs associated with charging phenomena around a charged specimen was attempted by performing electron holography and SE spectroscopy using the energy analyzer. The results suggest that it is possible to obtain the energy spectra of SEs using the analyzer and the charging states of a specimen by electron holography simultaneously.

Structural analysis of ion-implanted chemical-vapor-deposited diamond by transmission electron microscope

NASA Astrophysics Data System (ADS)

Jiang, N.; Deguchi, M.; Wang, C. L.; Won, J. H.; Jeon, H. M.; Mori, Y.; Hatta, A.; Kitabatake, M.; Ito, T.; Hirao, T.; Sasaki, T.; Hiraki, A.

1997-04-01

A transmission electron microscope (TEM) study of ion-implanted chemical-vapor-deposited (CVD) diamond is presented. CVD diamond used for transmission electron microscope observation was directly deposited onto Mo TEM grids. As-deposited specimens were irradiated by C (100 keV) ions at room temperature with a wide range of implantation doses (10 12-10 17/cm 2). Transmission electron diffraction (TED) patterns indicate that there exists a critical dose ( Dc) for the onset of amorphization of CVD diamond as a result of ion induced damage and the value of critical dose is confirmed to be about 3 × 10 15/cm 2. The ion-induced transformation process is clearly revealed by high resolution electron microscope (HREM) images. For a higher dose implantation (7 × 10 15/cm 2) a large amount of diamond phase is transformed into amorphous carbon and many tiny misoriented diamond blocks are found to be left in the amorphous solid. The average size of these misoriented diamond blocks is only about 1-2 nm. Further bombardment (10 17/cm 2) almost kills all of the diamond phase within the irradiated volume and moreover leads to local formation of micropolycrystalline graphite.