Pd-Ni-MWCNT nanocomposite thin films: preparation and structure

NASA Astrophysics Data System (ADS)

Kozłowski, Mirosław; Czerwosz, ElŻbieta; Sobczak, Kamil

2017-08-01

The properties of nanocomposite palladium-nickel-multi-walled (Pd-Ni-MWCNT) films deposited on aluminum oxide (Al2O3) substrate have been prepared and investigated. These films were obtained by 3 step process consisted of PVD/CVD/PVD methods. The morphology and structure of the obtained films were characterized by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) techniques at various stages of the film formation. EDX spectrometer was used to measurements of elements segregation in the obtained film. TEM and STEM (Scanning Transmission Electron Microscopy) observations showed MWCNTs decorated with palladium nanoparticles in the film obtained in the last step of film formation (final PVD process). The average size of the palladium nanoparticles observed both on MWCNTs and carbonaceous matrix does not exceed 5 nm. The research was conducted on the use of the obtained films as potential sensors of gases (e.g. H2, NH3, CO2) and bio-sensors or optical sensors.

Extraction of cellulose nanofibrils from dry softwood pulp using high shear homogenization.

PubMed

Zhao, Jiangqi; Zhang, Wei; Zhang, Xiaodan; Zhang, Xinxing; Lu, Canhui; Deng, Yulin

2013-09-12

The objective of this study was to extract cellulose nanofibrils (CNFs) from dry softwood pulp through a simple and environmentally friendly physical method of refining pretreatment coupled with high shear homogenization. An optical microscopy (OM) clearly showed the morphological development from the cellulose fibers to CNFs under repeated shear forces. The morphology, structure and properties of the obtained CNFs were comprehensively investigated using scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transformed infrared (FTIR) spectra, X-ray diffraction (XRD) and thermogravimetric (TG) analysis. The results indicated that the CNFs had diameters mainly ranged from 16 to 28nm. Compared with the pulp fibers, the CNFs exhibited a slightly higher crystallinity and a lower thermal stability. Moreover, a novel nanopaper with high optical transparency was prepared from the obtained CNFs, and a possible mechanism for the high optical transparency was discussed. Copyright © 2013 Elsevier Ltd. All rights reserved.

A facile synthesis of metal nanoparticle - graphene composites for better absorption of solar radiation

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

Sharma, Bindu; Mulla, Rafiq; Rabinal, M. K., E-mail: mkrabinal@yahoo.com

2015-06-24

Herein, a facile chemical approach has been adopted to prepare silver nanoparticles (AgNPs)- graphene (G) composite to study photothermal effect. Sodium borohydride (SBH), a strong reducing agent has been selected for this work. Effect of SBH concentrations on optical behavior of AgNPs-G composite was also investigated. Resultant materials were characterized by various techniques including X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), optical absorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM micrographs confirm wrapping of AgNPs into graphene whereas XRD analysis reveals their particle size variation between 47 nm to 69 nm. Optical studies throw a light on theirmore » strong absorption behavior towards solar radiation.« less

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.

Additive assisted hydrothermal synthesis, characterization and optical properties of one dimensional DyPO4:Ce3+ nanostructures

NASA Astrophysics Data System (ADS)

Khajuria, H.; Kumar, M.; Singh, R.; Ladol, J.; Nawaz Sheikh, H.

2018-05-01

One dimensional nanostructures of cerium doped dysprosium phosphate (DyPO4:Ce3+) were synthesized via hydrothermal route in the presence of different surfactants [sodium dodecyl sulfate (SDS), dodecyl sulfosuccinate (DSS), polyvinyl pyrollidone (PVP)] and solvent [ethylene glycol and water]. The prepared nanostructures were characterized by Powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), Field emission scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), UV-VIS-NIR absorption spectrophotometer and photoluminescence (PL) studies. The PXRD and FTIR results indicate purity, good crystallinity and effective doping of Ce3+ in nanostructures. SEM and TEM micrographs display nanorods, nanowires and nanobundles like morphology of DyPO4:Ce3+. Energy-dispersive X-ray spectra (EDS) of DyPO4:Ce3+nanostructures confirm the presence of dopant. UV-VIS-NIR absorption spectra of prepared compounds are used to calculate band gap and explore their optical properties. Luminescent properties of DyPO4:Ce3+ was studied by using PL emission spectra. The effect of additives and solvents on the uniformity, morphology and optical properties of the nanostructures were studied in detail.

Characterization of konjac glucomannan-ethyl cellulose film formation via microscopy.

PubMed

Xiao, Man; Wan, Li; Corke, Harold; Yan, Wenli; Ni, Xuewen; Fang, Yapeng; Jiang, Fatang

2016-04-01

Konjac glucomannan-ethyl cellulose (KGM-EC, 7:3, w/w) blended film shows good mechanical and moisture resistance properties. To better understand the basis for the KGM-EC film formation, optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atomic force microscopy (AFM) were used to observe the formation of the film from emulsion. Optical microscopy images showed that EC oil droplets were homogeneously dispersed in KGM water phase without obviously coalescence throughout the entire drying process. SEM images showed the surface and cross-sectional structures of samples maintained continuous and homogeneous appearance from the emulsion to dried film. AFM images indicated that KGM molecules entangled EC molecules in the emulsion. Interactions between KGM and EC improved the stability of KGM-EC emulsion, and contributed to uniformed structures of film formation. Based on these output information, a schematic model was built to elucidate KGM-EC film-forming process. Copyright © 2015 Elsevier B.V. All rights reserved.

Thin Films of Antimony-Tin Oxide as Counter-Electrodes for Proton Working Electrochromic Devices

DTIC Science & Technology

2002-01-01

diffraction and transmission electron microscopy (TEM). Electrochromic behavior is studied by means of cyclic voltamperometry coupled with ex situ optical... analysis , we noted that the Sn/Sb atomic ratio was relatively well preserved between target and grown films. Structural characterizations: Figure 1 shows the

Calcium copper-titanate thin film growth: tailoring of the operational conditions through nanocharacterization and substrate nature effects.

PubMed

Lo Nigro, Raffaella; Toro, Roberta G; Malandrino, Graziella; Fragalà, Ignazio L; Losurdo, Maria; Giangregorio, Michelaria M; Bruno, Giovanni; Raineri, Vito; Fiorenza, Patrick

2006-09-07

A novel approach based on a molten multicomponent precursor source has been applied for the MOCVD fabrication of high-quality CaCu(3)Ti(4)O(12) (CCTO) thin films on various substrates. The adopted in situ strategy involves a molten mixture consisting of Ca(hfa)(2).tetraglyme, Ti(tmhd)(2)(O-iPr)(2), and Cu(tmhd)(2) [Hhfa = 1,1,1,5,5,5-hexafluoro-2,4-pentanedione; tetraglyme = 2,5,8,11,14-pentaoxapentadecane; Htmhd = 2,2,6,6-tetramethyl-3,5-heptandione; O-iPr = isopropoxide] precursors. Film structural and morphological characterizations have been carried out by several techniques [X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM)], and in particular the energy filtered TEM mapping and X-ray energy dispersive (EDX) analysis in TEM mode provided a suitable correlation between nanostructural properties of CCTO films and deposition conditions and/or the substrate nature. Correlation between the nanostructure and optical/dielectric properties has been investigated exploiting spectroscopic ellipsometry.

Evolution of the substructure of a novel 12% Cr steel under creep conditions

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

Yadav, Surya Deo, E-mail: surya.yadav@tugraz.at; Kalácska, Szilvia, E-mail: kalacska@metal.elte.hu; Dománková, Mária, E-mail: maria.domankova@stuba.sk

2016-05-15

In this work we study the microstruture evolution of a newly developed 12% Cr martensitic/ferritic steel in as-received condition and after creep at 650 °C under 130 MPa and 80 MPa. The microstructure is described as consisting of mobile dislocations, dipole dislocations, boundary dislocations, precipitates, lath boundaries, block boundaries, packet boundaries and prior austenitic grain boundaries. The material is characterized employing light optical microscopy (LOM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). TEM is used to characterize the dislocations (mobile + dipole) inside the subgrains and XRD measurements are used tomore » the characterize mobile dislocations. Based on the subgrain boundary misorientations obtained from EBSD measurements, the boundary dislocation density is estimated. The total dislocation density is estimated for the as-received and crept conditions adding the mobile, boundary and dipole dislocation densities. Additionally, the subgrain size is estimated from the EBSD measurements. In this publication we propose the use of three characterization techniques TEM, XRD and EBSD as necessary to characterize all type of dislocations and quantify the total dislocation densty in martensitic/ferritic steels. - Highlights: • Creep properties of a novel 12% Cr steel alloyed with Ta • Experimental characterization of different types of dislocations: mobile, dipole and boundary • Characterization and interpretation of the substructure evolution using unique combination of TEM, XRD and EBSD.« less

Structural, morphological and optical properties of chromium oxide nanoparticles

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

Babukutty, Blessy; Parakkal, Fasalurahman; Nair, Swapna S., E-mail: swapna.s.nair@gmail.com

2015-06-24

Chromium oxide nanoparticles are synthesized by reduction route from chloride precursors with surfactant, trioctylphosphine oxide (TOPO). Structural and morphological characterization are analyzed using X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM). Transmission Electron micrographs show that the average grain size lies in the range 5nm to 10nm. Optical characterization has been done by UV-VIS spectrophotometer. Distinct optical absorptions of Cr{sup 3+} ions show hinting towards the presence of Cr{sub 2}O{sub 3}. Presence of oxygen is also confirmed from Electron Energy Loss Spectroscopy (EELS) studies.

Cd{sub 1−x}Mn{sub x}Te ultrasmall quantum dots growth in a silicate glass matrix by the fusion method

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

Dantas, Noelio Oliveira; Lima Fernandes, Guilherme de; Almeida Silva, Anielle Christine

2014-09-29

In this study, we synthesized Cd{sub 1−x}Mn{sub x}Te ultrasmall quantum dots (USQDs) in SiO{sub 2}-Na{sub 2}CO{sub 3}-Al{sub 2}O{sub 3}-B{sub 2}O{sub 3} glass system using the fusion method. Growth of these Cd{sub 1−x}Mn{sub x}Te USQDs was confirmed by optical absorption, atomic force microscopy (AFM), magnetic force microscopy (MFM), scanning transmission electron microscopy (TEM), and electron paramagnetic resonance (EPR) measurements. The blueshift of absorption transition with increasing manganese concentration gives evidence of incorporation of manganese ions (Mn{sup 2+}) in CdTe USQDs. AFM, TEM, and MFM confirmed, respectively, the formation of high quality Cd{sub 1−x}Mn{sub x}Te USQDs with uniformly distributed size and magneticmore » phases. Furthermore, EPR spectra showed six lines associated to the S = 5/2 spin half-filled d-state, characteristic of Mn{sup 2+}, and confirmed that Mn{sup 2+} are located in the sites core and surface of the CdTe USQD. Therefore, synthesis of high quality Cd{sub 1−x}Mn{sub x}Te USQDs may allow the control of optical and magnetic properties.« less

Phase control of austenitic chrome-nickel steel

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

Korkh, M. K., E-mail: KorkhMK@imp.uran.ru; Davidov, D. I., E-mail: davidov@imp.uran.ru; Korkh, J. V., E-mail: Korkh@imp.uran.ru

2015-10-27

The paper presents the results of the comparative study of the possibilities of different structural and magnetic methods for detection and visualization of the strain-induced martensitic phase in low carbon austenitic chromium-nickel steel. Results of TEM, SEM, optical microscopy, atomic and magnetic force microscopy, and magnetic measurements are presented. Amount of the magnetic strain-induced martensite was estimated. We pioneered magnetic force microscopic images of the single domain cluster distribution of the strain-induced martensite in austenite-ferrite materials.

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

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

NASA Astrophysics Data System (ADS)

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

2016-01-01

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

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

NASA Astrophysics Data System (ADS)

Johns, Steve; Shin, Wontak; Kane, Joshua J.; Windes, William E.; Ubic, Rick; Karthik, Chinnathambi

2018-07-01

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. To ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ∼60 μm. Discs 3 mm in diameter were then oxidized at temperatures between 575 °C and 625 °C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575 °C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

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

Johns, Steve; Shin, Wontak; Kane, Joshua J.

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

DOE PAGES

Johns, Steve; Shin, Wontak; Kane, Joshua J.; ...

2018-04-03

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

Transmission electron microscopy of unstained hybrid Au nanoparticles capped with PPAA (plasma-poly-allylamine): structure and electron irradiation effects.

PubMed

Gontard, Lionel C; Fernández, Asunción; Dunin-Borkowski, Rafal E; Kasama, Takeshi; Lozano-Pérez, Sergio; Lucas, Stéphane

2014-12-01

Hybrid (organic shell-inorganic core) nanoparticles have important applications in nanomedicine. Although the inorganic components of hybrid nanoparticles can be characterized readily using conventional transmission electron microscopy (TEM) techniques, the structural and chemical arrangement of the organic molecular components remains largely unknown. Here, we apply TEM to the physico-chemical characterization of Au nanoparticles that are coated with plasma-polymerized-allylamine, an organic compound with the formula C3H5NH2. We discuss the use of energy-filtered TEM in the low-energy-loss range as a contrast enhancement mechanism for imaging the organic shells of such particles. We also study electron-beam-induced crystallization and amorphization of the shells and the formation of graphitic-like layers that contain both C and N. The resistance of the samples to irradiation by high-energy electrons, which is relevant for optical tuning and for understanding the degree to which such hybrid nanostructures are stable in the presence of biomedical radiation, is also discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

Electron Microscopist | Center for Cancer Research

Cancer.gov

PROGRAM DESCRIPTION The Cancer Research Technology Program (CRTP) develops and implements emerging technology, cancer biology expertise and research capabilities to accomplish NCI research objectives. The CRTP is an outward-facing, multi-disciplinary hub purposed to enable the external cancer research community and provides dedicated support to NCI’s intramural Center for Cancer Research (CCR). The dedicated units provide electron microscopy, protein characterization, protein expression, optical microscopy and genetics. These research efforts are an integral part of CCR at the Frederick National Laboratory for Cancer Research (FNLCR). CRTP scientists also work collaboratively with intramural NCI investigators to provide research technologies and expertise. KEY ROLES/RESPONSIBILITIES - THIS POSITION IS CONTINGENT UPON FUNDING APPROVAL The Electron Microscopist will: Operate ultramicrotomes (Leica) and other instrumentation related to the preparation of embedded samples for EM (TEM and SEM) Operate TEM microscopes, (specifically Hitachi, FEI T20 and FEI T12) as well as SEM microscopes (Hitachi); task will include loading samples, screening, and performing data collection for a variety of samples: from cells to proteins Manage maintenance for the TEM and SEM microscopes Provide technical advice to investigators on sample preparation and data collection

Analysis on nonlinear optical properties of Cd (Zn) Se quantum dots synthesized using three different stabilizing agents

NASA Astrophysics Data System (ADS)

J, Joy Sebastian Prakash; G, Vinitha; Ramachandran, Murugesan; Rajamanickam, Karunanithi

2017-10-01

Three different stabilizing agents, namely, L-cysteine, Thioglycolic acid and cysteamine hydrochloride were used to synthesize Cd(Zn)Se quantum dots (QDs). It was characterized using UV-vis spectroscopy, x-ray diffraction (XRD) and transmission electron microscopy (TEM). The non-linear optical properties (non-linear absorption and non-linear refraction) of synthesized Cd(Zn)Se quantum dots were studied with z-scan technique using diode pumped continuous wavelaser system at a wavelength of 532 nm. Our (organic) synthesized quantum dots showed optical properties similar to the inorganic materials reported elsewhere.

Deformation microstructures of Barre granite: An optical, Sem and Tem study

USGS Publications Warehouse

Schedl, A.; Kronenberg, A.K.; Tullis, J.

1986-01-01

New scanning electron microscope techniques have been developed for characterizing ductile deformation microstructures in felsic rocks. In addition, the thermomechanical history of the macroscopically undeformed Barre granite (Vermont, U.S.A.) has been reconstructed based on examination of deformation microstructures using optical microscopy, scanning electron microscopy, and transmission electron microscopy. The microstructures reveal three distinct events: 1. (1) a low-stress, high-temperature event that produced subgrains in feldspars, and subgrains and recrystallized grains in quartz; 2. (2) a high-stress, low-temperature event that produced a high dislocation density in quartz and feldspars; and 3. (3) a lowest-temperature event that produced cracks, oriented primarily along cleavage planes in feldspars, and parallel to the macroscopic rift in quartz. The first two events are believed to reflect various stages in the intrusion and cooling history of the pluton, and the last may be related to the last stages of cooling, or to later tectonism. ?? 1986.

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

PubMed

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

2013-01-01

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

Microstructural, mechanical and electrochemical behaviour of a 7017 Al–Zn–Mg alloy of different tempers

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

Rout, Prasanta Kumar, E-mail: prasantonnet55@yahoo.com; Ghosh, M.M.; Ghosh, K.S., E-mail: ksghosh2001@yahoo.co.uk

2015-06-15

The aim of the investigation is to assess the microstructural features and associated physical, mechanical and electrochemical properties of a 7017 Al–Zn–Mg alloy of various tempers. A 7017 Al–Zn–Mg alloy was subjected to different ageing schedules to produce under-(T4), peak-(T6), over-(T7) and highly over-aged tempers. Optical microscopy, hardness measurement, electrical conductivity measurement, tensile testing and SEM fractographs, differential scanning calorimetry (DSC), transmission electron microscopy (TEM), and electrochemical polarization studies have been used to characterize the alloy tempers. Hardness measurement and tensile testing showed the characteristic age hardening phenomenon of aluminium alloys. Optical and TEM micrographs have revealed the variation inmore » size of matrix strengthening η′ (MgZn{sub 2}) and also the size and distribution of grain boundary η (MgZn{sub 2}) precipitate with ageing time. DSC thermograms exhibiting exothermic and endothermic peaks indicated the characteristic solid state reaction sequence of the 7017 alloy. Potentiodynamic polarization study of the 7017 alloy of various tempers in 3.5 wt.% NaCl solution at near neutral pH showed typical active metal dissolution behaviour, but at pH 12 an active–passive–transpassive transition behaviour has been observed. - Graphical abstract: TEM micrograph of the 7017 aluminium alloy of various tempers (a, b) under aged (T4), (c, d) peak aged (T6), (e, f) over aged (T7) and (g, h) highly over-aged. Display Omitted - Highlights: • 7017 Al-Zn-Mg alloy was subjected to different artificial ageing treatments. • Characterization of 7017 alloy tempers by hardness, tensile, DSC, TEM and electrochemical behaviour. • Structure-properties relationship of the 7017 Al-Zn-Mg alloy of various tempers.« less

Determination of dispersive optical constants of nanocrystalline CdSe (nc-CdSe) thin films

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

Sharma, Kriti; Al-Kabbi, Alaa S.; Saini, G.S.S.

2012-06-15

Highlights: ► nc-CdSe thin films are prepared by thermal vacuum evaporation technique. ► TEM analysis shows NCs are spherical in shape. ► XRD reveals the hexagonal (wurtzite) crystal structure of nc-CdSe thin films. ► The direct optical bandgap of nc-CdSe is 2.25 eV in contrast to bulk (1.7 eV). ► Dispersion of refractive index is discussed in terms of Wemple–DiDomenico single oscillator model. -- Abstract: The nanocrystalline thin films of CdSe are prepared by thermal evaporation technique at room temperature. These thin films are characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), X-raymore » diffraction (XRD) and photoluminescence spectroscopy (PL). The transmission spectra are recorded in the transmission range 400–3300 nm for nc-CdSe thin films. Transmittance measurements are used to calculate the refractive index (n) and absorption coefficient (α) using Swanepoel's method. The optical band gap (E{sub g}{sup opt}) has been determined from the absorption coefficient values using Tauc's procedure. The optical constants such as extinction coefficient (k), real (ε{sub 1}) and imaginary (ε{sub 2}) dielectric constants, dielectric loss (tan δ), optical conductivity (σ{sub opt}), Urbach energy (E{sub u}) and steepness parameter (σ) are also calculated for nc-CdSe thin films. The normal dispersion of refractive index is described using Wemple–DiDomenico single-oscillator model. Refractive index dispersion is further analysed to calculate lattice dielectric constant (ε{sub L}).« less

Rational design of Ag/TiO2 nanosystems by a combined RF-sputtering/sol-gel approach.

PubMed

Armelao, Lidia; Barreca, Davide; Bottaro, Gregorio; Gasparotto, Alberto; Maccato, Chiara; Tondello, Eugenio; Lebedev, Oleg I; Turner, Stuart; Van Tendeloo, Gustaaf; Sada, Cinzia; Stangar, Urska Lavrencic

2009-12-21

The present work is devoted to the preparation of Ag/TiO(2) nanosystems by an original synthetic strategy, based on the radio-frequency (RF) sputtering of silver particles on titania-based xerogels prepared by the sol-gel (SG) route. This approach takes advantage of the synergy between the microporous xerogel structure and the infiltration power characterizing RF-sputtering, whose combination enables the obtainment of a tailored dispersion of Ag-containing particles into the titania matrix. In addition, the system's chemico-physical features can be tuned further through proper ex situ thermal treatments in air at 400 and 600 degrees C. The synthesized composites are extensively characterized by the joint use of complementary techniques, that is, X-ray photoelectron and X-ray excited Auger electron spectroscopies (XPS, XE-AES), secondary ion mass spectrometry (SIMS), glancing incidence X-ray diffraction (GIXRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron diffraction (ED), high-angle annular dark field scanning TEM (HAADF-STEM), energy-filtered TEM (EF-TEM) and optical absorption spectroscopy. Finally, the photocatalytic performances of selected samples in the decomposition of the azo-dye Plasmocorinth B are preliminarily investigated. The obtained results highlight the possibility of tailoring the system characteristics over a broad range, directly influencing their eventual functional properties.

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

NASA Astrophysics Data System (ADS)

Osuntokun, Jejenija; Ajibade, Peter A.

2015-07-01

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

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

NASA Astrophysics Data System (ADS)

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

2010-07-01

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

Production and fabrication of 2500-lb Nb--Ti ingots to rod

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

Cordier, T.E.; McDonald, W.K.

Interest in Nb--Ti superconducting devices is exploding. This paper outlines the critical production criteria for this material. Areas discussed include ingot blending, melting, forging, extrusion, and rod reducing with emphasis on the metallurgical considerations affecting mechanical properties. Data are included relating process parameters to TEM finding as well as R.T. ductility and optical microscopy. (auth)

Quantitative Cryo-Scanning Transmission Electron Microscopy of Biological Materials.

PubMed

Elbaum, Michael

2018-05-11

Electron tomography provides a detailed view into the 3D structure of biological cells and tissues. Physical fixation by vitrification of the aqueous medium provides the most faithful preservation of biological specimens in the native, fully hydrated state. Cryo-microscopy is challenging, however, because of the sensitivity to electron irradiation and due to the weak electron scattering of organic material. Tomography is even more challenging because of the dependence on multiple exposures of the same area. Tomographic imaging is typically performed in wide-field transmission electron microscopy (TEM) mode with phase contrast generated by defocus. Scanning transmission electron microscopy (STEM) is an alternative mode based on detection of scattering from a focused probe beam, without imaging optics following the specimen. While careful configuration of the illumination and detectors is required to generate useful contrast, STEM circumvents the major restrictions of phase contrast TEM to very thin specimens and provides a signal that is more simply interpreted in terms of local composition and density. STEM has gained popularity in recent years for materials science. The extension of STEM to cryomicroscopy and tomography of cells and macromolecules is summarized herein. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enhanced Optical Breakdown in KB Cells Labeled with Folate-Targeted Silver/Dendrimer Composite Nanodevices

PubMed Central

Tse, Christine; Zohdy, Marwa J.; Ye, Jing Yong; O'Donnell, Matthew; Lesniak, Wojciech; Balogh, Lajos

2010-01-01

Enhanced optical breakdown of KB cells (a human oral epidermoid cancer cell known to overexpress folate receptors) targeted with silver/dendrimer composite nanodevices (CNDs) is described. CNDs {(Ag0}25-PAMAM_E5.(NH2)42(NGly)74(NFA)2.7} were fabricated by reactive encapsulation, using a biocompatible template of dendrimer-folic acid (FA) conjugates. Preferential uptake of the folate-targeted CNDs (of various treatment concentrations and surface functionality) by KB cells was visualized with confocal microscopy and transmission electron microscopy (TEM). Intracellular laser-induced optical breakdown (LIOB) threshold and dynamics were detected and characterized by high-frequency ultrasonic monitoring of resulting transient bubble events. When irradiated with a near-infrared (NIR), femtosecond laser, the CND-targeted KB cells acted as well-confined activators of laser energy, enhancing nonlinear energy absorption, exhibiting a significant reduction in breakdown threshold, and thus selectively promoting intracellular LIOB. PMID:20883823

Microstructure and composition analysis of low-Z/low-Z multilayers by combining hard and resonant soft X-ray reflectivity

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

Rao, P. N., E-mail: pnrao@rrcat.gov.in; Rai, S. K.; Srivastava, A. K.

2016-06-28

Microstructure and composition analysis of periodic multilayer structure consisting of a low electron density contrast (EDC) material combination by grazing incidence hard X-ray reflectivity (GIXR), resonant soft X-ray reflectivity (RSXR), and transmission electron microscopy (TEM) are presented. Measurements of reflectivity at different energies allow combining the sensitivity of GIXR data to microstructural parameters like layer thicknesses and interfacing roughness, with the layer composition sensitivity of RSXR. These aspects are shown with an example of 10-period C/B{sub 4}C multilayer. TEM observation reveals that interfaces C on B{sub 4}C and B{sub 4}C on C are symmetric. Although GIXR provides limited structural informationmore » when EDC between layers is low, measurements using a scattering technique like GIXR with a microscopic technique like TEM improve the microstructural information of low EDC combination. The optical constants of buried layers have been derived by RSXR. The derived optical constants from the measured RSXR data suggested the presence of excess carbon into the boron carbide layer.« less

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

Janeoo, Shashi; Sharma, Mamta, E-mail: mamta.phy85@gmail.com; Goswamy, J.

Polyaniline-indium oxide (In{sub 2}O{sub 3}/PANI) nanocomposite have been prepared by in-situ polymerization of aniline and as-synthesized In{sub 2}O{sub 3} nanoparticles. X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transformation infrared (FTIR) and UV/Vis spectroscopy techniques are used to investigate the structural and optical properties of In{sub 2}O{sub 3}/PANI nanocomposite. TEM analysis shows In{sub 2}O{sub 3} nanoparticles are embedded in PANI nanofibers. FTIR spectra show the good interactions between PANI nanofibers and In{sub 2}O{sub 3} nanoparticles. The band gap and electronic transitions in In{sub 2}O{sub 3}/PANI nanocomposite is determined by using UV/Vis spectra.

Consecutive light microscopy, scanning-transmission electron microscopy and transmission electron microscopy of traumatic human brain oedema and ischaemic brain damage.

PubMed

Castejon, O J; Castejon, H V; Diaz, M; Castellano, A

2001-10-01

Cortical biopsies of 11 patients with traumatic brain oedema were consecutively studied by light microscopy (LM) using thick plastic sections, scanning-transmission electron microscopy ((S)TEM) using semithin plastic sections and transmission electron microscopy (TEM) using ultrathin sections. Samples were glutaraldehyde-osmium fixed and embedded in Araldite or Epon. Thick sections were stained with toluidine-blue for light microscopy. Semithin sections were examined unstained and uncoated for (S)TEM. Ultrathin sections were stained with uranyl and lead. Perivascular haemorrhages and perivascular extravasation of proteinaceous oedema fluid were observed in both moderate and severe oedema. Ischaemic pyramidal and non-pyramidal nerve cells appeared shrunken, electron dense and with enlargement of intracytoplasmic membrane compartment. Notably swollen astrocytes were observed in all samples examined. Glycogen-rich and glycogen-depleted astrocytes were identified in anoxic-ischaemic regions. Dark and hydropic satellite, interfascicular and perivascular oligodendrocytes were also found. The status spongiosus of severely oedematous brain parenchyma observed by LM and (S)TEM was correlated with the enlarged extracellular space and disrupted neuropil observed by TEM. The (S)TEM is recommended as a suitable technique for studying pathological processes in the central nervous system and as an informative adjunct to LM and TEM.

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

PubMed

Sivakami, R; Dhanuskodi, S; Karvembu, R

2016-01-05

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

In quest of perfection in electron optics: a biographical sketch of Harald Rose on the occasion of his 80th birthday.

PubMed

Urban, Knut W

2015-04-01

This brief biographical sketch of Harald Rose on occasion of his 80th birthday describes some of the key events in an extraordinarily successful scientific life. Many of the theoretical concepts developed by him over the last 50 years have been fundamental for electron optics. Indeed, some of them have changed the whole complexion of this field and are fundamental to modern electron microscopy, both in TEM and in STEM mode. With this dedicated issue of Ultramicroscopy, the members of the electron microscopy community would like to thank Harald Rose for dedicating his professional life to their field and thereby enriching the life of those active in it. Copyright © 2015 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

Mineralogy and Microstructures of Shock-Induced Melt Veins in Chondrites

NASA Technical Reports Server (NTRS)

Sharp, Thomas G.

2000-01-01

The applicability of phase equilibrium data to the interpretation of shock-induced melt veins can only be tested by a detailed study of melt- vein mineralogy to see how high-pressure assemblages vary as a function of shock conditions inferred from other indicators. We have used transmission electron microscopy (TEM), analytical electron microscopy (AEM), scanning electron microscopy (SEM), electron microprobe analysis (EMA) and optical petrography to characterize the mineralogy, microstructures, and compositions of melt veins and associated high-pressure minerals in shocked chondrites and SNC meteorites. In the processes, we have gained a better understanding of what melt veining can tell us about shock conditions and we have discovered new mineral phases in chondritic and SNC meteorites.

High-temperature slow-strain-rate compression studies on CoAl-TiB2 composites

NASA Technical Reports Server (NTRS)

Mannan, S. K.; Kumar, K. S.; Whittenberger, J. D.

1990-01-01

Results are presented of compressive deformation tests performed on particulate-reinforced CoAl-TiB2 composites in the temperature range 1100-1300 K. Hot-pressed and postdeformation microstructures were characterized by TEM and by optical microscopy. It was found that the addition of TiB2 particles improves the deformation resistance of the matrix, due to dislocation-particle interactions.

Clean Transfer of Large Graphene Single Crystals for High-Intactness Suspended Membranes and Liquid Cells.

PubMed

Zhang, Jincan; Lin, Li; Sun, Luzhao; Huang, Yucheng; Koh, Ai Leen; Dang, Wenhui; Yin, Jianbo; Wang, Mingzhan; Tan, Congwei; Li, Tianran; Tan, Zhenjun; Liu, Zhongfan; Peng, Hailin

2017-07-01

The atomically thin 2D nature of suspended graphene membranes holds promising in numerous technological applications. In particular, the outstanding transparency to electron beam endows graphene membranes great potential as a candidate for specimen support of transmission electron microscopy (TEM). However, major hurdles remain to be addressed to acquire an ultraclean, high-intactness, and defect-free suspended graphene membrane. Here, a polymer-free clean transfer of sub-centimeter-sized graphene single crystals onto TEM grids to fabricate large-area and high-quality suspended graphene membranes has been achieved. Through the control of interfacial force during the transfer, the intactness of large-area graphene membranes can be as high as 95%, prominently larger than reported values in previous works. Graphene liquid cells are readily prepared by π-π stacking two clean single-crystal graphene TEM grids, in which atomic-scale resolution imaging and temporal evolution of colloid Au nanoparticles are recorded. This facile and scalable production of clean and high-quality suspended graphene membrane is promising toward their wide applications for electron and optical microscopy. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Kinetic precipitation of solution-phase polyoxomolybdate followed by transmission electron microscopy: a window to solution-phase nanostructure.

PubMed

Zhu, Yan; Cammers-Goodwin, Arthur; Zhao, Bin; Dozier, Alan; Dickey, Elizabeth C

2004-05-17

This study aimed to elucidate the structural nature of the polydisperse, nanoscopic components in the solution and the solid states of partially reduced polyoxomolybdate derived from the [Mo132] keplerate, [(Mo)Mo5]12-[Mo2 acetate]30. Designer tripodal hexamine-tris-crown ethers and nanoscopic molybdate coprecipitated from aqueous solution. These microcrystalline solids distributed particle radii between 2-30 nm as assayed by transmission electron microscopy (TEM). The solid materials and their particle size distributions were snap shots of the solution phase. The mother liquor of the preparation of the [Mo132] keplerate after three days revealed large species (r=20-30 nm) in the coprecipitate, whereas [Mo132] keplerate redissolved in water revealed small species (3-7 nm) in the coprecipitate. Nanoparticles of coprecipitate were more stable than solids derived solely from partially reduced molybdate. The TEM features of all material analyzed lacked facets on the nanometer length scale; however, the structures diffracted electrons and appeared to be defect-free as evidenced by Moiré patterns in the TEM images. Moiré patterns and size-invariant optical densities of the features in the micrographs suggested that the molybdate nanoparticles were vesicular.

Targeted nanodiamonds for identification of subcellular protein assemblies in mammalian cells

PubMed Central

Lake, Michael P.; Bouchard, Louis-S.

2017-01-01

Transmission electron microscopy (TEM) can be used to successfully determine the structures of proteins. However, such studies are typically done ex situ after extraction of the protein from the cellular environment. Here we describe an application for nanodiamonds as targeted intensity contrast labels in biological TEM, using the nuclear pore complex (NPC) as a model macroassembly. We demonstrate that delivery of antibody-conjugated nanodiamonds to live mammalian cells using maltotriose-conjugated polypropylenimine dendrimers results in efficient localization of nanodiamonds to the intended cellular target. We further identify signatures of nanodiamonds under TEM that allow for unambiguous identification of individual nanodiamonds from a resin-embedded, OsO4-stained environment. This is the first demonstration of nanodiamonds as labels for nanoscale TEM-based identification of subcellular protein assemblies. These results, combined with the unique fluorescence properties and biocompatibility of nanodiamonds, represent an important step toward the use of nanodiamonds as markers for correlated optical/electron bioimaging. PMID:28636640

On the chemical homogeneity of In xGa 1–xN alloys – Electron microscopy at the edge of technical limits

DOE PAGES

Specht, Petra; Kisielowski, Christian

2016-08-30

Ternary In xGa 1–xN alloys became technologically attractive when p-doping was achieved to produce blue and green light emitting diodes (LED)s. Starting in the mid 1990th, investigations of their chemical homogeneity were driven by the need to understand carrier recombination mechanisms in optical device structures to optimize their performance. Transmission electron microscopy (TEM) is the technique of choice to complement optical data evaluations, which suggests the coexistence of local carrier recombination mechanisms based on piezoelectric field effects and on indium clustering in the quantum wells of LEDs. We summarize the historic context of homogeneity investigations using electron microscopy techniques thatmore » can principally resolve the question of indium segregation and clustering in In xGa 1–xN alloys if optimal sample preparation and electron dose-controlled imaging techniques are employed together with advanced data evaluation.« less

Morphological study of the TK cholangiocarcinoma cell line with three-dimensional cell culture.

PubMed

Akiyoshi, Kohei; Kamada, Minori; Akiyama, Nobutake; Suzuki, Masafumi; Watanabe, Michiko; Fujioka, Kouki; Ikeda, Keiichi; Mizuno, Shuichi; Manome, Yoshinobu

2014-04-01

Cholangiocarcinoma is an intractable carcinoma originating from the bile duct epithelium. To gain an understanding of the cell biology of cholangiocarcinoma, in vitro cell culture is valuable. However, well‑characterized cell lines are limited. In the present study, the morphology of the TK cholangiocarcinoma cell line was analyzed by three‑dimensional culture. Dispersed TK cells were injected into a gelatin mesh scaffold and cultivated for 3‑20 days. The morphology of the TK cells was investigated by phase‑contrast microscopy, optical microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). TK cells were observed to proliferate three-dimensionally in the scaffold. The cells exhibited a globoid structure and attached to the scaffold. The SEM observation demonstrated typical microvilli and plicae on the surface of the structure. Light microscopy and TEM confirmed intercellular and cell‑to‑scaffold attachment in the three‑dimensional mesh. The culture also exhibited the formation of a duct-like structure covered by structured microvilli. In conclusion, three‑dimensional culture of TK cells demonstrated the morphological characteristics of cholangiocarcinoma in vitro. Production of high levels of carbohydrate antigen (CA)19‑9, CA50 and carcinoembryonic antigen was previously confirmed in the TK cell line. As a characteristic morphology was demonstrated in the present study, the TK cholangiocarcinoma cell line may be useful as an experimental model for further study of cholangiocarcinoma.

Near-ultraviolet micro-Raman study of diamond grown on GaN

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

Nazari, M., E-mail: m-n79@txstate.edu; Hancock, B. L.; Anderson, J.

2016-01-18

Ultraviolet (UV) micro-Raman measurements are reported of diamond grown on GaN using chemical vapor deposition. UV excitation permits simultaneous investigation of the diamond (D) and disordered carbon (DC) comprising the polycrystalline layer. From line scans of a cross-section along the diamond growth direction, the DC component of the diamond layer is found to be highest near the GaN-on-diamond interface and diminish with characteristic length scale of ∼3.5 μm. Transmission electron microscopy (TEM) of the diamond near the interface confirms the presence of DC. Combined micro-Raman and TEM are used to develop an optical method for estimating the DC volume fraction.

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.

To study the effect of dopant NiO concentration and duration of calcinations on structural and optical properties of MgO-NiO nanocomposites

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

Kumar, Rajesh, E-mail: rkkaushik06@gmail.com; Deptt. of Physics,Vaish College of Engineering, Rohtak-124001, Haryana; Praveen,

2016-05-06

In present work Magnesium oxide (MgO) samples were doped with different concentration of Transition metal Nickel Oxide(NiO) by using Chemical co-precipitation method. The doping levels were varied from NiO (5%, 10%, 15%) and all the samples were calcined at 600°C for 4hrs and 8hrs respectively. Structural analysis of these calcined materials is carried out by X-ray diffraction (XRD) techniques which reveals that average crystalline sizes are in nano region i.e. 21.77nm-31.13 nm and tabulated in table 1. The powder of calcined samples were also characterized by using various other techniques i.e. Scanning Electron Microscopy (SEM), Fourier Transformation Infrared Spectroscopy (FTIR), UV-Visiblemore » spectroscopy, Transmission Electron Microscopy (TEM) etc. The effects of dopant concentration, calcined temperature, calcinations duration on samples were studied and also investigate the effect of varying dopant concentration on morphology and optical properties of calcined nanomaterials. From results it was observed that the crystallite size of nanocomposites increases with increases dopant concentration or increases calcinations duration. The optical band gap decreases with increases sintering time and increase with increases dopant concentrations. TEM results coincide with XRD results and show that particles are polycrystalline in nature. FTIR spectra show that for all samples particles are pure in composition and transmission rate increases with calcinations duration.« less

The use of castor oil and ricinoleic acid in lead chalcogenide nanocrystal synthesis

NASA Astrophysics Data System (ADS)

Kyobe, Joseph W. M.; Mubofu, Egid B.; Makame, Yahya M. M.; Mlowe, Sixberth; Revaprasadu, Neerish

2016-08-01

A green solution-based thermolysis method for the synthesis of lead chalcogenide (PbE, E = S, Se, Te) nanocrystals in castor oil (CSTO) and its isolate ricinoleic acid (RA) is described. The blue shift observed from the optical spectra of CSTO and RA-capped PbE nanocrystals (NCs) confirmed the evidence of quantum confinement. The dimensions of PbE NCs obtained from NIR absorption spectra, transmission electron microscopy (TEM), and X-ray diffraction (XRD) studies were in good agreement. The particle sizes estimated were in the range of 20, 25, and 130 nm for castor oil-capped PbS, PbSe, and PbTe, respectively. Well-defined close to cubic-shaped particles were observed in the scanning electron microscopy (SEM) images of PbSe and PbTe nanocrystals. The high-resolution TEM and selective area electron diffraction (SAED) micrographs of the as-synthesized crystalline PbE NCs showed distinct lattice fringes with d-spacing distances corroborating with the standard values reported in literature.

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.

Opto-mechano-electrical tripling in ZnO nanowires probed by photocurrent spectroscopy in a high-resolution transmission electron microscope

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

Zhang, C.; Golberg, D., E-mail: xuzhi@iphy.ac.cn, E-mail: golberg.dmitri@nims.go.jp; Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1, Tsukuba, Ibaraki 3058577

2015-08-31

Photocurrent spectroscopy of individual free-standing ZnO nanowires inside a high-resolution transmission electron microscope (TEM) is reported. By using specially designed optical in situ TEM system capable of scanning tunneling microscopy probing paired with light illumination, opto-mechano-electrical tripling phenomenon in ZnO nanowires is demonstrated. Splitting of photocurrent spectra at around 3.3 eV under in situ TEM bending of ZnO nanowires directly corresponds to nanowire deformation and appearance of expanded and compressed nanowire sides. Theoretical simulation of a bent ZnO nanowire has an excellent agreement with the experimental data. The splitting effect could be explained by a change in the valence band structuremore » of ZnO nanowires due to a lattice strain. The strain-induced splitting provides important clues for future flexible piezo-phototronics.« less

Dependence of the electrical and optical properties on growth interruption in AlAs/In0.53Ga0.47As/InAs resonant tunneling diodes

PubMed Central

2011-01-01

The dependence of interface roughness of pseudomorphic AlAs/In0.53Ga0.47As/InAs resonant tunneling diodes [RTDs] grown by molecular beam epitaxy on interruption time was studied by current-voltage [I-V] characteristics, photoluminescence [PL] spectroscopy, and transmission electron microscopy [TEM]. We have observed that a splitting in the quantum-well PL due to island formation in the quantum well is sensitive to growth interruption at the AlAs/In0.53Ga0.47As interfaces. TEM images also show flatter interfaces with a few islands which only occur by applying an optimum value of interruption time. The symmetry of I-V characteristics of RTDs with PL and TEM results is consistent because tunneling current is highly dependent on barrier thickness and interface roughness. PMID:22112249

Dependence of the electrical and optical properties on growth interruption in AlAs/In0.53Ga0.47As/InAs resonant tunneling diodes.

PubMed

Zhang, Yang; Guan, Min; Liu, Xingfang; Zeng, Yiping

2011-11-23

The dependence of interface roughness of pseudomorphic AlAs/In0.53Ga0.47As/InAs resonant tunneling diodes [RTDs] grown by molecular beam epitaxy on interruption time was studied by current-voltage [I-V] characteristics, photoluminescence [PL] spectroscopy, and transmission electron microscopy [TEM]. We have observed that a splitting in the quantum-well PL due to island formation in the quantum well is sensitive to growth interruption at the AlAs/In0.53Ga0.47As interfaces. TEM images also show flatter interfaces with a few islands which only occur by applying an optimum value of interruption time. The symmetry of I-V characteristics of RTDs with PL and TEM results is consistent because tunneling current is highly dependent on barrier thickness and interface roughness.

Structure, Microsegregation, and Precipitates of an Alloy 690 ESR Ingot in Industrial Scale

NASA Astrophysics Data System (ADS)

Wang, Min; Zha, Xiangdong; Gao, Ming; Ma, Yingche; Liu, Kui; Li, Yiyi

2015-11-01

The structure, interdendritic, and intergranular segregation, and precipitates of an Alloy 690 electro-slag remelting (ESR) ingot in commercial scale (3t) were investigated by the optical microscopy, electroprobe microanalysis, scanning electron microscopy, and transmission electron microscopy (TEM) techniques. The results indicate that the central longitudinal section of the ESR ingot comprised the ramp-up, steady-state, and hot-top regions, which could be easily distinguished from each other through the macrostructures of them. In the interdendritic area, Cr and Ti were enriched, while Ni and Fe were depleted, and the nominal segregation indexes ( ζ i = C 0 i / C interdendritic i ) of Ti, Cr, and Ni were 0.40, 0.91, and 1.04, respectively, in the hot-top region where suffered the severest segregation. Nitrides, principally precipitated between dendrites, were identified as TiN by TEM and EDS. The morphology, size distribution, and volume fraction of them were determined as well. In terms of the intergranular area, Cr and C coexisted, while Ni and Fe were depleted. And the dendrite-like carbides continuously distributed on the interface between grains, which were identified as M23C6 by the selected area diffraction pattern.

Microanalytical study of a ferrous agricultural tool recovered from a historical site in Rio de Janeiro

NASA Astrophysics Data System (ADS)

Campos, G. N.; Solórzano, I. G.

The present work has as its objective a microanalytical study of a metallic archeological artifact using methods of optical microscopy (MO), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The object of the study corresponds to an agricultural tool (a hoe) from the Brazilian colonial period, dating from the late XVIII century, removed from an archeological site (Sítio Rochedo) in excavations conducted by researchers of the Brazilian Archeological Institute. Sample preparation required a meticulous procedure in view of the fragility of the object. The hoe has been suffering the action of oxidation-corrosion over the years, thereby making the impregnation of mineral sediments possible. A detailed metallographic analysis, coupled with spectroscopic SEM and TEM measurements, allows one to conclude that the hoe was made of puddle iron, retaining significant amount of slag. The hoe was probably made by African slaves who had metallurgical knowledge acquired from their ancestors under Portuguese colonization. The equi-axial microstructure of ferrite grains, together with the alignment of slag inclusions, strongly suggest a metal forming procedure conducted on low-carbon puddled iron, followed by heat treatment and then cooling at a slow rate.

New polyurethane nanocomposites based on soya oil.

PubMed

Mohammed, Issam Ahmed; Abd Khadir, Nurul Khizrien; Jaffar Al-Mulla, Emad Abbas

2014-01-01

New polyurethane (PU) nanocomposites were prepared from a dispersion of 0 - 5% montmorillonite (MMT) clay with isocyanate and soya oil polyol that was synthesized via transesterification of triglycerides to reduce petroleum dependence. FT-IR spectra indicate the presence of hydrogen bonding between nanoclay and the polymer matrix, whereas the exfoliated structure of clay layers was confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Optical microscopy, mechanical and thermal analyses were done to investigate significant improvement of the nanocomposites. The results showed PU-3% nanoclay (NC) showed optimum results in mechanical properties such as tensile and flexural strength but the lowest in impact strength.

Fabrication of plasmonic nanopore by using electron beam irradiation for optical bio-sensor

NASA Astrophysics Data System (ADS)

Choi, Seong Soo; Park, Myoung Jin; Han, Chul Hee; Oh, Seh Joong; Park, Nam Kyou; Park, Doo Jae; Choi, Soo Bong; Kim, Yong-Sang

2017-05-01

The Au nano-hole surrounded by the periodic nano-patterns would provide the enhanced optical intensity. Hence, the nano-hole surrounded with periodic groove patterns can be utilized as single molecule nanobio optical sensor device. In this report, the nano-hole on the electron beam induced membrane surrounded by periodic groove patterns were fabricated by focused ion beam technique (FIB), field emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM). Initially, the Au films with three different thickness of 40 nm, 60 nm, and 200 nm were deposited on the SiN film by using an electron beam sputter-deposition technique, followed by removal of the supporting SiN film. The nanopore was formed on the electron beam induced membrane under the FESEM electron beam irradiation. Nanopore formation inside the Au aperture was controlled down to a few nanometer, by electron beam irradiations. The optical intensities from the biomolecules on the surfaces including Au coated pyramid with periodic groove patterns were investigated via surface enhanced Raman spectroscopy (SERS). The fabricated nanopore surrounded by periodic patterns can be utilized as a next generation single molecule bio optical sensor.

Effects of multiple organic ligands on size uniformity and optical properties of ZnSe quantum dots

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

Archana, J., E-mail: archana.jayaram@yahoo.com; Navaneethan, M.; Hayakawa, Y.

2012-08-15

Highlights: ► Highly monodispersed ZnSe quantum dots have been synthesized by wet chemical route. ► Strong quantum confinement effect have been observed in ∼ 4 nm ZnSe quantum dots. ► Enhanced ultraviolet near band emission have been obtained using long chain polymer. -- Abstract: The effects of multi-ligands on the formation and optical transitions of ZnSe quantum dots have been investigated. The dots are synthesized using 3-mercapto-1,2-propanediol and polyvinylpyrrolidone ligands, and have been characterized by X-ray diffraction, transmission electron microscopy (TEM), UV–visible absorption spectroscopy, photoluminescence spectroscopy, and Fourier transform infrared spectroscopy. TEM reveals high monodispersion with an average size ofmore » 4 nm. Polymer-stabilized, organic ligand-passivated ZnSe quantum dots exhibit strong UV emission at 326 nm and strong quantum confinement in the UV–visible absorption spectrum. Uniform size and suppressed surface trap emission are observed when the polymer ligand is used. The possible growth mechanism is discussed.« less

First oxygen from lunar basalt

NASA Technical Reports Server (NTRS)

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

1993-01-01

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

Determination of the size, concentration, and refractive index of silica nanoparticles from turbidity spectra.

PubMed

Khlebtsov, Boris N; Khanadeev, Vitaly A; Khlebtsov, Nikolai G

2008-08-19

The size and concentration of silica cores determine the size and concentration of silica/gold nanoshells in final preparations. Until now, the concentration of silica/gold nanoshells with Stober's silica core has been evaluated through the material balance assumption. Here, we describe a method for simultaneous determination of the average size and concentration of silica nanospheres from turbidity spectra measured within the 400-600 nm spectral band. As the refractive index of silica nanoparticles is the key input parameter for optical determination of their concentration, we propose an optical method and provide experimental data on a direct determination of the refractive index of silica particles n = 1.475 +/- 0.005. Finally, we exemplify our method by determining the particle size and concentration for 10 samples and compare the results with transmission electron microscopy (TEM), atomic force microscopy (AFM), and dynamic light scattering data.

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

PubMed

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

2015-02-25

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

Correlative Light- and Electron Microscopy Using Quantum Dot Nanoparticles.

PubMed

Killingsworth, Murray C; Bobryshev, Yuri V

2016-08-07

A method is described whereby quantum dot (QD) nanoparticles can be used for correlative immunocytochemical studies of human pathology tissue using widefield fluorescence light microscopy and transmission electron microscopy (TEM). To demonstrate the protocol we have immunolabeled ultrathin epoxy sections of human somatostatinoma tumor using a primary antibody to somatostatin, followed by a biotinylated secondary antibody and visualization with streptavidin conjugated 585 nm cadmium-selenium (CdSe) quantum dots (QDs). The sections are mounted on a TEM specimen grid then placed on a glass slide for observation by widefield fluorescence light microscopy. Light microscopy reveals 585 nm QD labeling as bright orange fluorescence forming a granular pattern within the tumor cell cytoplasm. At low to mid-range magnification by light microscopy the labeling pattern can be easily recognized and the level of non-specific or background labeling assessed. This is a critical step for subsequent interpretation of the immunolabeling pattern by TEM and evaluation of the morphological context. The same section is then blotted dry and viewed by TEM. QD probes are seen to be attached to amorphous material contained in individual secretory granules. Images are acquired from the same region of interest (ROI) seen by light microscopy for correlative analysis. Corresponding images from each modality may then be blended to overlay fluorescence data on TEM ultrastructure of the corresponding region.

Self-accommodation of B19' martensite in Ti-Ni shape memory alloys - Part I. Morphological and crystallographic studies of the variant selection rule

NASA Astrophysics Data System (ADS)

Nishida, M.; Nishiura, T.; Kawano, H.; Inamura, T.

2012-06-01

The self-accommodation morphologies of B19‧ martensite in Ti-Ni alloys have been investigated by optical microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Twelve pairs of minimum units consisting of two habit plane variants (HPVs) with V-shaped morphology connected to a ? B19‧ type I variant accommodation twin were observed. Three types of self-accommodation morphologies, based on the V-shaped minimum unit, developed around one of the {111}B2 traces, which were triangular, rhombic and hexangular and consisted of three, four and six HPVs, respectively. In addition, the variant selection rule and the number of possible HPV combinations in each of these self-accommodation morphologies are discussed.

Quantitative characterization of nanoparticle agglomeration within biological media

NASA Astrophysics Data System (ADS)

Hondow, Nicole; Brydson, Rik; Wang, Peiyi; Holton, Mark D.; Brown, M. Rowan; Rees, Paul; Summers, Huw D.; Brown, Andy

2012-07-01

Quantitative analysis of nanoparticle dispersion state within biological media is essential to understanding cellular uptake and the roles of diffusion, sedimentation, and endocytosis in determining nanoparticle dose. The dispersion of polymer-coated CdTe/ZnS quantum dots in water and cell growth medium with and without fetal bovine serum was analyzed by transmission electron microscopy (TEM) and dynamic light scattering (DLS) techniques. Characterization by TEM of samples prepared by plunge freezing the blotted solutions into liquid ethane was sensitive to the dispersion state of the quantum dots and enabled measurement of agglomerate size distributions even in the presence of serum proteins where DLS failed. In addition, TEM showed a reduced packing fraction of quantum dots per agglomerate when dispersed in biological media and serum compared to just water, highlighting the effect of interactions between the media, serum proteins, and the quantum dots. The identification of a heterogeneous distribution of quantum dots and quantum dot agglomerates in cell growth medium and serum by TEM will enable correlation with the previously reported optical metrology of in vitro cellular uptake of this quantum dot dispersion. In this paper, we present a comparative study of TEM and DLS and show that plunge-freeze TEM provides a robust assessment of nanoparticle agglomeration state.

Phase behavior and transitions of self-assembling nano-structured materials

NASA Astrophysics Data System (ADS)

Duan, Hu

Homologous series of supramolecular nanostructures have been investigated by a combination of transmission electron microscopy (TEM), electron diffraction (ED), thermal polarized optical microscopy and X-ray diffraction (XRD). Materials include amphiphilic oligomers and polymer such as charged complexes, dipeptide dendrons semi-fluorinated dendron and polyethyleneimines. Upon microphase separation, they self-assemble into either cylindrical or spherical shapes, which co-organize into a 2D P6mm hexagonal columnar phase or 3D Pm 3¯ n and Im 3¯ m cubic phases. Correlation between the phase selection and molecular architecture is established accordingly. The order-disorder transition (ODT) is explored by rheometry and rheo-optical microscopy in a model polymeric compound poly(N-[3,4-bis(n-dodecan-1-yloxy)benzoyl]ethyleneimine). Shear alignment of the hexagonal columnar liquid crystalline phase along the velocity direction at low temperature and shear disordering in the vicinity of the ODT were observed. After cessation of shear, transformation back to the stable columnar phase follows a row-nucleation mechanism. The order-order transition process is explored in a monodendron that exhibits a hexagonal columnar and a weakly birefringent mesophase. Polarized DIC microscopy strongly supports an epitaxial relationship between them.

Vibrational properties of gold nanoparticles obtained by green synthesis

NASA Astrophysics Data System (ADS)

Alvarez, Ramón A. B.; Cortez-Valadez, M.; Bueno, L. Oscar Neira; Britto Hurtado, R.; Rocha-Rocha, O.; Delgado-Beleño, Y.; Martinez-Nuñez, C. E.; Serrano-Corrales, Luis Ivan; Arizpe-Chávez, H.; Flores-Acosta, M.

2016-10-01

This study reports the synthesis and characterization of gold nanoparticles through an ecological method to obtain nanostructures from the extract of the plant Opuntia ficus-indica. Colloidal nanoparticles show sizes that vary between 10-20 nm, and present various geometric morphologies. The samples were characterized through optical absorption, Raman Spectroscopy and Transmission Electron Microscopy (TEM). Additionally, low energy metallic clusters of Aun (n=2-20 atoms) were modeled by computational quantum chemistry. The theoretical results were obtained with Density Functional Theory (DFT). The predicted results of Au clusters show a tendency and are correlated with the experimental results concerning the optical absorption bands and Raman spectroscopy in gold nanoparticles.

Growth and Characterisation of GaAs/AlGaAs Core-shell Nanowires for Optoelectronic Device Applications

NASA Astrophysics Data System (ADS)

Jiang, Nian

III-V semiconductor nanowires have been investigated as key components for future electronic and optoelectronic devices and systems due to their direct band gap and high electron mobility. Amongst the III-V semiconductors, the planar GaAs material system has been extensively studied and used in industries. Accordingly, GaAs nanowires are the prime candidates for nano-scale devices. However, the electronic performance of GaAs nanowires has yet to match that of state-of-the-art planar GaAs devices. The present deficiency of GaAs nanowires is typically attributed to the large surface-to- volume ratio and the tendency for non-radiative recombination centres to form at the surface. The favoured solution of this problem is by coating GaAs nanowires with AlGaAs shells, which replaces the GaAs surface with GaAs/AlGaAs interface. This thesis presents a systematic study of GaAs/AlGaAs core-shell nanowires grown by metal organic chemical vapour deposition (MOCVD), including understanding the growth, and characterisation of their structural and optical properties. The structures of the nanowires were mainly studied by scanning electron microscopy and transmis- sion electron microscopy (TEM). A procedure of microtomy was developed to prepare the cross-sectional samples for the TEM studies. The optical properties were charac- terised by photoluminescence (PL) spectroscopy. Carrier lifetimes were measured by time-resolved PL. The growth of AlGaAs shell was optimised to obtain the best optical properties, e.g. the strongest PL emission and the longest minority carrier lifetimes. (Abstract shortened by ProQuest.).

Optical properties of template synthesized nanowalled ZnS microtubules

NASA Astrophysics Data System (ADS)

Kumar, Rajesh; Chakarvarti, S. K.

2007-12-01

Electrodeposition is a versatile technique combining low processing cost with ambient conditions that can be used to prepare metallic, polymeric and semiconducting nano/micro structures. In the present work, track-etch membranes (TEMs) of makrofol (KG) have been used as templates for synthesis of ZnS nanowalled microtubules using electrodeposition technique. The morphology of the microtubules was characterized by scanning electron microscopy. Size effects on the band gap of tubules have also been studied by UV-visible spectrophotometer.

Effect of Mo and Ti doping concentration on the structural and optical properties of ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Naz, Hina; Ali, Rai Nauman; Zhu, Xingqun; Xiang, Bin

2018-06-01

In this paper, we report the effect of single phase Mo and Ti doping concentration on the structural and optical properties of the ZnS nanoparticles. The structural and optical properties of the as-synthesized samples have been examined by x-ray diffraction, transmission electron microscopy (TEM), UV-visible near infrared absorption spectroscopy and x-ray photoelectron spectroscopy. TEM characterizations reveal a variation in the doped ZnS nanoparticle size distribution by utilizing different dopants of Mo and Ti. In absorption spectra, a clear red shift of 14 nm is observed with increasing Mo concentration as compared to pure ZnS nanoparticles, while by increasing Ti doping concentration, blue shift of 14 nm is obtained. Moreover, it demonstrates that the value of energy band gap decreases from 4.03 eV to 3.89 eV in case of Mo doping. However, the value of energy band gap have shown a remarkable increase from 4.11 eV to 4.27 eV with increasing Ti doping concentration. Our results provide a new pathway to understand the effect of Mo and Ti doping concentrations on the structural and optical properties of ZnS nanoparticles as it could be the key to tune the properties for future optoelectronic devices.

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

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

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

2015-12-15

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

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

Li, Shuning; Roy, Amitava; Lichtenberg, Henning

The micro-segmented flow technique was applied for continuous synthesis of ZnO micro- and nanoparticles with short residence times of 9.4 s and 21.4 s, respectively. The obtained particles were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Small angle X-ray scattering (SAXS) and photoluminescence spectroscopy were used to determine the size and optical properties of ZnO nanoparticles. In addition, extended X-ray absorption fine structure (EXAFS) spectroscopy was employed to investigate local structural properties. The EXAFS measurements reveal a larger degree of structural disorder in the nanoparticles than the microparticles. These structural changes should be taken into considerationmore » while evaluating the size-dependent visible emission of ZnO nanoparticles.« less

Synthesis of colloidal silver iron oxide nanoparticles--study of their optical and magnetic behavior.

PubMed

Kumar, Anil; Singhal, Aditi

2009-07-22

Silver iron oxide nanoparticles of fairly small size (average diameter approximately 1 nm) with narrow size distribution have been synthesized by the interaction of colloidal beta- Fe2O3 and silver nanoparticles. The surface morphology and size of these particles have been analyzed by using atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Their structural analysis has been carried out by employing x-ray diffraction (XRD), selected-area electron diffraction (SAED), optical and infrared (IR) spectroscopic techniques. The ageing of these particles exhibits the formation of self-assembly, possibly involving weak supramolecular interactions between Ag(I)O4 and Fe(III)O4 species. These particles display the onset of absorption in the near-infrared region and have higher absorption coefficient in the visible range compared to that of its precursors. Magnetic measurements reveal an interesting transition in their magnetic behavior from diamagnetic to superparamagnetic. The magnetic moment of these particles attains a limiting value of about 0.19 emu cm(-2), which is more than two times higher than that of colloidal beta- Fe2O3. With enhanced optical and magnetic properties, this system is suggested to have possible applications in optoelectronic and magnetic devices.

In-situ Isotopic Analysis at Nanoscale using Parallel Ion Electron Spectrometry: A Powerful New Paradigm for Correlative Microscopy

NASA Astrophysics Data System (ADS)

Yedra, Lluís; Eswara, Santhana; Dowsett, David; Wirtz, Tom

2016-06-01

Isotopic analysis is of paramount importance across the entire gamut of scientific research. To advance the frontiers of knowledge, a technique for nanoscale isotopic analysis is indispensable. Secondary Ion Mass Spectrometry (SIMS) is a well-established technique for analyzing isotopes, but its spatial-resolution is fundamentally limited. Transmission Electron Microscopy (TEM) is a well-known method for high-resolution imaging down to the atomic scale. However, isotopic analysis in TEM is not possible. Here, we introduce a powerful new paradigm for in-situ correlative microscopy called the Parallel Ion Electron Spectrometry by synergizing SIMS with TEM. We demonstrate this technique by distinguishing lithium carbonate nanoparticles according to the isotopic label of lithium, viz. 6Li and 7Li and imaging them at high-resolution by TEM, adding a new dimension to correlative microscopy.

Mesoporous CdS via Network of Self-Assembled Nanocrystals: Synthesis, Characterization and Enhanced Photoconducting Property.

PubMed

Patra, Astam K; Banerjee, Biplab; Bhaumik, Asim

2018-01-01

Semiconduction nanoparticles are intensively studied due to their huge potential in optoelctronic applications. Here we report an efficient chemical route for hydrothermal synthesis of aggregated mesoporous cadmium sulfide (CdS) nanoparticles using supramolecular-assembly of ionic and water soluble sodium salicylate as the capping agent. The nanostructure, mesophase, optical property and photoconductivity of these mesoporous CdS materials have been characterized by using small and wide angle powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N2-sorption, Raman analysis, Fourier transformed infrared (FT-IR), UV-Visible DSR spectroscopy, and photoconductivity measurement. Wide angle XRD pattern and high resolution TEM image analysis suggested that the particle size of the materials is within 10 nm and the nanoparticles are in well-crystallized cubic phase. Mesoporous CdS nanoparticles showed drastically enhanced photoelectrochemical response under visible light irradiation on entrapping a photosensitizer (dye) molecule in the interparticle spaces. Efficient synthesis strategy and the enhanced photo response in the mesoporous CdS material could facilitate the designing of other porous semiconductor oxide/sulfide and their applications in photon-to-electron conversion processes.

Microstructure Characterization and Stress Corrosion Evaluation of Autogenous and Hybrid Friction Stir Welded Al-Cu-Li 2195 Alloy

NASA Technical Reports Server (NTRS)

Li, Zhixian; Arbegast, William J.; Meletis, Efstathios I.

1997-01-01

Friction stir welding process is being evaluated for application on the Al-Cu-Li 2195 Super-Light Weight External Tank of the Space Transportation System. In the present investigation Al-Cu-Li 2195 plates were joined by autogenous friction stir welding (FSW) and hybrid FSW (friction stir welding over existing variable polarity plasma arc weld). Optical microscopy and transmission electron microscopy (TEM) were utilized to characterize microstructures of the weldments processed by both welding methods. TEM observations of autogenous FSW coupons in the center section of the dynamically-recrystallized zone showed an equiaxed recrystallized microstructure with an average grain size of approx. 3.8 microns. No T(sub 1), precipitates were present in the above-mentioned zone. Instead, T(sub B) and alpha precipitates were found in this zone with a lower population. Alternate immersion, anodic polarization, constant load, and slow strain tests were carried out to evaluate the general corrosion and stress-corrosion properties of autogenous and hybrid FSW prepared coupons. The experimental results will be discussed.

Synthesis and study of photovoltaic performance on various photoelectrode materials for DSSCs: Optimization of compact layer on nanometer thickness

NASA Astrophysics Data System (ADS)

Surya, Subramanian; Thangamuthu, Rangasamy; Senthil Kumar, Sakkarapalayam Murugesan; Murugadoss, Govindhasamy

2017-02-01

Dye-sensitized solar cells (DSSCs) have gained widespread attention in recent years because of their low production costs, ease of fabrication process and tuneable optical properties, such as colour and transparency. In this work, we explored a strategy wherein nanoparticles of pure TiO2, TiO2sbnd SnO2 nanocomposite, Sn (10%) doped TiO2 and SnO2 synthesized by the simple chemical precipitation method were employed as photoelectrodes to enhance the photovoltaic conversion efficiency of solar cells. The nanoparticles were characterized by different characterization techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM with EDX), transmission electron microscopy (TEM), high resolution electron microscopy (HR-TEM), UV-Visible absorbance (UV-vis), photoluminescence (PL), thermal gravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS) measurements. Moreover, we also demonstrated the effect of thin compact layer in DSSCs by architecture with various precursor materials of different concentrations. We found that the optimized compact layer material TDIP (titanium diisopropoxide) with a concentration of 0.3 M % is produced the highest efficiency of 2.25% for Sn (10%) doped TiO2 electron transport material (ETM) and 4.38% was achieved for pure TiO2 ETM using SnCl2 compact layer with 0.1 M concentrations.

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

NASA Astrophysics Data System (ADS)

Wang, Q.; Li, B.

2017-09-01

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

Improving the Mechanical Properties of Cu-15Ni-8Sn Alloys by Addition of Titanium

PubMed Central

Zhao, Chao; Zhang, Weiwen; Li, Daoxi; Luo, Zongqiang; Yang, Chao; Zhang, Datong

2017-01-01

The effect of Ti addition on the microstructure and mechanical properties of Cu-15Ni-8Sn alloys was investigated. Optical microscopy (OM), scanning electronic microscopy (SEM), and transmission electron microscopy (TEM) were used to determine grain size and distribution of the second phases in the alloys. The results indicate that the tensile properties of Cu-15Ni-8Sn alloys are improved significantly with Ti addition. Tensile elongation increased from 2.7% for the alloy without Ti to 17.9% for the alloy with 0.3% Ti, while tensile strength was maintained and even increased from 935 MPa to 1024 MPa. The improvement of the mechanical properties of Cu-15Ni-8Sn alloys by the addition of Ti is attributed to the grain refinement and suppression of discontinuous precipitation during heat treatment. PMID:28878192

Effect of Boron and Titanium Addition on the Hot Ductility of Low-Carbon Nb-Containing Steel

NASA Astrophysics Data System (ADS)

Liu, Wei-Jian; Li, Jing; Shi, Cheng-Bin; Huo, Xiang-Dong

2015-12-01

The effect of boron and titanium addition on the hot ductility of Nb-containing steel was investigated using hot tensile tests. The fracture surface and the quenched longitudinal microstructure were examined by optical microscopy (OM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results showed that both steel samples had the similar change from 1,100°C to 700°C. The hot ductility of Nb-containing steel with boron and titanium addition was higher than the steel without boron and titanium in the temperature range of 900-750°C. Because the formation of intergranular ferrite was inhibited by solute boron segregating on the grain boundary, the formation of TiN changed the distribution of Nb- and boron-containing precipitates and improved the amount of intragranular ferrite.

Decorating multi-walled carbon nanotubes with quantum dots for construction of multi-color fluorescent nanoprobes.

PubMed

Jia, Nengqin; Lian, Qiong; Tian, Zhong; Duan, Xin; Yin, Min; Jing, Lihong; Chen, Shouhui; Shen, Hebai; Gao, Mingyuan

2010-01-29

Novel multi-color fluorescent nanoprobes were prepared by electrostatically assembling differently sized CdTe quantum dots on polyethylenimine (PEI) functionalized multi-walled carbon nanotubes (MWNTs). The structural and optical properties of the nano-assemblies (MWNTs-PEI-CdTe) were characterized by transmission electron microscopy (TEM), electron diffraction spectra (EDS), Raman spectroscopy, confocal microscopy and photoluminescence spectroscopy (PL), respectively. Electrochemical impedance spectroscopy (EIS) was also applied to investigate the electrostatic assembling among oxidized MWNTs, PEI and CdTe. Furthermore, confocal fluorescence microscopy was used to monitor the nano-assemblies' delivery into tumor cells. It was found that the nano-assemblies exhibit efficient intracellular transporting and strong intracellular tracking. These properties would make this luminescent nano-assembly an excellent building block for the construction of intracellular nanoprobes, which could hold great promise for biomedical applications.

Synthesis, characterization and antibacterial property of ZnO:Mg nanoparticles

NASA Astrophysics Data System (ADS)

Kompany, A.; Madahi, P.; Shahtahmasbi, N.; Mashreghi, M.

2012-09-01

Sol-gel method was successfully used for the synthesis of ZnO nanoparticles (NPs) doped with different concentrations of Mg and the structural, optical and antibacterial properties of the nanoparticles were studied. The synthesized ZnO:Mg powders were characterized using x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transformation Infrared (FTIR) and UV-Vis spectroscopy. It was revealed that the samples have hexagonal Wurtzite structure, and the phase segregation takes place for 15% Mg content. TEM images show that the average size of the particles is about 50 nm. Also, the antibacterial activities of the nanoparticles were tested against Escherichia coli (Gram negative) cultures. ZnO:Mg nanofluid showed good antibacterial activity which increases with the increase of NPs concentration, and decreases slightly with the amount of Mg.

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.

Synthesis and characterization of some metal oxide nanocrystals by microwave irradiation

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

Rashad, M.; Gaber, A.; Abdelrahim, M. A.

2013-12-16

Copper oxide and cobalt oxide (CuO, Co3O4) nanocrystals (NCs) have been successfully prepared in a short time using microwave irradiation. The resulted powders of nanocrystals (NCs) were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Thermogravimetric analysis (TGA) measurements are also studied. Fourier-transform infrared (FT-IR) and UV–visible absorption spectroscopy of both kind of nanoparticels are illustrated. Optical absorption analysis indicated the direct band gap for both kinds of nanocrystals.

Crystalline phase transformation of colloidal cadmium sulfide nanocrystals

NASA Astrophysics Data System (ADS)

Ghali, M.; Eissa, A. M.; Mosaad, M. M.

2017-03-01

In this paper, we give a microscopic view concerning influence of the growth conditions on the physical properties of nanocrystals (NCs) thin films made of CdS, prepared using chemical bath deposition CBD technique. We show a crystalline phase transformation of CdS NCs from hexagonal wurtzite (W) structure to cubic zincblende (ZB) when the growth conditions change, particularly the solution pH values. This effect was confirmed using X-ray diffraction (XRD), transmission electron microscopy (TEM), optical absorption and photoluminescence (PL) measurements. The optical absorption spectra allow calculation of the bandgap value, Eg, where significant increase ˜200 meV in the CdS bandgap when transforming from Hexagonal to Cubic phase was found.

Age related optic nerve axonal loss in adult Brown Norway rats.

PubMed

Cepurna, William O; Kayton, Robert J; Johnson, Elaine C; Morrison, John C

2005-06-01

The effect of age on the number and morphology of optic nerve axons in adult Brown Norway rats (5-31 months old) (n=29) was examined using transmission electron microscopy (TEM). By manually counting every axon in areas representing 60% of the optic nerve cross-section, we found a significant negative correlation between age and axon count (R(2)=0.18, P<0.05). However, when the oldest animals were omitted, the relationship was no longer statistically significant. Simultaneously, the proportion of spontaneously degenerating axons increased at an exponential rate (R(2)=0.79, P<0.05), with significantly more degeneration in the 31-month group than in 5-month-old animals (ANOVA, P<0.05). This study demonstrates, using quantitative TEM methods, that optic nerve axonal numbers are relatively constant throughout the majority of the adult life of the Brown Norway rat, an increasingly popular strain for glaucoma research. Total axonal loss with aging is substantially less than that reported for other strains. The reduction in axonal numbers and the rate of axonal degeneration do not appear significantly altered until the last few months of life, failing to support some studies that have concluded that optic nerve axon loss in adult rats is linear. However, they do agree with other studies in the rat, and a similar study performed in non-human primate eyes, that concluded that aging changes in the optic nerve and retina follow a complex pattern. Therefore, the impact of animal age must be considered when modeling the course and pathophysiology of experimental glaucomatous optic nerve damage in rats.

Transmission electron microscopy of polymer blends and block copolymers

NASA Astrophysics Data System (ADS)

Gomez, Enrique Daniel

Transmission electron microscopy (TEM) of soft matter is a field that warrants further investigation. Developments in sample preparation, imaging and spectroscopic techniques could lead to novel experiments that may further our understanding of the structure and the role structure plays in the functionality of various organic materials. Unlike most hard materials, TEM of organic molecules is limited by the amount of radiation damage the material can withstand without changing its structure. Despite this limitation, TEM has been and will be a powerful tool to study polymeric materials and other soft matter. In this dissertation, an introduction of TEM for polymer scientists is presented. The fundamentals of interactions of electrons with matter are described using the Schrodinger wave equation and scattering cross-sections to fully encompass coherent and incoherent scattering. The intensity, which is the product of the wave function and its complex conjugate, shows no perceptible change due to the sample. Instead, contrast is generated through the optical system of the microscope by removing scattered electrons or by generating interference due to material-induced phase changes. Perhaps the most challenging aspect of taking TEM images, however, is sample preparation, because TEM experiments require materials with approximately 50 nm thickness. Although ultramicrotomy is a well-established powerful tool for preparing biological and polymeric sections for TEM, the development of cryogenic Focused Ion Beam may enable unprecedented cross-sectional TEM studies of polymer thin films on arbitrary substrates with nanometer precision. Two examples of TEM experiments of polymeric materials are presented. The first involves quantifying the composition profile across a lamellar phase obtained in a multicomponent blend of saturated poly(butadiene) and poly(isobutylene), stabilized by a saturated poly(butadiene) copolymer serving as a surfactant, using TEM and self-consistent field theory (SCFT). The liquid-like nature of this system at room temperature makes traditional staining methods for the enhancement of contrast ineffective. As an alternative, we take advantage of the large inelastic scattering cross-section of soft materials to generate contrast in zero-loss TEM images. Independent spatially resolved thickness measurements enable quantification of electron scattering. This enabled a comparison between the TEM data and predictions based on SCFT without any adjustable parameters. The second example involves the utilization of energy-filtered transmission electron microscopy (EFTEM) to compute elemental maps by taking advantage of ionization events. Elemental mapping of lithium is used to determine the distribution of salt in nanostructured poly(styrene-block-ethylene oxide) (SEO) copolymer/lithium salt electrolytes. Surprisingly, the concentration of lithium within a poly(ethylene oxide) (PEO) domain is found to be inhomogeneous; the salt is localized to the middle of the channels. Self-consistent field theory simulations suggest that localization of lithium is due to chain stretching at the interface, which increases with molecular weight. EFTEM and SCFT results show that the segregation of lithium salt to the middle of the PEO lamellae is greater for higher molecular weight polymers. This is correlated with the ionic conductivity of the copolymer electrolyte, which is found to show a higher conductivity for thinner lithium lamellae.

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.

Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

NASA Astrophysics Data System (ADS)

Lin, Chia-Hsuan; Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Moo-Chin; Ko, Horng-Huey

2017-12-01

The synthesis and optical properties of Mg-Al layered double hydroxide (LDH) precursor powders were investigated using X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution TEM (HRTEM), UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363-1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH)2](CO3)0.083.(H2O)0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL) spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

Interface inequivalence of the InP/InAlAs/InP staggered double heterostructure grown by metalorganic chemical vapor deposition

NASA Astrophysics Data System (ADS)

Böhrer, J.; Krost, A.; Heitz, R.; Heinrichsdorff, F.; Eckey, L.; Bimberg, D.; Cerva, H.

1996-02-01

The optical and structural properties of the normal InAlAs on InP and the inverted InP on the InAlAs staggered band lineup interface grown by metalorganic chemical vapor deposition (MOCVD) are compared by use of transmission electron microscopy (TEM), time integrated, and time resolved photoluminescence. TEM images show that both interfaces are dissimilar. The normal interface is very abrupt. The inverted interface shows an additional graded layer of about 2.5 nm in width of In1-xAlxAsyP1-y with x (0.48-0) and y (1.0-0.0). A large optical anisotropy exists because of the inequivalence of the two interfaces. The larger spatial separation of the carriers at the inverted interface is responsible for a smaller overlap of the electron and hole wave functions and for that reason a one order of magnitude longer e-h luminescence decay time of 45 ns is observed. The normal interface transition shifts approximately to the third root of excitation while the inverted interface transition shifts logarithmically.

Structural and Spectroscopic Studies of Sm3+/CdS Nanocrystallites in Sol-Gel TiO2-ZrO2 Matrix

NASA Astrophysics Data System (ADS)

Karthika, S.; Prathibha, Vasudevan; Ann, Mary K. A.; Viji, Vidyadharan; Biju, P. R.; Unnikrishnan, N. V.

2014-02-01

A sol-gel method was used to prepare titania-zirconia matrices doped with Sm3+/CdS nanocrystallites. The structural properties of the matrices were characterized using transmission electron microscopy (TEM), thermogravimetric analysis (TGA), differential thermal analysis (DTA), and Fourier-transform infrared spectroscopy studies. The thermal stability of the material was determined by TGA/DTA analysis. The absorption spectrum shows the characteristic peaks of the Sm3+ ions and the absorption peak corresponding to the CdS nanocrystallites. The optical bandgap and size of the CdS nanoparticles were calculated from the absorption spectrum. From TEM, the interplanar distance ( d) was estimated to be 3.533 Å, which matches with the (1 0 0) plane of bulk CdS. The measurements yield a nanocrystallite size of around 7.8 nm. The optical absorption and emission spectra confirmed the formation of CdS nanoparticles along with samarium ions in the titania-zirconia matrices. The fluorescence intensity of the samarium ions was found to be greatly enhanced by codoping with CdS nanocrystallites.

Physiochemical and optical properties of chitosan based graphene oxide bionanocomposite.

PubMed

Kumar, Santosh; Koh, Joonseok

2014-09-01

In the present investigation an ecofriendly approach and a simple homogeneous solution casting method led to the development of biodegradable chitosan/graphene oxide bionanocomposites. The formation of bionanocomposite was confirmed by UV-vis, FT-IR, Raman spectroscopy, XRD, and further evaluated by thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The circular dichroism (CD) study of chitosan/graphene oxide revealed that the intensity of the negative transition band at wavelength of 200-222 nm decreased with the different pH of chitosan/graphene oxide solutions. It was also found that the pH conditions affect the interaction between chitosan and graphene oxide. Optical properties of chitosan/graphene oxide are evaluated by photoluminescence (PL) spectroscopy which showed blue shift at excitation wavelength of 255 nm compared to graphene oxide. These results strongly suggest that the bionanocomposite materials may open new vistas in biotechnological, biosensor and biomedical applications. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Determination and identification of titanium dioxide nanoparticles in confectionery foods, marketed in South Korea, using inductively coupled plasma optical emission spectrometry and transmission electron microscopy.

PubMed

Kim, Namhoon; Kim, Changkyu; Jung, Soyoung; Park, Youngae; Lee, Youngju; Jo, Juyeon; Hong, Misun; Lee, Sangmi; Oh, Younghee; Jung, Kweon

2018-06-18

Food-grade titanium dioxide (TiO 2 ) is a common and widespread food additive in many processed foods, personal care products, and other industrial categories as it boosts the brightness and whiteness of colours. Although it is generally recognised as safe for humans, there is a growing interest in the health risks associated with its oral intake. This study quantified and identified TiO 2 nanoparticles present in confectionery foods, which are children's favourite foods, with inductively coupled plasma optical emission spectrometry (ICP-OES) and transmission electron microscopy (TEM). A reliable digestion method using hot sulphuric acid and a digestion catalyst (K 2 SO 4 :CuSO 4  = 9:1) was suggested for titanium analysis. Validations of the experimental method were quite acceptable in terms of linearity, recoveries, detection limits, and quantification limits. Of all the 88 analysed foods, TiO 2 was detected in 19 products, all except three declared TiO 2 in their labelling. The mean TiO 2 content of candies, chewing gums, and chocolates were 0.36 mg g -1 , 0.04 mg g -1 , and 0.81 mg g -1 , respectively. Whitish particles isolated from the confectionery foods were confirmed as TiO 2 nanoparticles via TEM and energy dispersive X-ray spectroscopy (EDX), in which nanosized particles (<100 nm) were identified.

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

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

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

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

Synthesis of SiC nanoparticles by SHG 532 nm Nd:YAG laser ablation of silicon in ethanol

NASA Astrophysics Data System (ADS)

Khashan, Khawla S.; Ismail, Raid A.; Mahdi, Rana O.

2018-06-01

In this work, colloidal spherical nanoparticles NPs of silicon carbide SiC have been synthesized using second harmonic generation 532 nm Nd:YAG laser ablation of silicon target dipped in ethanol solution at various laser fluences (1.5-5) J/cm2. X-Ray diffraction XRD, scanning electron microscopy SEM, transmission electron microscope TEM, Fourier transformed infrared spectroscopy FT-IR, Raman spectroscopy, photoluminescence PL spectroscopy, and UV-Vis absorption were employed to examine the structural, chemical and optical properties of SiC NPs. XRD results showed that all synthesised SiC nanoparticles are crystalline in nature and have hexagonal structure with preferred orientation along (103) plane. Raman investigation showed three characteristic peaks 764,786 and 954 cm-1, which are indexing to transverse optic TO phonon mode and longitudinal optic LO phonon mode of 4H-SiC structure. The optical absorption data showed that the values of optical energy gap of SiC nanoparticles prepared at 1.5 J/cm2 was 3.6 eV and was 3.85 eV for SiC synthesised at 5 J/cm2. SEM investigations confirmed that the nanoparticles synthesised at 5 J/cm2 are agglomerated to form larger particles. TEM measurements showed that SiC particles prepared at 1.5 J/cm2 have spherical shape with average size of 25 nm, while the particles prepared at 5 J/cm2 have an average size of 55 nm.

Structural, optical and dielectric investigation of CdFe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Sagadevan, Suresh; Pal, Kaushik; Zaman Chowdhury, Zaira; Enamul Hoque, Md

2017-07-01

A simple thermal decomposition technique has been executed for the synthesis of cadmium ferrite (CdFe2O4) nanoparticles. With the help of x-ray diffraction; scanning electron microscopy, energy-dispersive x-ray spectroscopy (EDS) and Fourier transform infrared spectroscopy the prepared nanoparticles were identified. The crystal size of the average particles aggregated and was found approximately to be 10-14 nm by means of XRD studies. However, the results of high-resolution transmission electron microscopy (HR-TEM) investigation ensured distinguished nanoparticles, and also the polycrystalline nature of those nanoparticles was confirmed by selected area diffraction (SAED) patterns. The scanning electron microscopy (SEM) images explored a random distribution of grains within the sample. Thin film surface topology of roughness and surface current measurement were studied by atomic force microscopy (TP-AFM, C-AFM). Hence, from the ultraviolet-visible (UV) spectroscopic absorption illustrated significant optical properties. Moreover, the optical energy band gap (E g) of CdFe2O4 nanoparticle was determined to be 1.74 eV. By studying the variation of dielectric constant and dielectric loss with respect to frequency, the CdFe2O4 nanoparticles electrical properties were analyzed. Analysis in the real and imaginary part of impedance explained their frequency and temperature dependence of the CdFe2O4 nanoparticles. The traditional solution-phase organometallic approach provides an effective way to synthesize high quality hydrophobic semiconductor-CdFe2O4 nanoparticles. Our simple, cost-effective approach is quite general, which is applicable to other nanomaterials, and it utilizes the currently mature in Nano-chemistry. The nanocomposite assemblies’ exhibit strong anisotropic optical and electrical properties are open up new possibilities in remarkable applications for optoelectronics in the near future.

Fabrication of Al/Mg/Al Composites via Accumulative Roll Bonding and Their Mechanical Properties

PubMed Central

Nie, Jinfeng; Liu, Mingxing; Wang, Fang; Zhao, Yonghao; Li, Yusheng; Cao, Yang; Zhu, Yuntian

2016-01-01

Al(1060)/Mg(AZ31)/Al(1060) multilayered composite was successfully produced using an accumulative roll bonding (ARB) process for up to four cycles at an elevated temperature (400 °C). The microstructure evolution of the composites and the bonding characteristics at the interfaces between Al and Mg layers with increasing ARB cycles were characterized through optical microscopy, field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). It was found that the grains of Al and Mg layers were significantly refined and Al3Mg2 and Al12 Mg17 intermetallic compound layers formed at the Al/Mg bonding interfaces. The strength increased gradually and the ultimate tensile strength (UTS) reached a maximum value of about 240 MPa at the third pass. Furthermore, the strengthening mechanism of the composite was analyzed based on the fracture morphologies. PMID:28774072

Synthesis, structural and optical properties of nanocrystalline vanadium doped zinc oxide aerogel

NASA Astrophysics Data System (ADS)

El Ghoul, J.; Barthou, C.; El Mir, L.

2012-06-01

We report the synthesis of vanadium-doped ZnO nanoparticles prepared by a sol-gel processing technique. In our approach, the water for hydrolysis was slowly released by esterification reaction followed by a supercritical drying in ethyl alcohol. Vanadium doping concentration of 10 at% has been investigated. After treatment in air at different temperatures, the obtained nanopowder was characterized by various techniques such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence (PL). Analysis by scanning electron microscopy at high resolution shows that the grain size increases with increasing temperature. Thus, in the case of thermal treatment at 500 °C in air, the powder with an average particle size of 25 nm shows a strong luminescence band in the visible range. The intensity and energy position of the obtained PL band depends on the temperature measurement increase. The mechanism of this emission band is discussed.

Attaching quantum dots to HER2 specific phage antibodies

NASA Astrophysics Data System (ADS)

Chu, Viet Ha; Nghiem, Thi Ha Lien; Huyen La, Thi; Dieu Thuy Ung, Thi; Huan Le, Quang; Thuan Tong, Kim; Liem Nguyen, Quang; Nhung Tran, Hong

2010-06-01

This work presents the results of the attachment of Qdot 655 ITKTM amino (PEG) quantum dots (QDs) (Invitrogen) and CdTe QDs (provided by Institute of Materials Science, VAST) to HER2 (Human Epidermal growth factor Receptor 2) specific phage antibodies (Abs) (provided by Institute of Biotechnology, VAST) in solution. The QDs were attached to the phage display specific HER2 Abs to form a complex QD-Ab. The QDs and complex QD-Ab were characterized by UV-VIS spectroscopy, transmission electron microscopy (TEM) and fluorescence microscopy. The fluorescence images show the QDs conjugated to the phage. Due to the QDs attaching to the surface, the phage dimensions were amplified, so its shape could be observed by optical microscopy. The complex QD-Ab was stable and lasted for a month. The results illustrate the value of the HER2 phage-QD complex as a cancer detection platform.

The Effect of Homogenization on the Corrosion Behavior of Al-Mg Alloy

NASA Astrophysics Data System (ADS)

Li, Yin; Hung, Yuanchun; Du, Zhiyong; Xiao, Zhengbing; Jia, Guangze

2018-04-01

The effect of homogenization on the corrosion behavior of 5083-O aluminum alloy is presented in this paper. The intergranular corrosion and exfoliation corrosion were used to characterize the discussed corrosion behavior of 5083-O aluminum alloy. The variations in the morphology, the kind and distribution of the precipitates, and the dislocation configurations in the samples after the homogenization were evaluated using optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The effects of the highly active grain boundary character distribution and the types of constituent particles on the corrosion are discussed on the basis of experimental observations. The results indicated that the corrosion behavior of 5083-O alloy was closely related to the microstructure obtained by the heat treatment. Homogenization carried out after casting had the optimal effect on the overall corrosion resistance of the material. Nevertheless, all samples could satisfy the requirements of corrosion resistance in marine applications.

Structural, optical, electrochemical and photovoltaic studies of spider web like Silver Indium Diselenide Quantum dots synthesized by ligand mediated colloidal sol-gel approach

NASA Astrophysics Data System (ADS)

Adhikari, Tham; Pathak, Dinesh; Wagner, Tomas; Jambor, Roman; Jabeen, Uzma; Aamir, Muhammad; Nunzi, Jean-Michel

2017-11-01

Silver indium diselenide quantum dots were successively synthesized by colloidal sol-gel method by chelating with organic ligand oleylamine (OLA). The particle size was studied by transmission electron microscopy (TEM) and the size was found about 10 nm. X-ray diffraction (XRD) was used to study crystalline structure of the nanocrystals. The grain size and morphology were further studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The elemental composition was studied by X-ray photon electron spectroscopy (XPS) and energy dispersive x-ray spectroscopy (EDAX). The capping property of OLA in nanocrystal was also demonstrated by Fourier Transform Infrared spectroscopy (FTIR). The band gap was calculated from both cyclic voltammetry and optical absorption and suggest quantum confinement. The solution processed bilayer thin film solar cells were fabricated with n-type Zinc oxide using doctor blading/spin coating method and their photovoltaic performance was studied. The best device sintered at 450 °C showed an efficiency 0.75% with current density of 4.54 mAcm-2, open-circuit voltage 0.44 V and fill factor 39.4%.

Fabrication of PbS quantum dots and their applications in solar cells based on ZnO nanorod arrays

NASA Astrophysics Data System (ADS)

Kumar, Dinesh; Chaudhary, Sujeet; Pandya, Dinesh K.

2018-05-01

An efficient, inexpensive and large area scalable approach based on sol-gel technique is presented to fabricate quantum dots (QDs) of PbS. Size of the QDs is tuned by the varying the bath concentrations in the range of 50-200 mM. Transmission electron microscopy (TEM) studies confirm the growth of spherically shaped ˜5.6 nm QDs at 50 mM bath concentration. The optical bandgap of the QDs is found to be ˜0.9 eV and corresponds to the size obtained from TEM studies. ZnO/PbS solar cells are fabricated by sensitizing the ZnO nanorods with PbS QDs. The fabricated solar cells demonstrate the highest open circuit voltage ˜200 mV and short circuit current density ˜0.81 µA/cm2.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Micro-CT scouting for transmission electron microscopy of human tissue specimens

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

Morales, A. G.; Stempinski, E. S.; XIAO, X.

Transmission electron microscopy (TEM) provides sub-nanometre-scale details in volumetric samples. Samples such as pathology tissue specimens are often stained with a metal element to enhance contrast, which makes them opaque to optical microscopes. As a result, it can be a lengthy procedure to find the region of interest inside a sample through sectioning. Here, we describe micro-CT scouting for TEM that allows noninvasive identification of regions of interest within a block sample to guide the sectioning step. In a tissue pathology study, a bench-top micro-CT scanner with 10 m resolution was used to determine the location of patches of themore » mucous membrane in osmium-stained human nasal scraping samples. Furthermore, once the regions of interest were located, the sample block was sectioned to expose that location, followed by ultra-thin sectioning and TEM to inspect the internal structure of the cilia of the membrane epithelial cells with nanometre resolution. This method substantially reduced the time and labour of the search process from typically 20 sections for light microscopy to three sections with no added sample preparation. Lay description Electron microscopy provides very high levels of detail in a small area, and thus the question of where to look in an opaque sample, such as a stained tissue specimen, needs to be answered by sectioning the sample in small steps and examining the sections under a light microscope, until the region of interest is found. The search process can be lengthy and labor intensive, especially for a study involving a large number of samples. Small areas of interest can be missed in the process if not enough regions are examined. We also describe a method to directly locate the region of interest within a whole sample using micro-CT imaging, bypassing the need of blindly sectioning. Micro-CT enables locating the region within 3D space; this information provides a guide for sectioning the sample to expose that precise location for high resolution electron microscopy imaging. In a human tissue specimen study, this method considerably reduced the time and labor of the search process.« less

Micro-CT scouting for transmission electron microscopy of human tissue specimens

DOE PAGES

Morales, A. G.; Stempinski, E. S.; XIAO, X.; ...

2016-02-08

Transmission electron microscopy (TEM) provides sub-nanometre-scale details in volumetric samples. Samples such as pathology tissue specimens are often stained with a metal element to enhance contrast, which makes them opaque to optical microscopes. As a result, it can be a lengthy procedure to find the region of interest inside a sample through sectioning. Here, we describe micro-CT scouting for TEM that allows noninvasive identification of regions of interest within a block sample to guide the sectioning step. In a tissue pathology study, a bench-top micro-CT scanner with 10 m resolution was used to determine the location of patches of themore » mucous membrane in osmium-stained human nasal scraping samples. Furthermore, once the regions of interest were located, the sample block was sectioned to expose that location, followed by ultra-thin sectioning and TEM to inspect the internal structure of the cilia of the membrane epithelial cells with nanometre resolution. This method substantially reduced the time and labour of the search process from typically 20 sections for light microscopy to three sections with no added sample preparation. Lay description Electron microscopy provides very high levels of detail in a small area, and thus the question of where to look in an opaque sample, such as a stained tissue specimen, needs to be answered by sectioning the sample in small steps and examining the sections under a light microscope, until the region of interest is found. The search process can be lengthy and labor intensive, especially for a study involving a large number of samples. Small areas of interest can be missed in the process if not enough regions are examined. We also describe a method to directly locate the region of interest within a whole sample using micro-CT imaging, bypassing the need of blindly sectioning. Micro-CT enables locating the region within 3D space; this information provides a guide for sectioning the sample to expose that precise location for high resolution electron microscopy imaging. In a human tissue specimen study, this method considerably reduced the time and labor of the search process.« less

Chemically functionalized ZnS quantum dots as new optical nanosensor of herbicides

NASA Astrophysics Data System (ADS)

Masteri-Farahani, M.; Mahdavi, S.; Khanmohammadi, H.

2018-03-01

Surface chemical functionalization of ZnS quantum dots (ZnS-QDs) with cysteamine hydrochloride resulted in the preparation of an optical nanosensor for detection of herbicides. Characterization of the functionalized ZnS-QDs was performed with physicochemical methods such as x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive x-ray (EDX) analysis, ultraviolet-visible (UV–vis) and photoluminescence (PL) spectroscopies. The optical band gap of the functionalized ZnS-QDs was determined by using Tauc plot as 4.1 eV. Addition of various herbicides resulted in the linearly fluorescence quenching of the functionalized ZnS-QDs according to the Stern-Volmer equation. The functionalized ZnS-QDs can be used as simple, rapid, and inexpensive nanosensor for practical detection and measurement of various herbicides.

Local sample thickness determination via scanning transmission electron microscopy defocus series.

PubMed

Beyer, A; Straubinger, R; Belz, J; Volz, K

2016-05-01

The usable aperture sizes in (scanning) transmission electron microscopy ((S)TEM) have significantly increased in the past decade due to the introduction of aberration correction. In parallel with the consequent increase of convergence angle the depth of focus has decreased severely and optical sectioning in the STEM became feasible. Here we apply STEM defocus series to derive the local sample thickness of a TEM sample. To this end experimental as well as simulated defocus series of thin Si foils were acquired. The systematic blurring of high resolution high angle annular dark field images is quantified by evaluating the standard deviation of the image intensity for each image of a defocus series. The derived dependencies exhibit a pronounced maximum at the optimum defocus and drop to a background value for higher or lower values. The full width half maximum (FWHM) of the curve is equal to the sample thickness above a minimum thickness given by the size of the used aperture and the chromatic aberration of the microscope. The thicknesses obtained from experimental defocus series applying the proposed method are in good agreement with the values derived from other established methods. The key advantages of this method compared to others are its high spatial resolution and that it does not involve any time consuming simulations. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

The potentials and challenges of electron microscopy in the study of atomic chains

NASA Astrophysics Data System (ADS)

Banhart, Florian; Torre, Alessandro La; Romdhane, Ferdaous Ben; Cretu, Ovidiu

2017-04-01

The article is a brief review on the potential of transmission electron microscopy (TEM) in the investigation of atom chains which are the paradigm of a strictly one-dimensional material. After the progress of TEM in the study of new two-dimensional materials, microscopy of free-standing one-dimensional structures is a new challenge with its inherent potentials and difficulties. In-situ experiments in the TEM allowed, for the first time, to generate isolated atomic chains consisting of metals, carbon or boron nitride. Besides having delivered a solid proof for the existence of atomic chains, in-situ TEM studies also enabled us to measure the electrical properties of these fundamental linear structures. While ballistic quantum conductivity is observed in chains of metal atoms, electrical transport in chains of sp1-hybridized carbon is limited by resonant states and reflections at the contacts. Although substantial progress has been made in recent TEM studies of atom chains, fundamental questions have to be answered, concerning the structural stability of the chains, bonding states at the contacts, and the suitability for applications in nanotechnology. Contribution to the topical issue "The 16th European Microscopy Congress (EMC 2016)", edited by Richard Brydson and Pascale Bayle-Guillemaud

Polarized Light Microscopy

NASA Technical Reports Server (NTRS)

Frandsen, Athela F.

2016-01-01

Polarized light microscopy (PLM) is a technique which employs the use of polarizing filters to obtain substantial optical property information about the material which is being observed. This information can be combined with other microscopy techniques to confirm or elucidate the identity of an unknown material, determine whether a particular contaminant is present (as with asbestos analysis), or to provide important information that can be used to refine a manufacturing or chemical process. PLM was the major microscopy technique in use for identification of materials for nearly a century since its introduction in 1834 by William Fox Talbot, as other techniques such as SEM (Scanning Electron Microscopy), FTIR (Fourier Transform Infrared spectroscopy), XPD (X-ray Powder Diffraction), and TEM (Transmission Electron Microscopy) had not yet been developed. Today, it is still the only technique approved by the Environmental Protection Agency (EPA) for asbestos analysis, and is often the technique first applied for identification of unknown materials. PLM uses different configurations in order to determine different material properties. With each configuration additional clues can be gathered, leading to a conclusion of material identity. With no polarizing filter, the microscope can be used just as a stereo optical microscope, and view qualities such as morphology, size, and number of phases. With a single polarizing filter (single polars), additional properties can be established, such as pleochroism, individual refractive indices, and dispersion staining. With two polarizing filters (crossed polars), even more can be deduced: isotropy vs. anisotropy, extinction angle, birefringence/degree of birefringence, sign of elongation, and anomalous polarization colors, among others. With the use of PLM many of these properties can be determined in a matter of seconds, even for those who are not highly trained. McCrone, a leader in the field of polarized light microscopy, often advised, If you cant determine a specific optical property of a particle after two minutes, move onto another configuration. Since optical properties can be seen so very quickly and easily under polarized light, it is only necessary to spend a maximum of two minutes on a technique to determine a particular property, though often only a few seconds are required.

Advantages and Disadvantages of using a Focused Ion Beam to Prepare TEM Samples From Irradiated U-10Mo Monolithic Nuclear Fuel

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

B. D. Miller; J. Gan; J. Madden

2012-05-01

Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and focused ion beam (FIB) milling were performed on an irradiated U-10Mo monolithic fuel to understand its irradiation microstructure. This is the first reported TEM work of irradiated fuel sample prepared using a FIB. Advantages and disadvantages of using the FIB to create TEM samples from this irradiated fuel will be presented along with some results from the work. Sample preparation techniques used to create SEM and FIB samples from the brittle irradiated monolithic sample will also be discussed.

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

One-step growth of nanosheet-assembled BiOCl/BiOBr microspheres for highly efficient visible photocatalytic performance

NASA Astrophysics Data System (ADS)

Zhang, Jinfeng; Lv, Jiali; Dai, Kai; Liang, Changhao; Liu, Qi

2018-02-01

In this work, we have developed a simple synthetic approach of nanosheet-assembled BiOCl/BiOBr microspheres by an ethylene glycol (EG)-assisted hydrothermal method. The crystalline form, morphology, chemical composition, optical performance and surface area of BiOCl/BiOBr microspheres were identified using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution TEM (HRTEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy spectra (EDX), UV-vis diffuse reflectance spectroscopy (DRS) analysis, high resolution X-ray photoelectron spectra (XPS) and N2 adsorption-desorption isotherms. BiOCl/BiOBr microspheres were nanosheet-assembled particles, which possessed visible light absorption under LED light irridation. Additionally, the methylene blue (MB) photodegradation performance of different BiOCl/BiOBr microspheres irradiated under 410 nm LED light arrays were investigated, the results exhibited that as-prepared BiOCl/BiOBr products showed higher catalytic effiency than pure BiOCl or BiOBr. By optimizing the composition ration of the BiOCl and BiOBr, up to 93% degradation rate can be obtained in the 40%BiOCl/BiOBr microspheres. Finally, the photocatalytic mechanism of BiOCl/BiOBr microspheres had been proposed.

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

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

Hojamberdiev, Mirabbos, E-mail: mirabbos_uz@yahoo.com; Zhu, Gangqiang; Xu, Yunhua

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

Quantitative analysis of nanoscale intranuclear structural alterations in hippocampal cells in chronic alcoholism via transmission electron microscopy imaging.

PubMed

Sahay, Peeyush; Shukla, Pradeep K; Ghimire, Hemendra M; Almabadi, Huda M; Tripathi, Vibha; Mohanty, Samarendra K; Rao, Radhakrishna; Pradhan, Prabhakar

2017-03-01

Chronic alcoholism is known to alter the morphology of the hippocampus, an important region of cognitive function in the brain. Therefore, to understand the effect of chronic alcoholism on hippocampal neural cells, we employed a mouse model of chronic alcoholism and quantified intranuclear nanoscale structural alterations in these cells. Transmission electron microscopy (TEM) images of hippocampal neurons were obtained, and the degree of structural alteration in terms of mass density fluctuation was determined using the light-localization properties of optical media generated from TEM imaging. The results, which were obtained at length scales ranging from ~30 to 200 nm, show that 10-12 week-old mice fed a Lieber-DeCarli liquid (alcoholic) diet had a higher degree of structural alteration than control mice fed a normal diet without alcohol. The degree of structural alteration became significantly distinguishable at a sample length of ~100 nm, which is the typical length scale of the building blocks of cells, such as DNA, RNA, proteins and lipids. Interestingly, different degrees of structural alteration at such length scales suggest possible structural rearrangement of chromatin inside the nuclei in chronic alcoholism.

Quantitative analysis of nanoscale intranuclear structural alterations in hippocampal cells in chronic alcoholism via transmission electron microscopy imaging

NASA Astrophysics Data System (ADS)

Sahay, Peeyush; Shukla, Pradeep K.; Ghimire, Hemendra M.; Almabadi, Huda M.; Tripathi, Vibha; Mohanty, Samarendra K.; Rao, Radhakrishna; Pradhan, Prabhakar

2017-04-01

Chronic alcoholism is known to alter the morphology of the hippocampus, an important region of cognitive function in the brain. Therefore, to understand the effect of chronic alcoholism on hippocampal neural cells, we employed a mouse model of chronic alcoholism and quantified intranuclear nanoscale structural alterations in these cells. Transmission electron microscopy (TEM) images of hippocampal neurons were obtained, and the degree of structural alteration in terms of mass density fluctuation was determined using the light-localization properties of optical media generated from TEM imaging. The results, which were obtained at length scales ranging from ~30 to 200 nm, show that 10-12 week-old mice fed a Lieber-DeCarli liquid (alcoholic) diet had a higher degree of structural alteration than control mice fed a normal diet without alcohol. The degree of structural alteration became significantly distinguishable at a sample length of ~100 nm, which is the typical length scale of the building blocks of cells, such as DNA, RNA, proteins and lipids. Interestingly, different degrees of structural alteration at such length scales suggest possible structural rearrangement of chromatin inside the nuclei in chronic alcoholism.

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.

Stacking fault related luminescence in GaN nanorods.

PubMed

Forsberg, M; Serban, A; Poenaru, I; Hsiao, C-L; Junaid, M; Birch, J; Pozina, G

2015-09-04

Optical and structural properties are presented for GaN nanorods (NRs) grown in the [0001] direction on Si(111) substrates by direct-current reactive magnetron sputter epitaxy. Transmission electron microscopy (TEM) reveals clusters of dense stacking faults (SFs) regularly distributed along the c-axis. A strong emission line at ∼3.42 eV associated with the basal-plane SFs has been observed in luminescence spectra. The optical signature of SFs is stable up to room temperatures with the activation energy of ∼20 meV. Temperature-dependent time-resolved photoluminescence properties suggest that the recombination mechanism of the 3.42 eV emission can be understood in terms of multiple quantum wells self-organized along the growth axis of NRs.

Chromatic Aberration Correction for Atomic Resolution TEM Imaging from 20 to 80 kV.

PubMed

Linck, Martin; Hartel, Peter; Uhlemann, Stephan; Kahl, Frank; Müller, Heiko; Zach, Joachim; Haider, Max; Niestadt, Marcel; Bischoff, Maarten; Biskupek, Johannes; Lee, Zhongbo; Lehnert, Tibor; Börrnert, Felix; Rose, Harald; Kaiser, Ute

2016-08-12

Atomic resolution in transmission electron microscopy of thin and light-atom materials requires a rigorous reduction of the beam energy to reduce knockon damage. However, at the same time, the chromatic aberration deteriorates the resolution of the TEM image dramatically. Within the framework of the SALVE project, we introduce a newly developed C_{c}/C_{s} corrector that is capable of correcting both the chromatic and the spherical aberration in the range of accelerating voltages from 20 to 80 kV. The corrector allows correcting axial aberrations up to fifth order as well as the dominating off-axial aberrations. Over the entire voltage range, optimum phase-contrast imaging conditions for weak signals from light atoms can be adjusted for an optical aperture of at least 55 mrad. The information transfer within this aperture is no longer limited by chromatic aberrations. We demonstrate the performance of the microscope using the examples of 30 kV phase-contrast TEM images of graphene and molybdenum disulfide, showing unprecedented contrast and resolution that matches image calculations.

Advanced electron microscopy characterization of nanomaterials for catalysis

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

Su, Dong

Transmission electron microscopy (TEM) has become one of the most powerful techniques in the fields of material science, inorganic chemistry and nanotechnology. In terms of resolutions, advanced TEM may reach a high spatial resolution of 0.05 nm, a high energy-resolution of 7 meV. In addition, in situ TEM can help researcher to image the process happened within 1 ms. This paper reviews the recent technical approaches of applying advanced TEM characterization on nanomaterials for catalysis. The text is organized according to the demanded information of nanocrystals from the perspective of application: for example, size, composition, phase, strain, and morphology. Themore » electron beam induced effect and in situ TEM are also introduced. As a result, I hope this review can help the scientists in related fields to take advantage of advanced TEM to their own researches.« less

Advanced electron microscopy characterization of nanomaterials for catalysis

DOE PAGES

Su, Dong

2017-04-01

Transmission electron microscopy (TEM) has become one of the most powerful techniques in the fields of material science, inorganic chemistry and nanotechnology. In terms of resolutions, advanced TEM may reach a high spatial resolution of 0.05 nm, a high energy-resolution of 7 meV. In addition, in situ TEM can help researcher to image the process happened within 1 ms. This paper reviews the recent technical approaches of applying advanced TEM characterization on nanomaterials for catalysis. The text is organized according to the demanded information of nanocrystals from the perspective of application: for example, size, composition, phase, strain, and morphology. Themore » electron beam induced effect and in situ TEM are also introduced. As a result, I hope this review can help the scientists in related fields to take advantage of advanced TEM to their own researches.« less

Stacking InAs quantum dots over ErAs semimetal nanoparticles on GaAs (0 0 1) using molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Zhang, Yuanchang; Eyink, Kurt G.; Grazulis, Lawrence; Hill, Madelyn; Peoples, Joseph; Mahalingam, Krishnamurthy

2017-11-01

Hybrid nanostructures are known to elicit an enhanced optical response. We study the directed alignment of ErAs metal nanoparticle (NP) and InAs quantum dot (QD) using molecular beam eptaxy (MBE) in a GaAs matrix. Due to high surface free energy caused by the crystal structure difference, overgrowth of an ErAs NP with GaAs forms a depression that condenses subsequent InAs adatoms to form an inverted QD self-aligned to the underlying ErAs NP. The ErAs NP growth, GaAs overgrowth, and InAs QD deposition were carefully controlled and studied with transmission electron microscopy (TEM) and atomic force microscopy (AFM) to investigate their effects on the QD-NP alignment.

Research on the Microstructures and Mechanical Properties of Ti Micro-Alloyed Cold Rolled Hot-Dip Galvanizing DP980 Steel

NASA Astrophysics Data System (ADS)

Han, Yun; Kuang, Shuang; Qi, Xiumei; Xie, Chunqian; Liu, Guanghui

Effects of galvanizing simulation parameters on microstructures and mechanical properties of Ti-microalloyed cold rolled hot-dip galvanizing DP980 steel were investigated in this study by optical microscopy (OM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) and tensile test. Moreover, the precipitation behavior of Ti in the experimental steel was also studied. The results show that, as the heating temperature increases, the tensile strength of experimental galvanizing DP980 steel decreases while the yield ratio and elongation of the steel are enhanced. The microstructures of experimental steels exhibit typical dual phase steel character and the volume fractions of MA islands are almost 30%. In addition, lots of nano-sized TiC precipitates can be found in the ferrite grains.

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

PubMed

Tanwar, Shivani; Ho, Ja-an Annie

2015-10-13

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

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

DOE PAGES

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

2017-03-09

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

Secretory glands and microvascular systems imaged in aqueous solution by atmospheric scanning electron microscopy (ASEM).

PubMed

Yamazawa, Toshiko; Nakamura, Naotoshi; Sato, Mari; Sato, Chikara

2016-12-01

Exocrine glands, e.g., salivary and pancreatic glands, play an important role in digestive enzyme secretion, while endocrine glands, e.g., pancreatic islets, secrete hormones that regulate blood glucose levels. The dysfunction of these secretory organs immediately leads to various diseases, such as diabetes or Sjögren's syndrome, by poorly understood mechanisms. Gland-related diseases have been studied by optical microscopy (OM), and at higher resolution by transmission electron microscopy (TEM) of Epon embedded samples, which necessitates hydrophobic sample pretreatment. Here, we report the direct observation of tissue in aqueous solution by atmospheric scanning electron microscopy (ASEM). Salivary glands, lacrimal glands, and pancreas were fixed, sectioned into slabs, stained with phosphotungstic acid (PTA), and inspected in radical scavenger d-glucose solution from below by an inverted scanning electron microscopy (SEM), guided by optical microscopy from above to target the tissue substructures. A 2- to 3-µm specimen thickness was visualized by the SEM. In secretory cells, cytoplasmic vesicles and other organelles were clearly imaged at high resolution, and the former could be classified according to the degree of PTA staining. In islets of Langerhans, the microvascular system used as an outlet by the secretory cells was also clearly observed. Microvascular system is also critically involved in the onset of diabetic complications and was clearly visible in subcutaneous tissue imaged by ASEM. The results suggest the use of in-solution ASEM for histology and to study vesicle secretion systems. Further, the high-throughput of ASEM makes it a potential tool for the diagnosis of exocrine and endocrine-related diseases. © 2016 Wiley Periodicals, Inc.

Static and Dynamic Electron Microscopy Investigations at the Atomic and Ultrafast Scales

NASA Astrophysics Data System (ADS)

Suri, Pranav Kumar

Advancements in the electron microscopy capabilities - aberration-corrected imaging, monochromatic spectroscopy, direct-electron detectors - have enabled routine visualization of atomic-scale processes with millisecond temporal resolutions in this decade. This, combined with progress in the transmission electron microscopy (TEM) specimen holder technology and nanofabrication techniques, allows comprehensive experiments on a wide range of materials in various phases via in situ methods. The development of ultrafast (sub-nanosecond) time-resolved TEM with ultrafast electron microscopy (UEM) has further pushed the envelope of in situ TEM to sub-nanosecond temporal resolution while maintaining sub-nanometer spatial resolution. A plethora of materials phenomena - including electron-phonon coupling, phonon transport, first-order phase transitions, bond rotation, plasmon dynamics, melting, and dopant atoms arrangement - are not yet clearly understood and could be benefitted with the current in situ TEM capabilities having atomic-level and ultrafast precision. Better understanding of these phenomena and intrinsic material dynamics (e.g. how phonons propagate in a material, what time-scales are involved in a first-order phase transition, how fast a material melts, where dopant atoms sit in a crystal) in new-generation and technologically important materials (e.g. two-dimensional layered materials, semiconductor and magnetic devices, rare-earth-element-free permanent magnets, unconventional superconductors) could bring a paradigm shift in their electronic, structural, magnetic, thermal and optical applications. Present research efforts, employing cutting-edge static and dynamic in situ electron microscopy resources at the University of Minnesota, are directed towards understanding the atomic-scale crystallographic structural transition and phonon transport in an iron-pnictide parent compound LaFeAsO, studying the mechanical stability of fast moving hard-drive heads in heat-assisted magnetic recording (HAMR) technology, exploring the possibility of ductile ceramics in magnesium oxide (MgO) nanomaterials, and revealing the atomic-structure of newly discovered rare-earth-element-free iron nitride (FeN) magnetic materials. Via atomic-resolution imaging and electron diffraction coupled with in situ TEM cooling on LaFeAsO, it was found that additional effects not related to the structural transition, namely dynamical scattering and electron channeling, can give signatures reminiscent of those typically associated with the symmetry change. UEM studies on LaFeAsO revealed direct, real-space imaging of the emergence and evolution of acoustic phonons and resolved dispersion behavior during propagation and scattering. Via UEM bright-field imaging, megahertz vibrational frequencies were observed upon laser-illumination in TEM specimens made out of HAMR devices which could be detrimental to their long-term thermal and structural reliability. Compression testing of 100-350 nm single-crystal MgO nanocubes shows size-dependent stresses and engineering strains of 4-13.8 GPa and 0.046-0.221 respectively at the first signs of yield accompanied by an absence of brittle fracture, which is a significant increase in plasticity of a brittle ceramic material. Atomic-scale characterization of FeN phases show that it is possible to detect interstitial locations of low atomic-number nitrogen atoms in iron crystal and hints at a development of novel routes (without involving rare-earth elements) for bulk permanent magnet synthesis.

Effect of high current density to defect generation of blue LED and its characterization with transmission electron microscope

NASA Astrophysics Data System (ADS)

Gunawan, R.; Sugiarti, E.; Isnaeni; Purawiardi, R. I.; Widodo, H.; Muslimin, A. N.; Yuliasari; Ronaldus, C. E.; Prastomo, N.; Hastuty, S.

2018-03-01

The optical, electrical and structural characteristics of InGaN-based blue light-emitting diodes (LEDs) were investigated to identify the degradation of LED before and after current injection. The sample was injected by high current of 200 A/cm2 for 5 and 20 minutes. It was observed that injection of current shifts light intensity and wavelength characteristics that indicated defect generation. Transmission Electron Microscopy (TEM) characterization was carried out in order to clarify the structure degradation caused by defect in active layer which consisted of 14 quantum well with thickness of about 5 nm and confined with barrier layer with thickness of about 12 nm. TEM results showed pre-existing defect in LED before injection with high current. Furthermore, discontinue and edge defect was found in dark spot region of LED after injection with high current.

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.

Synthesis and Optical Properties of MnS–ZnS and MnS–CdS Nanoparticles in Montmorillonite.

PubMed

Kabilaphat, Jirabhorn; Poosimma, Poonsuk; Khaorapapong, Nithima; Intachai, Sonchai; Ogawa, Makoto

2017-02-01

The incorporation of metal sulfide mixture, manganese sulfide and zinc sulfide (MnS–ZnS) or manganese sulfide and cadmium sulfide (MnS–CdS), in two types of montmorillonites (sodium montmorillonite and cetyltrimethylammonium modified montmorillonite) was investigated. The hybrids were characterized by powder X-ray diffraction, thermogravimetric-differential thermal analysis, transmission electron microscopy (TEM), and Raman, UV-visible and photoluminescence spectroscopies. The experimental evidences such as the expansion of the interlayer spaces and the presence of the absorption and photoluminescence due to MnS, ZnS and/or CdS revealed that the mixed metal sulfides formed in the interlayer space of montmorillonites. TEM images of the hybrids showed diskor plate-shaped nanoparticles with a mean diameter of ca. 2 nm. The increase of the luminescence intensities of the hybrids was assumed to be caused by quantum confinement effect in the interlayer space of montmorillonite.

A TEM Investigation of the Fine-Grained Matrix of the Martian Basaltic Breccia NWA 7034

NASA Technical Reports Server (NTRS)

Muttik, N.; Keller, L. P.; Agee, C. B.; McCubbin, F. M.; Santos, A. R.; Rahman, Z.

2014-01-01

The martian basaltic breccia NWA 7034 is characterized by fine-grained groundmass containing several different types of mineral grains and lithologic clasts. The matrix composition closely resembles Martian crustal rock and soil composition measured by recent rover and orbiter missions. The first results of NWA 7034 suggest that the brecciation of this martian meteorite may have formed due to eruptive volcanic processes; however, impact related brecciation processes have been proposed for paired meteorites NWA 7533 and NWA 7475]. Due to the very fine grain size of matrix, its textural details are difficult to resolve by optical and microprobe observations. In order to examine the potential nature of brecciation, transmission electron microscopy (TEM) studies combined with focused ion-beam technique (FIB) has been undertaken. Here we present the preliminary observations of fine-grained groundmass of NWA 7034 from different matrix areas by describing its textural and mineralogical variations and micro-structural characteristics.

Correlative microscopy of a carbide-free bainitic steel.

PubMed

Hofer, Christina; Bliznuk, Vitaliy; Verdiere, An; Petrov, Roumen; Winkelhofer, Florian; Clemens, Helmut; Primig, Sophie

2016-02-01

In this work a carbide-free bainitic steel was examined by a novel correlative microscopy approach using transmission Kikuchi diffraction (TKD) and transmission electron microscopy (TEM). The individual microstructural constituents could be identified by TKD based on their different crystal structure for bainitic ferrite and retained austenite and by image quality for the martensite-austenite (M-A) constituent. Subsequently, the same area was investigated in the TEM and a good match of these two techniques regarding the identification of the area position and crystal orientation could be proven. Additionally, the M-A constituent was examined in the TEM for the first time after preceded unambiguous identification using a correlative microscopy approach. The selected area diffraction pattern showed satellites around the main reflexes which might indicate a structural modulation. Copyright © 2015 Elsevier Ltd. All rights reserved.

Synthesis and characterization of PVK/AgNPs nanocomposites prepared by laser ablation.

PubMed

Abd El-Kader, F H; Hakeem, N A; Elashmawi, I S; Menazea, A A

2015-03-05

Nanocomposites of Poly (n-vinylcarbazole) PVK/Ag nanoparticles were prepared by laser ablation of a silver plate in aqueous solution of chlorobenzene. The influences of laser parameters such as; time of irradiation, source power and wavelength (photon energy) on structural, morphological and optical properties have been investigated using X-ray diffraction (XRD), Transmission electron microscopy (TEM), Ultraviolet-visible (UV-Vis) and Photoluminescence (PL). A correlation between the investigated properties has been discussed. XRD, TEM and PL indicated that the complexation between AgNPs and PVK in the composite system is possible. Only the reflection peak at 2θ=38° of AgNPs appeared in the composite nanoparticles while the other reflection peaks were destroyed. The nanoparticles shape and size distribution were evaluated from TEM images. TEM analysis revealed a lower average particle size at long laser irradiation time 40min and short laser wavelength 532nm together with high laser power 570mW. From UV-Visible spectra the values of absorption coefficient, absorption edge and energy tail were calculated. The reduction of band tail value with increasing the laser ablation parameters confirms the decrease of the disorder in such composite system. The PL and UV-Vis. spectra confirm that nanocomposite samples showed quantum confinement effect. Copyright © 2014 Elsevier B.V. All rights reserved.

Optical sensor based on a single CdS nanobelt.

PubMed

Li, Lei; Yang, Shuming; Han, Feng; Wang, Liangjun; Zhang, Xiaotong; Jiang, Zhuangde; Pan, Anlian

2014-04-23

In this paper, an optical sensor based on a cadmium sulfide (CdS) nanobelt has been developed. The CdS nanobelt was synthesized by the vapor phase transportation (VPT) method. X-Ray Diffraction (XRD) and Transmission Electron Microscopy (TEM) results revealed that the nanobelt had a hexagonal wurtzite structure of CdS and presented good crystal quality. A single nanobelt Schottky contact optical sensor was fabricated by the electron beam lithography (EBL) technique, and the device current-voltage results showed back-to-back Schottky diode characteristics. The photosensitivity, dark current and the decay time of the sensor were 4 × 10⁴, 31 ms and 0.2 pA, respectively. The high photosensitivity and the short decay time were because of the exponential dependence of photocurrent on the number of the surface charges and the configuration of the back to back Schottky junctions.

Progression in structural, magnetic and electrical properties of La-doped group IV elements

NASA Astrophysics Data System (ADS)

Deepapriya, S.; Annie Vinosha, P.; Rodney, John D.; Jerome Das, S.

2018-04-01

Progression of group IV elements such as zinc ferrite (ZnFe2O4), cobalt ferrite (CoFe2O4) was synthesized by doping lanthanum (La), via adopting a facile co-precipitation method. Doping hefty rare earth ion in spinel structure can amend to the physical properties of the lattice, which can be used in the enhancement of magnetic and electrical properties of the as-synthesized nanomaterial, it is vital to metamorphose and optimize its micro structural and magnetic features. The structural properties of the samples was analysed by powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), Transmission electron microscopy (TEM) and UV-visible spectral analysis (UV-vis) reveals the optical property and optical band gap. The magnetic properties were evaluated using a vibrating sample magnetometer (VSM), the presence of functional group was confirmed by FTIR. XRD analyses elucidates that the synthesized samples zinc and cobalt had a spinel structure. From TEM analyses the morphology and diameter of the particle was observed. The substituted rare earth ions in Zinc ferrite inhibit the grain growth of the materials in an efficient manner compared with that of the Cobalt ferrite.

The structural and optical properties of type III human collagen biosynthetic corneal substitutes

PubMed Central

Hayes, Sally; Lewis, Phillip; Islam, M. Mirazul; Doutch, James; Sorensen, Thomas; White, Tomas; Griffith, May; Meek, Keith M.

2015-01-01

The structural and optical properties of clinically biocompatible, cell-free hydrogels comprised of synthetically cross-linked and moulded recombinant human collagen type III (RHCIII) with and without the incorporation of 2-methacryloyloxyethyl phosphorylcholine (MPC) were assessed using transmission electron microscopy (TEM), X-ray scattering, spectroscopy and refractometry. These findings were examined alongside similarly obtained data from 21 human donor corneas. TEM demonstrated the presence of loosely bundled aggregates of fine collagen filaments within both RHCIII and RHCIII-MPC implants, which X-ray scattering showed to lack D-banding and be preferentially aligned in a uniaxial orientation throughout. This arrangement differs from the predominantly biaxial alignment of collagen fibrils that exists in the human cornea. By virtue of their high water content (90%), very fine collagen filaments (2–9 nm) and lack of cells, the collagen hydrogels were found to transmit almost all incident light in the visible spectrum. They also transmitted a large proportion of UV light compared to the cornea which acts as an effective UV filter. Patients implanted with these hydrogels should be cautious about UV exposure prior to regrowth of the epithelium and in-growth of corneal cells into the implants. PMID:26159106

Inducing fluorescence of uranyl acetate as a dual-purpose contrast agent for correlative light-electron microscopy with nanometre precision.

PubMed

Tuijtel, Maarten W; Mulder, Aat A; Posthuma, Clara C; van der Hoeven, Barbara; Koster, Abraham J; Bárcena, Montserrat; Faas, Frank G A; Sharp, Thomas H

2017-09-05

Correlative light-electron microscopy (CLEM) combines the high spatial resolution of transmission electron microscopy (TEM) with the capability of fluorescence light microscopy (FLM) to locate rare or transient cellular events within a large field of view. CLEM is therefore a powerful technique to study cellular processes. Aligning images derived from both imaging modalities is a prerequisite to correlate the two microscopy data sets, and poor alignment can limit interpretability of the data. Here, we describe how uranyl acetate, a commonly-used contrast agent for TEM, can be induced to fluoresce brightly at cryogenic temperatures (-195 °C) and imaged by cryoFLM using standard filter sets. This dual-purpose contrast agent can be used as a general tool for CLEM, whereby the equivalent staining allows direct correlation between fluorescence and TEM images. We demonstrate the potential of this approach by performing multi-colour CLEM of cells containing equine arteritis virus proteins tagged with either green- or red-fluorescent protein, and achieve high-precision localization of virus-induced intracellular membrane modifications. Using uranyl acetate as a dual-purpose contrast agent, we achieve an image alignment precision of ~30 nm, twice as accurate as when using fiducial beads, which will be essential for combining TEM with the evolving field of super-resolution light microscopy.

Microstructural and ultrastructural assessment of inferior alveolar nerve damage following nerve lateralization and implant placement: an experimental study in rabbits.

PubMed

Yoshimoto, Marcelo; Watanabe, Il-sei; Martins, Marília T; Salles, Marcos B; Ten Eyck, Gary R; Coelho, Paulo G

2009-01-01

The present study assessed damage to the inferior alveolar nerve (IAN) following nerve lateralization and implant placement surgery through optical and transmission electron microscopy (TEM). IAN lateralization was performed in 16 adult female rabbits (Oryctolagus cuniculus). During the nerve lateralization procedure, one implant was placed through the mandibular canal, and the IAN was replaced in direct contact with the implant. The implant was placed in the right mandible, and the left side was used as a control (no surgical procedure). After 8 weeks, the animals were sacrificed and samples were prepared for optical and TEM analysis of IAN structural damage. Histomorphometric analysis was performed to determine the number and cross-sectional dimensions of nerve fascicles and myelin sheath thickness between experimental and control groups. The different parameters were compared by one-way analysis of variance at the 95% significance level. Alterations in the perineural and endoneural regions of the IAN, with higher degrees of vascularization, were observed in the experimental group. TEM showed that the majority of the myelinated nerve fibers were not affected in the experimental samples. No significant variation in the number of fascicles was observed, significantly larger fascicle height and width were observed in the control group, and significantly thicker myelin sheaths were observed in the experimental samples. IAN lateralization resulted in substantial degrees of tissue disorganization at the microstructural level because of the presence of edema. However, at the ultrastructural level, small amounts of fiber degeneration were observed.

Growth of boron doped hydrogenated nanocrystalline cubic silicon carbide (3C-SiC) films by Hot Wire-CVD

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

Pawbake, Amit; Tata Institute of Fundamental Research, Colaba, Mumbai 400 005; Mayabadi, Azam

Highlights: • Boron doped nc-3C-SiC films prepared by HW-CVD using SiH{sub 4}/CH{sub 4}/B{sub 2}H{sub 6}. • 3C-Si-C films have preferred orientation in (1 1 1) direction. • Introduction of boron into SiC matrix retard the crystallanity in the film structure. • Film large number of SiC nanocrystallites embedded in the a-Si matrix. • Band gap values, E{sub Tauc} and E{sub 04} (E{sub 04} > E{sub Tauc}) decreases with increase in B{sub 2}H{sub 6} flow rate. - Abstract: Boron doped nanocrystalline cubic silicon carbide (3C-SiC) films have been prepared by HW-CVD using silane (SiH{sub 4})/methane (CH{sub 4})/diborane (B{sub 2}H{sub 6}) gasmore » mixture. The influence of boron doping on structural, optical, morphological and electrical properties have been investigated. The formation of 3C-SiC films have been confirmed by low angle XRD, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Fourier transform infra-red (FTIR) spectroscopy and high resolution-transmission electron microscopy (HR-TEM) analysis whereas effective boron doping in nc-3C-SiC have been confirmed by conductivity, charge carrier activation energy, and Hall measurements. Raman spectroscopy and HR-TEM analysis revealed that introduction of boron into the SiC matrix retards the crystallanity in the film structure. The field emission scanning electron microscopy (FE-SEM) and non contact atomic force microscopy (NC-AFM) results signify that 3C-SiC film contain well resolved, large number of silicon carbide (SiC) nanocrystallites embedded in the a-Si matrix having rms surface roughness ∼1.64 nm. Hydrogen content in doped films are found smaller than that of un-doped films. Optical band gap values, E{sub Tauc} and E{sub 04} decreases with increase in B{sub 2}H{sub 6} flow rate.« less

Chapter 14: Electron Microscopy on Thin Films for Solar Cells

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

Romero, Manuel; Abou-Ras, Daniel; Nichterwitz, Melanie

2016-07-22

This chapter overviews the various techniques applied in scanning electron microscopy (SEM) and transmission electron microscopy (TEM), and highlights their possibilities and also limitations. It gives the various imaging and analysis techniques applied on a scanning electron microscope. The chapter shows that imaging is divided into that making use of secondary electrons (SEs) and of backscattered electrons (BSEs), resulting in different contrasts in the images and thus providing information on compositions, microstructures, and surface potentials. Whenever aiming for imaging and analyses at scales of down to the angstroms range, TEM and its related techniques are appropriate tools. In many cases,more » also SEM techniques provide the access to various material properties of the individual layers, not requiring specimen preparation as time consuming as TEM techniques. Finally, the chapter dedicates to cross-sectional specimen preparation for electron microscopy. The preparation decides indeed on the quality of imaging and analyses.« less

Optical properties of ZnO/BaCO3 nanocomposites in UV and visible regions.

PubMed

Zak, Ali Khorsand; Hashim, Abdul Manaf; Darroudi, Majid

2014-01-01

Pure zinc oxide and zinc oxide/barium carbonate nanoparticles (ZnO-NPs and ZB-NPs) were synthesized by the sol-gel method. The prepared powders were characterized by X-ray diffraction (XRD), ultraviolet-visible (UV-Vis), Auger spectroscopy, and transmission electron microscopy (TEM). The XRD result showed that the ZnO and BaCO3 nanocrystals grow independently. The Auger spectroscopy proved the existence of carbon in the composites besides the Zn, Ba, and O elements. The UV-Vis spectroscopy results showed that the absorption edge of ZnO nanoparticles is redshifted by adding barium carbonate. In addition, the optical parameters including the refractive index and permittivity of the prepared samples were calculated using the UV-Vis spectra. 81.05.Dz; 78.40.Tv; 42.70.-a.

Preparation and optical characteristics of ZnSe nanocrystals doped glass by sol gel in situ crystallization method

NASA Astrophysics Data System (ADS)

Hao, Haiyan; Yao, Xi; Wang, Minqiang

2007-01-01

Homogeneous ZnSe nanocrystals doped SiO 2 glass was successfully prepared by sol-gel in situ crystallization method. The structure of the doped ZnSe nanocrystals was studied by X-ray diffraction (XRD). ZnSe nanocrystals in silica were about 4-10 nm analysed by transmission electron microscopy (TEM), which was consistent with the results of XRD estimated using Scherrer's formular. The quantum size effect in ZnSe nanocrystals was evidenced from the blue-shifts of the optical absorption edge, and the average size of ZnSe nanocrystals was estimated by the magnitude of blue shift according to the L.E. Brus' effective mass model. The size of ZnSe nanocrystals depending on annealing time and temperature was further discussed using XRF.

Tissue and cellular localization of tannins in Tunisian dates (Phoenix dactylifera L.) by light and transmission electron microscopy.

PubMed

Hammouda, Hédi; Alvarado, Camille; Bouchet, Brigitte; Kalthoum-Chérif, Jamila; Trabelsi-Ayadi, Malika; Guyot, Sylvain

2014-07-16

A histological approach including light microscopy and transmission electron microscopy (TEM) was used to provide accurate information on the localization of condensed tannins in the edible tissues and in the stone of date fruits (Phoenix dactylifera L.). Light microscopy was carried out on fresh tissues after staining by 4-dimethylaminocinnamaldehyde (DMACA) for a specific detection of condensed tannins. Thus, whether under light microscopy or transmission electron microscopy (TEM), results showed that tannins are not located in the epidermis but more deeply in the mesocarp in the vacuole of very large cells. Regarding the stones, tannins are found in a specific cell layer located at 50 μm from the sclereid cells of the testa.

Synthesis and characterization of graphene quantum dots/cobalt ferrite nanocomposite

NASA Astrophysics Data System (ADS)

Ramachandran, Shilpa; Sathishkumar, M.; Kothurkar, Nikhil K.; Senthilkumar, R.

2018-02-01

A facile method has been developed for the synthesis of a graphene quantum dots/cobalt ferrite nanocomposite. Graphene quantum dots (GQDs) were synthesized by a simple bottom-up method using citric acid, followed by the co-precipitation of cobalt ferrite nanoparticles on the graphene quantum dots. The morphology, structural analysis, optical properties, magnetic properties were investigated using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), UV-vis absorption spectroscopy, fluorescence spectroscopy, vibrating sample magnetometry (VSM) measurements. The synthesized nanocomposite showed good fluorescence and superparamagnetic properties, which are important for biomedical applications.

Synthesis by sol-gel process, structural and optical properties of nanoparticles of zinc oxide doped vanadium

NASA Astrophysics Data System (ADS)

El Ghoul, J.; Barthou, C.; El Mir, L.

2012-06-01

We report the elaboration of vanadium-doped ZnO nanoparticles prepared by a sol-gel processing technique. In our approach, the water for hydrolysis was slowly released by esterification reaction followed by a supercritical drying in ethyl alcohol. Vanadium doping concentration of 10 at.% has been investigated. After treatment in air at different temperatures, the obtained nanopowder was characterised by various techniques such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence (PL). Analysis by scanning electron microscopy at high resolution shows that the grain size increases with increasing temperature. Thus, in the case of thermal treatment at 500 °C in air, the powder with an average particle size of 25 nm shows a strong luminescence band in the visible range. The intensity and energy position of the obtained PL band depends on the temperature measurement increase. The mechanism of this emission band is discussed.

ZnO nanoparticles (ZnO-NPs) and their antifungal activity against coffee fungus Erythricium salmonicolor

NASA Astrophysics Data System (ADS)

Arciniegas-Grijalba, P. A.; Patiño-Portela, M. C.; Mosquera-Sánchez, L. P.; Guerrero-Vargas, J. A.; Rodríguez-Páez, J. E.

2017-06-01

In this work, a methodology of synthesis was designed to obtain ZnO nanoparticles (ZnO NPs) in a controlled and reproducible manner. The nanoparticles obtained were characterized using infrared spectroscopy, X-ray diffraction, and transmission electron microscopy (TEM). Also, we determined the antifungal capacity in vitro of zinc oxide nanoparticles synthesized, examining their action on Erythricium salmonicolor fungy causal of pink disease. To determine the effect of the quantity of zinc precursor used during ZnO NPs synthesis on the antifungal capacity, 0.1 and 0.15 M concentrations of zinc acetate were examined. To study the inactivation of the mycelial growth of the fungus, different concentrations of ZnO NPs of the two types of synthesized samples were used. The inhibitory effect on the growth of the fungus was determined by measuring the growth area as a function of time. The morphological change was observed with high-resolution optical microscopy (HROM), while TEM was used to observe changes in its ultrastructure. The results showed that a concentration of 9 mmol L-1 for the sample obtained from the 0.15 M and at 12 mmol L-1 for the 0.1 M system significantly inhibited growth of E. salmonicolor. In the HROM images a deformation was observed in the growth pattern: notable thinning of the fibers of the hyphae and a clumping tendency. The TEM images showed a liquefaction of the cytoplasmic content, making it less electron-dense, with the presence of a number of vacuoles and significant detachment of the cell wall.

The Effects of Helium Bubble Microstructure on Ductility in Annealed and HERF 21Cr-6Ni-9Mn Stainless Steel

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

Tosten, M.H.; Morgan, M.J.

1998-01-01

This study examined the effects of microstructure on the ambient temperature embrittlement from hydrogen isotopes and decay helium in 21Cr-6Ni-9Mn stainless steel. Hydrogen and tritium-exposed 21Cr-6Ni-9Mn stainless steel tensile samples were pulled to failure and then characterized by transmission electron microscopy (TEM) and optical microscopy. This study determined that ductility differences between annealed and high-energy-rate-forged (HERF) stainless steel containing tritium and its decay product, helium, could be related to differences in the helium bubble microstructures. The HERF microstructures were more resistant to tritium-induced embrittlement than annealed microstructures because the high number density of helium bubbles on dislocations trap tritium withinmore » the matrix and away from the grain boundaries.« less

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

NASA Astrophysics Data System (ADS)

Arulmozhi, K. T.; Mythili, N.

2013-12-01

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

Composite particles formed by complexation of poly(methacrylic acid) - stabilized magnetic fluid with chitosan: Magnetic material for bioapplications.

PubMed

Safarik, Ivo; Stepanek, Miroslav; Uchman, Mariusz; Slouf, Miroslav; Baldikova, Eva; Nydlova, Leona; Pospiskova, Kristyna; Safarikova, Mirka

2016-10-01

A simple procedure for the synthesis of magnetic fluid (ferrofluid) stabilized by poly(methacrylic acid) has been developed. This ferrofluid was used to prepare a novel type of magnetically responsive chitosan-based composite material. Both ferrofluid and magnetic chitosan composite were characterized by a combination of microscopy (optical microscopy, TEM, SEM), scattering (static and dynamic light scattering, SANS) and spectroscopy (FTIR) techniques. Magnetic chitosan was found to be a perspective material for various bioapplications, especially as a magnetic carrier for immobilization of enzymes and cells. Lipase from Candida rugosa was covalently attached after cross-linking and activation of chitosan using glutaraldehyde. Baker's yeast cells (Saccharomyces cerevisiae) were incorporated into the chitosan composite during its preparation; both biocatalysts were active after reaction with appropriate substrates. Copyright © 2016 Elsevier B.V. All rights reserved.

Structure Prediction of Self-Assembled Dye Aggregates from Cryogenic Transmission Electron Microscopy, Molecular Mechanics, and Theory of Optical Spectra.

PubMed

Friedl, Christian; Renger, Thomas; Berlepsch, Hans V; Ludwig, Kai; Schmidt Am Busch, Marcel; Megow, Jörg

2016-09-01

Cryogenic transmission electron microscopy (cryo-TEM) studies suggest that TTBC molecules self-assemble in aqueous solution to form single-walled tubes with a diameter of about 35 Å. In order to reveal the arrangement and mutual orientations of the individual molecules in the tube, we combine information from crystal structure data of this dye with a calculation of linear absorbance and linear dichroism spectra and molecular dynamics simulations. We start with wrapping crystal planes in different directions to obtain tubes of suitable diameter. This set of tube models is evaluated by comparing the resulting optical spectra with experimental data. The tubes that can explain the spectra are investigated further by molecular dynamics simulations, including explicit solvent molecules. From the trajectories of the most stable tube models, the short-range ordering of the dye molecules is extracted and the optimization of the structure is iteratively completed. The final structural model is a tube of rings with 6-fold rotational symmetry, where neighboring rings are rotated by 30° and the transition dipole moments of the chromophores form an angle of 74° with respect to the symmetry axis of the tube. This model is in agreement with cryo-TEM images and can explain the optical spectra, consisting of a sharp red-shifted J-band that is polarized parallel to to the symmetry axis of the tube and a broad blue-shifted H-band polarized perpendicular to this axis. The general structure of the homogeneous spectrum of this hybrid HJ-aggregate is described by an analytical model that explains the difference in redistribution of oscillator strength inside the vibrational manifolds of the J- and H-bands and the relative intensities and excitation energies of those bands. In addition to the particular system investigated here, the present methodology can be expected to aid the structure prediction for a wide range of self-assembled dye aggregates.

Microstructures of ancient and modern cast silver–copper alloys

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

Northover, S.M., E-mail: s.m.northover@open.ac.uk; Northover, J.P., E-mail: peter.northover@materials.ox.ac.uk

The microstructures of modern cast Sterling silver and of cast silver objects about 2500 years old have been compared using optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), energy dispersive X-ray microanalysis (EDX) and electron backscatter diffraction (EBSD). Microstructures of both ancient and modern alloys were typified by silver-rich dendrites with a few pools of eutectic and occasional cuprite particles with an oxidised rim on the outer surface. EBSD showed the dendrites to have a complex internal structure, often involving extensive twinning. There was copious intragranular precipitation within the dendrites, in themore » form of very fine copper-rich rods which TEM, X-ray diffraction (XRD), SEM and STEM suggest to be of a metastable face-centred-cubic (FCC) phase with a cube–cube orientation relationship to the silver-rich matrix but a higher silver content than the copper-rich β in the eutectic. Samples from ancient objects displayed a wider range of microstructures including a fine scale interpenetration of the adjoining grains not seen in the modern material. Although this study found no unambiguous evidence that this resulted from microstructural change produced over archaeological time, the copper supersaturation remaining after intragranular precipitation suggests that such changes, previously proposed for wrought and annealed material, may indeed occur in ancient silver castings. - Highlights: • Similar twinned structures and oxidised surfaces seen in ancient and modern cast silver • General precipitation of fine Cu-rich rods apparently formed by discontinuous precipitation is characteristic of as-cast silver. • The fine rods are cube-cube related to the matrix in contrast with the eutectic. • The silver-rich phase remains supersaturated with copper. • Possibly age-related grain boundary features seen in ancient cast silver.« less

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

PubMed

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

2012-07-01

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

Modulated structures and associated microstructures in the ferroelectric phase of Ba1-xSrxAl2O4 for 0.7 ≤ x ≤ 1.0

NASA Astrophysics Data System (ADS)

Tsukasaki, Hirofumi; Ishii, Yui; Tanaka, Eri; Kurushima, Kosuke; Mori, Shigeo

2016-01-01

In order to understand the ferroelectric and ferroelastic phases in Ba1-xSrxAl2O4 for 0.7 ≤ x ≤ 1.0, we have investigated the crystal structures and their associated microstructures of the ferroelectric and ferroelastic phases mainly by transmission electron microscopy (TEM) and scanning transmission electron microscopy-high-angle angular dark-field (STEM-HAADF) experiments, combined with powder X-ray diffraction experiments. Electron diffraction experiments showed that the ferroelectric and ferroelastic phases of Ba1-xSrxAl2O4 for 0.7 ≤ x ≤ 1.0 should be characterized as a modulated structure with the modulation vector of \\boldsymbol{{q}} = 0,1/2,0, whose space group should be monoclinic P21. High-resolution TEM experiments revealed that the microstructures in the monoclinic phase can be characterized as twin structures and nanometer-sized planar defects due to the monoclinic structure with the modulated structures, which are responsible for anomalous elastic behaviors and mechanoelectro-optical properties. In addition, subatomic-resolution STEM-HAADF images clearly indicated that the displacement of Al3+ ions involved in the AlO4 tetrahedra should play a crucial role in the formation of the modulated structures and twin structures.

ZnS, CdS and HgS nanoparticles via alkyl-phenyl dithiocarbamate complexes as single source precursors.

PubMed

Onwudiwe, Damian C; Ajibade, Peter A

2011-01-01

The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescence spectroscopy. The X-ray diffraction pattern showed that the prepared ZnS nanoparticles have a cubic sphalerite structure; the CdS indicates a hexagonal phase and the HgS show the presence of metacinnabar phase. The TEM image demonstrates that the ZnS nanoparticles are dot-shaped, the CdS and the HgS clearly showed a rice and spherical morphology respectively. The UV-Vis spectra exhibited a blue-shift with respect to that of the bulk samples which is attributed to the quantum size effect. The band gap of the samples have been calculated from absorption spectra and werefound to be about 4.33 eV (286 nm), 2.91 eV (426 nm) and 4.27 eV (290 nm) for the ZnS, CdS and HgS samples respectively.

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

PubMed Central

Onwudiwe, Damian C.; Ajibade, Peter A.

2011-01-01

The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescence spectroscopy. The X-ray diffraction pattern showed that the prepared ZnS nanoparticles have a cubic sphalerite structure; the CdS indicates a hexagonal phase and the HgS show the presence of metacinnabar phase. The TEM image demonstrates that the ZnS nanoparticles are dot-shaped, the CdS and the HgS clearly showed a rice and spherical morphology respectively. The UV-Vis spectra exhibited a blue-shift with respect to that of the bulk samples which is attributed to the quantum size effect. The band gap of the samples have been calculated from absorption spectra and werefound to be about 4.33 eV (286 nm), 2.91 eV (426 nm) and 4.27 eV (290 nm) for the ZnS, CdS and HgS samples respectively. PMID:22016607

New and unconventional approaches for advancing resolution in biological transmission electron microscopy by improving macromolecular specimen preparation and preservation.

PubMed

Massover, William H

2011-02-01

Resolution in transmission electron microscopy (TEM) now is limited by the properties of specimens, rather than by those of instrumentation. The long-standing difficulties in obtaining truly high-resolution structure from biological macromolecules with TEM demand the development, testing, and application of new ideas and unconventional approaches. This review concisely describes some new concepts and innovative methodologies for TEM that deal with unsolved problems in the preparation and preservation of macromolecular specimens. The selected topics include use of better support films, a more protective multi-component matrix surrounding specimens for cryo-TEM and negative staining, and, several quite different changes in microscopy and micrography that should decrease the effects of electron radiation damage; all these practical approaches are non-traditional, but have promise to advance resolution for specimens of biological macromolecules beyond its present level of 3-10 Å (0.3-1.0 nm). The result of achieving truly high resolution will be a fulfillment of the still unrealized potential of transmission electron microscopy for directly revealing the structure of biological macromolecules down to the atomic level. Published by Elsevier Ltd.

Electron microscopic diagnosis of human flavivirus encephalitis: use of confocal microscopy as an aid.

PubMed

Chu, C T; Howell, D N; Morgenlander, J C; Hulette, C M; McLendon, R E; Miller, S E

1999-10-01

The distinction between intracranial viral infections and inflammatory conditions requiring immunosuppression is important. Although specific laboratory reagents are readily available for some viruses, diagnosis of arbovirus infection is more difficult. Transmission electron microscopy (TEM) theoretically allows identification of viral particles independent of reagent availability, but it has limited sensitivity. We report two cases of human flavivirus encephalitis diagnosed by TEM. Laser scanning confocal microscopy (LSCM) was used in one case to survey unembedded tissue slices for focal abnormalities, from which fragments smaller than 1 mm2 were excised for epoxy embedding. This facilitated TEM identification of intracytoplasmic, budding, 35-40 nm spherical virus particles, confirmed by serology as St. Louis encephalitis. In contrast to mosquitoes and newborn mice, in which high viral loads are associated with minimal tissue responses, these biopsies showed florid angiodestructive inflammation and microgliosis, with rare virions in necrotic perivascular cells and astrocytes. To our knowledge, this represents the first ultrastructural study of St. Louis encephalitis in humans, indicating the potential value of LSCM-aided TEM.

Recent developments of the in situ wet cell technology for transmission electron microscopies.

PubMed

Chen, Xin; Li, Chang; Cao, Hongling

2015-03-21

In situ wet cells for transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) allow studying structures and processes in a liquid environment with high temporal and spatial resolutions, and have been attracting increasing research interests in many fields. In this review, we highlight the structural and functional developments of the wet cells for TEM and STEM. One of the key features of the wet cells is the sealing technique used to isolate the liquid sample from the TEM/STEM vacuum environments, thus the existing in situ wet cells are grouped by different sealing methods. In this study, the advantages and shortcomings of each type of in situ wet cells are discussed, the functional developments of different wet cells are presented, and the future trends of the wet cell technology are addressed. It is suggested that in the future the in situ wet cell TEM/STEM technology will have an increasing impact on frontier nanoscale research.

Demonstration of correlative atomic force and transmission electron microscopy using actin cytoskeleton

PubMed Central

Yamada, Yutaro; Konno, Hiroki; Shimabukuro, Katsuya

2017-01-01

In this study, we present a new technique called correlative atomic force and transmission electron microscopy (correlative AFM/TEM) in which a targeted region of a sample can be observed under AFM and TEM. The ultimate goal of developing this new technique is to provide a technical platform to expand the fields of AFM application to complex biological systems such as cell extracts. Recent advances in the time resolution of AFM have enabled detailed observation of the dynamic nature of biomolecules. However, specifying molecular species, by AFM alone, remains a challenge. Here, we demonstrate correlative AFM/TEM, using actin filaments as a test sample, and further show that immuno-electron microscopy (immuno-EM), to specify molecules, can be integrated into this technique. Therefore, it is now possible to specify molecules, captured under AFM, by subsequent observation using immuno-EM. In conclusion, correlative AFM/TEM can be a versatile method to investigate complex biological systems at the molecular level. PMID:28828286

High-resolution imaging by scanning electron microscopy of semithin sections in correlation with light microscopy.

PubMed

Koga, Daisuke; Kusumi, Satoshi; Shodo, Ryusuke; Dan, Yukari; Ushiki, Tatsuo

2015-12-01

In this study, we introduce scanning electron microscopy (SEM) of semithin resin sections. In this technique, semithin sections were adhered on glass slides, stained with both uranyl acetate and lead citrate, and observed with a backscattered electron detector at a low accelerating voltage. As the specimens are stained in the same manner as conventional transmission electron microscopy (TEM), the contrast of SEM images of semithin sections was similar to TEM images of ultrathin sections. Using this technique, wide areas of semithin sections were also observed by SEM, without the obstruction of grids, which was inevitable for traditional TEM. This study also applied semithin section SEM to correlative light and electron microscopy. Correlative immunofluorescence microscopy and immune-SEM were performed in semithin sections of LR white resin-embedded specimens using a FluoroNanogold-labeled secondary antibody. Because LR white resin is hydrophilic and electron stable, this resin is suitable for immunostaining and SEM observation. Using correlative microscopy, the precise localization of the primary antibody was demonstrated by fluorescence microscopy and SEM. This method has great potential for studies examining the precise localization of molecules, including Golgi- and ER-associated proteins, in correlation with LM and SEM. © 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.

Using transmission electron microscopy and 3View® to determine collagen fibril size and three-dimensional organization

PubMed Central

Mironov, Aleksandr; Cootes, Timothy F.; Holmes, David F.; Kadler, Karl E.

2017-01-01

Collagen fibrils are the major tensile element in vertebrate tissues where they occur as ordered bundles in the extracellular matrix. Abnormal fibril assembly and organization results in scarring, fibrosis, poor wound healing and connective tissue diseases. Transmission electron microscopy (TEM) is used to assess formation of the fibrils, predominantly by measuring fibril diameter. Here we describe an enhanced protocol for measuring fibril diameter as well as fibril-volume-fraction, mean fibril length, fibril cross-sectional shape, and fibril 3D organization that are also major determinants of tissue function. Serial section TEM (ssTEM) has been used to visualize fibril 3D-organization in vivo. However, serial block face-scanning electron microscopy (SBF-SEM) has emerged as a time-efficient alternative to ssTEM. The protocol described below is suitable for preparing tissues for TEM and SBF-SEM (by 3View®). We demonstrate the power of 3View® for studying collagen fibril organization in vivo and show how to find and track individual fibrils. Time scale: ~8 days from isolating the tissue to having a 3D image stack. PMID:23807286

Optical and TEM study of shock metamorphism from the Sedan test site

NASA Technical Reports Server (NTRS)

Gratz, A. J.

1992-01-01

Thus far, detailed petrologic studies of shock metamorphism have been performed on samples recovered from laboratory experiments and on a few natural impactites. The loading history of these samples is quite different: In particular, laboratory experiments spend only a short time (less than 1 microsec) at peak pressure, whereas natural impactites may have stress pulses from 0.1 - 1 ms. On the other hand, laboratory experiments have known stress histories; natural impactites do not. Natural samples are also subjected to thousands or millions of years of postshock annealing and/or weathering. A useful intermediate case is that of nuclear detonation. Stress pulses for these events can reach 0.1 ms or higher, and samples are obtained in pristine condition. All three types of loading produce stresses of hundreds of kilobars. Samples studied were taken from the Sedan nulcear test site, and consist of a coarse-grained granodiorite containing quartz, K-feldspar, cordierite, and hornblende. Samples were studied optically in this section, then were thinned with an ion mill and studied by transmission electron microscopy (TEM). Optically, quartz and K-feldspar displayed numerous sets of planar deformation features (PDF's) identical to the nondecorated PDF's seen in laboratory samples and many natural impactites. TEM study showed that the PDF's in quartz and feldspar corresponded to densely packed wide transformation lamellae identical to those described in laboratory studies. The transformation lamellae in both minerals were amorphous, with no sign of high-pressure phases. In the case of K-feldspar only, narrow sublamellae extended outward from some wide lamellae. Quartz, which was more abundant and studied more extensively, contained no shock-induced dislocations. Some planar features were also seen in cordierite, but could not be identified due to rapid beam damage. No shock defects were seen in hornblende in TEM. The shock-induced defects present at the Sedan site are very similar to those seen in shock recovery experiments, and also to those present at certain natural events (e.g., Meteor Crater). This suggests that shock deformation in quartz is not strongly dependent on shock pulse duration, and that laboratory recovery experiments are useful simulations of natural impact events.

Synthesis, photoluminescence and Magnetic properties of iron oxide (α-Fe2O3) nanoparticles through precipitation or hydrothermal methods

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Ammar, Salah; Gadri, Abdellatif

2018-07-01

In this work the iron oxide (α-Fe2O3) nanoparticles are synthesized using two different methods: precipitation and hydrothermal. Size, structural, optical and magnetic properties were determined and compared using X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR), Raman spectroscopy, Differential Thermal Analysis (DTA), Thermogravimetric Analysis (TGA), Ultraviolet-Visible (UV-Vis) analysis, Superconducting QUantum Interference Device (SQUID) magnetometer and Photoluminescence (PL). XRD data further revealed a rhombohedral (hexagonal) structure with the space group (R-3c) and showed an average size of 21 nm for hydrothermal samples and 33 nm for precipitation samples which concorded with TEM and SEM images. FT-IR confirms the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we have synthesized pure α-Fe2O3 but also to identify their phonon modes. The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. The decrease in the particle size of hematite of 33 nm for precipitation samples to 21 nm for hydrothermal samples is responsible for increasing the optical band gap of 1.94-2.10 eV where, the relation between them is inverse relationship. The products exhibited the attractive magnetic properties with good saturation magnetization, which were examined by a SQUID magnetometer. Photoluminescence measurements showed a strong emission band at 450 nm. Pure hematite prepared by hydrothermal method has smallest size, best crystallinity, highest band gap and best value of saturation magnetization compared to the hematite elaborated by the precipitation method.

Synthesis and cytotoxicity study of magnesium ferrite-gold core-shell nanoparticles.

PubMed

Nonkumwong, Jeeranan; Pakawanit, Phakkhananan; Wipatanawin, Angkana; Jantaratana, Pongsakorn; Ananta, Supon; Srisombat, Laongnuan

2016-04-01

In this work, the core-magnesium ferrite (MgFe2O4) nanoparticles were prepared by hydrothermal technique. Completed gold (Au) shell coating on the surfaces of MgFe2O4 nanoparticles was obtained by varying core/shell ratios via a reduction method. Phase identification, morphological evolution, optical properties, magnetic properties and cytotoxicity to mammalian cells of these MgFe2O4 core coated with Au nanoparticles were examined by using a combination of X-ray diffraction, scanning electron microscopy, transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy, UV-visible spectroscopy (UV-vis), vibrating sample magnetometry and resazurin microplate assay techniques. In general, TEM images revealed different sizes of the core-shell nanoparticles generated from various core/shell ratios and confirmed the completed Au shell coating on MgFe2O4 core nanoparticles via suitable core/shell ratio with particle size less than 100 nm. The core-shell nanoparticle size and the quality of coating influence the optical properties of the products. The UV-vis spectra of complete coated MgFe2O4-Au core-shell nanoparticles exhibit the absorption bands in the near-Infrared (NIR) region indicating high potential for therapeutic applications. Based on the magnetic property measurement, it was found that the obtained MgFe2O4-Au core-shell nanoparticles still exhibit superparamagnetism with lower saturation magnetization value, compared with MgFe2O4 core. Both of MgFe2O4 and MgFe2O4-Au core-shell also showed in vitro non-cytotoxicity to mouse areola fibroblast (L-929) cell line. Copyright © 2015 Elsevier B.V. All rights reserved.

Inverse thermoreversible mechanical stiffening and birefringence in methylcellulose/cellulose nanocrystal hydrogel.

PubMed

Hynninen, Ville; Hietala, Sami; McKee, Jason Robert; Murtomäki, Lasse; Rojas, Orlando J; Ikkala, Olli; Nonappa, Nonappa

2018-05-07

We show that composite hydrogels comprising methyl cellulose (MC) and cellulose nanocrystal (CNC) colloidal rods display a reversible and enhanced rheological storage modulus and optical birefringence upon heating, i.e., inverse thermoreversibility. Dynamic rheology, quantitative polarized optical microscopy (POM), isothermal titration calorimetry (ITC), circular dichroism (CD), and scanning and transmission electron microscopy (SEM and TEM) were used for characterization. The concentration of CNC in aqueous media was varied up to 3.5 wt % (i.e, keeping the concentration below the critical aq. concentration) while maintaining the MC aq. concentration at 1.0 wt %. At 20 °C, MC/CNC underwent gelation upon passing the CNC concentration of 1.5 wt %. At this point the storage modulus (G´) reached a plateau, and the birefringence underwent a stepwise increase, thus suggesting a percolative phenomenon. The storage modulus (G´) of the composite gels was an order of magnitude higher at 60 °C compared to that at 20 °C. ITC results suggested that at 60 °C, the CNC rods were entropically driven to interact with MC chains, which according to recent studies, collapse at this temperature into ring-like, colloidal-scale persistent fibrils with hollow cross-section. Consequently, the increased requirement for space and mutual alignment of components results in enhanced birefringence. At room temperature, ITC shows enthalpic binding between CNCs and MC with the latter comprising an aqueous, molecularly dispersed polymer chains that lead to looser and less birefringent material. TEM, SEM, and CD indicated CNC chiral fragments within MC/CNC composite gel. Thus, their space-filling, thermoreversible assembly within the MC network can be used to tune the rheological properties and to access liquid crystalline properties at low CNC concentrations.

Control of the shape and size of iron oxide (α-Fe2O3) nanoparticles synthesized through the chemical precipitation method

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

Hematite (α-Fe2O3) nanoparticles were synthesized via a simple chemical precipitation method. The impact of varying the concentration of precursor on the crystalline phase, size and morphology of α-Fe2O3 products was explored. The characteristic of the synthesized hematite nanoparticles were evaluated by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR) spectroscopy, Raman spectroscopy, Differential Thermal Analysis (DTA), Thermo Gravimetric Analysis (TGA), Ultraviolet-Visible (UV-Vis) analysis and Photoluminescence (PL). XRD data revealed a rhombohedral (hexagonal) structure with the space group R-3c in all samples. Uniform spherical like morphology was confirmed by TEM and SEM. The result revealed that the particle sizes were varied between 21 and 82 nm and that the increase in precursor concentration (FeCl3, 6H2O) is accompanied by an increase in the particle size of 21 nm for pure α-Fe2O3 synthesized with [Fe3+] = 0.05 M at 82 nm for pure α-Fe2O3 synthesized with [Fe3+] = 0.4 M. FT-IR confirms the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we have synthesized pure hematite but also to identify their phonon modes. The thermal behavior of compound was studied by using TGA/DTA results: The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. Besides, the optical investigation revealed that samples have an optical gap of about 2.1 eV and that this value varies as a function of the precursor concentration.

Quantification of Nanoscale Density Fluctuations in Biological Cells/Tissues: Inverse Participation Ratio (IPR) Analysis of Transmission Electron Microscopy Images and Implications for Early-Stage Cancer Detection

NASA Astrophysics Data System (ADS)

Pradhan, Prabhakar; Damania, Dhwanil; Joshi, Hrushikesh; Taflove, Allen; Roy, Hemant; Dravid, Vinayak; Backman, Vadim

2010-03-01

We report a study of the nanoscale mass density fluctuations of biological cells and tissues by quantifying their nanoscale light-localization properties. Transmission electron microscope (TEM) images of human cells and tissues are used to construct corresponding effective disordered optical lattices. Light-localization properties are studied by statistical analysis of the inverse participation ratio (IPR) of the eigenfunctions of these optical lattices at the nanoscales. Our results indicate elevation of the nanoscale disorder strength (e.g., refractive index fluctuations) in early carcinogenesis. Importantly, our results demonstrate that the increase in the nanoscale disorder represents the earliest structural alteration in cells undergoing carcinogenesis known to-date. Potential applications of the technique for early stage cancer detection will be discussed.

Microstructural studies of 35 degrees C copper Ni-Ti orthodontic wire and TEM confirmation of low-temperature martensite transformation.

PubMed

Brantley, William A; Guo, Wenhua; Clark, William A T; Iijima, Masahiro

2008-02-01

Previous temperature-modulated differential scanning calorimetry (TMDSC) study of nickel-titanium orthodontic wires revealed a large exothermic low-temperature peak that was attributed to transformation within martensitic NiTi. The purpose of this study was to use transmission electron microscopy (TEM) to verify this phase transformation in a clinically popular nickel-titanium wire, identify its mechanism and confirm other phase transformations found by TMDSC, and to provide detailed information about the microstructure of this wire. The 35 degrees C Copper nickel-titanium wire (Ormco) with cross-section dimensions of 0.016 in. x 0.022 in. used in the earlier TMDSC investigation was selected. Foils were prepared for TEM analyses by mechanical grinding, polishing, dimpling, ion milling and plasma cleaning. Standard bright-field and dark-field TEM images were obtained, along with convergent-beam electron diffraction patterns. A cryo-stage with the electron microscope (Phillips CM 200) permitted the specimen to be observed at -187, -45, and 50 degrees C, as well as at room temperature. Microstructures were also observed with an optical microscope and a scanning electron microscope. Room temperature microstructures had randomly oriented, elongated grains that were twinned. Electron diffraction patterns confirmed that phase transformations took place over temperature ranges previously found by TMDSC. TEM observations revealed a high dislocation density and fine-scale oxide particles, and that twinning is the mechanism for the low-temperature transformation in martensitic NiTi. TEM confirmed the low-temperature peak and other phase transformations observed by TMDSC, and revealed that twinning in martensite is the mechanism for the low-temperature peak. The high dislocation density and fine-scale oxide particles in the microstructure are the result of the wire manufacturing process.

Optical properties of embedded metal nanoparticles at low temperatures

NASA Astrophysics Data System (ADS)

Heilmann, A.; Kreibig, U.

2000-06-01

Metal nanoparticles (gold, silver, copper) that are embedded in an insulating organic host material exhibit optical plasma resonance absorption in the visible and near-infrared region. The spectral position, the half width and the intensity of the plasma resonance absorption all depend on the particle size, the particle shape, and the optical behavior of the cluster and the host material. The optical extinction of various gold, silver or copper particle assemblies embedded in plasma polymer or gelatin was measured at 4.2 K and 1.2 K as well as at room temperature. The packing density of several samples was high enough to resolve a reversible increase of the plasma resonance absorption intensity towards lower temperatures. Additionally, at larger silver particles D_m > 50 nm a significant blue shift of the plasma resonance absorption was measured. Particle size and shape distribution were determined by transmission electron microscopy (TEM). For the first time, simultaneous measurements of the electrical and optical properties at one and the same particle assembly were performed at low temperatures. Contrary to the increasing optical extinction, the d.c. conductivity decreased to two orders of magnitude. At silver particles embedded in a plasma polymer made from thiophene a significant photocurrent was measured.

Photo-induced changes in nano-copper oxide for optoelectronic applications

NASA Astrophysics Data System (ADS)

Hendi, A. A.; Rashad, M.

2018-06-01

Copper oxide (CuO) nanoparticles (NPs) have been prepared using microwave irradiation. A mother material was copper nitrate in distilled water. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used for characterizing the NPs powders. Thermal Gravimetric Analysis (TGA) and Differential Thermal Analysis (DTA) were measured for as-prepared CuO NPs. The obtained oxides NPs were confirmed produced during chemical precipitation by these characterizions. These NPs were dropped on top of glass substrate for measuring the optical characterizions. Both linear and nonlinear optical properties of the as-prepared CuO NP films were studied. The optical energy gap of the as-prepared CuO NP films is equal to 3.98 eV, which is higher than that of the bulk material. The effect of ultraviolet (UV) light irradiation on the CuO NP films was investigated at 2 and 5 h for study the photo-induced effect. The optical properties of CuO NP films were measured as a function of these UV irradiation time. The optical constants for as-prepared and irradiated CuO NP films were calculated which reflect the affect of UV irradiation time. As observed from these optical results, a highly forced for optoelectronic applications.

Correlative Magnetic Imaging of Heat-Assisted Magnetic Recording Media in Cross Section Using Lorentz TEM and MFM

DOE PAGES

Kim, Taeho Roy; Phatak, Charudatta; Petford-Long, Amanda K.; ...

2017-10-23

In order to increase the storage density of hard disk drives, a detailed understanding of the magnetic structure of the granular magnetic layer is essential. Here, we demonstrate an experimental procedure of imaging recorded bits on heat-assisted magnetic recording (HAMR) media in cross section using Lorentz transmission electron microscopy (TEM). With magnetic force microscopy and focused ion beam (FIB), we successfully targeted a single track to prepare cross-sectional TEM specimens. Then, we characterized the magnetic structure of bits with their precise location and orientation using Fresnel mode of Lorentz TEM. Here, this method can promote understanding of the correlation betweenmore » bits and their material structure in HAMR media to design better the magnetic layer.« less

Correlative Magnetic Imaging of Heat-Assisted Magnetic Recording Media in Cross Section Using Lorentz TEM and MFM

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

Kim, Taeho Roy; Phatak, Charudatta; Petford-Long, Amanda K.

In order to increase the storage density of hard disk drives, a detailed understanding of the magnetic structure of the granular magnetic layer is essential. Here, we demonstrate an experimental procedure of imaging recorded bits on heat-assisted magnetic recording (HAMR) media in cross section using Lorentz transmission electron microscopy (TEM). With magnetic force microscopy and focused ion beam (FIB), we successfully targeted a single track to prepare cross-sectional TEM specimens. Then, we characterized the magnetic structure of bits with their precise location and orientation using Fresnel mode of Lorentz TEM. Here, this method can promote understanding of the correlation betweenmore » bits and their material structure in HAMR media to design better the magnetic layer.« less

Electron tomography of whole cultured cells using novel transmission electron imaging technique.

PubMed

Okumura, Taiga; Shoji, Minami; Hisada, Akiko; Ominami, Yusuke; Ito, Sukehiro; Ushiki, Tatsuo; Nakajima, Masato; Ohshima, Takashi

2018-01-01

Since a three-dimensional (3D) cellular ultrastructure is significant for biological functions, it has been investigated using various electron microscopic techniques. Although transmission electron microscopy (TEM)-based techniques are traditionally used, cells must be embedded in resin and sliced into ultrathin sections in sample preparation processes. Block-face observation using a scanning electron microscope (SEM) has also been recently applied to 3D observation of cellular components, but this is a destructive inspection and does not allow re-examination. Therefore, we developed electron tomography using a transmission electron imaging technique called Plate-TEM. With Plate-TEM, the cells cultured directly on a scintillator plate are inserted into a conventional SEM equipped with a Plate-TEM observation system, and their internal structures are observed by detecting scintillation light produced by electrons passing through the cells. This technology has the following four advantages. First, the cells cultured on the plate can be observed at electron-microscopic resolution since they remain on the plate. Second, both surface and internal information can be obtained simultaneously by using electron- and photo-detectors, respectively, because a Plate-TEM detector is installed in an SEM. Third, the cells on the scintillator plate can also be inspected using light microscopy because the plate has transparent features. Finally, correlative observation with other techniques, such as conventional TEM, is possible after Plate-TEM observation because Plate-TEM is a non-destructive analysis technique. We also designed a sample stage to tilt the samples for tomography with Plate-TEM, by which 3D organization of cellular structures can be visualized as a whole cell. In the present study, Mm2T cells were investigated using our tomography system, resulting in 3D visualization of cell organelles such as mitochondria, lipid droplets, and microvilli. Correlative observations with various imaging techniques were also conducted by successive observations with light microscopy, SEM, Plate-TEM, and conventional TEM. Consequently, the Plate-TEM tomography technique encourages understanding of cellular structures at high resolution, which can contribute to cellular biological research. Copyright © 2017 Elsevier Ltd. All rights reserved.

Optical absorption and TEM studies of silver nanoparticle embedded BaO-CaF{sub 2}-P{sub 2}O{sub 5} glasses

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

Narayanan, Manoj Kumar, E-mail: manukokkal01@gmail.com; Shashikala, H. D.

Silver nanoparticle embedded 30BaO-20CaF{sub 2}-50P{sub 2}O{sub 5}-4Ag{sub 2}O-4SnO glasses were prepared by melt-quenching and subsequent heat treatment process. Silver-doped glasses were heat treated at temperatures 500 °C, 525°C and 550 °C for a fixed duration of 10 hours to incorporate metal nanoparticles into the glass matrix. Appearance and shift in peak positions of the surface plasmon resonance (SPR) bands in the optical absorption spectra of heat treated glass samples indicated that both formation and growth of nanoparticle depended on heat treatment temperature. Glass sample heat treated at 525 °C showed a SPR peak around 3 eV, which indicated that sphericalmore » nanoparticles smaller than 20 nm were formed inside the glass matrix. Whereas sample heat treated at 550 °C showed a size dependent red shift in SPR peak due to the presence of silver nanoparticles of size larger than 20 nm. Size of the nanoparticles calculated using full-width at half-maximum (FWHM) of absorption band showed a good agreement with the particle size obtained from transmission electron microscopy (TEM) analysis.« less

Green synthesis and characterization of ANbO3 (A = Na, K) nanopowders fabricated using a biopolymer

NASA Astrophysics Data System (ADS)

Khorrami, Gh. H.; Mousavi, M.; Khayatian, S. A.; Kompany, A.; Khorsand Zak, A.

2017-10-01

Lead-free sodium niobate (NaNbO3, NN) and potassium niobate (KNbO3, KN) nanopowders were successfully synthesized by a simple and green synthesis process in gelatin media. Gelatin, which is a biopolymer, was used as stabilizer. In order to determine the lowest calcination temperature needed to obtain pure NN and KN nanopowders, the produced gels were analyzed by thermogravometric analyzer (TGA). The produced gels were calcined at 500∘C and 600∘C. The structural and optical properties of the prepared powders were examined using X-ray diffraction (XRD) technique, transmission electron microscopy (TEM), and UV-Vis spectroscopy. The XRD results revealed that pure phase NN and KN nanopowders were formed at low temperature calcination of 500∘C and 600∘C, respectively. The Scherrer formula and size-strain plot (SSP) method were employed to estimate crystallite size and lattice strain of the samples. The TEM images show that the NN and KN samples calcined at 600∘C have cubic shape with an average particle size of 60.95 and 39.29 nm, respectively. The optical bandgap energy of the samples was calculated using UV-Vis diffused reflectance spectra of the samples and Kubelka-Munck relation.

Rapid and solvent-free solid-state synthesis and characterization of Zn3V2O8 nanostructures and their phenol red aqueous solution photodegradation

NASA Astrophysics Data System (ADS)

Mazloom, Fatemeh; Masjedi-Arani, Maryam; Salavati-Niasari, Masoud

2017-08-01

Zinc vanadate (Zn3V2O8) nanostructures have been successfully synthesized via simple, rapid and solvent-free solid-state method by using different complex precursors of Zn and NH4VO3 as novel starting materials. Effects of various zinc (II) Schiff base complex precursors and calcination temperatures were investigated to reach optimum condition. It was found that particle size and optical property of the as-prepared products could be greatly influenced via these parameters. The products were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectra, energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Photoluminescence and ultraviolet-visible (UV-Vis) spectroscopy. The photocatalytic activity of zinc vanadate nano and bulk structures were compared by degradation of phenol red aqueous solution.

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

NASA Astrophysics Data System (ADS)

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

2010-10-01

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

Effect of Ce doping on structural, optical and photocatalytic properties of ZnO nano-structures.

PubMed

Selvam, N Clament Sagaya; Vijaya, J Judith; Kennedy, L John

2014-03-01

A novel self-assembled pure and Ce doped ZnO nano-particles (NPs) were successfully synthesized by a simple low temperature co-precipitation method. The prepared photocatalysts were characterized by X-ray diffraction (XRD), High resolution scanning electron microscopy (HR-SEM), High resolution transmission electron microscopy (HR-TEM), diffuse reflectance spectroscopy (DRS) and Photoluminescence (PL) spectroscopy. The results indicated that the prepared photocatalysts shows a novel morphology, high crystallinity, uniform size distribution, and more defects. Photocatalytic degradation (PCD) of nonylphenol, a potent endocrine disrupting chemical in aqueous medium was investigated. Higher amount of oxygen defects exhibits enhanced PCD of nonylphenol. In addition, the influence of the Ce contents on the structure, morphology, absorption, emission and photocatalytic activity of ZnO nanoparticles (NPs) were investigated systematically. The relative PCD efficiency of pure ZnO, Ce-doped ZnO NPs and commercial TiO2 (Degussa P-25) have also been discussed.

Synthesis and characterization of Copper/Cobalt/Copper/Iron nanostructurated films with magnetoresistive properties

NASA Astrophysics Data System (ADS)

Ciupinǎ, Victor; Prioteasa, Iulian; Ilie, Daniela; Manu, Radu; Petrǎşescu, Lucian; Tutun, Ştefan Gabriel; Dincǎ, Paul; MustaÅ£ǎ, Ion; Lungu, Cristian Petricǎ; Jepu, IonuÅ£; Vasile, Eugeniu; Nicolescu, Virginia; Vladoiu, Rodica

2017-02-01

Copper/Cobalt/Copper/Iron thin films were synthesized in order to obtain nanostructured materials with special magnetoresistive properties. The multilayer films were deposited on silicon substrates. In this respect we used Thermionic Vacuum Arc Discharge Method (TVA). The benefit of this deposition technique is the ability to have a controlled range of thicknesses starting from few nanometers to hundreds of nanometers. The purity of the thin films was insured by a high vacuum pressure and a lack of any kind of buffer gas inside the coating chamber. The morphology and structure of the thin films were analyzed using Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) Techniques and Energy Dispersive X-ray Spectroscopy (EDXS). Magnetoresistive measurement results depict that thin films possess Giant Magneto-Resistance Effect (GMR). Magneto-Optic-Kerr Effect (MOKE) studies were performed to characterize the magnetic properties of these thin films.

Large-scale preparation of strawberry-like, AgNP-doped SiO2 microspheres using the electrospraying method

NASA Astrophysics Data System (ADS)

Ma, Zhijun; Ji, Huijiao; Tan, Dezhi; Dong, Guoping; Teng, Yu; Zhou, Jiajia; Guan, Miaojia; Qiu, Jianrong; Zhang, Ming

2011-07-01

In this paper, we report on a novel strategy for the preparation of silver nanoparticle-doped SiO2 microspheres (Ag-SMSs) with an interesting strawberry-like morphology using a simple and efficient electrospraying method. SEM (scanning electron microscopy), TEM (transmission electron microscopy), XRD (x-ray diffraction), EDS (energy-dispersive spectroscopy) and UV-vis spectra (ultraviolet-visible spectra) were applied to investigate the morphology, structure, composition and optical properties of the hybrid microspheres, and E. coli (Escherichia coli) was used as a model microbe to evaluate their antibacterial ability. The results showed that the Ag-SMSs were environmentally stable and washing resistant. The Ag-SMSs exhibited effective inhibition against proliferation of E. coli, and their antibacterial ability could be well preserved for a long time. The environmental stability, washing resistance, efficient antibacterial ability and simple but productive preparation method endowed the Ag-SMSs with great potential for practical biomedical applications.

Preparation and characterization of ultrafine nanoparticles of Cu doped lithium tetraborate

NASA Astrophysics Data System (ADS)

Khalilzadeh, Nasrin; Saion, Elias Bin; Mirabolghasemi, Hamed; Crouse, Karen A.; Shaari, Abdul Halim Bin; Hashim, Mansor Bin

This study details an innovative single-step thermal synthesis of nano-sized lithium tetraborate doped with 0.1 %wt copper and its characterization. The heating temperature for the synthesis of the nanoparticle material was optimized by variation between 200 and 850 °C. The optimum amount of polyvinyl pyrrolidone (PVP) the capping agent was determined to be 0.027 mol per 1 g LTB-Cu. The calcination time was 2 h. Characterization of the samples was carried out using Thermogravimetry Analysis (TGA), Derivative Thermogravimetry (DTG), Differential Scanning Calorimetry (DSC), Fourier Transform Infrared (FTIR) Spectroscopy, X-ray diffractometer (XRD), transmission electron microscopy (TEM) and Ultraviolet-Visible (UV-Vis) spectroscopy. The product was thermally stable above 450 °C. FTIR, XRD and TEM results confirmed the formation of pure nano-crystalline copper doped lithium tetraborate between 450 and 750 °C. The optical bandgap was estimated to be 5.02-6.05 eV in the presence of different amounts of PVP at various calcination temperatures.

Spectroscopic ellipsometry analysis of nanocrystalline silicon carbide obtained at low temperature

NASA Astrophysics Data System (ADS)

Kerdiles, S.; Madelon, R.; Rizk, R.

2001-12-01

Thin films of silicon carbide obtained by hydrogen-reactive magnetron sputtering with various substrate temperatures TS (100-600 °C) were analysed by transmission electron microscopy (TEM) and spectroscopic ellipsometry (SE). The TEM images show evidence of the growth of hydrogenated nanocrystalline silicon carbide (nc-SiC:H) deposited at TS as low as 300 °C, with an average grain size of 4-5 nm. The SE spectra were reproduced by using the Forouhi-Bloomer model and assuming a 7 nm thick overlayer with a void fraction of 45%. The observed increase of the refractive index with TS is assigned to the improvement of both crystallinity and compactness of the layer. The expected increase of the optical gap seems to be offset by the drop of hydrogen content, leaving the gap unchanged. The fabrication and characteristics of nc-SiC:H/c-Si diode are finally described and the data indicate a good rectifying behaviour, together with a low leakage current.

Hexagonal OsB 2: Sintering, microstructure and mechanical properties

DOE PAGES

Xie, Zhilin; Lugovy, Mykola; Orlovskaya, Nina; ...

2015-02-07

In this study, the metastable high pressure ReB 2-type hexagonal OsB 2 bulk ceramics was produced by spark plasma sintering. The phase composition, microstructure, and mechanical behavior of the sintered OsB 2 were studied by X-ray diffraction, optical microscopy, TEM, SEM, EDS, and nanoindentation. The produced ceramics was rather porous and contained a mixture of hexagonal (~80 wt.%) and orthorhombic (~20 wt.%) phases as identified by X-ray diffraction and EBSD analysis. Two boron-rich phases, which do not contain Os, were also identified by TEM and SEM/EDS analysis. Nanoindentation measurements yielded a hardness of 31 ± 9 GPa and Young’s modulusmore » of 574 ± 112 GPa, indicating that the material is rather hard and very stiff; but, it is very prone to crack formation and propagation, which is indicative of a very brittle nature of this material. Improvements in the sintering regime are required in order to produce dense, homogeneous and single phase hexagonal OsB 2 bulk ceramics.« less

Biodegradable Polycaprolactone-Titania Nanocomposites: Preparation, Characterization and Antimicrobial Properties

PubMed Central

Muñoz-Bonilla, Alexandra; Cerrada, María L.; Fernández-García, Marta; Kubacka, Anna; Ferrer, Manuel; Fernández-García, Marcos

2013-01-01

Nanocomposites obtained from the incorporation of synthesized TiO2 nanoparticles (≈10 nm average primary particle size) in different amounts, ranging from 0.5 to 5 wt.%, into a biodegradable polycaprolactone matrix are achieved via a straightforward and commercial melting processing. The resulting nanocomposites have been structurally and thermally characterized by transmission electron microscopy (TEM), wide/small angle X-ray diffraction (WAXS/SAXS, respectively) and differential scanning calorimetry (DSC). TEM evaluation provides evidence of an excellent nanometric dispersion of the oxide component in the polymeric matrix, with aggregates having an average size well below 100 nm. Presence of these TiO2 nanoparticles induces a nucleant effect during polymer crystallization. Moreover, the antimicrobial activity of nanocomposites has been tested using both UV and visible light against Gram-negative Escherichia coli bacteria and Gram-positive Staphylococcus aureus. The bactericidal behavior has been explained through the analysis of the material optical properties, with a key role played by the creation of new electronic states within the polymer-based nanocomposites. PMID:23629663

Antibacterial activity and morphological changes of Pseudomonas aeruginosa cells after exposure to Vernonia cinerea extract.

PubMed

Latha, Lachimanan Yoga; Darah, Ibrahim; Kassim, Mohd Jain Noordin Mohd; Sasidharan, Sreenivasan

2010-08-01

The antibacterial activity of Vernonia cinerea (L.) extract was investigated using the broth dilution method. The extract showed a favorable antimicrobial activity against Pseudomonas aeruginosa with a minimum inhibition concentration (MIC) value of 3.13 mg/mL. V. cinerea extract at (1/2), 1, or 2 times the MIC significantly inhibited bacterial growth with a noticeable drop in optical density (OD) of the bacterial culture, thus confirming the antibacterial activity of the extract on P. aeruginosa. Imaging using scanning (SEM) and transmission (TEM) electron microscopy was done to determine the major alterations in the microstructure of the extract-treated P. aeruginosa. The main abnormalities noted via SEM and TEM studies were the alteration in morphology of the bacterial cells. The main reason for this destruction was the severe alterations of the cell wall with the formation of holes, invaginations, and morphological disorganization caused by the extract. The authors conclude that the extract may be used as a candidate for the development of antimicrobial agents.

In situ TEM Raman spectroscopy and laser-based materials modification.

PubMed

Allen, F I; Kim, E; Andresen, N C; Grigoropoulos, C P; Minor, A M

2017-07-01

We present a modular assembly that enables both in situ Raman spectroscopy and laser-based materials processing to be performed in a transmission electron microscope. The system comprises a lensed Raman probe mounted inside the microscope column in the specimen plane and a custom specimen holder with a vacuum feedthrough for a tapered optical fiber. The Raman probe incorporates both excitation and collection optics, and localized laser processing is performed using pulsed laser light delivered to the specimen via the tapered optical fiber. Precise positioning of the fiber is achieved using a nanomanipulation stage in combination with simultaneous electron-beam imaging of the tip-to-sample distance. Materials modification is monitored in real time by transmission electron microscopy. First results obtained using the assembly are presented for in situ pulsed laser ablation of MoS 2 combined with Raman spectroscopy, complimented by electron-beam diffraction and electron energy-loss spectroscopy. Copyright © 2016 Elsevier B.V. All rights reserved.

Structure comparison of PMN-PT and PMN-PZT nanocrystals prepared by gel-combustion method at optimized temperatures

NASA Astrophysics Data System (ADS)

Ghasemifard, M.; Hosseini, S. M.; Bagheri-Mohagheghi, M. M.; Shahtahmasbi, N.

2009-09-01

We have synthesized and were performed a comparison of structures and optical properties between relaxor ferroelectric PMN-PT and PMN-PZT nanopowders. A gel-combustion method has been used to synthesize PMN-PT and PMN-PZT nanocrystalline with the perovskite structure. The precursors employed in the gel-combustion process were lead nitrate, magnesium acetate, niobium ammonium oxalate and zirconium nitrate. The nanopowders were characterized using the X-ray diffraction (XRD) and transmission electron microscopy (TEM) observation. Fourier transform infrared (FTIR) spectroscopy was employed to monitor the transformation of precursor solutions during the thermal reactions leading to the formation of perovskite phase.

Spectral analysis of scattered light from flowers' petals

NASA Astrophysics Data System (ADS)

Ozawa, Atsumi; Uehara, Tomomi; Sekiguchi, Fumihiko; Imai, Hajime

2009-07-01

A new method was developed for studying absorption characteristics of opaque samples based on the light scattering spectroscopy. Measurements were made in white, red and violet petals of Petunia hybrida, and gave the absorption spectra in a non-destructive manner without damaging the cell structures of the petal. The red petal has absorption peak at 550 nm and the violet has three absorption peaks: at 450, 670, and 550 nm. The results were discussed in correlation with the microscopic cell structures of the petal observed with optical microscope and transmission electron microscopy (TEM). Only the cells placed in the surface have the pigments giving the color of the petal.

Thermal magnetic field noise: electron optics and decoherence.

PubMed

Uhlemann, Stephan; Müller, Heiko; Zach, Joachim; Haider, Max

2015-04-01

Thermal magnetic field noise from magnetic and non-magnetic conductive parts close to the electron beam recently has been identified as a reason for decoherence in high-resolution transmission electron microscopy (TEM). Here, we report about new experimental results from measurements for a layered structure of magnetic and non-magnetic materials. For a simplified version of this setup and other situations we derive semi-analytical models in order to predict the strength, bandwidth and spatial correlation of the noise fields. The results of the simulations are finally compared to previous and new experimental data in a quantitative manner. Copyright © 2014 Elsevier B.V. All rights reserved.

UV-visible light-activated Ag-decorated, monodisperse TiO2 aggregates for treatment of the pharmaceutical oxytetracycline.

PubMed

Han, Changseok; Likodimos, Vlassis; Khan, Javed Ali; Nadagouda, Mallikarjuna N; Andersen, Joel; Falaras, Polycarpos; Rosales-Lombardi, Pablo; Dionysiou, Dionysios D

2014-10-01

Noble metal Ag-decorated, monodisperse TiO2 aggregates were successfully synthesized by an ionic strength-assisted, simple sol-gel method and were used for the photocatalytic degradation of the antibiotic oxytetracycline (OTC) under both UV and visible light (UV-visible light) irradiation. The synthesized samples were characterized by X-ray diffraction analysis (XRD); UV-vis diffuse reflectance spectroscopy; environmental scanning electron microscopy (ESEM); transmission electron microscopy (TEM); high-resolution TEM (HR-TEM); micro-Raman, energy-dispersive X-ray spectroscopy (EDS); and inductively coupled plasma optical emission spectrometry (ICP-OES). The results showed that the uniformity of TiO2 aggregates was finely tuned by the sol-gel method, and Ag was well decorated on the monodisperse TiO2 aggregates. The absorption of the samples in the visible light region increased with increasing Ag loading that was proportional to the amount of Ag precursor added in the solution over the tested concentration range. The Brunauer, Emmett, and Teller (The BET) surface area slightly decreased with increasing Ag loading on the TiO2 aggregates. Ag-decorated TiO2 samples demonstrated enhanced photocatalytic activity for the degradation of OTC under UV-visible light illumination compared to that of pure TiO2. The sample containing 1.9 wt% Ag showed the highest photocatalytic activity for the degradation of OTC under both UV-visible light and visible light illumination. During the experiments, the detected Ag leaching for the best TiO2-Ag photocatalyst was much lower than the National Secondary Drinking Water Regulation for Ag limit (0.1 mg L(-1)) issued by the US Environmental Protection Agency.

Microstructure analysis in the coupling region of fiber coupler with a novel electrical micro-heater

NASA Astrophysics Data System (ADS)

Shuai, Cijun; Gao, Chengde; Nie, Yi; Hu, Huanlong; Peng, Shuping

2011-12-01

Fused-tapered fiber coupler is widely used in optical-fiber communication, optical-fiber sensor and optical signal processing. Its optical performance is mainly determined by the glass properties in the coupling region. In this study, the effect of fused biconical taper (FBT) process on glass microstructure of fiber coupler was investigated by testing the microstructure of the cross-section of coupling region. The fiber coupler is fabricated with a novel home-designed electrical heater. Our experimental results show that the boundary between fiber core and fiber cladding become vague or indistinct after FBT under transmission electron microscopy (TEM) and Ge 2+ in fiber core diffuses into fiber cladding. Crystallizations are observed in coupling region under scanning electron microscope (SEM) and microscopic infrared (IR), and the micro crystallizations become smaller with the drawing speed increasing. The wave number of fiberglass increases after FBT and it is in proportion to the drawing speed. The analysis of the microstructure in the coupling region explored the mechanism of the improvement in the performance of fiber couplers which can be used for the guidance of fabrication process.

Investigation on structural, thermal, optical and sensing properties of meta-stable hexagonal MoO(3) nanocrystals of one dimensional structure.

PubMed

Chithambararaj, Angamuthuraj; Bose, Arumugam Chandra

2011-01-01

Hexagonal molybdenum oxide (h-MoO(3)) was synthesized by a solution based chemical precipitation technique. Analysis by X-ray diffraction (XRD) confirmed that the as-synthesized powder had a metastable hexagonal structure. The characteristic vibrational band of Mo-O was identified from Fourier transform infrared spectroscopy (FT-IR). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images clearly depicted the morphology and size of h-MoO(3.) The morphology study showed that the product comprises one-dimensional (1D) hexagonal rods. From the electron energy loss spectroscopy (EELS) measurement, the elemental composition was investigated and confirmed from the characteristic peaks of molybdenum and oxygen. Thermogravimetric (TG) analysis on metastable MoO(3) revealed that the hexagonal phase was stable up to 430 °C and above this temperature complete transformation into a highly stable orthorhombic phase was achieved. The optical band gap energy was estimated from the Kubelka-Munk (K-M) function and was found to be 2.99 eV. Finally, the ethanol vapor-sensing behavior was investigated and the sensing response was found to vary linearly as a function of ethanol concentration in the parts per million (ppm) range.

Synthesis, spectral and thermal studies of pyridyl adducts of Zn(II) and Cd(II) dithiocarbamates, and their use as single source precursors for ZnS and CdS nanoparticles.

PubMed

Onwudiwe, Damian C; Strydom, Christien A; Oluwafemi, Oluwatobi S; Hosten, Eric; Jordaan, Anine

2014-06-21

The synthesis, spectroscopic characterisation, and thermal studies of pyridyl adducts of Zn(II) and Cd(II) complexes of N-ethyl-N-phenyl dithiocarbamate, represented as [ZnL2py] and [CdL2py2], are reported. Single-crystal X-ray structural analysis of the Zn compound showed that it is five-coordinate with four sulphurs from dithiocarbamate and one nitrogen from pyridine in a distorted square pyramidal geometry. The thermogravimetric studies indicate that the zinc and cadmium compounds undergo fast weight loss, and the temperature at maximum rate of decomposition is at 277 °C and 265 °C respectively, to give the metal (Zn or Cd) sulphide residues. These compounds were used as single molecule precursors to produce nanocrystalline MS (M = Zn, Cd) after thermolysis in hexadecylamine. The morphological and optical properties of the resulting MS nanocrystallites were investigated using transmission electron microscopy (TEM), scanning electron microscopy (SEM), UV-Vis absorption and photoluminescence (PL) spectroscopy, and powdered X-ray diffraction (XRD). By varying the growth time, the temporal evolution of the optical properties and morphology of the nanocrystals were investigated.

Novel synthesis and characterization of pristine Cu nanoparticles for the non-enzymatic glucose biosensor.

PubMed

Dayakar, T; Rao, K Venkateswara; Bikshalu, K; Rajendar, V; Park, Si-Hyun

2017-07-01

Non enzymatic electrochemical glucose sensing was developed based on pristine Cu Nanopartilces (NPs)/Glassy Carbon Electrode (GCE) which can be accomplished by simple green method via ocimum tenuiflorum leaf extract. Then, the affect of leaf extract addition on improving Structural, Optical and electrochemical properties of pristine cu NPs was investigated. The synthesized Cu NPs were characterized with X-ray diffraction (X-ray), Uv-Visible spectroscopy (Uv-Vis), Fourier transformation infrared spectroscopy (FTIR), Particle size distribution (PSA), Scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDS), Transmission electron microscopy (TEM) for structural optical and morphological studies respectively. The synthesized Cu NPs were coated over glassy carbon electrode (GCE) to study the electrochemical response of glucose by cyclic voltammetry and ampherometer. The results indicates that the modified biosensor shows a remarkable sensitivity (1065.21 μA mM -1  cm -2 ), rapid response time (<3s), wide linear range (1 to 7.2 mM), low detection limit (0.038 μM at S/N = 3). Therefore, the prepared Cu NPs by the Novel Bio-mediated route were exploited to construct a non-enzymatic glucose biosensor for sustainable clinical field applications.

Innovative Linear Low Density Polyethylene Nanocomposite Films Reinforced with Organophilic Layered Double Hydroxides: Fabrication, Morphology and Enhanced Multifunctional Properties.

PubMed

Xie, Jiazhuo; Wang, Haijun; Wang, Zhou; Zhao, Qinghua; Yang, Yuechao; Waterhouse, Geoffrey I N; Hao, Lei; Xiao, Zihao; Xu, Jing

2018-01-08

Herein, we reported the successful development of novel nanocomposite films based on linear low density polyethylene (LLDPE) with enhanced anti-drop, optical, mechanical, thermal and water vapor barrier properties by introducing organophilic layered double hydroxides (OLDHs) nanosheets. OLDHs loadings were varied from 0-6 wt.%. Structural analyses using the Fourier transform infrared spectrum (FT-IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) indicated that the OLDHs nanosheets were homogeneously dispersed with an ordered alignment in the LLDPE matrix. The LLDPE film containing 2 wt.% OLDHs (denoted as OLDHs-2) showed the optimal mechanical, thermal and water vapor barrier properties, whilst the anti-drop and optical performance of the films improved with increasing OLDHs content. The enhanced antidrop properties of the composite films relative to pristine LLDPE can be expected to effectively reduce agricultural losses to disease when the films are applied as agricultural films, whilst the superior light transmittance and water-retaining properties of the composite films will boost agricultural production. Results presented suggest that multifunctional LLDPE/OLDHs nanocomposites show great promise as low cost agricultural plastic films.

Effect of Zn doping on structural, optical and thermal properties of CeO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ramasamy, V.; Vijayalakshmi, G.

2015-09-01

The undoped and Zn doped CeO2 nanoparticles were synthesized by chemical precipitation method at room temperature. The undoped and Zn doped CeO2 nanoparticles have been characterized by X-ray powder diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), ultraviolet visible and photoluminescence (PL) spectroscopy, Fourier transform infrared spectroscopy (FTIR) and thermogravimetry and differential thermal analysis (TG-DTA). The cubic fluorite structures of the CeO2 nanoparticles were determined by XRD. The influence of particle size on structural parameters such as lattice parameter (a), inter planar distance (d), dislocation density (δ), microstrain (ε), lattice strain (η) and texture co-efficient (TC) were also determined. The lattice strains were determined by Williamson-Hall plot method. The effect of Zn doping with shifting of the bands were observed by UV-Vis spectroscopy and also their optical band gap were determined. The emission spectra and energy band diagram of the undoped and Zn doped samples were derived from PL spectroscopy. The structural bond vibrations of undoped and Zn doped CeO2 nanoparticles were analyzed by FTIR spectroscopy. The thermal property (weight loss and decomposition) of the sample is observed by TG-DTA curve.

Correlative fluorescence microscopy and scanning transmission electron microscopy of quantum-dot-labeled proteins in whole cells in liquid.

PubMed

Dukes, Madeline J; Peckys, Diana B; de Jonge, Niels

2010-07-27

Correlative fluorescence microscopy and transmission electron microscopy (TEM) is a state-of-the-art microscopy methodology to study cellular function, combining the functionality of light microscopy with the high resolution of electron microscopy. However, this technique involves complex sample preparation procedures due to its need for either thin sections or frozen samples for TEM imaging. Here, we introduce a novel correlative approach capable of imaging whole eukaryotic cells in liquid with fluorescence microscopy and with scanning transmission electron microscopy (STEM); there is no additional sample preparation necessary for the electron microscopy. Quantum dots (QDs) were bound to epidermal growth factor (EGF) receptors of COS7 fibroblast cells. Fixed whole cells in saline water were imaged with fluorescence microscopy and subsequently with STEM. The STEM images were correlated with fluorescence images of the same cellular regions. QDs of dimensions 7x12 nm were visible in a 5 microm thick layer of saline water, consistent with calculations. A spatial resolution of 3 nm was achieved on the QDs.

Correlative Fluorescence Microscopy and Scanning Transmission Electron Microscopy of Quantum Dot Labeled Proteins in Whole Cells in Liquid

PubMed Central

Dukes, Madeline J.; Peckys, Diana B.; de Jonge, Niels

2010-01-01

Correlative fluorescence microscopy and transmission electron microscopy (TEM) is a state-of-the-art microscopy methodology to study cellular function, combining the functionality of light microscopy with the high resolution of electron microscopy. However, this technique involves complex sample preparation procedures due to its need for either thin sections or frozen samples for TEM imaging. Here, we introduce a novel correlative approach capable of imaging whole eukaryotic cells in liquid with fluorescence microscopy and with scanning transmission electron microscopy (STEM); there is no additional sample preparation necessary for the electron microscopy. Quantum dots (QDs) were bound to epidermal growth factor (EGF) receptors of COS7 fibroblast cells. Fixed whole cells in saline water were imaged with fluorescence microscopy and subsequently with STEM. The STEM images were correlated with fluorescence images of the same cellular regions. QDs of dimensions 7 × 12 nm were visible in a 5 μm thick layer of saline water, consistent with calculations. A spatial resolution of 3 nm was achieved on the QDs. PMID:20550177

Electron holography—basics and applications

NASA Astrophysics Data System (ADS)

Lichte, Hannes; Lehmann, Michael

2008-01-01

Despite the huge progress achieved recently by means of the corrector for aberrations, allowing now a true atomic resolution of 0.1 nm, hence making it an unrivalled tool for nanoscience, transmission electron microscopy (TEM) suffers from a severe drawback: in a conventional electron micrograph only a poor phase contrast can be achieved, i.e. phase structures are virtually invisible. Therefore, conventional TEM is nearly blind for electric and magnetic fields, which are pure phase objects. Since such fields provoked by the atomic structure, e.g. of semiconductors and ferroelectrics, largely determine the solid state properties, hence the importance for high technology applications, substantial object information is missing. Electron holography in TEM offers the solution: by superposition with a coherent reference wave, a hologram is recorded, from which the image wave can be completely reconstructed by amplitude and phase. Now the object is displayed quantitatively in two separate images: one representing the amplitude, the other the phase. From the phase image, electric and magnetic fields can be determined quantitatively in the range from micrometre down to atomic dimensions by all wave optical methods that one can think of, both in real space and in Fourier space. Electron holography is pure wave optics. Therefore, we discuss the basics of coherence and interference, the implementation into a TEM, the path of rays for recording holograms as well as the limits in lateral and signal resolution. We outline the methods of reconstructing the wave by numerical image processing and procedures for extracting the object properties of interest. Furthermore, we present a broad spectrum of applications both at mesoscopic and atomic dimensions. This paper gives an overview of the state of the art pointing at the needs for further development. It is also meant as encouragement for those who refrain from holography, thinking that it can only be performed by specialists in highly specialized laboratories. In fact, a modern TEM built for atomic resolution and equipped with a field emitter or a Schottky emitter, well aligned by a skilled operator, can deliver good holograms. Running commercially available image processing software and mathematics programs on a laptop-computer is sufficient for reconstruction of the amplitude and phase images and extracting desirable object information.

Imaging plasmodesmata with high-resolution scanning electron microscopy.

PubMed

Barton, Deborah A; Overall, Robyn L

2015-01-01

High-resolution scanning electron microscopy (HRSEM) is an effective tool to investigate the distribution of plasmodesmata within plant cell walls as well as to probe their complex, three-dimensional architecture. It is a useful alternative to traditional transmission electron microscopy (TEM) in which plasmodesmata are sectioned to reveal their internal substructures. Benefits of adopting an HRSEM approach to studies of plasmodesmata are that the specimen preparation methods are less complex and time consuming than for TEM, many plasmodesmata within a large region of tissue can be imaged in a single session, and three-dimensional information is readily available without the need for reconstructing TEM serial sections or employing transmission electron tomography, both of which are lengthy processes. Here we describe methods to prepare plant samples for HRSEM using pre- or postfixation extraction of cellular material in order to visualize plasmodesmata embedded within plant cell walls.

Quantification of transendothelial migration using three-dimensional confocal microscopy.

PubMed

Cain, Robert J; d'Água, Bárbara Borda; Ridley, Anne J

2011-01-01

Migration of cells across endothelial barriers, termed transendothelial migration (TEM), is an important cellular process that underpins the pathology of many disease states including chronic inflammation and cancer metastasis. While this process can be modeled in vitro using cultured cells, many model systems are unable to provide detailed visual information of cell morphologies and distribution of proteins such as junctional markers, as well as quantitative data on the rate of TEM. Improvements in imaging techniques have made microscopy-based assays an invaluable tool for studying this type of detailed cell movement in physiological processes. In this chapter, we describe a confocal microscopy-based method that can be used to assess TEM of both leukocytes and cancer cells across endothelial barriers in response to a chemotactic gradient, as well as providing information on their migration into a subendothelial extracellular matrix, designed to mimic that found in vivo.

Controlling of ZnO nanostructures by solute concentration and its effect on growth, structural and optical properties

NASA Astrophysics Data System (ADS)

Kumar, Yogendra; Rana, Amit Kumar; Bhojane, Prateek; Pusty, Manojit; Bagwe, Vivas; Sen, Somaditya; Shirage, Parasharam M.

2015-10-01

ZnO nanostructured films were prepared by a chemical bath deposition method on glass substrates without any assistance of either microwave or high pressure autoclaves. The effect of solute concentration on the pure wurtzite ZnO nanostructure morphologies is studied. The control of the solute concentration helps to control the nanostructure to form nano-needles, and -rods. X-ray diffraction (XRD) studies revealed highly c-axis oriented thin films. Scanning electron microscopy (SEM) confirms the modification of the nanostructure dependent on the concentration. Transmission electron microscopy (TEM) results show the single crystalline electron diffraction pattern, indicating high quality nano-material. UV-vis results show the variation in the band gap from 3.20 eV to 3.14 eV with increasing concentration as the nanostructures change from needle- to rod-like. Photoluminescence (PL) data indicate the existence of defects in the nanomaterials emitting light in the yellow-green region, with broad UV and visible spectra. A sharp and strong peak is observed at ˜438 cm-1 by Raman spectroscopy, assigned to the {{{{E}}}2}{{high}} optical mode of ZnO, the characteristic peak for the highly-crystalline wurtzite hexagonal phase. The solute concentration significantly affects the formation of defect states in the nanostructured films, and as a result, it alters the structural and optical properties. Current-voltage characteristics alter with the measurement environment, indicating potential sensor applications.

Single Step In Situ Synthesis and Optical Properties of Polyaniline/ZnO Nanocomposites

PubMed Central

Kaith, B. S.; Rajput, Jaspreet

2014-01-01

Polyaniline/ZnO nanocomposites were prepared by in situ oxidative polymerization of aniline monomer in the presence of different weight percentages of ZnO nanostructures. The steric stabilizer added to prevent the agglomeration of nanostructures in the polymer matrix was found to affect the final properties of the nanocomposite. ZnO nanostructures of various morphologies and sizes were prepared in the absence and presence of sodium lauryl sulphate (SLS) surfactant under different reaction conditions like in the presence of microwave radiation (microwave oven), under pressure (autoclave), under vacuum (vacuum oven), and at room temperature (ambient condition). The conductivity of these synthesized nanocomposites was evaluated using two-probe method and the effect of concentration of ZnO nanostructures on conductivity was observed. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and UV-visible (UV-VIS) spectroscopy techniques were used to characterize nanocomposites. The optical energy band gap of the nanocomposites was calculated from absorption spectra and ranged between 1.5 and 3.21 eV. The reported values depicted the blue shift in nanocomposites as compared to the band gap energies of synthesized ZnO nanostructures. The present work focuses on the one-step synthesis and potential use of PANI/ZnO nanocomposite in molecular electronics as well as in optical devices. PMID:24523653

Preparation, characterization, and optical properties of gold, silver, and gold-silver alloy nanoshells having silica cores.

PubMed

Kim, Jun-Hyun; Bryan, William W; Lee, T Randall

2008-10-07

This report describes the structural and optical properties of a series of spherical shell/core nanoparticles in which the shell is comprised of a thin layer of gold, silver, or gold-silver alloy, and the core is comprised of a monodispersed silica nanoparticle. The silica core particles were prepared using the Stöber method, functionalized with terminal amine groups, and then seeded with small gold nanoparticles (approximately 2 nm in diameter). The gold-seeded silica particles were coated with a layer of gold, silver, or gold-silver alloy via solution-phase reduction of an appropriate metal ion or mixture of metal ions. The size, morphology, and elemental composition of the composite nanoparticles were characterized by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, thermal gravimetric analysis (TGA), dynamic light scattering (DLS), and transmission electron microscopy (TEM). The optical properties of the nanoparticles were analyzed by UV-vis spectroscopy, which showed strong absorptions ranging from 400 nm into the near-IR region, where the position of the plasmon band reflected not only the thickness of the metal shell, but also the nature of the metal comprising the shell. Importantly, the results demonstrate a new strategy for tuning the position of the plasmon resonance without having to vary the core diameter or the shell thickness.

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

PubMed

Kobler, A; Kübel, C

2017-02-01

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

Direct and continuous synthesis of VO2 nanoparticles

NASA Astrophysics Data System (ADS)

Powell, M. J.; Marchand, P.; Denis, C. J.; Bear, J. C.; Darr, J. A.; Parkin, I. P.

2015-11-01

Monoclinic VO2 nanoparticles are of interest due to the material's thermochromic properties, however, direct synthesis routes to VO2 nanoparticles are often inaccessible due to the high synthesis temperatures or long reaction times required. Herein, we present a two-step synthesis route for the preparation of monoclinic VO2 nanoparticles using Continuous Hydrothermal Flow Synthesis (CHFS) followed by a short post heat treatment step. A range of particle sizes, dependent on synthesis conditions, were produced from 50 to 200 nm by varying reaction temperatures and the residence times in the process. The nanoparticles were characterised by powder X-ray diffraction, Raman and UV/Vis spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The nanoparticles were highly crystalline with rod and sphere-like morphologies present in TEM micrographs, with the size of both the rod and spherical particles being highly dependent on both reaction temperature and residence time. SEM micrographs showed the surface of the powders produced from the CHFS process to be highly uniform. The samples were given a short post synthesis heat treatment to ensure that they were phase pure monoclinic VO2, which led to them exhibiting a large and reversible switch in optical properties (at near-IR wavelengths), which suggests that if such materials can be incorporated into coatings or in composites, they could be used for fenestration in architectural applications.

Direct and continuous synthesis of VO2 nanoparticles.

PubMed

Powell, M J; Marchand, P; Denis, C J; Bear, J C; Darr, J A; Parkin, I P

2015-11-28

Monoclinic VO2 nanoparticles are of interest due to the material's thermochromic properties, however, direct synthesis routes to VO2 nanoparticles are often inaccessible due to the high synthesis temperatures or long reaction times required. Herein, we present a two-step synthesis route for the preparation of monoclinic VO2 nanoparticles using Continuous Hydrothermal Flow Synthesis (CHFS) followed by a short post heat treatment step. A range of particle sizes, dependent on synthesis conditions, were produced from 50 to 200 nm by varying reaction temperatures and the residence times in the process. The nanoparticles were characterised by powder X-ray diffraction, Raman and UV/Vis spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The nanoparticles were highly crystalline with rod and sphere-like morphologies present in TEM micrographs, with the size of both the rod and spherical particles being highly dependent on both reaction temperature and residence time. SEM micrographs showed the surface of the powders produced from the CHFS process to be highly uniform. The samples were given a short post synthesis heat treatment to ensure that they were phase pure monoclinic VO2, which led to them exhibiting a large and reversible switch in optical properties (at near-IR wavelengths), which suggests that if such materials can be incorporated into coatings or in composites, they could be used for fenestration in architectural applications.

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

NASA Astrophysics Data System (ADS)

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

2017-10-01

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

Synthesis of noble metal nanoparticles

NASA Astrophysics Data System (ADS)

Bahadory, Mozhgan

Improved methods were developed for the synthesis of noble metal nanoparticles. Laboratory experiments were designed for introducing of nanotechnology into the undergraduate curriculum. An optimal set of conditions for the synthesis of clear yellow colloidal silver was investigated. Silver nanoparticles were obtained by borohydride reduction of silver nitrate, a method which produces particles with average size of 12+/-2 nm, determined by Transmission Electron Microscopy (TEM). The plasmon absorbance is at 397 nm and the peak width at half maximum (PWHM) is 70-75 nm. The relationship between aggregation and optical properties was determined along with a method to protect the particles using polyvinylpyrrolidone (PVP). A laboratory experiment was designed in which students synthesize yellow colloidal silver, estimate particle size using visible spectroscopy, and study aggregation effects. The synthesis of the less stable copper nanoparticles is more difficult because copper nanopaticles are easily oxidized. Four methods were used for the synthesis of copper nanoparticles, including chemical reduction with sodium borohydride, sodium borohydride with potassium iodide, isopropyl alcohol with cetyltrimethylammonium bormide (CTAB) and reducing sugars. The latter method was also the basis for an undergraduate laboratory experiment. For each reaction, the dependence of stability of the copper nanoparticles on reagent concentrations, additives, relative amounts of reactants, and temperature is explored. Atomic force microscopy (AFM), TEM and UV-Visible Spectroscopy were used to characterize the copper nanoparticles. A laboratory experiment to produce copper nanoparticles from household chemicals was developed.

Synthesis and Characterization of Nanofibrous Polyaniline Thin Film Prepared by Novel Atmospheric Pressure Plasma Polymerization Technique

PubMed Central

Park, Choon-Sang; Kim, Dong Ha; Shin, Bhum Jae; Tae, Heung-Sik

2016-01-01

This work presents a study on the preparation of plasma-polymerized aniline (pPANI) nanofibers and nanoparticles by an intense plasma cloud type atmospheric pressure plasma jets (iPC-APPJ) device with a single bundle of three glass tubes. The nano size polymer was obtained at a sinusoidal wave with a peak value of 8 kV and a frequency of 26 kHz under ambient air. Discharge currents, photo-sensor amplifier, and optical emission spectrometer (OES) techniques were used to analyze the plasma produced from the iPC-APPJ device. Field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), gas chromatography-mass spectrometry (GC-MS), and gel permeation chromatography (GPC) techniques were used to analyze the pPANI. FE-SEM and TEM results show that pPANI has nanofibers, nanoparticles morphology, and polycrystalline characteristics. The FT-IR and GC-MS analysis show the characteristic polyaniline peaks with evidence that some quinone and benzene rings are broken by the discharge energy. GPC results show that pPANI has high molecular weight (Mw), about 533 kDa with 1.9 polydispersity index (PDI). This study contributes to a better understanding on the novel growth process and synthesis of uniform polyaniline nanofibers and nanoparticles with high molecular weights using the simple atmospheric pressure plasma polymerization technique. PMID:28787838

Structural, optical and morphological characterization of Cu-doped α-Fe2O3 nanoparticles synthesized through co-precipitation technique

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

2017-11-01

Pure and copper (Cu concentration varying from 2 to 8%) doped hematite (α-Fe2O3) nanocrystals were synthesized through co-precipitation method using simple equipment. X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR), Raman spectroscopy, Differential Thermal Analysis (DTA), Thermo Gravimetric Analysis (TGA) and Ultraviolet-Visible (UV-Vis) techniques were used to characterize the synthesized samples. XRD measurements confirm that all the prepared nanocrystals consist only in nanocrystalline hematite phase. These results along with TEM and SEM show that the size of the nanoparticles decreases with Cu-doping down to 21 nm. FT-IR confirm the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we synthesized pure and Cu-doped hematite but also to identify their phonon modes. The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. The UV-Vis absorption measurements confirm that the decrease of particle size is accompanied by a decrease in the band gap value from 2.12 eV for pure α-Fe2O3 down to 1.91 eV for 8% Cu-doped α-Fe2O3. 8% Cu-doped hematite had the smallest size, the best crystallinity and the lowest band gap.

Synthesis and Characterization of Nanofibrous Polyaniline Thin Film Prepared by Novel Atmospheric Pressure Plasma Polymerization Technique.

PubMed

Park, Choon-Sang; Kim, Dong Ha; Shin, Bhum Jae; Tae, Heung-Sik

2016-01-11

This work presents a study on the preparation of plasma-polymerized aniline (pPANI) nanofibers and nanoparticles by an intense plasma cloud type atmospheric pressure plasma jets (iPC-APPJ) device with a single bundle of three glass tubes. The nano size polymer was obtained at a sinusoidal wave with a peak value of 8 kV and a frequency of 26 kHz under ambient air. Discharge currents, photo-sensor amplifier, and optical emission spectrometer (OES) techniques were used to analyze the plasma produced from the iPC-APPJ device. Field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), gas chromatography-mass spectrometry (GC-MS), and gel permeation chromatography (GPC) techniques were used to analyze the pPANI. FE-SEM and TEM results show that pPANI has nanofibers, nanoparticles morphology, and polycrystalline characteristics. The FT-IR and GC-MS analysis show the characteristic polyaniline peaks with evidence that some quinone and benzene rings are broken by the discharge energy. GPC results show that pPANI has high molecular weight ( M w ), about 533 kDa with 1.9 polydispersity index (PDI). This study contributes to a better understanding on the novel growth process and synthesis of uniform polyaniline nanofibers and nanoparticles with high molecular weights using the simple atmospheric pressure plasma polymerization technique.

Enhanced dispersion of multiwall carbon nanotubes in natural rubber latex nanocomposites by surfactants bearing phenyl groups.

PubMed

Mohamed, Azmi; Anas, Argo Khoirul; Bakar, Suriani Abu; Ardyani, Tretya; Zin, Wan Manshol W; Ibrahim, Sofian; Sagisaka, Masanobu; Brown, Paul; Eastoe, Julian

2015-10-01

Here is presented a systematic study of the dispersibility of multiwall carbon nanotubes (MWCNTs) in natural rubber latex (NR-latex) assisted by a series of single-, double-, and triple-sulfosuccinate anionic surfactants containing phenyl ring moieties. Optical polarising microscopy, field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Raman spectroscopy have been performed to obtain the dispersion-level profiles of the MWCNTs in the nanocomposites. Interestingly, a triple-chain, phenyl-containing surfactant, namely sodium 1,5-dioxo-1,5-bis(3-phenylpropoxy)-3-((3-phenylpropoxy)carbonyl) pentane-2-sulfonate (TCPh), has a greater capacity the stabilisation of MWCNTs than a commercially available single-chain sodium dodecylbenzenesulfonate (SDBS) surfactant. TCPh provides significant enhancements in the electrical conductivity of nanocomposites, up to ∼10(-2) S cm(-1), as measured by a four-point probe instrument. These results have allowed compilation of a road map for the design of surfactant architectures capable of providing the homogeneous dispersion of MWCNTs required for the next generation of polymer-carbon-nanotube materials, specifically those used in aerospace technology. Copyright © 2015 Elsevier Inc. All rights reserved.

Effect of Nb on microstructure and yield strength of a high temperature tempered martensitic steel

NASA Astrophysics Data System (ADS)

Wang, Qian; Sun, Yu; Zhang, Chuanyou; Wang, Qingfeng; Zhang, Fucheng

2018-04-01

Martensitic steels based on a composition of 25CrMo47NbVTi with different concentrations of Nb (0.003%–0.060%) were quenched (Q) at 900 °C and tempered (T) at 700 °C to obtain oil country tubular goods (OCTG) with higher yield strength. The precipitation and microstructures were characterized and quantified by optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and x-ray diffraction (XRD). The results show that the increased Nb content led to an enhanced overall precipitation, the rising solution-precipitation temperature, the increased mass or volume fraction of the Nb-containing precipitates, and the decreased average diameter of Nb-containing particles. With the enhanced precipitation of small sized Nb-containing particles, the austenite grain and corresponding martensitic packet and block were evidently refined. In addition, the dislocation density increased slightly with increasing Nb addition. The yield strength was experimentally measured and quantitatively estimated. The findings based on theoretical calculations indicated that as a consequence of intensified strengthening from grain boundaries, precipitates and dislocations, the yield strength was enhanced significantly by Nb addition.

Submerged Arc Stainless Steel Strip Cladding—Effect of Post-Weld Heat Treatment on Thermal Fatigue Resistance

NASA Astrophysics Data System (ADS)

Kuo, I. C.; Chou, C. P.; Tseng, C. F.; Lee, I. K.

2009-03-01

Two types of martensitic stainless steel strips, PFB-132 and PFB-131S, were deposited on SS41 carbon steel substrate by a three-pass submerged arc cladding process. The effects of post-weld heat treatment (PWHT) on thermal fatigue resistance and hardness were evaluated by thermal fatigue and hardness testing, respectively. The weld metal microstructure was investigated by utilizing optical microscopy, scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM). Results showed that, by increasing the PWHT temperature, hardness decreased but there was a simultaneous improvement in weldment thermal fatigue resistance. During tempering, carbide, such as (Fe, Cr)23C6, precipitated in the weld metals and molybdenum appeared to promote (Fe, Cr, Mo)23C6 formation. The precipitates of (Fe, Cr, Mo)23C6 revealed a face-centered cubic (FCC) structure with fine grains distributed in the microstructure, thereby effectively increasing thermal fatigue resistance. However, by adding nickel, the AC1 temperature decreased, causing a negative effect on thermal fatigue resistance.

Investigating the transverse optical structure of spider silk micro-fibers using quantitative optical microscopy

NASA Astrophysics Data System (ADS)

Little, Douglas J.; Kane, Deb M.

2017-01-01

The transverse optical structure of two orb-weaver (family Araneidae) spider dragline silks was investigated using a variant of the inverse-scattering technique. Immersing the silks in a closely refractive index-matched liquid, the minimum achievable image contrast was greater than expected for an optically homogeneous silk, given what is currently known about the optical absorption of these silks. This "excess contrast" indicated the presence of transverse optical structure within the spider silk. Applying electromagnetic scattering theory to a transparent double cylinder, the minimum achievable irradiance contrast for the Plebs eburnus and Argiope keyserlingi dragline silks was determined to be consistent with step index refractive index contrasts of 1-4×10-4 and 6-7×10-4, respectively, supposing outer-layer thicknesses consistent with previous TEM studies (50 nm and 100 nm, respectively). The possibility of graded index refractive index contrasts within the spider silks is also discussed. This is the strongest evidence, to date, that there is a refractive index contrast associated with the layered morphology of spider silks and/or variation of proportion of nanocrystalline components within the spider silk structure. The method is more generally applicable to optical micro-fibers, including those with refractive index variations on a sub-wavelength scale.

Scanning transmission X-ray, laser scanning, and transmission electron microscopy mapping of the exopolymeric matrix of microbial biofilms.

PubMed

Lawrence, J R; Swerhone, G D W; Leppard, G G; Araki, T; Zhang, X; West, M M; Hitchcock, A P

2003-09-01

Confocal laser scanning microscopy (CLSM), transmission electron microscopy (TEM), and soft X-ray scanning transmission X-ray microscopy (STXM) were used to map the distribution of macromolecular subcomponents (e.g., polysaccharides, proteins, lipids, and nucleic acids) of biofilm cells and matrix. The biofilms were developed from river water supplemented with methanol, and although they comprised a complex microbial community, the biofilms were dominated by heterotrophic bacteria. TEM provided the highest-resolution structural imaging, CLSM provided detailed compositional information when used in conjunction with molecular probes, and STXM provided compositional mapping of macromolecule distributions without the addition of probes. By examining exactly the same region of a sample with combinations of these techniques (STXM with CLSM and STXM with TEM), we demonstrate that this combination of multimicroscopy analysis can be used to create a detailed correlative map of biofilm structure and composition. We are using these correlative techniques to improve our understanding of the biochemical basis for biofilm organization and to assist studies intended to investigate and optimize biofilms for environmental remediation applications.

The Interior Analysis and 3-D Reconstruction of Internally-Mixed Light-Absorbing Atmospheric Particles

NASA Astrophysics Data System (ADS)

Conny, J. M.; Collins, S. M.; Anderson, I.; Herzing, A.

2010-12-01

Carbon-containing atmospheric particles may either absorb solar or outgoing long-wave radiation or scatter solar radiation, and thus, affect Earth’s radiative balance in multiple ways. Light-absorbing carbon that is common in urban air particles such as industrial coke dust, road dust, and diesel soot, often exists in the same particle with other phases that contain, for example, aluminum, calcium, iron, and sulfur. While the optical properties of atmospheric particles in general depend on overall particle size and shape, the inhomogeneity of chemical phases within internally-mixed particles may also greatly affect particle optical properties. In this study, a series of microscopic approaches were used to identify individual light-absorbing coarse-mode particles and to assess their interior structure and composition. Particle samples were collected in 2004 from one of the U.S. EPA’s Los Angeles Particulate Matter Supersites, and were likely affected substantially by road dust and construction dust. First, bright-field and dark-field light microscopy and computer-controlled scanning electron microscopy (SEM) with energy-dispersive x-ray spectroscopy (EDX) were used to distinguish predominantly light-absorbing carbonaceous particles from other particle types such as mineral dust, sea salt, and brake wear. Second, high-resolution SEM-EDX elemental mapping of individual carbonaceous particles was used to select particles with additional elemental phases that exhibited spatial inhomogeneity. Third, focused ion-beam SEM (FIB-SEM) with EDX was used to slice through selected particles to expose interior surfaces and to determine the spatial distribution of element phases throughout the particles. Fourth, study of the interior phases of a particle was augmented by the transmission electron microscopy (TEM) of a thin section of the particle prepared by FIB-SEM. Here, electron energy loss spectroscopy with TEM was used to study chemical bonding in the carbonaceous phase. Finally, automated serial slicing and imaging in the FIB-SEM generated a stack of secondary electron images of the particles’ interior surfaces that allowed for the 3-D reconstruction of the particles, a process known as FIB tomography. Interior surface of light-absorbing carbonaceous particle from FIB-SEM analysis.

Biocompatible magnetofluorescent probes: luminescent silicon quantum dots coupled with superparamagnetic iron(III) oxide.

PubMed

Erogbogbo, Folarin; Yong, Ken-Tye; Hu, Rui; Law, Wing-Cheung; Ding, Hong; Chang, Ching-Wen; Prasad, Paras N; Swihart, Mark T

2010-09-28

Luminescent silicon quantum dots (SiQDs) are gaining momentum in bioimaging applications, based on their unique combination of optical properties and biocompatibility. Here, we report the development of a multimodal probe that combines the optical properties of silicon quantum dots with the superparamagnetic properties of iron oxide nanoparticles to create biocompatible magnetofluorescent nanoprobes. Multiple nanoparticles of each type are coencapsulated within the hydrophobic core of biocompatible phospholipid-polyethyleneglycol (DSPE-PEG) micelles. The size distribution and composition of the magnetofluorescent nanoprobes were characterized by transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS). Enhanced cellular uptake of these probes in the presence of a magnetic field was demonstrated in vitro. Their luminescence stability in a prostate cancer tumor model microenvironment was demonstrated in vivo. This paves the way for multimodal silicon quantum-dot-based nanoplatforms for a variety of imaging and delivery applications.

Ion polished Cr/Sc attosecond multilayer mirrors for high water window reflectivity

DOE PAGES

Guggenmos, Alexander; Radünz, Stefan; Rauhut, Roman; ...

2014-01-20

Recent advances in the development of attosecond soft X-ray sources ranging into the water window spectral range, between the 1s states of carbon and oxygen (284 eV–543 eV), are also driving the development of suited broadband multilayer optics for steering and shaping attosecond pulses. The relatively low intensity of current High Harmonic Generation (HHG) soft X-ray sources calls for an efficient use of photons, thus the development of low-loss multilayer optics is of uttermost importance. Here, we report about the realization of broadband Cr/Sc attosecond multilayer mirrors with nearly atomically smooth interfaces by an optimized ion beam deposition and assistedmore » interface polishing process. This yields to our knowledge highest multilayer mirror reflectivity at 300 eV near normal incidence. The results are verified by transmission electron microscopy (TEM) and soft/hard X-ray reflectometry.« less

Ion polished Cr/Sc attosecond multilayer mirrors for high water window reflectivity

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

Guggenmos, Alexander; Radünz, Stefan; Rauhut, Roman

Recent advances in the development of attosecond soft X-ray sources ranging into the water window spectral range, between the 1s states of carbon and oxygen (284 eV–543 eV), are also driving the development of suited broadband multilayer optics for steering and shaping attosecond pulses. The relatively low intensity of current High Harmonic Generation (HHG) soft X-ray sources calls for an efficient use of photons, thus the development of low-loss multilayer optics is of uttermost importance. Here, we report about the realization of broadband Cr/Sc attosecond multilayer mirrors with nearly atomically smooth interfaces by an optimized ion beam deposition and assistedmore » interface polishing process. This yields to our knowledge highest multilayer mirror reflectivity at 300 eV near normal incidence. The results are verified by transmission electron microscopy (TEM) and soft/hard X-ray reflectometry.« less

Nano Electronics on Atomically Controlled van der Waals Quantum Heterostructures

DTIC Science & Technology

2015-03-30

for the structural of the atomically sharp interface between hBN and Bi2Te3. Finally, we have developed unprecedentedly clean graphene supercoductor...crystals by MBE method. We also use transmission electron microscopy (TEM) analysis for the structural of the atomically sharp interface between hBN and...by MBE method. We also use transmission electron microscopy (TEM) analysis for the structural of the atomically sharp interface between hBN and Bi2Te3

Retinal Toxicity of Acai Fruit (Euterpe Oleracea) Dye Concentrations in Rabbits: Basic Principles of a New Dye for Chromovitrectomy in Humans.

PubMed

Caiado, Rafael R; Peris, Cristiane S; Lima-Filho, Acácio Alves Souza; Urushima, Joao Guilherme Palma; Novais, Eduardo; Badaró, Emmerson; Maia, André; Sinigaglia-Coimbra, Rita; Watanabe, Sung Eun S; Rodrigues, Eduardo B; Farah, Michel Eid; Maia, Mauricio

2017-08-01

Evaluate toxicity of acai fruit (Euterpe oleracea) dye concentrations in a rabbit model. Rabbits were injected intravitreously with 10%, 25%, and 35% acai dye concentrations. Control eyes received balanced salt solution (BSS). Electroretinogram (ERG), fundus imaging, fluorescein angiography (FA), optical coherence tomography (OCT), and light and transmission electron microscopy (LM/TEM) were performed. Fundus imaging showed increased vitreous opacity with increased dye concentrations. FA and OCT showed normality with all concentrations. Comparisons between BSS and dye concentrations were analyzed using Kruskal-Wallis and Mood's median test (p < 0.05). At 24 h, ERGs showed reduced amplitudes from baseline in all eyes. Median b-wave amplitudes nonsignificantly decreased and latency increased with 10% and 25%; findings were significant (p < 0.05) for 35%. LM and TEM showed no abnormalities for 10% and 25%. With 35%, TEM showed ganglion cell edema at 24 h that resolved after 7 days. Vacuolization, multilamellar bodies, and nerve bundle damage occurred at 24 h/7 days in the inner nuclear layer. Mitochondrial cristae disruption occurred in the inner photoreceptor segment at 24 h that decreased by 7 days. Ten and twenty-five percent concentrations were safe and may improve identification of the posterior hyaloid and internal limiting membrane during chromovitrectomy in humans.

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.

Preparation of herpes simplex virus-infected primary neurons for transmission electron microscopy.

PubMed

Miranda-Saksena, Monica; Boadle, Ross; Cunningham, Anthony L

2014-01-01

Transmission electron microscopy (TEM) provides the resolution necessary to identify both viruses and subcellular components of cells infected with many types of viruses, including herpes simplex virus. Recognized as a powerful tool in both diagnostic and research-based virology laboratories, TEM has made possible the identification of new viruses and has contributed to the elucidation of virus life cycle and virus-host cell interaction. Whilst there are many sample preparation techniques for TEM, conventional processing using chemical fixation and resin embedding remains a useful technique, available in virtually all EM laboratories, for studying virus/cell ultrastructure. In this chapter, we describe the preparation of herpes simplex virus-infected primary neurons, grown on plastic cover slips, to allow sectioning of neurons and axons in their growth plane. This technique allows TEM examination of cell bodies, axons, growth cones, and varicosities, providing powerful insights into virus-cell interaction.

Quantitative Transmission Electron Microscopy of Nanoparticles and Thin-Film Formation in Electroless Metallization of Polymeric Surfaces

NASA Astrophysics Data System (ADS)

Dutta, Aniruddha; Heinrich, Helge; Kuebler, Stephen; Grabill, Chris; Bhattacharya, Aniket

2011-03-01

Gold nanoparticles(Au-NPs) act as nucleation sites for electroless deposition of silver on functionalized SU8 polymeric surfaces. Here we report the nanoscale morphology of Au and Ag nanoparticles as studied by Transmission Electron Microscopy (TEM). Scanning TEM with a high-angle annular dark-field detector is used to obtain atomic number contrast. From the intensity-calibrated plan-view scanning TEM images we determine the mean thickness and the volume distribution of the Au-NPs on the surface of the functionalized polymer. We also report the height and the radius distribution of the gold nanoparticles obtained from STEM images taking into consideration the experimental errors. The cross sectional TEM images yield the density and the average distance of the Au and Ag nanoparticles on the surface of the polymer. Supported by grant NSF, Chemistry Division.

Visualising reacting single atoms under controlled conditions: Advances in atomic resolution in situ Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM)

NASA Astrophysics Data System (ADS)

Boyes, Edward D.; Gai, Pratibha L.

2014-02-01

Advances in atomic resolution Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM) for probing gas-solid catalyst reactions in situ at the atomic level under controlled reaction conditions of gas environment and temperature are described. The recent development of the ESTEM extends the capability of the ETEM by providing the direct visualisation of single atoms and the atomic structure of selected solid state heterogeneous catalysts in their working states in real-time. Atomic resolution E(S)TEM provides a deeper understanding of the dynamic atomic processes at the surface of solids and their mechanisms of operation. The benefits of atomic resolution-E(S)TEM to science and technology include new knowledge leading to improved technological processes with substantial economic benefits, improved healthcare, reductions in energy needs and the management of environmental waste generation. xml:lang="fr"

The importance of transmission electron microscopy analysis of spermatozoa: Diagnostic applications and basic research.

PubMed

Moretti, Elena; Sutera, Gaetano; Collodel, Giulia

2016-06-01

This review is aimed at discussing the role of ultrastructural studies on human spermatozoa and evaluating transmission electron microscopy as a diagnostic tool that can complete andrology protocols. It is clear that morphological sperm defects may explain decreased fertilizing potential and acquire particular value in the field of male infertility. Electron microscopy is the best method to identify systematic or monomorphic and non-systematic or polymorphic sperm defects. The systematic defects are characterized by a particular anomaly that affects the vast majority of spermatozoa in a semen sample, whereas a heterogeneous combination of head and tail defects found in variable percentages are typically non-systematic or polymorphic sperm defects. A correct diagnosis of these specific sperm alterations is important for choosing the male infertility's therapy and for deciding to turn to assisted reproduction techniques. Transmission electron microscopy (TEM) also represents a valuable method to explore the in vitro effects of different compounds (for example drugs with potential spermicidal activity) on the morphology of human spermatozoa. Finally, TEM used in combination with immunohistochemical techniques, integrates structural and functional aspects that provide a wide horizon in the understanding of sperm physiology and pathology. transmission electron microscopy: TEM; World Health Organization: WHO; light microscopy: LM; motile sperm organelle morphology examination: MSOME; intracytoplasmic morphologically selected sperm injection: IMSI; intracytoplasmic sperm injection: ICSI; dysplasia of fibrous sheath: DFS; primary ciliary dyskinesia: PCD; outer dense fibers: ODF; assisted reproduction technologies: ART; scanning electron microscopy: SEM; polyvinylpirrolidone: PVP; tert-butylhydroperoxide: TBHP.

Evolution of Immiscibly Blended Functionalized Polymers with Respect to Cure Parameters and Formulation

NASA Astrophysics Data System (ADS)

Heller, Nicholas Walter Medicus

Powder coatings are becoming ubiquitous in the coating marketplace due to the absence of solvents in their formulation, but they have yet to see implementation in low-reflectance outdoor applications. This demand could be met by utilizing polymer blends formulated with low loadings of matting agents and pigments. The goal of this research is a thorough characterization of prototype low-reflectance coatings through several analytical techniques. Prototypical thermoset blends consist of functionalized polyurethanes rendered immiscible by differences in polar and hydrogen bonding characteristics, resulting in a surface roughened by droplet domains. Analysis of both pigmented and control clear films was performed. This research project had three primary aims: (1) determine the composition of the resin components of the polymer blend; (2) to monitor the evolution of domains before and during curing of clear polymer blends; (3) to monitor the evolution of these domains when pigments are added to these blends. The clear films enabled unhindered analysis by Fourier transform infrared (FTIR) and Raman spectroscopy on the binder. However, these domains provided no spectroscopic signatures despite their observation by optical microscopy. This necessitated the development of a new procedure for cross-section preparation that leaves no contamination from polishing media, which enabled Raman mapping of the morphology via an introduced marker peak from styrene monomer. The clears were analyzed as a powder and as films that were quenched at various cure-times using FTIR, Raman, transmission electron microscopy (TEM), and thermomechanical methods to construct a model of coating evolution based on cure parameters and polymer dynamics. Domains were observed in the powder, and underwent varying rates of coarsening as the cure progressed. TEM, scanning electron microscopy and thermomechanical methods were also used on pigmented systems at different states of the cure, including in powder form. TEM analysis additionally revealed the encapsulation of pigment particles by the domains, which helped explain the interaction between phase separation and pigment materials. The knowledge gained from fundamental characterization could be used to enable future generations of durable powder coatings with dead matte finishes.

Shock Deformation and Volcanism across the Cretaceous - Transition.

NASA Astrophysics Data System (ADS)

Huffman, Alan Royce

1990-01-01

The cause of the Cretaceous-Tertiary (K/T) transition remains one of the most controversial scientific topics in the geosciences. Geological and geophysical evidence associated with the K/T boundary have been used to argue that the extinctions were caused by meteor impact or volcanism. The goal of this study was to assess the viability of a volcanic model for the K/T transition. Comparison of natural and experimentally-shocked quartz and feldspar using optical and transmission electron microscopy (TEM) revealed that the optical and statistical character of shock-induced microstructures in volcanic rocks are different from both classic impact microstructures, and from the Raton K/T samples. A series of 31 high-explosive (HE) shock-recovery experiments at pressures to 25 GPa and temperatures to 750^circC were completed on samples of granite and quartzite. TEM and optical microscopy reveal that pre-shock temperature and pulse duration have a first-order effect on the development of shock-induced microstructures in quartz and feldspar. Application of the experimental results to natural shock-induced microstructures indicates that the volcanic microstructures are probably produced at elevated temperatures and shock pressures that do not exceed 15 GPa. The results also suggest that the Raton K/T deposits were produced at pressures below about 25 GPa. Analysis of samples from the K/T transition at DSDP Site 527 and correlations between biostratigraphy, isotopes, and the data from this study suggest that the decline in marine productivity over an extended period of time may be due to climate changes induced by basaltic volcanism. The eruption of the Deccan Traps is a viable mechanism for the K/T extinctions, and the correlation of flood basalts with every major biotic crisis in the last 250 Ma supports the link between these two phenomena. Eruption of flood basalts enriched in F, Cl, CO_2 , and SO_2, could disrupt the terrestrial ecosystem, and could produce effects including elevated pCO_2, acid rain, ozone depletion, lower ocean alkalinity, and climatic change, which can explain the observation of stepped or gradual extinction.

Scanning EM of non-heavy metal stained biosamples: Large-field of view, high contrast and highly efficient immunolabeling

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

Kuipers, Jeroen; Boer, Pascal de; Giepmans, Ben N.G., E-mail: b.n.g.giepmans@umcg.nl

Scanning electron microscopy (SEM) is increasing its application in life sciences for electron density measurements of ultrathin sections. These are traditionally analyzed with transmission electron microscopy (TEM); by most labs, SEM analysis still is associated with surface imaging only. Here we report several advantages of SEM for thin sections over TEM, both for structural inspection, as well as analyzing immuno-targeted labels such as quantum dots (QDs) and gold, where we find that QD-labeling is ten times more efficient than gold-labeling. Furthermore, we find that omitting post-staining with uranyl and lead leads to QDs readily detectable over the ultrastructure, but undermore » these conditions ultrastructural contrast was even almost invisible in TEM examination. Importantly, imaging in SEM with STEM detection leads to both outstanding QDs and ultrastructural contrast. STEM imaging is superior over back-scattered electron imaging of these non-contrasted samples, whereas secondary electron detection cannot be used at all. We conclude that examination of ultrathin sections by SEM, which may be immunolabeled with QDs, will allow rapid and straightforward analysis of large fields with more efficient labeling than can be achieved with immunogold. The large fields of view routinely achieved with SEM, but not with TEM, allows straightforward raw data sharing using virtual microscopy, also known as nanotomy when this concerns EM data in the life sciences. - Highlights: • High resolution and large fields of view via nanotomy or virtual microscopy. • Highly relevant for EM‐datasets where information density is high. • Sample preparation with low contrast good for STEM, not TEM. • Quantum dots now stand out in STEM‐based detection. • 10 Times more efficient labeling with quantum dots compared to gold.« less

Effect of He+ fluence on surface morphology and ion-irradiation induced defect evolution in 7075 aluminum alloys

NASA Astrophysics Data System (ADS)

Ni, Kai; Ma, Qian; Wan, Hao; Yang, Bin; Ge, Junjie; Zhang, Lingyu; Si, Naichao

2018-02-01

The evolution of microstructure for 7075 aluminum alloys with 50 Kev helium ions irradiation were studied by using optical microscopy (OM), scanning electron microscopy (SEM), x-ray diffraction (XRD) and transmission electron microscopy (TEM). The fluences of 1 × 1015, 1 × 1016 and 1 × 1017 ions cm-2 were selected, and irradiation experiments were conducted at room temperatures. The transmission process of He+ ions was simulated by using SRIM software, including distribution of ion ranges, energy losses and atomic displacements. Experimental results show that irradiated pits and micro-cracks were observed on irradiation sample surface, and the size of constituent particles (not including Mg2Si) decreased with the increasing dose. The x-ray diffraction results of the pair of peaks is better resolved in irradiated samples might indicate that the stressed structure consequence due to crystal defects (vacancies and interstitials) after He+ implantation. TEM observation indicated that the density of MgZn2 phase was significantly reduced after helium ion irradiation which is harmful to strength. Besides, the development of compressive stress produced a large amount of dislocation defects in the 1015 ions cm-2 sample. Moreover, higher fluence irradiation produced more dislocations in sample. At fluence of 1016 ions cm-2, dislocation wall formed by dislocation slip and aggregation in the interior of grains, leading to the refinement of these grains. As fluence increased to 1017 ions cm-2, dislocation loops were observed in pinned dislocation. Moreover, dislocation as effective defect sink, irradiation-induced vacancy defects aggregated to these sinks, and resulted in the formation of helium bubbles in dislocation.

Dopant concentration dependent optical and X-Ray induced photoluminescence in Eu3+ doped La2Zr2O7

NASA Astrophysics Data System (ADS)

Pokhrel, Madhab; Brik, Mikhail; Mao, Yuanbing

2015-03-01

Herein, we will be presenting the dopant (Eu) concentration dependent high density La2Zr2O7 nanoparticles for optical and X-ray scintillation applications by use of X - ray diffraction, Raman, FTIR, scanning electron microscope (SEM), transmission electron microscopy (TEM), optically and X-ray excited photoluminescence (PL). Several theoretical methods have been used in order to investigate the structural, electronic, optical, elastic, dynamic properties of Eu doped La2Zr2O7. It is observed that Eu: La2Zr2O7 shows an intense red luminescence under 258, 322, 394 and 465 nm excitation. The optical intensity of Eu: La2Zr2O7 depends on the dopant concentration of Eu3+. Following high energy excitation with X-rays, Eu: La2Zr2O7 shows an atypical Eu PL response (scintillation) with a red emission. The intense color emission of Eu obtained under 258 nm excitation, the X-ray induced luminescence property along with reportedly high density of La2Zr2O7, makes these nanomaterials attractive for optical and X-ray applications. The authors thank the support from the Defense Threat Reduction Agency (DTRA) of the U.S. Department of Defense (Award #HDTRA1-10-1-0114).

Appendix B: Summary of TEM Particle Size Distribution Datasets

EPA Pesticide Factsheets

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

Thermal behavior of aerosol particles from biomass burning during the BBOP campaign using transmission electron microscopy

NASA Astrophysics Data System (ADS)

Adachi, K.; Ishimoto, H.; Sedlacek, A. J., III; Kleinman, L. I.; Chand, D.; Hubbe, J. M.; Buseck, P. R.

2017-12-01

Aerosol samples were collected from wildland and agricultural biomass fires in North America during the 2013 Biomass Burning Observation Project (BBOP). We show in-situ shape and size changes and variations in the compositions of individual particles before and after heating using a transmission electron microscope (TEM). The responses of aerosol particles to heating are important for measurements of their chemical, physical, and optical properties, classification, and determination of origin. However, the thermal behavior of organic aerosol particles is largely unknown. We provide a method to analyze such thermal behavior through heating from room temperature to >600°C by using a heating holder within TEM. The results indicate that individual tar balls (TB; spherical organic material) from biomass burning retained, on average, up to 30% of their volume when heated to 600°C. Chemical analysis reveals that K and Na remained in the residues, whereas S and O were lost. In contrast to bulk sample measurements of carbonaceous particles using thermal/optical carbon analyzers, our single-particle results imply that many individual organic particles consist of multiple types of organic matter having different thermal stabilities. Our results also suggest that because of their thermal stability, some organic particles may not be detectable by using aerosol mass spectrometry or thermal/optical carbon analyzers. This result can lead to an underestimate of the abundance of TBs and other organic particles, and therefore biomass burning may have a greater influence than is currently recognized in regional and global climate models.

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

PubMed Central

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

2016-01-01

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

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

PubMed

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

2016-07-14

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

Plasmonics and SERS activity of post-transition metal nanoparticles

NASA Astrophysics Data System (ADS)

Bezerra, A. G.; Machado, T. N.; Woiski, T. D.; Turchetti, D. A.; Lenz, J. A.; Akcelrud, L.; Schreiner, W. H.

2018-05-01

Nanoparticles of the post-transition metals, In, Sn, Pb, and Bi, and of the metalloid Sb were produced by laser ablation synthesis in solution (LASiS) and tested for localized surface plasmon resonances (LSPR) and surface-enhanced Raman scattering (SERS). The nanoparticles were characterized by UV-Vis optical absorption, dynamic light scattering (DLS), and transmission electron microscopy (TEM). Several organic and biological molecules were tested, and SERS activity was demonstrated for all tested nanoparticles and molecules. The Raman enhancement factor for each nanoparticle class and molecule was experimentally determined. The search for new plasmonic nanostructures is important mainly for life sciences-related applications and this study expands the range of SERS active systems.

Hybride magnetic nanostructure based on amino acids functionalized polypyrrole

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

Nan, Alexandrina, E-mail: alexandrina.nan@itim-cj.ro; Bunge, Alexander; Turcu, Rodica

Conducting polypyrrole is especially promising for many commercial applications because of its unique optical, electric, thermal and mechanical properties. We report the synthesis and characterization of novel pyrrole functionalized monomers and core-shell hybrid nanostructures, consisting of a conjugated polymer layer (amino acids functionalized pyrrole copolymers) and a magnetic nanoparticle core. For functionalization of the pyrrole monomer we used several amino acids: tryptophan, leucine, phenylalanine, serine and tyrosine. These amino acids were linked via different types of hydrophobic linkers to the nitrogen atom of the pyrrole monomer. The magnetic core-shell hybrid nanostructures are characterized by various methods such as FTIR spectroscopy,more » transmission electron microscopy (TEM) and magnetic measurements.« less

Cooperative infrared to visible upconversion and visible to near-infrared quantum cutting in Tb and Yb co-doped glass containing Ag nanoparticles

NASA Astrophysics Data System (ADS)

Pan, Z.; Sekar, G.; Akrobetu, R.; Mu, R.; Morgan, S. H.

2011-10-01

Tb, Yb, and Ag co-doped glass nano-composites were synthesized in a lithium-lanthanum-aluminosilicate glass matrix (LLAS) by a melt-quench technique. Ag nanoparticles (NPs) were formed in the glass matrix and confirmed by optical absorption and transmission electron microscopy (TEM). Plasmon enhanced luminescence was observed. Cooperative infrared to visible upconversion and visible to near-infrared quantum cutting were studied for samples with different thermal annealing times. Because the Yb3+ emission at 940 - 1020 nm is matched well with the band gap of crystalline Si, the quantum cutting effect may have its potential application in silicon-based solar cells.

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

NASA Astrophysics Data System (ADS)

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

2017-10-01

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

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

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

Pan, Xiaoqing

2015-06-30

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

One-dimensional nanoferroic rods; synthesis and characterization

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Seddik, U.; Okasha, N.; Imam, N. G.

2015-11-01

One-dimensional nanoferroic rods of BaTiO3 were synthesized by improved citrate auto-combustion technology using tetrabutyl titanate. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FTIR) have been used to characterize the prepared sample. The results indicated that the crystal structure of BaTiO3 is tetragonal phase with an average crystallite size of 47 nm. SEM image gives a cauliflower-like morphology of the agglomerated nanorods. The stoichiometry of the chemical composition of the BaTiO3 ceramic was confirmed by EDX. TEM micrograph exhibited that BaTiO3 nanoparticles have rod-like shape with an average length of 120 nm and width of 43 nm. AFM was used to investigate the surface topography and its roughness. The topography image in 3D showed that the BaTiO3 particles have a rod shape with an average particle size of 116 nm which in agreement with 3D TEM result.

Detailed Investigation of Core-Shell Precipitates in a Cu-Containing High Entropy Alloy

NASA Astrophysics Data System (ADS)

Alam, T.; Gwalani, B.; Viswanathan, G.; Fraser, H.; Banerjee, R.

2018-05-01

Due to the competing influences of configurational entropy and enthalpy of mixing, in recent years, secondary (including intermetallic) phases have been reported in many high entropy alloy (HEA) systems. These secondary phases offer great potential in terms of strengthening the HEA beyond the solid solution strengthening effects, and as such are of great interest in regards to alloy design for engineering applications. The present research investigates novel nano-scale core-shell precipitates forming within the disordered bcc matrix phase of an Al2CrCuFeNi2 HEA, utilizing complementary high-resolution microscopy techniques of atom probe tomography (APT) and transmission electron microscopy (TEM). The size, morphology, and local chemistry of these core-shell precipitates was measured by APT, and the composition was further corroborated by high-resolution scanning transmission electron microscopy-energy dispersive spectroscopy in an aberration-corrected TEM. Furthermore, high-resolution TEM imaging of the core-shell structure indicates that the Cu-rich core exhibits a bcc crystal structure.

A simple approach to characterizing block copolymer assemblies: graphene oxide supports for high contrast multi-technique imaging†

PubMed Central

Patterson, Joseph P.; Sanchez, Ana M.; Petzetakis, Nikos; Smart, Thomas P.; Epps, Thomas H.; Portman, Ian

2013-01-01

Block copolymers are well-known to self-assemble into a range of 3-dimensional morphologies. However, due to their nanoscale dimensions, resolving their exact structure can be a challenge. Transmission electron microscopy (TEM) is a powerful technique for achieving this, but for polymeric assemblies chemical fixing/staining techniques are usually required to increase image contrast and protect specimens from electron beam damage. Graphene oxide (GO) is a robust, water-dispersable, and nearly electron transparent membrane: an ideal support for TEM. We show that when using GO supports no stains are required to acquire high contrast TEM images and that the specimens remain stable under the electron beam for long periods, allowing sample analysis by a range of electron microscopy techniques. GO supports are also used for further characterization of assemblies by atomic force microscopy. The simplicity of sample preparation and analysis, as well as the potential for significantly increased contrast background, make GO supports an attractive alternative for the analysis of block copolymer assemblies. PMID:24049544

Correlative scanning-transmission electron microscopy reveals that a chimeric flavivirus is released as individual particles in secretory vesicles.

PubMed

Burlaud-Gaillard, Julien; Sellin, Caroline; Georgeault, Sonia; Uzbekov, Rustem; Lebos, Claude; Guillaume, Jean-Marc; Roingeard, Philippe

2014-01-01

The intracellular morphogenesis of flaviviruses has been well described, but flavivirus release from the host cell remains poorly documented. We took advantage of the optimized production of an attenuated chimeric yellow fever/dengue virus for vaccine purposes to study this phenomenon by microscopic approaches. Scanning electron microscopy (SEM) showed the release of numerous viral particles at the cell surface through a short-lived process. For transmission electron microscopy (TEM) studies of the intracellular ultrastructure of the small number of cells releasing viral particles at a given time, we developed a new correlative microscopy method: CSEMTEM (for correlative scanning electron microscopy - transmission electron microscopy). CSEMTEM analysis suggested that chimeric flavivirus particles were released as individual particles, in small exocytosis vesicles, via a regulated secretory pathway. Our morphological findings provide new insight into interactions between flaviviruses and cells and demonstrate that CSEMTEM is a useful new method, complementary to SEM observations of biological events by intracellular TEM investigations.

Correlative Scanning-Transmission Electron Microscopy Reveals that a Chimeric Flavivirus Is Released as Individual Particles in Secretory Vesicles

PubMed Central

Burlaud-Gaillard, Julien; Sellin, Caroline; Georgeault, Sonia; Uzbekov, Rustem; Lebos, Claude; Guillaume, Jean-Marc; Roingeard, Philippe

2014-01-01

The intracellular morphogenesis of flaviviruses has been well described, but flavivirus release from the host cell remains poorly documented. We took advantage of the optimized production of an attenuated chimeric yellow fever/dengue virus for vaccine purposes to study this phenomenon by microscopic approaches. Scanning electron microscopy (SEM) showed the release of numerous viral particles at the cell surface through a short-lived process. For transmission electron microscopy (TEM) studies of the intracellular ultrastructure of the small number of cells releasing viral particles at a given time, we developed a new correlative microscopy method: CSEMTEM (for correlative scanning electron microscopy - transmission electron microscopy). CSEMTEM analysis suggested that chimeric flavivirus particles were released as individual particles, in small exocytosis vesicles, via a regulated secretory pathway. Our morphological findings provide new insight into interactions between flaviviruses and cells and demonstrate that CSEMTEM is a useful new method, complementary to SEM observations of biological events by intracellular TEM investigations. PMID:24681578

Identification and Ultrastructural Characterization of a Novel Nuclear Degradation Complex in Differentiating Lens Fiber Cells

PubMed Central

Costello, M. Joseph; Brennan, Lisa A.; Gilliland, Kurt O.; Johnsen, Sönke; Kantorow, Marc

2016-01-01

An unresolved issue in structural biology is how the encapsulated lens removes membranous organelles to carry out its role as a transparent optical element. In this ultrastructural study, we establish a mechanism for nuclear elimination in the developing chick lens during the formation of the organelle-free zone. Day 12–15 chick embryo lenses were examined by high-resolution confocal light microscopy and thin section transmission electron microscopy (TEM) following fixation in 10% formalin and 4% paraformaldehyde, and then processing for confocal or TEM as described previously. Examination of developing fiber cells revealed normal nuclei with dispersed chromatin and clear nucleoli typical of cells in active ribosome production to support protein synthesis. Early signs of nuclear degradation were observed about 300 μm from the lens capsule in Day 15 lenses where the nuclei display irregular nuclear stain and prominent indentations that sometimes contained a previously undescribed macromolecular aggregate attached to the nuclear envelope. We have termed this novel structure the nuclear excisosome. This complex by confocal is closely adherent to the nuclear envelope and by TEM appears to degrade the outer leaflet of the nuclear envelope, then the inner leaflet up to 500 μm depth. The images suggest that the nuclear excisosome separates nuclear membrane proteins from lipids, which then form multilamellar assemblies that stain intensely in confocal and in TEM have 5 nm spacing consistent with pure lipid bilayers. The denuded nucleoplasm then degrades by condensation and loss of structure in the range 600 to 700 μm depth producing pyknotic nuclear remnants. None of these stages display any classic autophagic vesicles or lysosomes associated with nuclei. Uniquely, the origin of the nuclear excisosome is from filopodial-like projections of adjacent lens fiber cells that initially contact, and then appear to fuse with the outer nuclear membrane. These filopodial-like projections appear to be initiated with a clathrin-like coat and driven by an internal actin network. In summary, a specialized cellular organelle, the nuclear excisosome, generated in part by adjacent fiber cells degrades nuclei during fiber cell differentiation and maturation. PMID:27536868

Multi Length Scale Imaging of Flocculated Estuarine Sediments; Insights into their Complex 3D Structure

NASA Astrophysics Data System (ADS)

Wheatland, Jonathan; Bushby, Andy; Droppo, Ian; Carr, Simon; Spencer, Kate

2015-04-01

Suspended estuarine sediments form flocs that are compositionally complex, fragile and irregularly shaped. The fate and transport of suspended particulate matter (SPM) is determined by the size, shape, density, porosity and stability of these flocs and prediction of SPM transport requires accurate measurements of these three-dimensional (3D) physical properties. However, the multi-scaled nature of flocs in addition to their fragility makes their characterisation in 3D problematic. Correlative microscopy is a strategy involving the spatial registration of information collected at different scales using several imaging modalities. Previously, conventional optical microscopy (COM) and transmission electron microscopy (TEM) have enabled 2-dimensional (2D) floc characterisation at the gross (> 1 µm) and sub-micron scales respectively. Whilst this has proven insightful there remains a critical spatial and dimensional gap preventing the accurate measurement of geometric properties and an understanding of how structures at different scales are related. Within life sciences volumetric imaging techniques such as 3D micro-computed tomography (3D µCT) and focused ion beam scanning electron microscopy [FIB-SEM (or FIB-tomography)] have been combined to characterise materials at the centimetre to micron scale. Combining these techniques with TEM enables an advanced correlative study, allowing material properties across multiple spatial and dimensional scales to be visualised. The aims of this study are; 1) to formulate an advanced correlative imaging strategy combining 3D µCT, FIB-tomography and TEM; 2) to acquire 3D datasets; 3) to produce a model allowing their co-visualisation; 4) to interpret 3D floc structure. To reduce the chance of structural alterations during analysis samples were first 'fixed' in 2.5% glutaraldehyde/2% formaldehyde before being embedding in Durcupan resin. Intermediate steps were implemented to improve contrast and remove pore water, achieved by the addition of heavy metal stains and washing samples in a series of ethanol solutions and acetone. Gross-scale characterisation involved scanning samples using a Nikon Metrology HM X 225 µCT. For micro-scale analysis a working surface was revealed by microtoming the sample. Ultrathin sections were then collected and analysed using a JEOL 1200 Ex II TEM, and FIB-tomography datasets obtained using an FEI Quanta 3D FIB-SEM. Finally, to locate the surface and relate TEM and FIB-tomography datasets to the original floc, samples were rescanned using the µCT. Image processing was initially conducted in ImageJ. Following this datasets were imported into Amira 5.5 where pixel intensity thresholding allowed particle-matrix boundaries to be defined. Using 'landmarks' datasets were then registered to enable their co-visualisation in 3D models. Analysis of registered datasets reveals the complex non-fractal nature of flocs, whose properties span several of orders of magnitude. Primary particles are organised into discrete 'bundles', the arrangement of which directly influences their gross morphology. This strategy, which allows the co-visualisation of spatially registered multi-scale 3D datasets, provides unique insights into the true nature floc which would other have been impossible.

Indigenous Carbonaceous Matter in the Nakhla Mars Meteorite

NASA Technical Reports Server (NTRS)

Clemett, S. J.; Thomas-Keprta, K. L.; Rahman, Z.; Le, L.; Wentworth, S. J.; Gibson, E. K.; McKay, D. S.

2016-01-01

Detailed microanalysis of the Martian meteorite Nakhla has shown there are morphologically distinct carbonaceous features spatially associated with low-T aqueous alteration phases including salts and id-dingsite. A comprehensive suite of analytical instrumentation including optical microscopy, field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) spectroscopy, focused ion beam (FIB) microscopy, transmission electron microscopy (TEM), two-step laser mass spectrometry (mu-L(sup 2)MS), laser mu-Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), and nanoscale secondary ion mass spectrometry (NanoSIMS) are being used to characterize the carbonaceous matter and host mineralogy. The search for carbonaceous matter on Mars has proved challenging. Viking Landers failed to unambiguously detect simple organics at either of the two landing sites although the Martian surface is estimated to have acquired at least 10(exp15) kg of C as a consequence of meteoritic accretion over the last several Ga. The dearth of organics at the Martian surface has been attributed to various oxidative processes including UV photolysis and peroxide activity. Consequently, investigations of Martian organics need to be focused on the sub-surface regolith where such surface processes are either severely attenuated or absent. Fortuitously since Martian meteorites are derived from buried regolith materials they provide a unique opportunity to study Martian organic geochemistry.

Characterization of 380nm UV-LEDs grown on free-standing GaN by atmospheric-pressure metal-organic chemical vapor deposition

NASA Astrophysics Data System (ADS)

Shieh, C. Y.; Li, Z. Y.; Kuo, H. C.; Chang, J. Y.; Chi, G. C.

2014-03-01

We reported the defects and optical characterizations of the ultraviolet light-emitting diodes grown on free-standing GaN substrate (FS-GaN) and sapphire. Cross-sectional transmission electron microscopy (TEM) images showed that the total defect densities of grown UV LEDs on FS-GaN and sapphire including edge, screw and mixed type were 3.6×106 cm-2 and 5.5×108 cm-2. When substrate of UV LEDs was changed from sapphire to FS-GaN, it can be clearly found that the crystallography of GaN epilayers was drastically different from that GaN epilayers on sapphire. Besides, the microstructures or indium clustering can be not observed at UV LEDs on FS-GaN from TEM measurement. The internal quantum efficiency of UVLEDs on FS-GaN and sapphire were 34.8 % and 39.4 % respectively, which attributed to indium clustering in multi-layers quantum wells (MQWs) of UV LEDs on sapphire. The relationship between indiumclustering and efficiency droop were investigated by temperature-dependent electroluminescence (TDEL) measurements.

Characteristics of Mg-doped and In-Mg co-doped p-type GaN epitaxial layers grown by metal organic chemical vapour deposition

NASA Astrophysics Data System (ADS)

Chung, S. J.; Senthil Kumar, M.; Lee, Y. S.; Suh, E.-K.; An, M. H.

2010-05-01

Mg-doped and In-Mg co-doped p-type GaN epilayers were grown using the metal organic chemical vapour deposition technique. The effect of In co-doping on the physical properties of p-GaN layer was examined by high resolution x-ray diffraction (HRXRD), transmission electron microscopy (TEM), Hall effect, photoluminescence (PL) and persistent photoconductivity (PPC) at room temperature. An improved crystalline quality and a reduction in threading dislocation density are evidenced upon In doping in p-GaN from HRXRD and TEM images. Hole conductivity, mobility and carrier density also significantly improved by In co-doping. PL studies of the In-Mg co-doped sample revealed that the peak position is blue shifted to 3.2 eV from 2.95 eV of conventional p-GaN and the PL intensity is increased by about 25%. In addition, In co-doping significantly reduced the PPC effect in p-type GaN layers. The improved electrical and optical properties are believed to be associated with the active participation of isolated Mg impurities.

Optical properties of thin films of zinc oxide quantum dots and polydimethylsiloxane: UV-blocking and the effect of cross-linking.

PubMed

Eita, Mohamed; El Sayed, Ramy; Muhammed, Mamoun

2012-12-01

Thin films of polydimethylsiloxane (PDMS) and ZnO quantum dots (QDs) were built up as multilayers by spin-coating. The films are characterized by a UV-blocking ability that increases with increasing number of bilayers. Photoluminescence (PL) emission spectra of the thin films occur at 522 nm, which is the PL wavelength of the ZnO QDs dispersion, but with a lower intensity and a quantum yield (QY) less than 1% that of the dispersion. Cross-linking has introduced new features to the absorption spectra in that the absorption peak was absent. These changes were attributed to the morphological and structural changes revealed by transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR), respectively. TEM showed that the ZnO particle size in the film increased from 7 (±2.7) nm to 16 (±7.8) upon cross-linking. The FTIR spectra suggest that ZnO QDs are involved in the cross-linking of PDMS and that the surface of the ZnO QDs has been chemically modified. Copyright © 2012 Elsevier Inc. All rights reserved.

Combinatorial study of low-refractive Mg-F-Si-O nano-composites deposited by magnetron co-sputtering from compound targets

NASA Astrophysics Data System (ADS)

Mertin, Stefan; Länzlinger, Tony; Sandu, Cosmin S.; Scartezzini, Jean-Louis; Muralt, Paul

2018-03-01

Deposition of nano-composite Mg-F-Si-O films on optical grade silica glass was studied employing RF magnetron co-sputtering from magnesium fluoride (MgF2) and fused silica (SiO2) targets. The aim was to obtain a stable and reliable sputtering process for optical coatings exhibiting a refractive index lower than the one of quartz glass (1.46 at 550 nm) without adding gaseous fluorine to the deposition process. The two magnetrons were installed in a confocal way at 45° off-axis with respect to a static substrate, thus creating a lateral gradient in the thin-film composition. The deposited Mg-F-Si-O coatings were structurally analysed by electron dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The obtained films consist of MgF2 nanocrystals embedded in a SiO2-rich amorphous matrix. Spectroscopic ellipsometry and spectrophotometry measurements showed that they are highly transparent exhibiting a very-low extinction coefficient k and a refractive index n in the desired range between the one of MgF2 (1.38) and SiO2 (1.46). Films with n = 1.424 and 1.435 at 550 nm were accomplished with absorption below the detection threshold.

Hybrid structure of white layer in high carbon steel - Formation mechanism and its properties.

PubMed

Hossain, Rumana; Pahlevani, Farshid; Witteveen, Evelien; Banerjee, Amborish; Joe, Bill; Prusty, B Gangadhara; Dippenaar, Rian; Sahajwalla, Veena

2017-10-16

This study identifies for the first time, the hybrid structure of the white layer in high carbon steel and describes its formation mechanism and properties. The so-called 'white layer' in steel forms during high strain rate deformation and appears featureless under optical microscopy. While many researchers have investigated the formation of the white layer, there has been no definitive study, nor is there sufficient evidence to fully explain the formation, structure and properties of the layer. In this study, the formation, morphology and mechanical properties of the white layer was determined following impact testing, using a combination of optical and SE- microscopy, HR-EBSD, TKD and TEM as well as nano-indentation hardness measurements and FE modelling. The phase transformation and recrystallization within and near the white layer was also investigated. The microstructure of the steel in the white layer consisted of nano-sized grains of martensite. A very thin layer of austenite with nano sized grains was identified within the white layer by HR-EBSD techniques, the presence of which is attributed to a thermally-induced reverse phase transformation. Overall, the combination of phase transformations, strain hardening and grain refinement led to a hybrid structure and an increase in hardness of the white layer.

Synthesis of Silver and Gold Nanoparticles Using Antioxidants from Blackberry, Blueberry, Pomegranate, and Turmeric Extracts

EPA Science Inventory

Greener synthesis of Ag and Au nanoparticles is described using antioxidants from blackberry, blueberry, pomegranate, and turmeric extracts. The synthesized particles were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution TEM (HR...

High-temperature effects on the light transmission through sapphire optical fiber

DOE PAGES

Wilson, Brandon A.; Petrie, Christian M.; Blue, Thomas E.

2018-03-13

Single crystal sapphire optical fiber was tested at high temperatures (1500°C) to determine its suitability for optical instrumentation in high-temperature environments. Broadband light transmission (450-2300 nm) through sapphire fiber was measured as a function of temperature as a test of the fiber's ability to survive and operate in high-temperature environments. Upon heating sapphire fiber to 1400°C, large amounts of light attenuation were measured across the entire range of light wavelengths that were tested. SEM and TEM images of the heated sapphire fiber indicated that a layer had formed at the surface of the fiber, most likely due to a chemicalmore » change at high temperatures. The microscopy results suggest that the surface layer may be in the form of aluminum hydroxide. Subsequent tests of sapphire fiber in an inert atmosphere showed minimal light attenuation at high temperatures along with the elimination of any surface layers on the fiber, indicating that the air atmosphere is indeed responsible for the increased attenuation and surface layer formation at high temperatures.« less

High-temperature effects on the light transmission through sapphire optical fiber

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

Wilson, Brandon A.; Petrie, Christian M.; Blue, Thomas E.

Single crystal sapphire optical fiber was tested at high temperatures (1500°C) to determine its suitability for optical instrumentation in high-temperature environments. Broadband light transmission (450-2300 nm) through sapphire fiber was measured as a function of temperature as a test of the fiber's ability to survive and operate in high-temperature environments. Upon heating sapphire fiber to 1400°C, large amounts of light attenuation were measured across the entire range of light wavelengths that were tested. SEM and TEM images of the heated sapphire fiber indicated that a layer had formed at the surface of the fiber, most likely due to a chemicalmore » change at high temperatures. The microscopy results suggest that the surface layer may be in the form of aluminum hydroxide. Subsequent tests of sapphire fiber in an inert atmosphere showed minimal light attenuation at high temperatures along with the elimination of any surface layers on the fiber, indicating that the air atmosphere is indeed responsible for the increased attenuation and surface layer formation at high temperatures.« less

Growth, morphological and optical characteristics of ZnSSe nanorods

NASA Astrophysics Data System (ADS)

Chen, Lin-Jer; Dai, Jia-Heng

2017-02-01

Zinc seledide sulfide (ZnSxSe1-x) nanorods with wurtzite structure were synthesized by a low temperature solvothermal pathway. In a typical condition of solvothermal at 180 °C for 8 h, the ZnSxSe1-x was composed of nanorods 10-15 nm in diameter and 50-75 nm length. These results indicate that the nanoscale of ZnSSe nanocrystals may contribute to the solvothermal process and exhibit a tunable photoluminescence (PL) and band gap that depends on the variation of reaction conditions. The work suggests a promising route to single-mode "mirror-less" amplified spontaneous emission (ASE) from inorganic nanomaterials with the Cholesteric liquid crystals (CLC) providing additional potential functionality. The obtained products are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-visible spectroscopy, and X-ray photoelectron spectroscopy (XPS). This approach for solvothermal growth can also be used with primary ZnSSe nanorods to achieve tunable optical properties and can likely be extended to nanomaterials of different shapes and other optical devices.

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

NASA Astrophysics Data System (ADS)

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

2011-10-01

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

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

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

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

Influence of graphene quantum dots on electrical properties of polymer composites

NASA Astrophysics Data System (ADS)

Arthisree, D.; Joshi, Girish M.

2017-07-01

We successfully prepared synthetic nanocomposite (SNC) by dispersing graphene quantum dots (GQD) in cellulose acetate (CA) polymer system. The dispersion and occupied network of GQD were foreseen by microscopic techniques. The variation of plane to crossed linked array network was observed by the polarizing optical microscopic (POM) technique. The scanning electron microscopy (SEM) revealed the leaves like impressions of GQD in host polymer system. The series network of GQD occupied in CA at higher resolution was confirmed by transmission electron microscopy (TEM). The two dimensional (2D) topographic images demonstrated an entangled polymer network to plane morphology. The variation in surface roughness was evaluated from the dimensional (3D) topography. The influence of temperature on AC conductivity with highest value (4  ×  10-5 S cm-1), contributes to the decrease in activation energy. The DC conductivity obeys the percolation criteria co-related to the GQD loading by weight fraction. Furthermore, this synthetic nanocomposite is feasible for the development of sensing and electrical applications.

Fabrication of GaAs/Al0.3Ga0.7As multiple quantum well nanostructures on (100) si substrate using a 1-nm InAs relief layer.

PubMed

Oh, H J; Park, S J; Lim, J Y; Cho, N K; Song, J D; Lee, W; Lee, Y J; Myoung, J M; Choi, W J

2014-04-01

Nanometer scale thin InAs layer has been incorporated between Si (100) substrate and GaAs/Al0.3Ga0.7As multiple quantum well (MQW) nanostructure in order to reduce the defects generation during the growth of GaAs buffer layer on Si substrate. Observations based on atomic force microscopy (AFM) and transmission electron microscopy (TEM) suggest that initiation and propagation of defect at the Si/GaAs interface could be suppressed by incorporating thin (1 nm in thickness) InAs layer. Consequently, the microstructure and resulting optical properties improved as compared to the MQW structure formed directly on Si substrate without the InAs layer. It was also observed that there exists some limit to the desirable thickness of the InAs layer since the MQW structure having thicker InAs layer (4 nm-thick) showed deteriorated properties.

Simple fabrication process for 2D ZnO nanowalls and their potential application as a methane sensor.

PubMed

Chen, Tse-Pu; Chang, Sheng-Po; Hung, Fei-Yi; Chang, Shoou-Jinn; Hu, Zhan-Shuo; Chen, Kuan-Jen

2013-03-20

Two-dimensional (2D) ZnO nanowalls were prepared on a glass substrate by a low-temperature thermal evaporation method, in which the fabrication process did not use a metal catalyst or the pre-deposition of a ZnO seed layer on the substrate. The nanowalls were characterized for their surface morphology, and the structural and optical properties were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence (PL). The fabricated ZnO nanowalls have many advantages, such as low growth temperature and good crystal quality, while being fast, low cost, and easy to fabricate. Methane sensor measurements of the ZnO nanowalls show a high sensitivity to methane gas, and rapid response and recovery times. These unique characteristics are attributed to the high surface-to-volume ratio of the ZnO nanowalls. Thus, the ZnO nanowall methane sensor is a potential gas sensor candidate owing to its good performance.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Jingle-bell-shaped ferrite hollow sphere with a noble metal core: Simple synthesis and their magnetic and antibacterial properties

NASA Astrophysics Data System (ADS)

Li, Siheng; Wang, Enbo; Tian, Chungui; Mao, Baodong; Kang, Zhenhui; Li, Qiuyu; Sun, Guoying

2008-07-01

In this paper, a simple strategy is developed for rational fabrication of a class of jingle-bell-shaped hollow structured nanomaterials marked as Ag@ MFe 2O 4 ( M=Ni, Co, Mg, Zn), consisting of ferrite hollow shells and metal nanoparticle cores, using highly uniform colloidal Ag@C microspheres as template. The final composites were obtained by direct adsorption of metal cations Fe 3+ and M 2+ on the surface of the Ag@C spheres followed by calcination process to remove the middle carbon shell and transform the metal ions into pure phase ferrites. The as-prepared composites were characterized by X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray analysis (EDX), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis spectroscopy and SQUID magnetometer. The results showed that the composites possess the magnetic property of the ferrite shell and the optical together with antibacterial property of the Ag core.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

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

Budhi, Sridhar; Peeraphatdit, Chorthip; Pylypenko, Svitlana

2014-02-07

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

Modification of the Interfacial Interaction between Carbon Fiber and Epoxy with Carbon Hybrid Materials

PubMed Central

Yu, Kejing; Wang, Menglei; Wu, Junqing; Qian, Kun; Sun, Jie; Lu, Xuefeng

2016-01-01

The mechanical properties of the hybrid materials and epoxy and carbon fiber (CF) composites were improved significantly as compared to the CF composites made from unmodified epoxy. The reasons could be attributed to the strong interfacial interaction between the CF and the epoxy composites for the existence of carbon nanomaterials. The microstructure and dispersion of carbon nanomaterials were characterized by transmission electron microscopy (TEM) and optical microscopy (OM). The results showed that the dispersion of the hybrid materials in the polymer was superior to other carbon nanomaterials. The high viscosity and shear stress characterized by a rheometer and the high interfacial friction and damping behavior characterized by dynamic mechanical analysis (DMA) indicated that the strong interfacial interaction was greatly improved between fibers and epoxy composites. Remarkably, the tensile tests presented that the CF composites with hybrid materials and epoxy composites have a better reinforcing and toughening effect on CF, which further verified the strong interfacial interaction between epoxy and CF for special structural hybrid materials. PMID:28335217

Green chemistry approach for the synthesis of ZnO-carbon dots nanocomposites with good photocatalytic properties under visible light.

PubMed

Bozetine, Hakima; Wang, Qi; Barras, Alexandre; Li, Musen; Hadjersi, Toufik; Szunerits, Sabine; Boukherroub, Rabah

2016-03-01

We report on a simple and one-pot synthetic method to produce ZnO/carbon quantum dots (ZnO/CQDs) nanocomposites. The morphological features and chemical composition of the nanocomposites were characterized using X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analyses (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The optical properties of the nanocomposites were examined using UV-visible (UV-vis) spectrophotometry. The photocatalytic activity of the ZnO/CQDs was evaluated for the degradation of a model organic pollutant, rhodamine B, under visible light irradiation at room temperature. The highly efficient photodegradation capability of the nanocomposite was demonstrated by comparison with ZnO particles, prepared using identical experimental conditions. Overall, the present approach adheres to green chemistry principles and the nanocomposite holds promise for the development of remarkably efficient catalytic systems. Copyright © 2015 Elsevier Inc. All rights reserved.

Three-dimensional imaging of dislocation propagation during crystal growth and dissolution

PubMed Central

Schenk, Anna S.; Kim, Yi-Yeoun; Kulak, Alexander N.; Campbell, James M.; Nisbet, Gareth; Meldrum, Fiona C.; Robinson, Ian K.

2015-01-01

Atomic level defects such as dislocations play key roles in determining the macroscopic properties of crystalline materials 1,2. Their effects range from increased chemical reactivity 3,4 to enhanced mechanical properties 5,6. Dislocations have been widely studied using traditional techniques such as X-ray diffraction and optical imaging. Recent advances have enabled atomic force microscopy to study single dislocations 7 in two-dimensions (2D), while transmission electron microscopy (TEM) can now visualise strain fields in three-dimensions (3D) with near atomic resolution 8–10. However, these techniques cannot offer 3D imaging of the formation or movement of dislocations during dynamic processes. Here, we describe how Bragg Coherent Diffraction Imaging (BCDI) 11,12 can be used to visualize in 3D, the entire network of dislocations present within an individual calcite crystal during repeated growth and dissolution cycles. These investigations demonstrate the potential of BCDI for studying the mechanisms underlying the response of crystalline materials to external stimuli. PMID:26030304

Simple Fabrication Process for 2D ZnO Nanowalls and Their Potential Application as a Methane Sensor

PubMed Central

Chen, Tse-Pu; Chang, Sheng-Po; Hung, Fei-Yi; Chang, Shoou-Jinn; Hu, Zhan-Shuo; Chen, Kuan-Jen

2013-01-01

Two-dimensional (2D) ZnO nanowalls were prepared on a glass substrate by a low-temperature thermal evaporation method, in which the fabrication process did not use a metal catalyst or the pre-deposition of a ZnO seed layer on the substrate. The nanowalls were characterized for their surface morphology, and the structural and optical properties were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence (PL). The fabricated ZnO nanowalls have many advantages, such as low growth temperature and good crystal quality, while being fast, low cost, and easy to fabricate. Methane sensor measurements of the ZnO nanowalls show a high sensitivity to methane gas, and rapid response and recovery times. These unique characteristics are attributed to the high surface-to-volume ratio of the ZnO nanowalls. Thus, the ZnO nanowall methane sensor is a potential gas sensor candidate owing to its good performance. PMID:23519350

Electrical and optical properties of ITO and ITO/Cr-doped ITO films

NASA Astrophysics Data System (ADS)

Caricato, A. P.; Cesaria, M.; Luches, A.; Martino, M.; Maruccio, G.; Valerini, D.; Catalano, M.; Cola, A.; Manera, M. G.; Lomascolo, M.; Taurino, A.; Rella, R.

2010-12-01

In this paper we report on the effects of the insertion of Cr atoms on the electrical and optical properties of indium tin oxide (ITO) films to be used as electrodes in spin-polarized light-emitting devices. ITO films and ITO(80 nm)/Cr-doped ITO(20 nm) bilayers and Cr-doped ITO films with a thickness of 20 nm were grown by pulsed ArF excimer laser deposition. The optical, structural, morphological and electrical properties of ITO films and ITO/Cr-doped structures were characterized by UV-Visible transmission and reflection spectroscopy, transmission electron microscopy (TEM), atomic force microscopy (AFM) and Hall-effect analysis. For the different investigations, the samples were deposited on different substrates like silica and carbon coated Cu grids. ITO films with a thickness of 100 nm, a resistivity as low as ˜4×10-4 Ω cm, an energy gap of ˜4.3 eV and an atomic scale roughness were deposited at room temperature without any post-deposition process. The insertion of Cr into the ITO matrix in the upper 20 nm of the ITO matrix induced variations in the physical properties of the structure like an increase of average roughness (˜0.4-0.5 nm) and resistivity (up to ˜8×10-4 Ω cm). These variations were correlated to the microstructure of the Cr-doped ITO films with particular attention to the upper 20 nm.

Biological interactions of quantum dot nanoparticles in skin and in human epidermal keratinocytes

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

Zhang, Leshuai W.; Yu, William W.; Colvin, Vicki L.

2008-04-15

Quantum dots nanoparticles have novel optical properties for biomedical applications and electronics, but little is known about their skin permeability and interaction with cells. QD621 are nail-shaped nanoparticles that contain a cadmium/selenide core with a cadmium sulfide shell coated with polyethylene glycol (PEG) and are soluble in water. QD were topically applied to porcine skin flow-through diffusion cells to assess penetration at 1 {mu}M, 2 {mu}M and 10 {mu}M for 24 h. QD were also studied in human epidermal keratinocytes (HEK) to determine cellular uptake, cytotoxicity and inflammatory potential. Confocal microscopy depicted the penetration of QD621 through the uppermost stratummore » corneum (SC) layers of the epidermis and fluorescence was found primarily in the SC and near hair follicles. QD were found in the intercellular lipid bilayers of the SC by transmission electron microscopy (TEM). Inductively coupled plasma-optical emission spectroscopy (ICP-OES) analysis for cadmium (Cd) and fluorescence for QD both did not detect Cd nor fluorescence signal in the perfusate at any time point or concentration. In HEK, viability decreased significantly (p < 0.05) from 1.25 nM to 10nM after 24 h and 48 h. There was a significant increase in IL-6 at 1.25 nM to 10 nM, while IL-8 increased from 2.5nM to 10nM after 24 h and 48 h. TEM of HEK treated with 10 nM of QD621 at 24 h depicted QD in cytoplasmic vacuoles and at the periphery of the cell membranes. These results indicate that porcine skin penetration of QD621 is minimal and limited primarily to the outer SC layers, yet if the skin were damaged allowing direct QD exposure to skin or keratinocytes, an inflammatory response could be initiated.« less

A single-phase white light emitting Pr3+ doped Ba2CaWO6 phosphor: synthesis, photoluminescence and optical properties

NASA Astrophysics Data System (ADS)

Sreeja, E.; Vidyadharan, Viji; Jose, Saritha K.; George, Anns; Joseph, Cyriac; Unnikrishnan, N. V.; Biju, P. R.

2018-04-01

Pr3+ doped Ba2CaWO6 phosphor were prepared by traditional high-temperature solid-state reaction technique. The structure evolution was systematically investigated by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis. The X-ray powder diffraction patterns indicate that the prepared phosphors crystallized in the cubic double-perovskite structure. The functional groups were identified using FTIR spectra and the elements present in the composition were confirmed by the EDS profile. The morphology of the phosphor was identified using SEM and TEM analysis. The PL spectra illustrated that these phosphors could be efficiently excited by charge transfer band of host and the maximum luminescence intensity was observed at 0.06 wt% of Pr3+ ion. Upon the charge transfer band excitation, emission spectra showed peaks at 489, 532, 647, 685 and 737 nm corresponding to 3P0→3H4, 3P1→3H5, 3P0→3F2, 3P0→3F3 and 3P0→3F4 transitions respectively. The concentration quenching of Ba2CaWO6:Pr3+ phosphor can be mainly attributed to dipole-dipole interaction. The CIE coordinates were estimated to be close to the white region. The decay curves are well fitted with double exponential decay models. The standard and modified Judd-Ofelt (JO) theories were used to determine the Judd-Ofelt intensity parameters, radiative transition probabilities and branching ratios. The optical properties indicate that Ba2CaWO6:Pr3+ phosphors can produce white light emission from a single phase host and its potential application for solid-state lighting and display devices.

Correlative Electron and Fluorescence Microscopy of Magnetotactic Bacteria in Liquid: Toward In Vivo Imaging

PubMed Central

Woehl, Taylor J.; Kashyap, Sanjay; Firlar, Emre; Perez-Gonzalez, Teresa; Faivre, Damien; Trubitsyn, Denis; Bazylinski, Dennis A.; Prozorov, Tanya

2014-01-01

Magnetotactic bacteria biomineralize ordered chains of uniform, membrane-bound magnetite or greigite nanocrystals that exhibit nearly perfect crystal structures and species-specific morphologies. Transmission electron microscopy (TEM) is a critical technique for providing information regarding the organization of cellular and magnetite structures in these microorganisms. However, conventional TEM can only be used to image air-dried or vitrified bacteria removed from their natural environment. Here we present a correlative scanning TEM (STEM) and fluorescence microscopy technique for imaging viable cells of Magnetospirillum magneticum strain AMB-1 in liquid using an in situ fluid cell TEM holder. Fluorescently labeled cells were immobilized on microchip window surfaces and visualized in a fluid cell with STEM, followed by correlative fluorescence imaging to verify their membrane integrity. Notably, the post-STEM fluorescence imaging indicated that the bacterial cell wall membrane did not sustain radiation damage during STEM imaging at low electron dose conditions. We investigated the effects of radiation damage and sample preparation on the bacteria viability and found that approximately 50% of the bacterial membranes remained intact after an hour in the fluid cell, decreasing to ~30% after two hours. These results represent a first step toward in vivo studies of magnetite biomineralization in magnetotactic bacteria. PMID:25358460

Correlative Electron and Fluorescence Microscopy of Magnetotactic Bacteria in Liquid: Toward In Vivo Imaging

DOE PAGES

Woehl, Taylor J.; Kashyap, Sanjay; Firlar, Emre; ...

2014-10-31

Magnetotactic bacteria biomineralize ordered chains of uniform, membrane-bound magnetite or greigite nanocrystals that exhibit nearly perfect crystal structures and species-specific morphologies. Transmission electron microscopy (TEM) is a critical technique for providing information regarding the organization of cellular and magnetite structures in these microorganisms. However, conventional TEM can only be used to image air-dried or vitrified bacteria removed from their natural environment. Here we present a correlative scanning TEM (STEM) and fluorescence microscopy technique for imaging viable cells of Magnetospirillum magneticum strain AMB-1 in liquid using an in situ fluid cell TEM holder. Fluorescently labeled cells were immobilized on microchip windowmore » surfaces and visualized in a fluid cell with STEM, followed by correlative fluorescence imaging to verify their membrane integrity. Notably, the post-STEM fluorescence imaging indicated that the bacterial cell wall membrane did not sustain radiation damage during STEM imaging at low electron dose conditions. We investigated the effects of radiation damage and sample preparation on the bacteria viability and found that approximately 50% of the bacterial membranes remained intact after an hour in the fluid cell, decreasing to ~30% after two hours. These results represent a first step toward in vivo studies of magnetite biomineralization in magnetotactic bacteria.« less

Comparative studies of thin film growth on aluminium by AFM, TEM and GDOES characterization

NASA Astrophysics Data System (ADS)

Qi, Jiantao; Thompson, George E.

2016-07-01

In this present study, comparative studies of trivalent chromium conversion coating formation, associated with aluminium dissolution process, have been investigated using atomic force microscopy (AFM), transmission electron microscopy (TEM) and glow-discharge optical emission spectroscopy (GDOES). High-resolution electron micrographs revealed the evident and uniform coating initiation on the whole surface after conversion treatment for only 30 s, although a network of metal ridges was created by HF etching pre-treatment. In terms of conversion treatment process on electropolished aluminium, constant kinetics of coating growth, ∼0.30 ± 0.2 nm/s, were found after the prolonged conversion treatment for 600 s. The availability of electrolyte anions for coating deposition determined the growth process. Simultaneously, a proceeding process of aluminium dissolution during conversion treatment, of ∼0.11 ± 0.02 nm/s, was found for the first time, indicating constant kinetics of anodic reactions. The distinct process of aluminium consumption was assigned with loss of corrosion protection of the deposited coating material as evidenced in the electrochemical impedance spectroscopy. Based on the present data, a new mechanism of coating growth on aluminium was proposed, and it consisted of an activation period (0-30 s), a linear growth period (0.30 nm/s, up for 600 s) and limited growth period (0.17 nm/s, 600-1200 s). In addition, the air-drying post-treatment and a high-vacuum environment in the microscope revealed a coating shrinkage, especially in the coatings after conversion treatments for longer time.

One-Step Synthesis of Titanium Oxyhydroxy-Fluoride Rods and Research on the Electrochemical Performance for Lithium-ion Batteries and Sodium-ion Batteries.

PubMed

Li, Biao; Gao, Zhan; Wang, Dake; Hao, Qiaoyan; Wang, Yan; Wang, Yongkun; Tang, Kaibin

2015-12-01

Titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O rods with a hexagonal tungsten bronze (HTB) structure, was synthesized via a facile one-step solvothermal method. The structure, morphology, and component of the products were characterized by X-ray powder diffraction (XRD), thermogravimetry (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), inductively coupled plasma optical emission spectroscopy (ICP-OES), ion chromatograph, energy-dispersive X-ray (EDX) analyses, and so on. Different rod morphologies which ranged from nanoscale to submicron scale were simply obtained by adjusting reaction conditions. With one-dimension channels for Li/Na intercalation/de-intercalation, the electrochemical performance of titanium oxyhydroxy-fluoride for both lithium-ion batteries (LIBs) and sodium-ion batteries (SIBs) was also studied. Electrochemical tests revealed that, for LIBs, titanium oxyhydroxy-fluoride exhibited a stabilized reversible capacity of 200 mAh g(-1) at 25 mA g(-1) up to 120 cycles in the electrode potential range of 3.0-1.2 V and 140 mAh g(-1) at 250 mA g(-1) up to 500 cycles, especially; for SIBs, a high capacity of 100 mAh g(-1) was maintained at 25 mA g(-1) after 115 cycles in the potential range of 2.9-0.5 V.

Characterization of V-shaped defects in 4H-SiC homoepitaxial layers

DOE PAGES

Zhang, Lihua; Su, Dong; Kisslinger, Kim; ...

2014-12-04

Synchrotron white beam x-ray topography images show that faint needle-like surface morphological features observed on the Si-face of 4H-SiC homoepitaxial layers using Nomarski optical microscopy are associated with V shaped stacking faults in the epilayer. KOH etching of the V shaped defect reveals small oval pits connected by a shallow line which corresponding to the surface intersections of two partial dislocations and the stacking fault connecting them. Transmission electron microscopy (TEM) specimens from regions containing the V shaped defects were prepared using focused ion beam milling, and stacking sequences of (85), (50) and (63) are observed at the faulted regionmore » with high resolution TEM. In order to study the formation mechanism of V shaped defect, low dislocation density 4H-SiC substrates were chosen for epitaxial growth, and the corresponding regions before and after epitaxy growth are compared in SWBXT images. It is found that no defects in the substrate are directly associated with the formation of the V shaped defect. Simulation results of the contrast from the two partial dislocations associated with V shaped defect in synchrotron monochromatic beam x-ray topography reveals the opposite sign nature of their Burgers vectors. Therefore, a mechanism of 2D nucleation during epitaxy growth is postulated for the formation of the V shaped defect, which requires elimination of non-sequential 1/4[0001] bilayers from the original structure to create the observed faulted stacking sequence.« less

Characterization of V-shaped defects in 4H-SiC homoepitaxial layers

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

Zhang, Lihua; Su, Dong; Kisslinger, Kim

Synchrotron white beam x-ray topography images show that faint needle-like surface morphological features observed on the Si-face of 4H-SiC homoepitaxial layers using Nomarski optical microscopy are associated with V shaped stacking faults in the epilayer. KOH etching of the V shaped defect reveals small oval pits connected by a shallow line which corresponding to the surface intersections of two partial dislocations and the stacking fault connecting them. Transmission electron microscopy (TEM) specimens from regions containing the V shaped defects were prepared using focused ion beam milling, and stacking sequences of (85), (50) and (63) are observed at the faulted regionmore » with high resolution TEM. In order to study the formation mechanism of V shaped defect, low dislocation density 4H-SiC substrates were chosen for epitaxial growth, and the corresponding regions before and after epitaxy growth are compared in SWBXT images. It is found that no defects in the substrate are directly associated with the formation of the V shaped defect. Simulation results of the contrast from the two partial dislocations associated with V shaped defect in synchrotron monochromatic beam x-ray topography reveals the opposite sign nature of their Burgers vectors. Therefore, a mechanism of 2D nucleation during epitaxy growth is postulated for the formation of the V shaped defect, which requires elimination of non-sequential 1/4[0001] bilayers from the original structure to create the observed faulted stacking sequence.« less

Reactive Oxygen Species Mediated Bacterial Biofilm Inhibition via Zinc Oxide Nanoparticles and Their Statistical Determination

PubMed Central

Dwivedi, Sourabh; Wahab, Rizwan; Khan, Farheen; Mishra, Yogendra K.; Musarrat, Javed; Al-Khedhairy, Abdulaziz A.

2014-01-01

The formation of bacterial biofilm is a major challenge in clinical applications. The main aim of this study is to describe the synthesis, characterization and biocidal potential of zinc oxide nanoparticles (NPs) against bacterial strain Pseudomonas aeruginosa. These nanoparticles were synthesized via soft chemical solution process in a very short time and their structural properties have been investigated in detail by using X-ray diffraction and transmission electron microscopy measurements. In this work, the potential of synthesized ZnO-NPs (∼10–15 nm) has been assessed in-vitro inhibition of bacteria and the formation of their biofilms was observed using the tissue culture plate assays. The crystal violet staining on biofilm formation and its optical density revealed the effect on biofilm inhibition. The NPs at a concentration of 100 µg/mL significantly inhibited the growth of bacteria and biofilm formation. The biofilm inhibition by ZnO-NPs was also confirmed via bio-transmission electron microscopy (Bio-TEM). The Bio-TEM analysis of ZnO-NPs treated bacteria confirmed the deformation and damage of cells. The bacterial growth in presence of NPs concluded the bactericidal ability of NPs in a concentration dependent manner. It has been speculated that the antibacterial activity of NPs as a surface coating material, could be a feasible approach for controlling the pathogens. Additionally, the obtained bacterial solution data is also in agreement with the results from statistical analytical methods. PMID:25402188

Reactive oxygen species mediated bacterial biofilm inhibition via zinc oxide nanoparticles and their statistical determination.

PubMed

Dwivedi, Sourabh; Wahab, Rizwan; Khan, Farheen; Mishra, Yogendra K; Musarrat, Javed; Al-Khedhairy, Abdulaziz A

2014-01-01

The formation of bacterial biofilm is a major challenge in clinical applications. The main aim of this study is to describe the synthesis, characterization and biocidal potential of zinc oxide nanoparticles (NPs) against bacterial strain Pseudomonas aeruginosa. These nanoparticles were synthesized via soft chemical solution process in a very short time and their structural properties have been investigated in detail by using X-ray diffraction and transmission electron microscopy measurements. In this work, the potential of synthesized ZnO-NPs (∼ 10-15 nm) has been assessed in-vitro inhibition of bacteria and the formation of their biofilms was observed using the tissue culture plate assays. The crystal violet staining on biofilm formation and its optical density revealed the effect on biofilm inhibition. The NPs at a concentration of 100 µg/mL significantly inhibited the growth of bacteria and biofilm formation. The biofilm inhibition by ZnO-NPs was also confirmed via bio-transmission electron microscopy (Bio-TEM). The Bio-TEM analysis of ZnO-NPs treated bacteria confirmed the deformation and damage of cells. The bacterial growth in presence of NPs concluded the bactericidal ability of NPs in a concentration dependent manner. It has been speculated that the antibacterial activity of NPs as a surface coating material, could be a feasible approach for controlling the pathogens. Additionally, the obtained bacterial solution data is also in agreement with the results from statistical analytical methods.

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

PubMed

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

2017-08-01

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

Dispersion of Co/CNTs via strong electrostatic adsorption method: Thermal treatment effect

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

Akbarzadeh, Omid, E-mail: omid.akbarzadeh63@gmail.com; Abdullah, Bawadi, E-mail: bawadi-abdullah@petronas.com.my; Subbarao, Duvvuri, E-mail: duvvuri-subbarao@petronas.com.my

The effect of different thermal treatment temperature on the structure of multi-walled carbon nanotubes (MWCNTs) and Co particle dispersion on CNTs support is studied using Strong electrostatic adsorption (SEA) method. The samples tested by N{sub 2}-adsorption, field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). N{sub 2}-adsorption results showed BET surface area increased using thermal treatment and TEM images showed that increasing the thermal treatment temperature lead to flaky CNTs and defects introduced on the outer surface and Co particle dispersion increased.

Structural properties of GaAsN grown on (001) GaAs by metalorganic molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Ok, Young-Woo; Choi, Chel-Jong; Seong, Tae-Yeon; Uesugi, K.; Suemune, I.

2001-07-01

Detailed transmission electron microscopy (TEM) and transmission electron diffraction (TED) examination has been made of metalorganic molecular beam epitaxial GaAsN layers grown on (001) GaAs substrates. TEM results show that lateral composition modulation occurs in the GaAs1-xNx layer (x 6.75%). It is shown that increasing N composition and Se (dopant) concentration leads to poor crystallinity. It is also shown that the addition of Se increases N composition. Atomic force microscopy (AFM) results show that the surfaces of the samples experience a morphological change from faceting to islanding, as the N composition and Se concentration increase. Based on the TEM and AFM results, a simple model is given to explain the formation of the lateral composition modulation.

Electron microscopy of the amphibian model systems Xenopus laevis and Ambystoma mexicanum.

PubMed

Kurth, Thomas; Berger, Jürgen; Wilsch-Bräuninger, Michaela; Kretschmar, Susanne; Cerny, Robert; Schwarz, Heinz; Löfberg, Jan; Piendl, Thomas; Epperlein, Hans H

2010-01-01

In this chapter we provide a set of different protocols for the ultrastructural analysis of amphibian (Xenopus, axolotl) tissues, mostly of embryonic origin. For Xenopus these methods include: (1) embedding gastrulae and tailbud embryos into Spurr's resin for TEM, (2) post-embedding labeling of methacrylate (K4M) and cryosections through adult and embryonic epithelia for correlative LM and TEM, and (3) pre-embedding labeling of embryonic tissues with silver-enhanced nanogold. For the axolotl (Ambystoma mexicanum) we present the following methods: (1) SEM of migrating neural crest (NC) cells; (2) SEM and TEM of extracellular matrix (ECM) material; (3) Cryo-SEM of extracellular matrix (ECM) material after cryoimmobilization; and (4) TEM analysis of hyaluronan using high-pressure freezing and HABP labeling. These methods provide exemplary approaches for a variety of questions in the field of amphibian development and regeneration, and focus on cell biological issues that can only be answered with fine structural imaging methods, such as electron microscopy. Copyright © 2010 Elsevier Inc. All rights reserved.

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

PubMed

Grant, Timothy; Rohou, Alexis; Grigorieff, Nikolaus

2018-03-07

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

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

PubMed Central

2018-01-01

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

Survival and Intra-Nuclear Trafficking of Burkholderia pseudomallei: Strategies of Evasion from Immune Surveillance?

PubMed

Vadivelu, Jamuna; Vellasamy, Kumutha Malar; Thimma, Jaikumar; Mariappan, Vanitha; Kang, Wen-Tyng; Choh, Leang-Chung; Shankar, Esaki M; Wong, Kum Thong

2017-01-01

During infection, successful bacterial clearance is achieved via the host immune system acting in conjunction with appropriate antibiotic therapy. However, it still remains a tip of the iceberg as to where persistent pathogens namely, Burkholderia pseudomallei (B. pseudomallei) reside/hide to escape from host immune sensors and antimicrobial pressure. We used transmission electron microscopy (TEM) to investigate post-mortem tissue sections of patients with clinical melioidosis to identify the localisation of a recently identified gut microbiome, B. pseudomallei within host cells. The intranuclear presence of B. pseudomallei was confirmed using transmission electron microscopy (TEM) of experimentally infected guinea pig spleen tissues and Live Z-stack, and ImageJ analysis of fluorescence microscopy analysis of in vitro infection of A549 human lung epithelial cells. TEM investigations revealed intranuclear localization of B. pseudomallei in cells of infected human lung and guinea pig spleen tissues. We also found that B. pseudomallei induced actin polymerization following infection of A549 human lung epithelial cells. Infected A549 lung epithelial cells using 3D-Laser scanning confocal microscopy (LSCM) and immunofluorescence microscopy confirmed the intranuclear localization of B. pseudomallei. B. pseudomallei was found within the nuclear compartment of host cells. The nucleus may play a role as an occult or transient niche for persistence of intracellular pathogens, potentially leading to recurrrent episodes or recrudescence of infection.

Survival and Intra-Nuclear Trafficking of Burkholderia pseudomallei: Strategies of Evasion from Immune Surveillance?

PubMed Central

Vadivelu, Jamuna; Vellasamy, Kumutha Malar; Thimma, Jaikumar; Mariappan, Vanitha; Kang, Wen-Tyng; Choh, Leang-Chung; Wong, Kum Thong

2017-01-01

Background During infection, successful bacterial clearance is achieved via the host immune system acting in conjunction with appropriate antibiotic therapy. However, it still remains a tip of the iceberg as to where persistent pathogens namely, Burkholderia pseudomallei (B. pseudomallei) reside/hide to escape from host immune sensors and antimicrobial pressure. Methods We used transmission electron microscopy (TEM) to investigate post-mortem tissue sections of patients with clinical melioidosis to identify the localisation of a recently identified gut microbiome, B. pseudomallei within host cells. The intranuclear presence of B. pseudomallei was confirmed using transmission electron microscopy (TEM) of experimentally infected guinea pig spleen tissues and Live Z-stack, and ImageJ analysis of fluorescence microscopy analysis of in vitro infection of A549 human lung epithelial cells. Results TEM investigations revealed intranuclear localization of B. pseudomallei in cells of infected human lung and guinea pig spleen tissues. We also found that B. pseudomallei induced actin polymerization following infection of A549 human lung epithelial cells. Infected A549 lung epithelial cells using 3D-Laser scanning confocal microscopy (LSCM) and immunofluorescence microscopy confirmed the intranuclear localization of B. pseudomallei. Conclusion B. pseudomallei was found within the nuclear compartment of host cells. The nucleus may play a role as an occult or transient niche for persistence of intracellular pathogens, potentially leading to recurrrent episodes or recrudescence of infection. PMID:28045926

Influence of organic solvent on optical and structural properties of ultra-small silicon dots synthesized by UV laser ablation in liquid.

PubMed

Intartaglia, Romuald; Bagga, Komal; Genovese, Alessandro; Athanassiou, Athanassia; Cingolani, Roberto; Diaspro, Alberto; Brandi, Fernando

2012-11-28

Ultra small silicon nanoparticles (Si-NPs) with narrow size distribution are prepared in a one step process by UV picosecond laser ablation of silicon bulk in liquid. Characterization by electron microscopy and absorption spectroscopy proves Si-NPs generation with an average size of 2 nm resulting from an in situ photofragmentation effect. In this context, the current work aims to explore the liquid medium (water and toluene) effect on the Si-NPs structure and on the optical properties of the colloidal solution. Si-NPs with high pressure structure (s.g. Fm3m) and diamond-like structure (s.g. Fd3m), in water, and SiC moissanite 3C phase (s.g. F4[combining macron]3m) in toluene are revealed by the means of High-Resolution TEM and HAADF-STEM measurements. Optical investigations show that water-synthesized Si-NPs have blue-green photoluminescence emission characterized by signal modulation at a frequency of 673 cm(-1) related to electron-phonon coupling. The synthesis in toluene leads to generation of Si-NPs embedded in the graphitic carbon-polymer composite which has intrinsic optical properties at the origin of the optical absorption and luminescence of the obtained colloidal solution.

Spin angular momentum transfer from TEM00 focused Gaussian beams to negative refractive index spherical particles

PubMed Central

Ambrosio, Leonardo A.; Hernández-Figueroa, Hugo E.

2011-01-01

We investigate optical torques over absorbent negative refractive index spherical scatterers under the influence of linear and circularly polarized TEM00 focused Gaussian beams, in the framework of the generalized Lorenz-Mie theory with the integral localized approximation. The fundamental differences between optical torques due to spin angular momentum transfer in positive and negative refractive index optical trapping are outlined, revealing the effect of the Mie scattering coefficients in one of the most fundamental properties in optical trapping systems. PMID:21833372

Preparation of electrospun pyrochlore-structure KGdTa2O7:Eu3+ phosphor: the optical and structural properties for white light emitting diode applications.

PubMed

Yim, Chul Jin; Unithrattil, Sanjith; Chung, Woon Jin; Im, Won Bin

2013-12-01

Red emitting nanofibers, KGdTa2O7:Eu3+ were synthesized by electrospinning technique followed by heat treatment. As-prepared uniform fiber precursor with diameter ranging from about 700 nm to about 900 nm were calcined after removing organic species by calcination. The fiber surface become rough and diameter decreased to about 250-340 nm range due to decomposition of organic species and formation of inorganic phase. Morphology, structural and photoluminescent properties of fibers were analyzed using thermogravimetric and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and photoluminescence (PL). TG-DTA analysis indicates that KGdTa2O7:Eu3+ began to crystalize at 520 degrees C. Fibers annealed at 900 degrees C formed well crystallized uniform fibers. Under ultraviolet excitation KGdTa2O7:Eu3+ exhibits red emission due to transitions in 4f states of Eu3+. The excitation band is dominated by the Eu(3+)--O2-charge transfer band peaked at 289 nm. The emission peak is in the region that is ideal for red light emission.

Synthesis and Cs-Corrected Scanning Transmission Electron Microscopy Characterization of Multimetallic Nanoparticles

NASA Astrophysics Data System (ADS)

Khanal, Subarna; Bhattarai, Nabraj; Velázquez-Salazar, Jesus; Jose-Yacaman, Miguel; Subarna Khanal Team

2014-03-01

Multimetallic nanoparticles have been attracted greater attention both in materials science and nanotechnology due to its unique electronic, optical, biological, and catalytic properties lead by physiochemical interactions among different atoms and phases. The distinct features of multimetallic nanoparticles enhanced synergetic properties, large surface to volume ratio and quantum size effects ultimately lead to novel and wide range of possibilities for different applications than monometallic counterparts. For instance, PtPd, Pt/Cu, Au-Au3Cu, AgPd/Pt, AuCu/Pt and many other multimetallic nanoparticles have raised interest for their various applications in fuel cells, ethanol and methanol oxidation reactions, hydrogen storage, and so on. The nanostructures were analyzed by transmission electron microscopy (TEM) and by aberration-corrected scanning transmission electron microscopy (Cs-corrected STEM), in combination with high angle annular dark field (HAADF), bright field (BF), energy dispersive X-ray spectroscopy (EDS), and electron energy loss spectroscopy (EELS) detectors. These techniques allowed us to probe the structure at the atomic level of the nanoparticles revealing new structural information and elemental composition of the nanoparticles. The authors would like to acknowledge NSF grants DMR-1103730, ``Alloys at the Nanoscale: The Case of Nanoparticles Second Phase'' and NSF PREM Grant # DMR 0934218.

Solid-state transformation of Fe-rich intermetallic phases in Al–5.0Cu–0.6Mn squeeze cast alloy with variable Fe contents during solution heat treatment

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

Lin, Bo; School of Mechanical Engineering, Gui Zhou University, Guiyang 550000; Zhang, Weiwen, E-mail: mewzhang@scut.edu.cn

2015-06-15

The Al–5.0 wt.% Cu–0.6 wt.% Mn alloys with a variable Fe content were prepared by squeeze casting. Optical microscopy (OM), Deep etching technique, scanning electron microscopy(SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to examine the solid-state transformation of Fe-rich intermetallics during the solution heat treatment. The results showed that the Chinese script-like α-Fe, Al{sub 6}(FeMn) and needle-like Al{sub 3}(FeMn) phases transform to a new Cu-rich β-Fe (Al{sub 7}Cu{sub 2}(FeMn)) phase during solution heat treatment. The possible reaction and overall transformation kinetics of the solid-state phase transformation for the Fe-rich intermetallics were investigated. - Graphical abstract: Displaymore » Omitted - Highlights: • The α-Fe, Al{sub 6}(FeMn) and Al{sub 3}(FeMn) phases change to the β-Fe phases. • Possible reactions of Fe phases during solution heat treatment are discussed. • The overall fractional transformation rate follows an Avrami curve.« less

Growth, characterization and estimation of lattice strain and size in CdS nanoparticles: X-ray peak profile analysis

NASA Astrophysics Data System (ADS)

Solanki, Rekha Garg; Rajaram, Poolla; Bajpai, P. K.

2018-05-01

This work is based on the growth, characterization and estimation of lattice strain and crystallite size in CdS nanoparticles by X-ray peak profile analysis. The CdS nanoparticles were synthesized by a non-aqueous solvothermal method and were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman and UV-visible spectroscopy. XRD confirms that the CdS nanoparticles have the hexagonal structure. The Williamson-Hall (W-H) method was used to study the X-ray peak profile analysis. The strain-size plot (SSP) was used to study the individual contributions of crystallite size and lattice strain from the X-rays peaks. The physical parameters such as strain, stress and energy density values were calculated using various models namely, isotropic strain model, anisotropic strain model and uniform deformation energy density model. The particle size was estimated from the TEM images to be in the range of 20-40 nm. The Raman spectrum shows the characteristic optical 1LO and 2LO vibrational modes of CdS. UV-visible absorption studies show that the band gap of the CdS nanoparticles is 2.48 eV. The results show that the crystallite size estimated from Scherrer's formula, W-H plots, SSP and the particle size calculated by TEM images are approximately similar.

Microscopy based studies on the interaction of bio-based silver nanoparticles with Bombyx mori Nuclear Polyhedrosis virus.

PubMed

Tamilselvan, Selvaraj; Ashokkumar, Thirunavukkarasu; Govindaraju, Kasivelu

2017-04-01

In the present investigation, silver nanoparticles (AgNPs) interactions with Bombyx mori Nuclear Polyhedrosis virus (BmNPV) were characterized using High-Resolution Scanning Electron Microscopy (HR-SEM), Energy Dispersive X-ray Analysis (EDAX), Transmission Electron Microscopy (TEM), Atomic Force Microcopy (AFM) and Confocal Microscope (CM). HR-SEM study reveals that the biosynthesized AgNPs have interacted with BmNPV and were found on the surface. TEM micrographs of normal and viral polyhedra treated with AgNPs showed that the nanoparticles were accumulated in the membrane and it was noted that some of the AgNPs successfully penetrated the membrane by reaching the capsid of BmNPV. AFM and confocal microscopy studies reveal that the disruption in the shell membrane tends to lose its stability due to exposure of AgNPs to BmNPV. Copyright © 2017 Elsevier B.V. All rights reserved.

Nanoscale insights on one- and two-dimensional material structures

NASA Astrophysics Data System (ADS)

Floresca, Herman Carlo

The race for smaller, faster and more efficient devices has led researchers to explore the possibilities of utilizing nanostructures for scaling. These one-dimensional and two-dimensional materials have properties that are attractive for this purpose but are still not well controlled. Control comes with a complete understanding of the materials' electrical, thermal, optical and structural characteristics but is difficult to obtain due to their small scale. This work is intended to help researchers overcome the difficulty in studying nanostructures by providing techniques for analysis and insights of nanostructures that have not been previously available. Two nanostructures were studied: silicon nanowires and graphene. The nanowires were prepared for cross-section transmission electron microscopy (TEM) to discover the effects that controlled oxidation has on the dimensions and shape of the nanowires. Since cross-section TEM is not able to provide information about surface structure, a method for manipulating the wires with orientation control was developed. With this ability, all three orthogonal views of the nanowire were compiled for a comprehensive study on its structure in terms of shape and surface roughness. Graphene was used for a two-dimensional analytical technique that took advantage of customized computer programs for data acquisition, measurement and display. With the information provided, distinctions between grain boundary types in polycrystalline graphene were made and supported by statistical information from the software's output. It was also applied to a growth series of graphene samples in conjunction with scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) maps. The results help point to origins of graphene's polycrystalline nature. This dissertation concludes with a thought towards the future by highlighting a method that can help analyze nanostructures, which may become incorporated into the structures of large devices. The fold-out method is a TEM sample preparation technique utilizing a focused ion beam (FIB) for site specific thinning across a large sample area. Its process is demonstrated along with advantages over conventional methods.

Allochthonous Addition of Meteoritic Organics to the Lunar Regolith

NASA Technical Reports Server (NTRS)

Thomas-Keprta, K. L.; Clemett, S.; Ross, D. K.; Le, L.; Rahman, Z.; McKay, D. S.; Gibson, E. K.; Gonzalez, C.

2013-01-01

Preparation of lunar samples 74220,861 was discussed in detail in [3, 4]. Our analysis sequence was as follows: optical microscopy, UV fluorescence imaging, -Raman, FESEM-EDX imaging and mapping, FETEMEDX imaging and mapping of a Focused Ion Beam (FIB) extracted section, and NanoSIMs analysis. We observed fluffytextured C-rich regions of interest (ROI) on three different volcanic glass beads. Each ROI was several m2 in size and fluoresced when exposed to UV. Using FESEM/EDX, the largest ROI measured 36 m and was located on an edge of a plateau located on the uppermost surface of the bead. The ROI was covered on one edge by a siliceous filament emanating from the plateau surface indicating it was attached to the bead while on the Moon. EDX mapping of the ROI shows it is composed primarily of heterogeneously distributed C. Embedded with the carbonaceous phase are localized concentrations of Si, Fe, Al and Ti indicating the presence of glass and/or minerals grains. -Raman showed strong D- and G-bands and their associated second order bands; intensity and location of these bands indicates the carbonaceous matter is structurally disorganized. A TEM thin section was extracted from the surface of a glass bead using FIB microscopy. High resolution TEM imaging and selected area electron diffraction demonstrate the carbonaceous layer to be amorphous; it lacked any long or short range order characteristic of micro- or nanocrystalline graphite. Additionally TEM imaging also revealed the presence of submicron mineral grains, typically < 50 nm in size, dispersed within the carbonaceous layer. NanoSIMs data will be presented and discussed at the meeting. Given the noted similarities between the carbonaceous matter present on 74220 glass beads and meteoritic kerogen, we suggest the allochthonous addition of meteoritic organics as the most probable source for the C-rich ROIs.

Nanoparticles generated by laser in liquids as contrast medium and radiotherapy intensifiers

NASA Astrophysics Data System (ADS)

Restuccia, Nancy; Torrisi, Lorenzo

2018-01-01

The synthesis of Au and Ag nanoparticles (NP) though laser ablation in liquids as a function the laser parameters is presented. Spherical NPs with diameter distribution within 1 and 100 nm were prepared by laser ablation in water. The nanoparticles characterization was performed using optical spectroscopy and electronic microscopy (SEM and TEM) measurements. Studies of the possible use of metallic nanoparticles as intensifier of diagnostics imaging contrast medium and absorbing dose from ionizing radiations in traditional radiotherapy and protontherapy are presented. Examples of in vitro (in tissue equivalent materials) and in vivo (in mice), were conducted thank to simulation programs permitting to evaluate the enhancement of efficiency in imaging and therapy as a function of the NPs concentrations and irradiation conditions.

Highly-branched anisotropic hybrid nanoparticles at surfaces.

NASA Astrophysics Data System (ADS)

Tsukruk, Vladimir

2009-03-01

We present a brief overview of our recent studies on combined hybrid anisotropic structures composed of inorganic nanoparticles and highly branched molecules such as modified silsesquioxanes polyhedra cores (POSS) with mixed hydrophobic-hydrophilic tails and silver nanowires with functionalized star block copolymer with embedded gold nanoparticles (nanocobs). We demonstrate two-stage melting of that branched POSS and their ability to form monolayer and multilayered LB structures. On the other hand, we observed that silver-BCP-gold nanocobs display extremely bright Raman scattering caused by surface enhanced Raman effect with very different longitudinal and transversal optical properties as revealed by high-resolution confocal Raman microscopy. To study these hybrid nanostructures we applied combined AFM, SEM, TEM, XPS, SERS, UV-vis, and XR techniques.

Tunable Properties of Exfoliated Polyvinylalcohol Nanocomposites by In Situ Coprecipitation of Layered Double Hydroxides

NASA Astrophysics Data System (ADS)

Liu, Jiajia; Yuen, Richard K. K.; Hu, Yuan

2017-10-01

Poly(vinyl alcohol) (PVA) nanocomposites were prepared by a “one step” method based on the coprecipitation of layered double hydroxide (LDH) nanosheets in the polymer aqueous solution. The morphology, fire resistance properties, mechanical and optical properties of the PVA/LDH nanocomposites were studied. The LDH nanosheets were homogeneously dispersed in the PVA matrix as indicated by X-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) characterization. Meanwhile, the peak of heat release rate (pHRR) and total heat release (THR) were decreased by 58% and 28%, respectively. Storage modulus at 30 °C was increased, and the transmittance of more than 90% at the visible region was obtained upon addition of 5 wt% LDH.

Modelling the excitation field of an optical resonator

NASA Astrophysics Data System (ADS)

Romanini, Daniele

2014-06-01

Assuming the paraxial approximation, we derive efficient recursive expressions for the projection coefficients of a Gaussian beam over the Gauss--Hermite transverse electro-magnetic (TEM) modes of an optical cavity. While previous studies considered cavities with cylindrical symmetry, our derivation accounts for "simple" astigmatism and ellipticity, which allows to deal with more realistic optical systems. The resulting expansion of the Gaussian beam over the cavity TEM modes provides accurate simulation of the excitation field distribution inside the cavity, in transmission, and in reflection. In particular, this requires including counter-propagating TEM modes, usually neglected in textbooks. As an illustrative application to a complex case, we simulate reentrant cavity configurations where Herriott spots are obtained at cavity output. We show that the case of an astigmatic cavity is also easily modelled. To our knowledge, such relevant applications are usually treated under the simplified geometrical optics approximation, or using heavier numerical methods.

Characterization of microbially Fe(III)-reduced nontronite: Environmental cell-transmission electron microscopy study

USGS Publications Warehouse

Kim, Jin-wook; Furukawa, Yoko; Daulton, Tyrone L.; Lavoie, Dawn L.; Newell, Steven W.

2003-01-01

Microstructural changes induced by the microbial reduction of Fe(III) in nontronite by Shewanella oneidensis were studied using environmental cell (EC)-transmission electron microscopy (TEM), conventional TEM, and X-ray powder diffraction (XRD). Direct observations of clays by EC-TEM in their hydrated state allowed for the first time an accurate and unambiguous TEM measurement of basal layer spacings and the contraction of layer spacing caused by microbial effects, most likely those of Fe(III) reduction. Non-reduced and Fe(III)-reduced nontronite, observed by EC-TEM, exhibited fringes with mean d001 spacings of 1.50 nm (standard deviation, σ = 0.08 nm) and 1.26 nm (σ = 0.10 nm), respectively. In comparison, the same samples embedded with Nanoplast resin, sectioned by microtome, and observed using conventional TEM, displayed layer spacings of 1.0–1.1 nm (non-reduced) and 1.0 nm (reduced). The results from Nanoplast-embedded samples are typical of conventional TEM studies, which have measured nearly identical layer spacings regardless of Fe oxidation state. Following Fe(III) reduction, both EC- and conventional TEM showed an increase in the order of nontronite selected area electron diffraction patterns while the images exhibited fewer wavy fringes and fewer layer terminations. An increase in stacking order in reduced nontronite was also suggested by XRD measurements. In particular, the ratio of the valley to peak intensity (v/p) of the 1.7 nm basal 001 peak of ethylene glycolated nontronite was measured at 0.65 (non-reduced) and 0.85 (microbially reduced).

Silver nanoparticle production by Rhizopus stolonifer and its antibacterial activity against extended spectrum {beta}-lactamase producing (ESBL) strains of Enterobacteriaceae

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

Banu, Afreen; Rathod, Vandana, E-mail: drvandanarathod@rediffmail.com; Ranganath, E.

Highlights: {yields} Silver nanoparticle production by using Rhizopus stolonifer. {yields} Antibacterial activity of silver nanoparticles against extended spectrum {beta}-lactamase producing (ESBL) strains of Enterobacteriaceae. {yields} Synergistic effect of antibiotics with silver nanoparticles towards ESBL-strains. {yields} Characterization of silver nanoparticles made by UV-vis spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transformed infrared (FTIR) spectroscopy, atomic force microscopy (AFM). -- Abstract: This report focuses on the synthesis of silver nanoparticles using the fungus, Rhizopus stolonifer and its antimicrobial activity. Research in nanotechnology highlights the possibility of green chemistry pathways to produce technologically important nanomaterials. Characterization of newly synthesized silvermore » nanoparticles was made by UV-visible absorption spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), Fourier transform infrared (FTIR) spectroscopy and atomic force microscope (AFM). TEM micrograph revealed the formation of spherical nanoparticles with size ranging between 3 and 20 nm. The biosynthesized silver nanoparticles (AgNPs) showed excellent antibacterial activity against ESBL-strains which includes E. coli, Proteus. sp. and Klebsiella sp.« less

Transmission Electron Microscopy of Minerals and Rocks

NASA Astrophysics Data System (ADS)

McLaren, Alex C.

1991-04-01

Of the many techniques that have been applied to the study of crystal defects, none has contributed more to our understanding of their nature and influence on the physical and chemical properties of crystalline materials than transmission electron microscopy (TEM). TEM is now used extensively by an increasing number of earth scientists for direct observation of defect microstructures in minerals and rocks. Transmission Electron Microscopy of Rocks and Minerals is an introduction to the principles of the technique and is the only book to date on the subject written specifically for geologists and mineralogists. The first part of the book deals with the essential physics of the transmission electron microscope and presents the basic theoretical background required for the interpretation of images and electron diffraction patterns. The final chapters are concerned with specific applications of TEM in mineralogy and deal with such topics as planar defects, intergrowths, radiation-induced defects, dislocations and deformation-induced microstructures. The examples cover a wide range of rock-forming minerals from crustal rocks to those in the lower mantle, and also take into account the role of defects in important mineralogical and geological processes.

Optically active substituted polyacetylene@carbon nanotube hybrids: Preparation, characterization and infrared emissivity property study

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

Bu, Xiaohai; Zhou, Yuming, E-mail: ymzhou@seu.edu.cn; Zhang, Tao

Optically active substituted polyacetylene@multiwalled carbon nanotubes (SPA@MWCNTs) nanohybrids were fabricated by wrapping helical SPA copolymers onto the surface of modified nanotubes through ester bonding linkage. SPA copolymer based on chiral phenylalanine and serine was pre-polymerized by a rhodium zwitterion catalyst in THF, and evidently proved to possess strong optical activity and adopt a predominately one-handed helical conformation. Various characterizations including Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and transmission electron microscopy (TEM) demonstrated that the SPA had been covalently grafted onto the nanotubes without destroying their original graphite structure. The wrapped SPA was found tomore » exhibit an enhancement in thermal stability and still maintained considerable optical activity after grafting. The infrared emissivity property of the nanohybrids at 8–14 μm was investigated in addition. The results indicated that the SPA@MWCNTs hybrid matrix could possess a much lower infrared emissivity value (ε=0.707) than raw MWCNTs, which might be due to synergistic effect of the unique helical conformation of optically active SPA and strengthened interfacial interaction between the organic polymers and inorganic nanoparticles. - Graphical abstract: Optically active SPA@MWCNTs nanohybrids with low infrared emissivity. - Highlights: • Synthesis of optically active SPA copolymer derived from serine and phenylalanine. • Preparation and characterization of optically active SPA@MWCNTs nanohybrids. • Application study of the SPA@MWCNTs nanohybrids (ε=0.707) in lowering the infrared emissivity.« less

FIB-SEM imaging of carbon nanotubes in mouse lung tissue.

PubMed

Købler, Carsten; Saber, Anne Thoustrup; Jacobsen, Nicklas Raun; Wallin, Håkan; Vogel, Ulla; Qvortrup, Klaus; Mølhave, Kristian

2014-06-01

Ultrastructural characterisation is important for understanding carbon nanotube (CNT) toxicity and how the CNTs interact with cells and tissues. The standard method for this involves using transmission electron microscopy (TEM). However, in particular, the sample preparation, using a microtome to cut thin sample sections for TEM, can be challenging for investigation of regions with agglomerations of large and stiff CNTs because the CNTs cut with difficulty. As a consequence, the sectioning diamond knife may be damaged and the uncut CNTs are left protruding from the embedded block surface excluding them from TEM analysis. To provide an alternative to ultramicrotomy and subsequent TEM imaging, we studied focused ion beam scanning electron microscopy (FIB-SEM) of CNTs in the lungs of mice, and we evaluated the applicability of the method compared to TEM. FIB-SEM can provide serial section volume imaging not easily obtained with TEM, but it is time-consuming to locate CNTs in the tissue. We demonstrate that protruding CNTs after ultramicrotomy can be used to locate the region of interest, and we present FIB-SEM images of CNTs in lung tissue. FIB-SEM imaging was applied to lung tissue from mice which had been intratracheally instilled with two different multiwalled CNTs; one being short and thin, and the other longer and thicker. FIB-SEM was found to be most suitable for detection of the large CNTs (Ø ca. 70 nm), and to be well suited for studying CNT agglomerates in biological samples which is challenging using standard TEM techniques.

Study of cobalt effect on structural and optical properties of Dy doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Kumar, Pawan; Pandey, Praveen C.

2018-05-01

The present study has been carried out to investigate the effect of Co doping on structural and optical properties of Dy doped ZnO nanoparticles. We have prepared pure Zinc oxide, Dy (1%) doped ZnO and Dy (1%) doped ZnO co-doped with Co(2%) with the help of simple sol-gel combustion method. The structural analysis carried out using X-ray diffraction spectra (XRD) indicates substitution of Dy and Co at Zn site of ZnO crystal structure and hexagonal crystal structure without any secondary phase formation in all the samples. The surface morphology was analyzed by transmission electron microscopy (TEM). Absorption study indicates that Dy doping causes a small shift in band edge, while Co co-doping results significant change is absorption edge as well as introduce defect level absorption in the visible region. The band gap of samples decreases due to Dy and Co doping, which can be attributed to defect level formation below the conduction band in the system.

Investigations on structural, optical and magnetic properties of Dy-doped zinc ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Vinosha, P. Annie; Deepapriya, S.; Rodney, John. D.; Das, S. Jerome

2018-04-01

A persuasive and thriftily feasible homogeneous co-precipitation route was adopted to fabricate dysprosium (Dy) doped zinc ferrite (Zn1-xDyxFe2O4)nanoparticles in order to examine their structural, optical and magnetic properties. Theas-synthesized Zn1-xDyxFe2O4 was studied for its momentous applications in photo-degradation of organic Methylene Blue (MB) dye. The paper marksthe connotation of zinc ferrite nanocatalyst in Photo-Fenton degradation. The chemical composition of dysprosium has a decisive feature of this research work. From X-ray diffraction analysis (XRD), spinel phase formation of theas-synthesized Zn1-xDyxFe2O4 nanoparticles was observedand the crystallite size was foundto increase as the doping concentration increased. Theabsorption bands peaked between 600-400 cm-l waspragmatic by Fourier Transform Infrared spectral analysis (FTIR). Transmission Electron Microscopy (TEM) micrograph elucidated the morphology and the speck size of as-synthesized nanoparticles. Surface area and pore size were determined by Brunauer-Emmett-Teller (BET) technique.

Optical and electrical properties of GaN-based light emitting diodes grown on micro- and nano-scale patterned Si substrate

NASA Astrophysics Data System (ADS)

Chiu, Ching-Hsueh; Lin, Chien-Chung; Deng, Dongmei; Kuo, Hao-Chung; Lau, Kei-May

2011-10-01

We investigate the optical and electrical characteristics of the GaN-based light emitting diodes (LEDs) grown on Micro and Nano-scale Patterned silicon substrate (MPLEDs and NPLEDs). The transmission electron microscopy (TEM) images reveal the suppression of threading dislocation density in InGaN/GaN structure on nano-pattern substrate due to nanoscale epitaxial lateral overgrowth (NELOG). The plan-view and cross-section cathodoluminescence (CL) mappings show less defective and more homogeneous active quantum well region growth on nano-porous substrates. From temperature dependent photoluminescence (PL) and low temperature time-resolved photoluminescence (TRPL) measurement, NPLEDs has better carrier confinement and higher radiative recombination rate than MPLEDs. In terms of device performance, NPLEDs exhibits smaller electroluminescence (EL) peak wavelength blue shift, lower reverse leakage current and decreases efficiency droop compared with the MPLEDs. These results suggest the feasibility of using NPSi for the growth of high quality and power LEDs on Si substrates.

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

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

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

2004-05-01

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

Shape and crystallographic orientation of nanodiamonds for quantum sensing.

PubMed

Ong, S Y; Chipaux, M; Nagl, A; Schirhagl, R

2017-05-03

Nanodiamonds with dimensions down to a few tens of nanometers containing nitrogen-vacancy (NV) color centers have revealed their potential as powerful and versatile quantum sensors with a unique combination of spatial resolution and sensitivity. The NV centers allow transducing physical properties, such as strain, temperature, and electric or magnetic field, to an optical transition that can be detected in the single photon range. For example, this makes it possible to sense a single electron spin or a few nuclear spins by detecting their magnetic resonance. The location and orientation of these defects with respect to the diamond surface play a crucial role in interpreting the data and predicting their sensitivities. Despite its relevance, the geometry of these nanodiamonds has never been thoroughly investigated. Without accurate data, spherical models have been applied to interpret or predict results in the past. With the use of High Resolution Transmission Electron Microscopy (HR-TEM), Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM), we investigated nanodiamonds with an average hydrodynamic diameter of 25 nm (the most common type for quantum sensing) and found a flake-like geometry, with 23.2 nm and 4.5 nm being the average lateral and vertical dimensions. We have also found evidence for a preferred crystallographic orientation of the main facet in the (110) direction. Furthermore, we discuss the consequences of this difference in geometry on diamond-based applications. Shape not only influences the creation efficiency of nitrogen-vacancy centers and their quantum coherence properties (and thus sensing performance), but also the optical properties of the nanodiamonds, their interaction with living cells, and their surface chemistry.

Enhanced broadband near-infrared luminescence from Pr3+-doped tellurite glass with silver nanoparticles

NASA Astrophysics Data System (ADS)

Cheng, Pan; Zhou, Yaxun; Zhou, Minghan; Su, Xiue; Zhou, Zizhong; Yang, Gaobo

2017-11-01

Pr3+-doped tellurite glasses containing metallic silver NPs were synthesized by the conventional melt-quenching technique. Structural, thermal and optical properties of the synthesized glass samples were characterized by X-Ray diffraction (XRD) curves, Raman spectra, differential scanning calorimeter (DSC) curves, transmission electron microscopy (TEM) images, UV/Vis/NIR absorption and near-infrared fluorescence emission spectra. The XRD curves confirmed the amorphous structural nature of the synthesized glasses, the Raman spectra identified the presence of different vibrational groups, the DSC curves verified the good thermal stability, and the TEM images revealed the nucleated silver NPs with average diameter about 10 nm dispersed in the glass matrix and its surface Plasmon resonance (SPR) absorption band was located at around 510 nm. Besides, Judd-Ofelt intensity parameters Ωt (t = 2, 4, 6) and other important spectroscopic parameters like transition probability, radiative lifetime, branching ratio were calculated to evaluate the radiative properties of Pr3+ levels from the measured optical absorption spectra. It was found that Pr3+-doped tellurite glasses could emit an ultra-broadband fluorescence extending from 1250 to 1650 nm under the 488 nm excitation, and this fluorescence emission increased further with the introduction of silver NPs. The enhanced fluorescence was mainly attributed to the increased local electric field around Pr3+ induced by silver NPs. The present results demonstrate that Pr3+-Ag codoped tellurite glass is a promising candidate for the near-infrared band ultra-broadband fiber amplifiers covering the expanded low-loss communication window.

High-energy ball milling technique for ZnO nanoparticles as antibacterial material

PubMed Central

Salah, Numan; Habib, Sami S; Khan, Zishan H; Memic, Adnan; Azam, Ameer; Alarfaj, Esam; Zahed, Nabeel; Al-Hamedi, Salim

2011-01-01

Nanoparticles of zinc oxide (ZnO) are increasingly recognized for their utility in biological applications. In this study, the high-energy ball milling (HEBM) technique was used to produce nanoparticles of ZnO from its microcrystalline powder. Four samples were ball milled for 2, 10, 20, and 50 hours, respectively. The structural and optical modifications induced in the ‘as synthesized’ nanomaterials were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM), and photoluminescence emission spectra (PL). SEM and TEM results show a gradual decrease in particle size from around 600 to ∼30 nm, with increased milling time. The initial microstructures had random shapes, while the final shape became quite spherical. XRD analysis showed ZnO in a hexagonal structure, broadening in the diffracted peaks and going from larger to smaller particles along with a relaxation in the lattice constant c. The value of c was found to increase from 5.204 to 5.217 Å with a decrease in particle size (600 to ∼30 nm). PL result showed a new band at around 365 nm, whose intensity is found to increase as the particles size decreases. These remarkable structural and optical modifications induced in ZnO nanoparticles might prove useful for various applications. The increase in c value is an important factor for increasing the antibacterial effects of ZnO, suggesting that the HEBM technique is quite suitable for producing these nanoparticles for this purpose. PMID:21720499

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

PubMed

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

2018-06-07

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

Importance of microscopy in durability studies of solidified and stabilized contaminated soils

USGS Publications Warehouse

Klich, I.; Wilding, L.P.; Drees, L.R.; Landa, E.R.

1999-01-01

Solidification/stabilization (S/S) is recognized by the U.S. EPA as a best demonstrated available technology for the containment of contaminated soils and other hazardous wastes that cannot be destroyed by chemical, thermal, or biological means. Despite the increased use of S/S technologies, little research has been conducted on the weathering and degradation of solidified and stabilized wastes once the treated materials have been buried. Published data to verify the performance and durability of landfilled treated wastes over time are rare. In this preliminary study, optical and electron microscopy (scanning electron microscopy [SEM], transmission electron microscopy [TEM] and electron probe microanalyses [EPMA]) were used to evaluate weathering features associated with metal-bearing contaminated soil that had been solidified and stabilized with Portland cement and subsequently buried on site, stored outdoors aboveground, or achieved in a laboratory warehouse for up to 6 yr. Physical and chemical alteration processes identified include: freeze-thaw cracking, cracking caused by the formation of expansive minerals such as ettringite, carbonation, and the movement of metals from waste aggregates into the cement micromass. Although the extent of degradation after 6 yr is considered slight to moderate, results of this study show that the same environmental concerns that affect the durability of concrete must be considered when evaluating the durability and permanence of the solidification and stabilization of contaminated soils with cement. In addition, such evaluations cannot be based on leaching and chemical analyses alone. The use of all levels of microscopic analyses must be incorporated into studies of the long-term performance of S/S technologies.Solidification/stabilization (S/S) is recognized by the U.S. EPA as a best demonstrated available technology for the containment of contaminated soils and other hazardous wastes that cannot be destroyed by chemical, thermal, or biological means. Despite the increased use of S/S technologies, little research has been conducted on the weathering and degradation of solidified and stabilized wastes once the treated materials have been buried. Published data to verify the performance and durability of landfilled treated wastes over time are rare. In this preliminary study, optical and electron microscopy (scanning electron microscopy [SEM], transmission electron microscopy [TEM] and electron probe microanalyses [EPMA]) were used to evaluate weathering features associated with metal-bearing contaminated soil that had been solidified and stabilized with Portland cement and subsequently buried on site, stored outdoors aboveground, or archived in a laboratory, warehouse for up to 6 yr. Physical and chemical alteration processes identified include: freeze-thaw cracking, cracking caused by the formation of expansive minerals such as ettringite, carbonation, and the movement of metals from waste aggregates into the cement micromass. Although the extent of degradation after 6 yr is considered slight to moderate, results of this study show that the same environmental concerns that affect the durability of concrete must be considered when evaluating the durability and permanence of the solidification and stabilization of contaminated soils with cement. In addition, such evaluations cannot be based on leaching and chemical analyses alone. The use of all levels of microscopic analyses must be incorporated into studies of the long-term performance of S/S technologies.

Do it yourself: optical spectrometer for physics undergraduate instruction in nanomaterial characterization

NASA Astrophysics Data System (ADS)

Yeti Nuryantini, Ade; Cahya Septia Mahen, Ea; Sawitri, Asti; Wahid Nuryadin, Bebeh

2017-09-01

In this paper, we report on a homemade optical spectrometer using diffraction grating and image processing techniques. This device was designed to produce spectral images that could then be processed by measuring signal strength (pixel intensity) to obtain the light source, transmittance, and absorbance spectra of the liquid sample. The homemade optical spectrometer consisted of: (i) a white LED as a light source, (ii) a cuvette or sample holder, (iii) a slit, (iv) a diffraction grating, and (v) a CMOS camera (webcam). In this study, various concentrations of a carbon nanoparticle (CNP) colloid were used in the particle size sample test. Additionally, a commercial optical spectrometer and tunneling electron microscope (TEM) were used to characterize the optical properties and morphology of the CNPs, respectively. The data obtained using the homemade optical spectrometer, commercial optical spectrometer, and TEM showed similar results and trends. Lastly, the calculation and measurement of CNP size were performed using the effective mass approximation (EMA) and TEM. These data showed that the average nanoparticle sizes were approximately 2.4 nm and 2.5 ± 0.3 nm, respectively. This research provides new insights into the development of a portable, simple, and low-cost optical spectrometer that can be used in nanomaterial characterization for physics undergraduate instruction.

Differences in Physical and Biochemical Properties of Thermus scotoductus SA-01 Cultured with Dielectric or Convection Heating.

PubMed

Cockrell, Allison L; Fitzgerald, Lisa A; Cusick, Kathleen D; Barlow, Daniel E; Tsoi, Stanislav D; Soto, Carissa M; Baldwin, Jeffrey W; Dale, Jason R; Morris, Robert E; Little, Brenda J; Biffinger, Justin C

2015-09-01

A thermophile, Thermus scotoductus SA-01, was cultured within a constant-temperature (65°C) microwave (MW) digester to determine if MW-specific effects influenced the growth and physiology of the organism. As a control, T. scotoductus cells were also cultured using convection heating at the same temperature as the MW studies. Cell growth was analyzed by optical density (OD) measurements, and cell morphologies were characterized using electron microscopy imaging (scanning electron microscopy [SEM] and transmission electron microscopy [TEM]), dynamic light scattering (DLS), and atomic force microscopy (AFM). Biophysical properties (i.e., turgor pressure) were also calculated with AFM, and biochemical compositions (i.e., proteins, nucleic acids, fatty acids) were analyzed by attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy. Gas chromatography-mass spectrometry (GC-MS) was used to analyze the fatty acid methyl esters extracted from cell membranes. Here we report successful cultivation of a thermophile with only dielectric heating. Under the MW conditions for growth, cell walls remained intact and there were no indications of membrane damage or cell leakage. Results from these studies also demonstrated that T. scotoductus cells grown with MW heating exhibited accelerated growth rates in addition to altered cell morphologies and biochemical compositions compared with oven-grown cells. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

Transmission/Scanning Transmission Electron Microscopy | Materials Science

Science.gov Websites

imaging such as high resolution TEM. Transmission electron diffraction patterns help to determine the microstructure of a material and its defects. Phase-contrast imaging or high-resolution (HR) TEM imaging gives high scattering angle can be collected to form high-resolution, chemically sensitive, atomic number (Z

PROPOSED ASTM METHOD FOR THE DETERMINATION OF ASBESTOS IN AIR BY TEM AND INFORMATION ON INTERFERING FIBERS

EPA Science Inventory

The draft of the ASTM Test Method for air entitled: "Airborne Asbestos Concentration in Ambient and Indoor Atmospheres as Determined by Transmission Electron Microscopy Direct Transfer (TEM)" (ASTM Z7077Z) is an adaptation of the International Standard, ISO 10312. It is currently...

Correlative transmission electron microscopy and electrical properties study of switchable phase-change random access memory line cells

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

Oosthoek, J. L. M.; Kooi, B. J., E-mail: B.J.Kooi@rug.nl; Voogt, F. C.

2015-02-14

Phase-change memory line cells, where the active material has a thickness of 15 nm, were prepared for transmission electron microscopy (TEM) observation such that they still could be switched and characterized electrically after the preparation. The result of these observations in comparison with detailed electrical characterization showed (i) normal behavior for relatively long amorphous marks, resulting in a hyperbolic dependence between SET resistance and SET current, indicating a switching mechanism based on initially long and thin nanoscale crystalline filaments which thicken gradually, and (ii) anomalous behavior, which holds for relatively short amorphous marks, where initially directly a massive crystalline filament ismore » formed that consumes most of the width of the amorphous mark only leaving minor residual amorphous regions at its edges. The present results demonstrate that even in (purposely) thick TEM samples, the TEM sample preparation hampers the probability to observe normal behavior and it can be debated whether it is possible to produce electrically switchable TEM specimen in which the memory cells behave the same as in their original bulk embedded state.« less

Correlative transmission electron microscopy and electrical properties study of switchable phase-change random access memory line cells

NASA Astrophysics Data System (ADS)

Oosthoek, J. L. M.; Voogt, F. C.; Attenborough, K.; Verheijen, M. A.; Hurkx, G. A. M.; Gravesteijn, D. J.; Kooi, B. J.

2015-02-01

Phase-change memory line cells, where the active material has a thickness of 15 nm, were prepared for transmission electron microscopy (TEM) observation such that they still could be switched and characterized electrically after the preparation. The result of these observations in comparison with detailed electrical characterization showed (i) normal behavior for relatively long amorphous marks, resulting in a hyperbolic dependence between SET resistance and SET current, indicating a switching mechanism based on initially long and thin nanoscale crystalline filaments which thicken gradually, and (ii) anomalous behavior, which holds for relatively short amorphous marks, where initially directly a massive crystalline filament is formed that consumes most of the width of the amorphous mark only leaving minor residual amorphous regions at its edges. The present results demonstrate that even in (purposely) thick TEM samples, the TEM sample preparation hampers the probability to observe normal behavior and it can be debated whether it is possible to produce electrically switchable TEM specimen in which the memory cells behave the same as in their original bulk embedded state.

Radiation induced deposition of copper nanoparticles inside the nanochannels of poly(acrylic acid)-grafted poly(ethylene terephthalate) track-etched membranes

NASA Astrophysics Data System (ADS)

Korolkov, Ilya V.; Güven, Olgun; Mashentseva, Anastassiya A.; Atıcı, Ayse Bakar; Gorin, Yevgeniy G.; Zdorovets, Maxim V.; Taltenov, Abzal A.

2017-01-01

Poly(ethylene terephthalate) PET, track-etched membranes (TeMs) with 400 nm average pore size were UV-grafted with poly(acrylic acid) (PAA) after oxidation of inner surfaces by H2O2/UV system. Carboxylate groups of grafted PAA chains were easily complexed with Cu2+ ions in aqueous solutions. These ions were converted into metallic copper nanoparticles (NPs) by radiation-induced reduction of copper ions in aqueous-alcohol solution by gamma rays in the dose range of 46-250 kGy. Copper ions chelating with -COOH groups of PAA chains grafted on PET TeMs form polymer-metal ion complex that prevent the formation of agglomerates during reduction of copper ions to metallic nanoparticles. The detailed analysis by X-Ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed the deposition of copper nanoparticles with the average size of 70 nm on the inner surface of nanochannels of PET TeMs. Samples were also investigated by FTIR, ESR spectroscopies to follow copper ion reduction.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Liquid crystal-based glucose biosensor functionalized with mixed PAA and QP4VP brushes.

PubMed

Khan, Mashooq; Park, Soo-Young

2015-06-15

4-Cyano-4'-pentylbiphenyl (5CB) in a transmission electron microscopy (TEM) grid was developed for glucose detection by coating with a monolayer of mixed polymer brushes using poly(acrylicacid-b-4-cynobiphenyl-4'-oxyundecylacrylate) (PAA-b-LCP) and quaternized poly(4-vinylpyridine-b-4-cynobiphenyl-4'-oxyundecylacrylate) (QP4VP-b-LCP) (LCP stands for liquid crystal polymer) at the 5CB/aqueous interface. The resultant 5CB in TEM grid was functionalized with the PAA and QP4VP brushes, which were strongly anchored by the LCP block. The PAA brush rendered the 5CB/aqueous interface pH-responsive and the QP4VP brush immobilized glucose oxidase (GOx) through electrostatic interactions without the aid of coupling agents. The glucose was detected through a homeotropic-to-planar orientational transition of the 5CB observed through a polarized optical microscope (POM) under crossed polarizers. The optimum immobilization with a 0.78 µM GOx solution on the dual-brush-coated TEM grid enabled glucose detection at concentrations higher than 0.5 mM with response times shorter than 180 s. This TEM grid glucose sensor provided a linear response of birefringence of the 5CB to glucose concentrations ranging from 0.5 to 11 mM with a Michaelis-Menten constant (Km) of 1.67 mM. This new and sensitive glucose biosensor has the advantages of low production cost, simple enzyme immobilization, high enzyme sensitivity and stability, and easy detection with POM, and may be useful for prescreening the glucose level in the human body. Copyright © 2015 Elsevier B.V. All rights reserved.

Nanocuvette: A Functional Ultrathin Liquid Container for Transmission Electron Microscopy.

PubMed

Wadell, Carl; Inagaki, Satoshi; Nakamura, Tomiro; Shi, Ji; Nakamura, Yoshio; Sannomiya, Takumi

2017-02-28

Advances in TEM techniques have spurred a renewed interest in a wide variety of research fields. A rather recent track within these endeavors is the use of TEM for in situ imaging in liquids. In this article, we show the fabrication of a liquid cell for TEM observations which we call the nanocuvette. The structure consists of a nanohole film sandwiched by carbon films, sealing liquid in the holes. The hole film can be produced using a variety of materials, tailored for the desired application. Since the fabrication is based on self-assembly, it is both cheap and straightforward. Compared to previously reported liquid cells, this structure allows for thinner liquid layers with better controlled cell structures, making it possible to achieve a high resolution even at lower acceleration voltages and electron doses. We demonstrate a resolution corresponding to an information transfer up to ∼2 nm at 100 kV for molecular imaging. Apart from the advantages arising from the thin liquid layer, the nanocuvette also enables the possibility to study liquid-solid interfaces at the side walls of the nanoholes. We illustrate the possibilities of the nanocuvette by studying several model systems: electron beam induced growth dynamics of silver nanoparticles in salt solution, polymer deposition from solution, and imaging of nonstained antibodies in solution. Finally, we show how the inclusion of a plasmonically active gold layer in the nanocuvette structure enables optical confirmation of successful liquid encapsulation prior to TEM studies. The nanocuvette provides an easily fabricated and flexible platform which can help further the understanding of reactions, processes, and conformation of molecules and atoms in liquid environments.

Experimental shock deformation in zircon: a transmission electron microscopic study

NASA Astrophysics Data System (ADS)

Leroux, H.; Reimold, W. U.; Koeberl, C.; Hornemann, U.; Doukhan, J.-C.

1999-06-01

In recent years, apparently shock-induced and, thus, impact-characteristic microdeformations, in the form of planar microdeformation features and so-called strawberry (granular) texture, have been observed in zircons in rocks from confirmed impact structures and from the K/ T boundary. The nature of the planar microdeformations in this mineral is, however, still unknown, and critical information is needed regarding the shock pressure range in which these deformation effects are produced. We experimentally shock deformed two series of thin zircon (ZrSiO 4) target plates, cut perpendicular to the c-axis, at shock pressures of 20, 40, and 60 GPa. The recovered samples were characterized by optical and scanning electron microscopy. In addition, one sample series was studied by transmission electron microscopy (TEM). Microdeformation effects observed at 20 GPa include pervasive micro-cleavage and dislocation patterns. Plastic deformation is indicated by a high density of straight dislocations in glide configuration. The dominant glide systems are <100>{010}. Micro-cleavages, induced by shear stresses during the compression stage, occur mostly in the {100} planes. The large density of dislocations at crack tips shows that plastic deformation was initiated by the micro-cracking processs. At 40 GPa, the sample was partly transformed from the zircon (z) to a scheelite (CaWO 4)-type (s) structure. Planar deformation features (PDFs) containing an amorphous phase of zircon composition are present in the not yet transformed zircon relics. The phase with scheelite structure, initiated in the {100} planes of zircon, consists of thin (0.1 to several μm) bands that crosscut the zircon matrix. The phase transformation is displacive (martensitic) and can be related by {100} z // {112} s and [001] z // <110> s. The scheelite structure phase is densely twinned, with twins in the (112) plane. The 60-GPa sample consists completely of the scheelite structure phase. Crosscutting and displacing relationships between twins and PDFs demonstrate that PDFs are formed in the zircon structure, i.e., before the phase transformation to the scheelite structure occurred, most likely at the shock front. Crystallographic orientations of optically visible planar features in zircon, in comparison with orientations of planar defects at the TEM scale, suggest that the optically visible features are more likely planar microfractures than PDFs.

Lattice Matched Iii-V IV Semiconductor Heterostructures: Metalorganic Chemical Vapor Deposition and Remote Plasma Enhanced Chemical Vapor Deposition.

NASA Astrophysics Data System (ADS)

Choi, Sungwoo

1992-01-01

This thesis describes the growth and characterization of wide gap III-V compound semiconductors such as aluminum gallium arsenide (Al_{rm x} Ga_{rm 1-x}As), gallium nitride (GaN), and gallium phosphide (GaP), deposited by the metalorganic chemical vapor deposition (MOCVD) and remote plasma enhanced chemical vapor deposition (Remote PECVD). In the first part of the thesis, the optimization of GaAs and Al_{rm x}Ga _{rm 1-x}As hetero -epitaxial layers on Ge substrates is described in the context of the application in the construction of cascade solar cells. The emphasis on this study is on the trade-offs in the choice of the temperature related to increasing interdiffusion/autodoping and increasing perfection of the epilayer with increasing temperature. The structural, chemical, optical, and electrical properties of the heterostructures are characterized by x-ray rocking curve measurement, scanning electron microscopy (SEM), electron beam induced current (EBIC), cross-sectional transmission electron microscopy (X-TEM), Raman spectroscopy, secondary ion mass spectrometry (SIMS), and steady-state and time-resolved photoluminescence (PL). Based on the results of this work the optimum growth temperature is 720^circC. The second part of the thesis describes the growth of GaN and GaP layers on silicon and sapphire substrates and the homoepitaxy of GaP by remote PECVD. I have designed and built an ultra high vacuum (UHV) deposition system which includes: the gas supply system, the pumping system, the deposition chamber, the load-lock chamber, and the waste disposal system. The work on the deposition of GaN on Si and sapphire focuses onto the understanding of the growth kinetics. In addition, Auger electron spectroscopy (AES) for surface analysis, x-ray diffraction methods and microscopic analyses using SEM and TEM for structural characterization, infrared (IR) and ultraviolet (UV) absorption measurements for optical characterization, and electrical characterization results on the GaN films are presented. In the deposition GaP thin films by remote PECVD, trimethylgallium and in-situ generated phosphine precursors are employed as source gases which permits homo- and heteroepitaxial growth as substrate temperature of 590-620^ circC. Also, the growth kinetics of gallium phosphide is discussed. As in the case of GaN, the surface, structural, chemical, optical, and electrical properties are characterized and the results are discussed.

A top-down method to fabricate SrAl2O4:Eu2+,Dy3+ nanosheets from commercial blocky phosphors

NASA Astrophysics Data System (ADS)

Zhang, Haoran; Xue, Zhiping; Lei, Bingfu; Dong, Hanwu; Zhang, Haiming; Deng, Suqing; Zheng, Mingtao; Liu, Yingliang; Xiao, Yong

2014-09-01

By using commercial SrAl2O4:Eu2+,Dy3+ phosphor as raw material, we have developed a novel and simple top-down method to fabricate SrAl2O4:Eu2+,Dy3+ nanosheets that are useful for potential practical applications, especially as fluorescent labels for biomolecules and mechano-optical nano-devices. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDX) results demonstrate that the treated samples are still pure-phase of SrAl2O4:Eu2+,Dy3+. The field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) results indicate that the treated SrAl2O4:Eu2+,Dy3+ phosphors are built up by nanosheets bundles. Excitation and emission spectra, afterglow emission spectra and decay curves are used to analyze the luminescence properties of SrAl2O4:Eu2+,Dy3+ nanosheets, and the results show that, compared with commercial samples, the treated samples show similar spectra characteristic including the spectra shapes and the band position. Furthermore, the fluorescence and afterglow intensity of SrAl2O4:Eu2+,Dy3+ nanosheets can be tuned linearly by changing the circumstance temperatures, which further indicates its potential applications in fiber-optical thermometer materials.

Development of CdS Nanostructures by Thermal Decomposition of Aminocaproic Acid-Mixed Cd-Thiourea Complex Precursor: Structural, Optical and Photocatalytic Characterization.

PubMed

Patel, Jayesh D; Mighri, Frej; Ajji, Abdellah; Chaudhuri, Tapas K

2015-04-01

The present work deals with two different CdS nanostructures produced via hydrothermal and solvothermal decompositions of aminocaproic acid (ACA)-mixed Cd-thiourea complex precursor at 175 °C. Both nanostructures were extensively characterized for their structural, morphological and optical properties. The powder X-ray diffraction characterization showed that the two CdS nanostructures present a wurtzite morphology. Scanning electron microscopy and energy-dispersive X-ray characterizations revealed that the hydrothermal decomposition produced well-shaped CdS flowers composed of six dendritic petals, and the solvothermal decomposition produced CdS microspheres with close stoichiometric chemical composition. The UV-vis absorption and photoluminescence spectra of CdS dendritic flowers and microsphere nanostructures showed that both nanostructures present a broad absorption between 200 and 700 nm and exhibit strong green emissions at 576 and 520 nm upon excitations at 290 nm and 260 nm, respectively. The transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) characterizations confirmed that CdS microspheres were mesoporous and were composed of small nanocrystals. A possible growth mechanism in the formation of the CdS nanostructures was proposed based on morphology evolution as a function of the reaction time. Furthermore, the as-synthesized CdS nanostructures were found to exhibit highly efficient photocatalytic activities for the degradation of methyl orange (MeO) and rhodamine B (RhB) dyes.

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.

Preparation and optical properties of indium tin oxide/epoxy nanocomposites with polyglycidyl methacrylate grafted nanoparticles.

PubMed

Tao, Peng; Viswanath, Anand; Schadler, Linda S; Benicewicz, Brian C; Siegel, Richard W

2011-09-01

Visibly highly transparent indium tin oxide (ITO)/epoxy nanocomposites were prepared by dispersing polyglycidyl methacrylate (PGMA) grafted ITO nanoparticles into a commercial epoxy resin. The oleic acid stabilized, highly crystalline, and near monodisperse ITO nanoparticles were synthesized via a nonaqueous synthetic route with multigram batch quantities. An azido-phosphate ligand was synthesized and used to exchange with oleic acid on the ITO surface. The azide terminal group allows for the grafting of epoxy resin compatible PGMA polymer chains via Cu(I) catalyzed alkyne-azide "click" chemistry. Transmission electron microscopy (TEM) observation shows that PGMA grafted ITO particles were homogeneously dispersed within the epoxy matrix. Optical properties of ITO/epoxy nanocomposites with different ITO concentrations were studied with an ultraviolet-visible-near-infrared (UV-vis-NIR) spectrometer. All the ITO/epoxy nanocomposites show more than 90% optical transparency in the visible light range and absorption of UV light from 300 to 400 nm. In the near-infrared region, ITO/epoxy nanocomposites demonstrate low transmittance and the infrared (IR) transmission cutoff wavelength of the composites shifts toward the lower wavelength with increased ITO concentration. The ITO/epoxy nanocomposites were applied onto both glass and plastic substrates as visibly transparent and UV/IR opaque optical coatings.

Ion-beam-assisted deposition of Au nanocluster/Nb 2O 5 thin films with nonlinear optical properties

NASA Astrophysics Data System (ADS)

Cotell, C. M.; Schiestel, S.; Carosella, C. A.; Flom, S.; Hubler, G. K.; Knies, D. L.

1997-05-01

Gold nanocluster thin films (˜ 200 nm thickness) consisting of metal clusters ˜ 5 nm in size embedded in a matrix of Nb 2O 5 were deposited by ion beam-assisted deposition (IBAD) by coevaporation of Au and Nb with O 2+ ion bombardment. The microstructure and optical characteristics of these films were examined as-deposited and after annealing at 600°C. Annealing crystallized the amorphous oxide matrix and ripened the nanoclusters. A strong linear absorption at the wavelength of the surface plasmon resonance for Au developed as a result of annealing. The linear optical behavior was modeled using Mie scattering theory. Good agreement was found between the nanocluster sizes predicted by the theory and the particle sizes observed experimentally using transmission electron microscopy (TEM). The nonlinear optical (NLO) properties of the nanocluster films were probed experimentally using degenerate four wave mixing and nonlinear transmission. The wavelength was near the peak of the surface plasmon resonance as measured by VIS/UV spectroscopy. Values of | χxxxx(3)| were 7.3 × 10 -8 and 3.0 × 10 -10 esu for annealed and unannealed samples, respe The dominant mechanism for the nonlinear response was change in dielectric constant due to the generation of a distribution of hot, photoexcited electrons.

A portable cryo-plunger for on-site intact cryogenic microscopy sample preparation in natural environments.

PubMed

Comolli, Luis R; Duarte, Robert; Baum, Dennis; Luef, Birgit; Downing, Kenneth H; Larson, David M; Csencsits, Roseann; Banfield, Jillian F

2012-06-01

We present a modern, light portable device specifically designed for environmental samples for cryogenic transmission-electron microscopy (cryo-TEM) by on-site cryo-plunging. The power of cryo-TEM comes from preparation of artifact-free samples. However, in many studies, the samples must be collected at remote field locations, and the time involved in transporting samples back to the laboratory for cryogenic preservation can lead to severe degradation artifacts. Thus, going back to the basics, we developed a simple mechanical device that is light and easy to transport on foot yet effective. With the system design presented here we are able to obtain cryo-samples of microbes and microbial communities not possible to culture, in their near-intact environmental conditions as well as in routine laboratory work, and in real time. This methodology thus enables us to bring the power of cryo-TEM to microbial ecology. Copyright © 2011 Wiley Periodicals, Inc.

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

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

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

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

Microstructural characterization of Ti-6Al-4V metal chips by focused ion beam (FIB) and transmission electron microscopy (TEM)

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

Schneider, Judy; Dong, Lei; Howe, Jane Y

2011-01-01

The microstructure of the secondary deformation zone (SDZ) near the cutting surface in metal chips of Ti-6Al-4V formed during machining was investigated using focused ion beam (FIB) specimen preparation and transmission electron microscopy (TEM) imaging. Use of the FIB allowed precise extraction of the specimen across this region to reveal its inhomogeneous microstructure resulting from the non-uniform distribution of strain, strain rate, and temperature generated during the cutting process. Initial imaging from conventional TEM foil preparation revealed microstructures ranging from heavily textured to regions of fine grains. Using FIB preparation, the transverse microstructure could be interpreted as fine grains nearmore » the cutting surface which transitioned to coarse grains toward the free surface. At the cutting surface a 10 nm thick recrystallized layer was observed capping a 20 nm thick amorphous layer.« less

Magnetic mapping of iron in rodent spleen

PubMed Central

Blissett, Angela R.; Ollander, Brooke; Penn, Brittany; McTigue, Dana M.; Agarwal, Gunjan

2016-01-01

Evaluation of iron distribution and density in biological tissues is important to understand the pathogenesis of a variety of diseases and the fate of exogenously administered iron-based carriers and contrast agents. Iron distribution in tissues is typically characterized via histochemical (Perl’s) stains or immunohistochemistry for ferritin, the major iron storage protein. A more accurate mapping of iron can be achieved via ultrastructural transmission electron microscopy (TEM) based techniques, which involve stringent sample preparation conditions. In this study, we elucidate the capability of magnetic force microscopy (MFM) as a label-free technique to map iron at the nanoscale level in rodent spleen tissue. We complemented and compared our MFM results with those obtained using Perl’s staining and TEM. Our results show how MFM mapping corresponded to sizes of iron-rich lysosomes at a resolution comparable to that of TEM. In addition MFM is compatible with tissue sections commonly prepared for routine histology. PMID:27890658

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

Yin, Congfei; Liang, Xiaojuan, E-mail: lxj6126@126

The titanate, is a material of interest for various energy applications, including photovoltaics, catalysts, and high-rate energy storage devices. Herein, its related materials, CuO/CaTi{sub 4}O{sub 9} [CCTO] thin films, were successfully fabricated on SrTiO{sub 3} (100) substrates by RF magnetron sputtering assisted with subsequent oxygen annealing. This obtained CCTO thin films were then systemically studied by X-ray powder diffraction (XRD), atomic force microscopy (AFM), scan electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and high-resolution transmission electron microscopy (HRTEM). It was found that CuO and CaTi{sub 4}O{sub 9} (001) particles were closely accumulated together on the surface of the substrate inmore » the annealing process after comparing with that of the as-prepared thin film, which was verified by SEM and AFM results. Furthermore, we investigated the third-order nonlinear optical (NLO) properties of the as-prepared and annealed CCTO thin film by means of the Z-scan technique using 650 nm femtosecond laser pulse. Post-deposition oxygen annealing was found to modify the morphological characteristics of the films, resulting in enhancing their NLO properties. The observation of NLO performance of annealed CCTO thin film indicates that RF magnetron sputtering is a feasible method for the fabrication of optical thin films, which can be expanded to fabricate other NLO materials from the corresponding dispersions. Naturally, we concluded that the CCTO thin film occupy a better NLO property, and thus enlarge its application in nonlinear optics. - Highlights: • The CCTO thin film was prepared using the RF magnetron sputtering and oxygen annealing. • The film was prepared on the SrTiO{sub 3}(100) substrates with a Ca{sub 2}CuO{sub 3} target. • The oxygen annealing was found can effectively enhance the film quality and NLO property. • The film was characterized using XPS, SEM, AFM, TEM, XRD and Z-scan techniques.« less

High-resolution high-sensitivity elemental imaging by secondary ion mass spectrometry: from traditional 2D and 3D imaging to correlative microscopy

NASA Astrophysics Data System (ADS)

Wirtz, T.; Philipp, P.; Audinot, J.-N.; Dowsett, D.; Eswara, S.

2015-10-01

Secondary ion mass spectrometry (SIMS) constitutes an extremely sensitive technique for imaging surfaces in 2D and 3D. Apart from its excellent sensitivity and high lateral resolution (50 nm on state-of-the-art SIMS instruments), advantages of SIMS include high dynamic range and the ability to differentiate between isotopes. This paper first reviews the underlying principles of SIMS as well as the performance and applications of 2D and 3D SIMS elemental imaging. The prospects for further improving the capabilities of SIMS imaging are discussed. The lateral resolution in SIMS imaging when using the microprobe mode is limited by (i) the ion probe size, which is dependent on the brightness of the primary ion source, the quality of the optics of the primary ion column and the electric fields in the near sample region used to extract secondary ions; (ii) the sensitivity of the analysis as a reasonable secondary ion signal, which must be detected from very tiny voxel sizes and thus from a very limited number of sputtered atoms; and (iii) the physical dimensions of the collision cascade determining the origin of the sputtered ions with respect to the impact site of the incident primary ion probe. One interesting prospect is the use of SIMS-based correlative microscopy. In this approach SIMS is combined with various high-resolution microscopy techniques, so that elemental/chemical information at the highest sensitivity can be obtained with SIMS, while excellent spatial resolution is provided by overlaying the SIMS images with high-resolution images obtained by these microscopy techniques. Examples of this approach are given by presenting in situ combinations of SIMS with transmission electron microscopy (TEM), helium ion microscopy (HIM) and scanning probe microscopy (SPM).

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Fundamental metallurgical aspects of axial splitting in zircaloy cladding

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

Chung, H. M.

Fundamental metallurgical aspects of axial splitting in irradiated Zircaloy cladding have been investigated by microstructural characterization and analytical modeling, with emphasis on application of the results to understand high-burnup fuel failure under RIA situations. Optical microscopy, SEM, and TEM were conducted on BWR and PWR fuel cladding tubes that were irradiated to fluence levels of 3.3 x 10{sup 21} n cm{sup {minus}2} to 5.9 x 10{sup 21} n cm{sup {minus}2} (E > 1 MeV) and tested in hot cell at 292--325 C in Ar. The morphology, distribution, and habit planes of macroscopic and microscopic hydrides in as-irradiated and posttest claddingmore » were determined by stereo-TEM. The type and magnitude of the residual stress produced in association with oxide-layer growth and dense hydride precipitation, and several synergistic factors that strongly influence axial-splitting behavior were analyzed. The results of the microstructural characterization and stress analyses were then correlated with axial-splitting behavior of high-burnup PWR cladding reported for simulated-RIA conditions. The effects of key test procedures and their implications for the interpretation of RIA test results are discussed.« less

An approach for scalable production of silver (Ag) decorated WS2 nanosheets

NASA Astrophysics Data System (ADS)

Sumesh, C. K.; Kapatel, Sanni; Chaudhari, Arti

2018-05-01

In the Present study we report the synthesis of Ag nanoparticles (NPs) decorated WS2 nanosheets by sonochemical exfoliation followed by simple chemical reduction process at room temperature. The morphology and microstructure of the as-synthesized Ag-WS2 nanocomposite were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and optical absorption (UV-Vis.) spectroscopy. X-ray and TEM analysis shows the presence of Ag with significant peak over 38.08°, 44.22°, 64.37° and 77.33° at 2θ angle for (111), (200), (220) and (311) respectively. The Ag nanoparticles are randomly distributed throughout the surface of the WS2 nanosheets without undergoing further oxidation during the formation of composites. The formation of Ag-WS2 nanocomposites shows a clear blue shift in the absorption as we obtained the characteristics absorption valleys at 456, 536 and 631 nm from the UV Vis spectroscopy analysis compared to pure WS2 nanosheets. Henceforth a facile method for the Ag decoration on WS2 nanosheets was put forward and briefly discussed. The proposed synthesis method is very promising for the low cost and large-scale synthesis of other noble metal incorporation TMDC compounds.

Analysis of Peroxisome Biogenesis in Pollen by Confocal Microscopy and Transmission Electron Microscopy.

PubMed

Jia, Peng-Fei; Li, Hong-Ju; Yang, Wei-Cai

2017-01-01

Peroxisome is an essential single-membrane bound organelle in most eukaryotic cells and functions in diverse cellular processes. De novo formation, division, and turnover of peroxisomes contribute to its biogenesis, morphology, and population regulation. In plants, peroxisome plays multiple roles, including metabolism, development, and stress response. Defective peroxisome biogenesis and development retard plant growth, adaption, and reproduction. Through tracing the subcellular localization of fluorescent reporter tagged matrix protein of peroxisome, fluorescence microscopy is a reliable and fast way to detect peroxisome biogenesis. Further fine-structural observation of peroxisome by TEM enables researchers to observe the detailed ultrastructure of its morphology and spatial contact with other organelles. Pollen grain is a specialized structure where two small sperm cells are enclosed in the cytoplasm of a large vegetative cell. Two features make pollen grain a good system to study peroxisome biogenesis: indispensable requirement of peroxisome for germination on the stigma and homogeneity. Here, we describe the methods of studying peroxisome biogenesis in Arabidopsis pollen grains by fluorescent live-imaging with confocal laser scanning microscopy (CLSM) and by DAB-staining based transmission electron microscopy (TEM).

Systemic and Microvascular Effects of Resuscitation with Blood Products After Severe Hemorrhage in Rats

DTIC Science & Technology

2014-01-01

thickness, blood flow, and microvascular permeability were studied using intravital microscopy. Hemodynamics and coagulation tests (rotational...Microcirculation; packed red blood cells; intravital microscopy; ROTEM; plasma proteins; rats. Current US military guidance for the resuscitation of warfighters...was used for coagulation assays (rotational thromboelast- ometry [ROTEM], TEM Innovations GmbH, Germany). Intravital Microscopy and Animal Preparation

Strengthening Mechanisms and Their Relative Contributions to the Yield Strength of Microalloyed Steels

NASA Astrophysics Data System (ADS)

Lu, Junfang; Omotoso, Oladipo; Wiskel, J. Barry; Ivey, Douglas G.; Henein, Hani

2012-09-01

Microalloyed steels are used widely in oil and gas pipelines. They are a class of high-strength, low-carbon steels that contain small additions (in amounts less than 0.1 wt pct) of Nb, Ti, and/or V. The steels may contain other alloying elements, such as Mo, in amounts exceeding 0.1 wt pct. Precipitation in these steels can be controlled through thermomechanical-controlled processing, leading to precipitates with sizes that range from several microns to a few nanometers. Microalloyed steels have good strength, good toughness, and excellent weldability, which are attributed in part to the presence of the nanosized carbide and carbonitride precipitates. Because of their fine sizes, wide particle size distribution, and low volume fractions, conventional microscopic methods are not satisfactory for quantifying these precipitates. Matrix dissolution is a promising alternative to extract the precipitates for quantification. Relatively large volumes of material can be analyzed so that statistically significant quantities of precipitates of different sizes are collected. In this article, the microstructure features of a series of microalloyed steels (X70, X80, and X100) as well as a Grade 100 steel are characterized using optical microscopy (OM) and scanning electron microscopy (SEM). A chemical dissolution technique is used to extract the precipitates from the steels. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) are combined to analyze the chemical composition of these precipitates. Rietveld refinement of the XRD patterns is used to quantify fully the relative amounts of these precipitates. The size distribution of the nanosized precipitates is quantified using dark-field imaging (DF) in the TEM. The effects of microalloying content, finish rolling temperature (FRT), and coiling temperature (CT)/interrupted cooling temperature (ICT) on the grain size and the amount of nanoprecipitation are discussed. Individual strengthening contributions from grain size effects, solid-solution strengthening, and precipitation strengthening are quantified to understand fully the strengthening mechanisms for these steels.

Post-ion beam induced degradation of copper layers in transmission electron microscopy specimens

NASA Astrophysics Data System (ADS)

Seidel, F.; Richard, O.; Bender, H.; Vandervorst, W.

2015-11-01

Copper containing transmission electron microscopy (TEM) specimens frequently show corrosion after focused ion beam (FIB) preparation. This paper reveals that the corrosion product is a Cu-S phase growing over the specimen surface. The layer is identified by energy-dispersive x-ray spectroscopy, and lattice spacing indexing of power spectra patterns. The corrosion process is further studied by TEM on cone-shaped specimens, which are intentionally stored after FIB preparation with S flakes for short time. Furthermore, a protective method against corrosion is developed by varying the time in the FIB vacuum and the duration of a subsequent plasma cleaning.

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.

The ultrastructural features of the premalignant oral lesions.

PubMed

Olinici, Doiniţa; Cotrutz, Carmen Elena; Mihali, Ciprian Valentin; Grecu, Vasile Bogdan; Botez, Emanuela Ana; Stoica, Laura; Onofrei, Pavel; Condurache, Oana; Dimitriu, Daniela Cristina

2018-01-01

Premalignant oral lesions are among the most important risk factors for the development of oral squamocellular carcinoma. Recent population studies indicate a significant rise in the prevalence of leukoplakia, erythroplakia/erythroleukoplakia, actinic cheilitis, submucous fibrosis and erosive lichen planus. Since standard histopathological examination has numerous limitations regarding the accurate appreciation of potential malignant transformation, the present study aims to aid these evaluations using the transmission electron microscopy (TEM) technique, which emphasizes ultrastructural changes pertaining to this pathology. Oral mucosa fragments collected from 43 patients that were clinically and histopathologically diagnosed with leukoplakia, erosive actinic cheilitis and erosive lichen planus have been processed through the classic technique for the examination using TEM and were examined using a Philips CM100 transmission electron microscope. The electron microscopy study has confirmed the histopathological diagnosis of the tissue samples examined using photonic microscopy and has furthermore revealed a series of ultrastructural details that on the one hand indicate the tendency for malignant transformation, and on the other reveal characteristic features of tumor development. All the details furnished by TEM complete the overall picture of morphological changes, specific to these lesions, indicating the importance of using these techniques in establishing both a correct diagnosis and prognosis.

Microstructural observation of fuel cell catalyst inks by Cryo-SEM and Cryo-TEM.

PubMed

Shimanuki, Junichi; Takahashi, Shinichi; Tohma, Hajime; Ohma, Atsushi; Ishihara, Ayumi; Ito, Yoshiko; Nishino, Yuri; Miyazawa, Atsuo

2017-06-01

In order to improve the electricity generation performance of fuel cell electric vehicles, it is necessary to optimize the microstructure of the catalyst layer of a polymer electrolyte fuel cell. The catalyst layer is formed by a wet coating process using catalyst inks. Therefore, it is very important to observe the microstructure of the catalyst ink. In this study, the morphology of carbon-supported platinum (Pt/C) particles in catalyst inks with a different solvent composition was investigated by cryogenic scanning electron microscopy (cryo-SEM). In addition, the morphology of the ionomer, which presumably influences the formation of agglomerated Pt/C particles in a catalyst ink, was investigated by cryogenic transmission electron microscopy (cryo-TEM). The results of a cryo-SEM observation revealed that the agglomerated Pt/C particles tended to become coarser with a higher 1-propanol (NPA) weight fraction. The results of a cryo-TEM observation indicated that the actual ionomer dispersion in a catalyst ink formed a network structure different from that of the ionomer in the solvent. © The Author 2017. 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.

Green synthesis and characterization of graphene nanosheets

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

Tavakoli, Farnosh; Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir; Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran

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

Revealing 3D Ultrastructure and Morphology of Stem Cell Spheroids by Electron Microscopy.

PubMed

Jaros, Josef; Petrov, Michal; Tesarova, Marketa; Hampl, Ales

2017-01-01

Cell culture methods have been developed in efforts to produce biologically relevant systems for developmental and disease modeling, and appropriate analytical tools are essential. Knowledge of ultrastructural characteristics represents the basis to reveal in situ the cellular morphology, cell-cell interactions, organelle distribution, niches in which cells reside, and many more. The traditional method for 3D visualization of ultrastructural components, serial sectioning using transmission electron microscopy (TEM), is very labor-intensive due to contentious TEM slice preparation and subsequent image processing of the whole collection. In this chapter, we present serial block-face scanning electron microscopy, together with complex methodology for spheroid formation, contrasting of cellular compartments, image processing, and 3D visualization. The described technique is effective for detailed morphological analysis of stem cell spheroids, organoids, as well as organotypic cell cultures.

Effect of Cold-rolling on Mechanical Properties and Microstructure of an Al-12%Si-0.2%Mg Alloy

NASA Astrophysics Data System (ADS)

Liao, Hengcheng; Cai, Mingdong; Jing, Qiumin; Ding, Ke

2011-11-01

Effect of multi-pass cold-rolling on the mechanical properties and microstructure of a near-eutectic Al-12%Si-0.2%Mg casting alloy was investigated. Optical microscopy, SEM, and TEM were employed to resolve the as-rolled microstructure, and the microstructure of samples after aging treatment. It has been found that Brinell hardness increases considerably with rolling reduction ratio; and further annealing leads to a remarkable drop in hardness. Two mechanisms, namely precipitation hardening and recovery softening, were found to develop simultaneously in the subsequent aging treatment following cold rolling. In contrast, recovery softening dominated the aging of cold-rolled specimen with prior intermediate annealing. Tensile properties were also performed to measure the effect of cold rolling and subsequent aging treatment.

Visible-light photocatalytic activity of graphene oxide-wrapped Bi2WO6 hierarchical microspheres

NASA Astrophysics Data System (ADS)

Zhai, Jiali; Yu, Hongwen; Li, Haiyan; Sun, Lei; Zhang, Kexin; Yang, Hongjun

2015-07-01

A facile approach of fabricating homogeneous graphene oxide (GO)-wrapped Bi2WO6 microspheres (GO/Bi2WO6) is developed. The transmission electron microscopy (TEM) results show that a heterojunction interface between GO and Bi2WO6. The UV-vis diffuse reflection spectra (DRS) reveal that the as-prepared GO/Bi2WO6 composites own more intensive absorption in the visible light range compared with pure Bi2WO6. These characteristic structural and optical properties endow GO/Bi2WO6 composites with enhanced photocatalytic activity. The enhanced photocatalytic activity of the GO/Bi2WO6 is attributed predominantly to the synergetic effect between GO and Bi2WO6, causing rapid generation and separation of photo-generated charge carriers.

Influence of Hot Plastic Deformation in γ and (γ + α) Area on the Structure and Mechanical Properties of High-Strength Low-Alloy (HSLA) Steel.

PubMed

Sas, Jan; Kvačkaj, Tibor; Milkovič, Ondrej; Zemko, Michal

2016-11-30

The main goal of this study was to develop a new processing technology for a high-strength low-alloy (HSLA) steel in order to maximize the mechanical properties attainable at its low alloy levels. Samples of the steel were processed using thermal deformation schedules carried out in single-phase (γ) and dual-phase (γ + α) regions. The samples were rolled at unconventional finishing temperatures, their final mechanical properties were measured, and their strength and plasticity behavior was analyzed. The resulting microstructures were observed using optical and transmission electron microscopy (TEM). They consisted of martensite, ferrite and (NbV)CN precipitates. The study also explored the process of ferrite formation and its influence on the mechanical properties of the material.

Electron and Fluorescence Microscopy of Extracellular Glucan and Aryl-Alcohol Oxidase during Wheat-Straw Degradation by Pleurotus eryngii

PubMed Central

Barrasa, J. M.; Gutiérrez, A.; Escaso, V.; Guillén, F.; Martínez, M. J.; Martínez, A. T.

1998-01-01

The ligninolytic fungus Pleurotus eryngii grown in liquid medium secreted extracellular polysaccharide (87% glucose) and the H2O2-producing enzyme aryl-alcohol oxidase (AAO). The production of both was stimulated by wheat-straw. Polyclonal antibodies against purified AAO were obtained, and a complex of glucanase and colloidal gold was prepared. With these tools, the localization of AAO and extracellular glucan in mycelium from liquid medium and straw degraded under solid-state fermentation conditions was investigated by transmission electron microscopy (TEM) and fluorescence microscopy. These studies revealed that P. eryngii produces a hyphal sheath consisting of a thin glucan layer. This sheath appeared to be involved in both mycelial adhesion to the straw cell wall during degradation and AAO immobilization on hyphal surfaces, with the latter evidenced by double labeling. AAO distribution during differential degradation of straw tissues was observed by immunofluorescence microscopy. Finally, TEM immunogold studies confirmed that AAO penetrates the plant cell wall during P. eryngii degradation of wheat straw. PMID:9435085

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

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

The Effect of Precipitate Evolution on Austenite Grain Growth in RAFM Steel.

PubMed

Yan, Biyu; Liu, Yongchang; Wang, Zejun; Liu, Chenxi; Si, Yonghong; Li, Huijun; Yu, Jianxing

2017-09-01

To study the effects of various types of precipitates and precipitate evolution behavior on austenite (size and phase fraction) in reduced activation ferritic/martensitic (RAFM) steel, RAFM steel was heated to various austenitizing temperatures. The microstructures of specimens were observed using optical microscopy (OM) and transmission electron microscopy (TEM). The results indicate that the M 23 C₆ and MX precipitates gradually coarsen and dissolve into the matrix as the austenitizing temperatures increase. The M 23 C₆ precipitates dissolve completely at 1100 °C, while the MX precipitates dissolve completely at 1200 °C. The evolution of two types of precipitate has a significant effect on the size of austenite. Based on the Zener pinning model, the effect of precipitate evolution on austenite grain size is quantified. It was found that the coarsening and dissolution of M 23 C₆ and MX precipitates leads to a decrease in pinning pressure on grain boundaries, facilitating the rapid growth of austenite grains. The austenite phase fraction is also affected by the coarsening and dissolution of precipitates.

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

The Effect of Precipitate Evolution on Austenite Grain Growth in RAFM Steel

PubMed Central

Yan, Biyu; Liu, Yongchang; Wang, Zejun; Liu, Chenxi; Si, Yonghong; Li, Huijun; Yu, Jianxing

2017-01-01

To study the effects of various types of precipitates and precipitate evolution behavior on austenite (size and phase fraction) in reduced activation ferritic/martensitic (RAFM) steel, RAFM steel was heated to various austenitizing temperatures. The microstructures of specimens were observed using optical microscopy (OM) and transmission electron microscopy (TEM). The results indicate that the M23C6 and MX precipitates gradually coarsen and dissolve into the matrix as the austenitizing temperatures increase. The M23C6 precipitates dissolve completely at 1100 °C, while the MX precipitates dissolve completely at 1200 °C. The evolution of two types of precipitate has a significant effect on the size of austenite. Based on the Zener pinning model, the effect of precipitate evolution on austenite grain size is quantified. It was found that the coarsening and dissolution of M23C6 and MX precipitates leads to a decrease in pinning pressure on grain boundaries, facilitating the rapid growth of austenite grains. The austenite phase fraction is also affected by the coarsening and dissolution of precipitates. PMID:28862680

Synthesis of ZnO nanosphere for picomolar level detection of bovine serum albumin.

PubMed

Sasmal, Milan; Maiti, Tapas Kumar; Bhattacharyya, Tarun Kanti

2015-01-01

In this paper, we demonstrate an electrical detection technique based on solution processed zinc oxide nanosphere for ultra-low level detection of bovine serum albumin (BSA). Our sensor device works on the basis of the variation of conductance of the ZnO nanosphere with different concentration of BSA. The morphological and structural characterizations of ZnO nanosphere were carried out by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction (XRD). Circular dichroism (CD) spectroscopy was performed to investigate the chemical interaction between the BSA and zinc oxide nanosphere. Optical detection was performed using absorbance and Fourier transform infrared spectroscopy (FTIR) studies. Our device exhibits sensitivity 0.126 nA/pM, lower limit of detection (LOD) 10 pM and the fast response time around 5 s, confirming the highest sensitivity for BSA detection achieved so far. Sensing mechanism is governed on the basis of the charge transfer phenomenon between BSA and ZnO. All measurements were carried out at 1 V bias for low power operation.

High Order in a Self-Assembled Iridium(III) Complex Gelator Towards Nanostructured IrO2 Thin Films.

PubMed

Scarpelli, Francesca; Ionescu, Andreea; Aiello, Iolinda; La Deda, Massimo; Crispini, Alessandra; Ghedini, Mauro; Brunelli, Elvira; Sesti, Settimio; Godbert, Nicolas

2017-10-18

The preparation and characterization of a new metallogelator based on the Ir III discrete cyclometalated complex [(ppy) 2 Ir(bpy)](CH 3 CH 2 OCH 2 CO 2 ) are reported, where H(ppy) is 2-phenylpiridine and bpy is 2,2'-bipyridine, which is used as an ancillary ligand. The compound is able to self-assemble in water in a range of concentrations between 3 % and 6 % w/w, creating a luminescent ordered supramolecular gel. The gel and xerogel architectures were investigated through polarized optical microscopy (POM), SEM and TEM microscopies coupled with powder X-ray diffraction. The gel supramolecular organization is characterized by columnar tetragonal strands, already present at high dilution conditions, of cations surrounded by counteranions. These strands, in turn, are self-assembled in an oblique columnar cell upon gelification. The xerogel thin films obtained upon complete dehydration maintained the gel supramolecular order and can be used as a precursor for the preparation of nanostructured IrO 2 thin films. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

TiO2/SiO2 porous composite thin films: Role of TiO2 areal loading and modification with gold nanospheres on the photocatalytic activity

NASA Astrophysics Data System (ADS)

Levchuk, Irina; Sillanpää, Mika; Guillard, Chantal; Gregori, Damia; Chateau, Denis; Parola, Stephane

2016-10-01

The aim of the work was to study photocatalytic activity of composite TiO2/Au/SiO2 thin films. Coatings were prepared using sol-gel technique. Physicochemical parameters of coatings were characterized using UV-vis spectrometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectrometry (XPS), inductively coupled plasma optical emission spectroscopy (ICP-OES), ellipsometry, tactile measurements, goniometry and diffuse reflectance measurements. The photocatalytic activity of the films was tested in batch mode using aqueous solution of formic acid. Changes of formic acid concentration were determined by means of high pressure liquid chromatography (HPLC). Increase of initial degradation rate of formic acid was detected for TiO2/Au/SiO2 films with gold nanoparticle's load 0.5 wt.% and 1.25 wt.%. However, deeper insights using more detailed characterization of these coatings demonstrated that the improvement of the photocatalytic activity is more probably attributed to an increase in the areal loading of TiO2.

Strain softening during tension in cold drawn Cu–Ag alloys

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

Chang, L.L., E-mail: lilichang@sdu.edu.cn; Wen, S.; Li, S.L.

2015-10-15

Experiments were conducted on Cu–0.1wt.%Ag alloys to evaluate the influence of producing procedures and annealing conditions on microstructure evolution and mechanical properties of Cu–Ag alloys. Optical microscopy (OM), electron back-scattered diffraction (EBSD), X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used for microstructural evaluation and mechanical properties were characterized by tensile tests. The results indicated that hot-extruded Cu–Ag alloys had a typical dynamic recrystallized microstructure with equiaxed grains. Cold drawing at room temperature leaded to partial recrystallized microstructure with a mixture of coarse and fine grains. The dominate {001}<100 > cubic texture formed during hot extrusion was changed tomore » be {112}<111 > copper texture by cold drawing. Strain softening occurred during room temperature tension of cold drawn Cu–Ag alloys with an average grain size of 13–19.7 μm. - Highlights: • Strain softening occurred during tension of Cu–Ag alloys with coarse grain size. • Work hardening was observed in hot-extruded and annealed Cu–0.1wt.%Ag alloys. • Strain softening was ascribed to dynamic recovery and dynamic recrystallization.« less

Synthesis of poly acrylic acid modified silver nanoparticles and their antimicrobial activities.

PubMed

Ni, Zhihui; Wang, Zhihua; Sun, Lei; Li, Binjie; Zhao, Yanbao

2014-08-01

Poly acrylic acid modified silver (Ag/PAA) nanoparticles (NPs) have been successfully synthesized in the aqueous solution by using tannic acid as a reductant. The structure, morphology and composition of Ag/PAA NPs were characterized by various techniques such as X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible absorption spectroscopy (UV-vis) and thermogravimetry analysis (TGA). The results show that PAA/Ag NPs have a quasi-ball shape with an average diameter of 10 nm and exhibit well crystalline, and the reaction conditions have some effect on products morphology and size distribution. In addition, the as-synthesized Ag/PAA NPs antimicrobial activities against Escherichia coli (E. coli), Pseudomonas aeruginosa (P. aeruginosa) and Staphylococcus aureus (S. aureus) were evaluated by the methods of broth dilution, cup diffusion, optical density (OD600) and electron microscopy observation. The as-synthesized Ag/PAA NPs exhibit excellent antibacterial activity. The antimicrobial mechanism may be attributed to the damaging of bacterial cell membrane and causing leakage of cytoplasm. Copyright © 2014 Elsevier B.V. All rights reserved.

Mechanisms of decoherence in electron microscopy.

PubMed

Howie, A

2011-06-01

The understanding and where possible the minimisation of decoherence mechanisms in electron microscopy were first studied in plasmon loss, diffraction contrast images but are of even more acute relevance in high resolution TEM phase contrast imaging and electron holography. With the development of phase retrieval techniques they merit further attention particularly when their effect cannot be eliminated by currently available energy filters. The roles of electronic excitation, thermal diffuse scattering, transition radiation and bremsstrahlung are examined here not only in the specimen but also in the electron optical column. Terahertz-range aloof beam electronic excitation appears to account satisfactorily for recent observations of decoherence in electron holography. An apparent low frequency divergence can emerge for the calculated classical bremsstrahlung event probability but can be ignored for photon wavelengths exceeding the required coherence distance or path lengths in the equipment. Most bremsstrahlung event probabilities are negligibly important except possibly in large-angle bending magnets or mandolin systems. A more reliable procedure for subtracting thermal diffuse scattering from diffraction pattern intensities is proposed. Copyright © 2010 Elsevier B.V. All rights reserved.

Scalable high-mobility MoS2 thin films fabricated by an atmospheric pressure chemical vapor deposition process at ambient temperature

NASA Astrophysics Data System (ADS)

Huang, Chung-Che; Al-Saab, Feras; Wang, Yudong; Ou, Jun-Yu; Walker, John C.; Wang, Shuncai; Gholipour, Behrad; Simpson, Robert E.; Hewak, Daniel W.

2014-10-01

Nano-scale MoS2 thin films are successfully deposited on a variety of substrates by atmospheric pressure chemical vapor deposition (APCVD) at ambient temperature, followed by a two-step annealing process. These annealed MoS2 thin films are characterized with scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), micro-Raman, X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-VIS-NIR spectrometry, photoluminescence (PL) and Hall Effect measurement. Key optical and electronic properties of APCVD grown MoS2 thin films are determined. This APCVD process is scalable and can be easily incorporated with conventional lithography as the deposition is taking place at room temperature. We also find that the substrate material plays a significant role in the crystalline structure formation during the annealing process and single crystalline MoS2 thin films can be achieved by using both c-plane ZnO and c-plane sapphire substrates. These APCVD grown nano-scale MoS2 thin films show great promise for nanoelectronic and optoelectronic applications.

Synthesis of mesoporous Mn/TiO2 nanocomposites and investigating the photocatalytic properties in aqueous systems.

PubMed

Oseghe, Ekemena Oghenovoh; Ndungu, Patrick Gathura; Jonnalagadda, Sreekanth Babu

2015-01-01

Mesoporous 20 wt% Mn/TiO2 nanocomposites were synthesized adopting modified sol-gel method at different pH (pH = 2, 7 and 11) conditions and calcined at 400 °C. Based on the characteristics of the 20 wt% Mn/TiO2 nanocomposites synthesized at pH 11, same procedure was adopted for the synthesis of different wt% Mn/TiO2. The nanocomposite samples and their surface properties were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), mapping, inductively coupled plasma optical emission spectrometry (ICP-OES), Fourier transform infrared (FTIR), and fluorescence spectrometry. The nanocomposites existed in the anatase phase of TiO2 with no peak assigned to Mn on the diffractogram. The photocatalytic activities of the materials were evaluated by monitoring degradation of a model dye (methylene blue (MB)) in presence of visible light and ozone. The nanocomposite synthesized under neutral condition (pH = 7) exhibited the best photocatalytic activity resulting from its relatively smaller crystal size (5.98 nm) and larger pore volume (0.30 cm(3)/g). One percentage of weight Mn/TiO2 showed 100% decolouration of MB in the presence of O3 after 100 min.

Using Graphene Liquid Cell Transmission Electron Microscopy to Study in Situ Nanocrystal Etching.

PubMed

Hauwiller, Matthew R; Ondry, Justin C; Alivisatos, A Paul

2018-05-17

Graphene liquid cell electron microscopy provides the ability to observe nanoscale chemical transformations and dynamics as the reactions are occurring in liquid environments. This manuscript describes the process for making graphene liquid cells through the example of graphene liquid cell transmission electron microscopy (TEM) experiments of gold nanocrystal etching. The protocol for making graphene liquid cells involves coating gold, holey-carbon TEM grids with chemical vapor deposition graphene and then using those graphene-coated grids to encapsulate liquid between two graphene surfaces. These pockets of liquid, with the nanomaterial of interest, are imaged in the electron microscope to see the dynamics of the nanoscale process, in this case the oxidative etching of gold nanorods. By controlling the electron beam dose rate, which modulates the etching species in the liquid cell, the underlying mechanisms of how atoms are removed from nanocrystals to form different facets and shapes can be better understood. Graphene liquid cell TEM has the advantages of high spatial resolution, compatibility with traditional TEM holders, and low start-up costs for research groups. Current limitations include delicate sample preparation, lack of flow capability, and reliance on electron beam-generated radiolysis products to induce reactions. With further development and control, graphene liquid cell may become a ubiquitous technique in nanomaterials and biology, and is already being used to study mechanisms governing growth, etching, and self-assembly processes of nanomaterials in liquid on the single particle level.

Atom-counting in High Resolution Electron Microscopy:TEM or STEM - That's the question.

PubMed

Gonnissen, J; De Backer, A; den Dekker, A J; Sijbers, J; Van Aert, S

2017-03-01

In this work, a recently developed quantitative approach based on the principles of detection theory is used in order to determine the possibilities and limitations of High Resolution Scanning Transmission Electron Microscopy (HR STEM) and HR TEM for atom-counting. So far, HR STEM has been shown to be an appropriate imaging mode to count the number of atoms in a projected atomic column. Recently, it has been demonstrated that HR TEM, when using negative spherical aberration imaging, is suitable for atom-counting as well. The capabilities of both imaging techniques are investigated and compared using the probability of error as a criterion. It is shown that for the same incoming electron dose, HR STEM outperforms HR TEM under common practice standards, i.e. when the decision is based on the probability function of the peak intensities in HR TEM and of the scattering cross-sections in HR STEM. If the atom-counting decision is based on the joint probability function of the image pixel values, the dependence of all image pixel intensities as a function of thickness should be known accurately. Under this assumption, the probability of error may decrease significantly for atom-counting in HR TEM and may, in theory, become lower as compared to HR STEM under the predicted optimal experimental settings. However, the commonly used standard for atom-counting in HR STEM leads to a high performance and has been shown to work in practice. Copyright © 2017 Elsevier B.V. All rights reserved.

Novel method for measurement of transistor gate length using energy-filtered transmission electron microscopy

NASA Astrophysics Data System (ADS)

Lee, Sungho; Kim, Tae-Hoon; Kang, Jonghyuk; Yang, Cheol-Woong

2016-12-01

As the feature size of devices continues to decrease, transmission electron microscopy (TEM) is becoming indispensable for measuring the critical dimension (CD) of structures. Semiconductors consist primarily of silicon-based materials such as silicon, silicon dioxide, and silicon nitride, and the electrons transmitted through a plan-view TEM sample provide diverse information about various overlapped silicon-based materials. This information is exceedingly complex, which makes it difficult to clarify the boundary to be measured. Therefore, we propose a simple measurement method using energy-filtered TEM (EF-TEM). A precise and effective measurement condition was obtained by determining the maximum value of the integrated area ratio of the electron energy loss spectrum at the boundary to be measured. This method employs an adjustable slit allowing only electrons with a certain energy range to pass. EF-TEM imaging showed a sharp transition at the boundary when the energy-filter’s passband centre was set at 90 eV, with a slit width of 40 eV. This was the optimum condition for the CD measurement of silicon-based materials involving silicon nitride. Electron energy loss spectroscopy (EELS) and EF-TEM images were used to verify this method, which makes it possible to measure the transistor gate length in a dynamic random access memory manufactured using 35 nm process technology. This method can be adapted to measure the CD of other non-silicon-based materials using the EELS area ratio of the boundary materials.

In Situ Electron Microscopy of Lactomicroselenium Particles in Probiotic Bacteria.

PubMed

Nagy, Gabor; Pinczes, Gyula; Pinter, Gabor; Pocsi, Istvan; Prokisch, Jozsef; Banfalvi, Gaspar

2016-06-30

Electron microscopy was used to test whether or not (a) in statu nascendi synthesized, and in situ measured, nanoparticle size does not differ significantly from the size of nanoparticles after their purification; and (b) the generation of selenium is detrimental to the bacterial strains that produce them. Elemental nano-sized selenium produced by probiotic latic acid bacteria was used as a lactomicroselenium (lactomicroSel) inhibitor of cell growth in the presence of lactomicroSel, and was followed by time-lapse microscopy. The size of lactomicroSel produced by probiotic bacteria was measured in situ and after isolation and purification. For these measurements the TESLA BS 540 transmission electron microscope was converted from analog (aTEM) to digital processing (dTEM), and further to remote-access internet electron microscopy (iTEM). Lactobacillus acidophilus produced fewer, but larger, lactomicroSel nanoparticles (200-350 nm) than Lactobacillus casei (L. casei), which generated many, smaller lactomicroSel particles (85-200 nm) and grains as a cloudy, less electrodense material. Streptococcus thermophilus cells generated selenoparticles (60-280 nm) in a suicidic manner. The size determined in situ in lactic acid bacteria was significantly lower than those measured by scanning electron microscopy after the isolation of lactomicroSel particles obtained from lactobacilli (100-500 nm), but higher relative to those isolated from Streptococcus thermopilus (50-100 nm). These differences indicate that smaller lactomicroSel particles could be more toxic to the producing bacteria themselves and discrepancies in size could have implications with respect to the applications of selenium nanoparticles as prebiotics.

Symposium LL: Nanowires--Synthesis Properties Assembly and Application

DTIC Science & Technology

2010-09-10

dedicated hard x - ray microscopy beamline is operated in partnership with the Advanced Photon Source to provide fluorescence, diffraction, and...characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X - ray diffraction (XRD) measurements, proving it to be...Investigation of Preferred Growth Direction of GaN Nanorods by Synchrotron X - ray Reciprocal Space Mapping. Yuri Sohn1, Sanghwa Lee1, Chinkyo Kim1 and Dong

Fibre-optic nonlinear optical microscopy and endoscopy.

PubMed

Fu, L; Gu, M

2007-06-01

Nonlinear optical microscopy has been an indispensable laboratory tool of high-resolution imaging in thick tissue and live animals. Rapid developments of fibre-optic components in terms of growing functionality and decreasing size provide enormous opportunities for innovations in nonlinear optical microscopy. Fibre-based nonlinear optical endoscopy is the sole instrumentation to permit the cellular imaging within hollow tissue tracts or solid organs that are inaccessible to a conventional optical microscope. This article reviews the current development of fibre-optic nonlinear optical microscopy and endoscopy, which includes crucial technologies for miniaturized nonlinear optical microscopy and their embodiments of endoscopic systems. A particular attention is given to several classes of photonic crystal fibres that have been applied to nonlinear optical microscopy due to their unique properties for ultrashort pulse delivery and signal collection. Furthermore, fibre-optic nonlinear optical imaging systems can be classified into portable microscopes suitable for imaging behaving animals, rigid endoscopes that allow for deep tissue imaging with minimally invasive manners, and flexible endoscopes enabling imaging of internal organs. Fibre-optic nonlinear optical endoscopy is coming of age and a paradigm shift leading to optical microscope tools for early cancer detection and minimally invasive surgery.

Bi-layered collagen nano-structured membrane prototype collagen matrix 10826® for soft tissue regeneration in rabbits: an in vivo ultra-structural study of the early healing phase.

PubMed

De Santis, D; Menchini Fabris, G B; Lotti, J; Palumbo, C; Ferretti, M; Castellani, R; Lotti, T; Zanotti, G; Gelpi, F; Covani, C; Nocini, P F

Collagen Matrix (CM) 10826 is a nanostructured bi-layered collagen membrane obtained from type I and III porcine collagen, which in vitro has shown to have the potential to be a substitute and/or stimulant for soft oral tissue regeneration. The objective of this study was to evaluate the in vivo potential and safety of this membrane for soft tissue regeneration in the early stage of wound healing. Two soft tissue wounds (test and control) were created on the back skin of 5 rabbits (female New Zealand White Rabbits specific pathogen free). All wounds were protected by a special poly-tetra-fluoro-ethylene (PTFE) healing camera. On each rabbit on the test side CM-10826 was used, while on the control side conventional treatment (an autologous pedicle graft) was performed. The healing process was observed clinically after 2 and 6 days, and Magnetic Resonance Imaging (MRI) was performed after this period. After 7 days, animals were sacrificed and specimens were analyzed with light optic microscopy (LM), Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). These in vivo trials on rabbits confirmed that CM-10826 is well tolerated, without signs of histological inflammatory reaction and proved to be able to accelerate the spontaneous repair of the skin defect taken as the control. The light-optic and ultra-microscopy of serial biopsies showed that the new matrix is biocompatible and is able to function as a scaffold inducing soft tissue regeneration. In conclusion this study demonstrates that CM-10826 promote early soft tissue regeneration and suggests it is a potential constituent for human autologous keratinocytes seeded derma bioequivalent. It protects the wound from injuries and bacterial contamination accelerating healing process. As a clinical relevance, we consider that the quality of life of patients will be improved avoiding the use of major autologous grafts, reducing the hospitalization time and morbidity.

Hollow Au/Ag nanostars displaying broad plasmonic resonance and high surface-enhanced Raman sensitivity

NASA Astrophysics Data System (ADS)

Garcia-Leis, Adianez; Torreggiani, Armida; Garcia-Ramos, Jose Vicente; Sanchez-Cortes, Santiago

2015-08-01

Bimetallic Au/Ag hollow nanostar (HNS) nanoparticles with different morphologies were prepared in this work. These nanoplatforms were obtained by changing the experimental conditions (concentration of silver and chemical reductors, hydroxylamine and citrate) and by using Ag nanostars as template nanoparticles (NPs) through galvanic replacement. The goal of this research was to create bimetallic Au/Ag star-shaped nanoparticles with advanced properties displaying a broader plasmonic resonance, a cleaner exposed surface, and a high concentration of electromagnetic hot spots on the surface provided by the special morphology of nanostars. The size, shape, and composition of Ag as well as their optical properties were studied by extinction spectroscopy, hyperspectral dark field microscopy, transmission and scanning electron microscopy (TEM and SEM), and energy dispersive X-ray spectroscopy (EDX). Finally, the surface-enhanced Raman scattering (SERS) activity of these HNS was investigated by using thioflavin T, a biomarker of the β-amyloid fibril formation, responsible for Alzheimer's disease. Lucigenin, a molecule displaying different SERS activities on Au and Ag, was also used to explore the presence of these metals on the NP surface. Thus, a relationship between the morphology, plasmon resonance and SERS activity of these new NPs was made.Bimetallic Au/Ag hollow nanostar (HNS) nanoparticles with different morphologies were prepared in this work. These nanoplatforms were obtained by changing the experimental conditions (concentration of silver and chemical reductors, hydroxylamine and citrate) and by using Ag nanostars as template nanoparticles (NPs) through galvanic replacement. The goal of this research was to create bimetallic Au/Ag star-shaped nanoparticles with advanced properties displaying a broader plasmonic resonance, a cleaner exposed surface, and a high concentration of electromagnetic hot spots on the surface provided by the special morphology of nanostars. The size, shape, and composition of Ag as well as their optical properties were studied by extinction spectroscopy, hyperspectral dark field microscopy, transmission and scanning electron microscopy (TEM and SEM), and energy dispersive X-ray spectroscopy (EDX). Finally, the surface-enhanced Raman scattering (SERS) activity of these HNS was investigated by using thioflavin T, a biomarker of the β-amyloid fibril formation, responsible for Alzheimer's disease. Lucigenin, a molecule displaying different SERS activities on Au and Ag, was also used to explore the presence of these metals on the NP surface. Thus, a relationship between the morphology, plasmon resonance and SERS activity of these new NPs was made. Electronic supplementary information (ESI) available: The SERS spectra of ThT on A-E samples are provided at two different excitations: 532 and 785 nm (Fig. S1). See DOI: 10.1039/c5nr02819a

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

PubMed

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

2018-05-06

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

Influence of perfluorocarbons on Carbamazepine and Benzodiazepine for a neuro-lung protective strategy.

PubMed

Natchimuthu, V; Thomas, Sabu; Ramalingam, Murugan; Ravi, S

2017-09-01

Lennox-Gastaut syndrome (LGS) is commonly characterized by a triad of features including multiple seizure types, intellectual disability or regression. LGS type of seizures is epilepsy which is due to abnormal vibrations occurring in seizures. During the time of such abnormal vibrations, both the seizures and the lungs suffer a lack in oxygen content to a considerable extent. This results in prolonged vibrations and loses of nervous control. As a neuro-lung protective strategy, a novel attempt has been made to enrich both seizures and lungs with oxygen content through the support of Perfluorodecalin (an excellent oxygen carrier) C 10 F 18 (PFD) and Perfluorohexane C 6 F 14 (PFH) along with an enhancement in the antiepileptic activity by the two chosen antiepileptic drugs (AEDs) Carbamazepine (CBZ) and Benzodiazepine (BDZ). Perfluorodecalin C 10 F 18 (PFD) and Perfluorohexane C 6 F 14 (PFH) emulsions were prepared by sonication process with combination of nonionic emulsifier, Lecithin (l-α-phosphatidylcholine) as a surfactant in Aqueous phase medium. These emulsions were mixed with Carbamazepine (CBZ) and Benzodiazepine (BDZ) drugs maintained at a temperature of about -20°C to 20°C and were set to slow evaporation process. The products are subjected to Optical microscope, Transmission electron microscopy (TEM) and Scanning Electron Microscope (SEM) - Energy dispersive X-ray Spectroscopy (EDS). Study reveals the co-existence of fluorine and drug ensuring the oxygen uptake by the drug. Morphology of TEM, Optical microscopic images and the particle diameter estimated through Image_J confirms this analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

Optical characterization of CdS nanoparticles embedded into the comb-type amphiphilic graft copolymer

NASA Astrophysics Data System (ADS)

Kalaycı, Özlem A.; Duygulu, Özgür; Hazer, Baki

2013-01-01

This study refers to the synthesis and characterization of a novel organic/inorganic hybrid nanocomposite material containing cadmium sulfide (CdS) nanoparticles. For this purpose, a series of polypropylene (PP)-g-polyethylene glycol (PEG), PP-g-PEG comb-type amphiphilic graft copolymers were synthesized. PEGs with Mn = 400, 2000, 3350, and 8000 Da were used and the graft copolymers obtained were coded as PPEG400, PPEG2000, PPEG3350, and PPEG8000. CdS nanoparticles were formed in tetrahydrofuran solution of PP-g-PEG amphiphilic comb-type copolymer by the reaction between aqueous solutions of Na2S and Cd(CH3COO)2 simultaneously. Micelle formation of PPEG2000 comb-type amphiphilic graft copolymer in both solvent/non-solvent (petroleum ether-THF) by transmission electron microscopy (TEM). The optical characteristics, size morphology, phase analysis, and dispersion of CdS nanoparticles embedded in PPEG400, PPEG2000, PPEG3350, and PPEG8000 comb-type amphiphilic graft copolymer micelles were determined by high resolution TEM (HRTEM), energy dispersive spectroscopy, UV-vis spectroscopy, and fluorescence emission spectroscopy techniques. The aggregate size of PPEG2000-CdS is between 10 and 50 nm; however, in the case of PPEG400-CdS, PPEG3350-CdS, and PPEG8000-CdS samples, it is up to approximately 100 nm. The size of CdS quantum dots in the aggregates for PPEG2000 and PPEG8000 samples was observed as 5 nm by HRTEM analysis, and this result was also supported by UV-vis absorbance spectra and fluorescence emission spectra.

Electron Microscopy Characterization of Vanadium Dioxide Thin Films and Nanoparticles

NASA Astrophysics Data System (ADS)

Rivera, Felipe

Vanadium dioxide (VO_2) is a material of particular interest due to its exhibited metal to insulator phase transition at 68°C that is accompanied by an abrupt and significant change in its electronic and optical properties. Since this material can exhibit a reversible drop in resistivity of up to five orders of magnitude and a reversible drop in infrared optical transmission of up to 80%, this material holds promise in several technological applications. Solid phase crystallization of VO_2 thin films was obtained by a post-deposition annealing process of a VO_{x,x approx 2} amorphous film sputtered on an amorphous silicon dioxide (SiO_2) layer. Scanning electron microscopy (SEM) and electron-backscattered diffraction (EBSD) were utilized to study the morphology of the solid phase crystallization that resulted from this post-deposition annealing process. The annealing parameters ranged in temperature from 300°C up to 1000°C and in time from 5 minutes up to 12 hours. Depending on the annealing parameters, EBSD showed that this process yielded polycrystalline vanadium dioxide thin films, semi-continuous thin films, and films of isolated single-crystal particles. In addition to these films on SiO_2, other VO_2 thin films were deposited onto a-, c-, and r-cuts of sapphire and on TiO_2(001) heated single-crystal substrates by pulsed-laser deposition (PLD). The temperature of the substrates was kept at ˜500°C during deposition. EBSD maps and orientation imaging microscopy were used to study the epitaxy and orientation of the VO_2 grains deposited on the single crystal substrates, as well as on the amorphous SiO_2 layer. The EBSD/OIM results showed that: 1) For all the sapphire substrates analyzed, there is a predominant family of crystallographic relationships wherein the rutile VO_2{001} planes tend to lie parallel to the sapphire's {10-10} and the rutile VO_2{100} planes lie parallel to the sapphire's {1-210} and {0001}. Furthermore, while this family of relationships accounts for the majority of the VO_2 grains observed, due to the sapphire substrate's geometry there were variations within these rules that changed the orientation of VO_2 grains with respect to the substrate's normal direction. 2) For the TiO_2, a substrate with a lower lattice mismatch, we observe the expected relationship where the rutile VO_2 [100], [110], and [001] crystal directions lie parallel to the TiO_2 substrate's [100], [110], and [001] crystal directions respectively. 3) For the amorphous SiO_2 layer, all VO_2 crystals that were measurable (those that grew to the thickness of the deposited film) had a preferred orientation with the the rutile VO_2[001] crystal direction tending to lie parallel to the plane of the specimen. The use of transmission electron microscopy (TEM) is presented as a tool for further characterization studies of this material and its applications. In this work TEM diffraction patterns taken from cross-sections of particles of the a- and r-cut sapphire substrates not only solidified the predominant family mentioned, but also helped lift the ambiguity present in the rutile VO_2{100} axes. Finally, a focused-ion beam technique for preparation of cross-sectional TEM samples of metallic thin films deposited on polymer substrates is demonstrated.

Theory of the spatial resolution of (scanning) transmission electron microscopy in liquid water or ice layers.

PubMed

de Jonge, Niels

2018-04-01

The sample dependent spatial resolution was calculated for transmission electron microscopy (TEM) and scanning TEM (STEM) of objects (e.g., nanoparticles, proteins) embedded in a layer of liquid water or amorphous ice. The theoretical model includes elastic- and inelastic scattering, beam broadening, and chromatic aberration. Different contrast mechanisms were evaluated as function of the electron dose, the detection angle, and the sample configuration. It was found that the spatial resolution scales with the electron dose to the -1/4th power. Gold- and carbon nanoparticles were examined in the middle of water layers ranging from 0.01--10 µm thickness representing relevant classes of experiments in both materials science and biology. The optimal microscope settings differ between experimental configurations. STEM performs the best for gold nanoparticles for all layer thicknesses, while carbon is best imaged with phase-contrast TEM for thin layers but bright field STEM is preferred for thicker layers. The resolution was also calculated for a water layer enclosed between thin membranes. The influence of chromatic aberration correction for TEM was examined as well. The theory is broadly applicable to other types of materials and sample configurations. Copyright © 2018 Elsevier B.V. All rights reserved.

Nanoparticle Immobilization for Controllable Experiments in Liquid-Cell Transmission Electron Microscopy.

PubMed

Robertson, Alex W; Zhu, Guomin; Mehdi, B Layla; Jacobs, Robert M J; De Yoreo, James; Browning, Nigel D

2018-06-22

We demonstrate that silanization can control the adhesion of nanostructures to the SiN windows compatible with liquid-cell transmission electron microscopy (LC-TEM). Formation of an (3-aminopropyl)triethoxysilane (APTES) self-assembled monolayer on a SiN window, producing a surface decorated with amino groups, permits strong adhesion of Au nanoparticles to the window. Many of these nanoparticles remain static, undergoing minimal translation or rotation during LC-TEM up to high electron beam current densities due to the strong interaction between the APTES amino group and Au. We then use this technique to perform a direct comparative LC-TEM study on the behavior of ligand and nonligand-coated Au nanoparticles in a Au growth solution. While the ligand coated nanoparticles remain consistent even under high electron beam current densities, the naked nanoparticles acted as sites for secondary Au nucleation. These nucleated particles decorated the parent nanoparticle surface, forming consecutive monolayer assemblies of ∼2 nm diameter nanoparticles, which sinter into the parent particle when the electron beam was shut off. This method for facile immobilization of nanostructures for LC-TEM study will permit more sophisticated and controlled in situ experiments into the properties of solid-liquid interfaces in the future.

Operando observations of solid-state electrochemical reactions in Li-ion batteries by spatially resolved TEM EELS and electron holography.

PubMed

Yamamoto, Kazuo; Iriyama, Yasutoshi; Hirayama, Tsukasa

2017-02-08

All-solid-state Li-ion batteries having incombustible solid electrolytes are promising energy storage devices because they have significant advantages in terms of safety, lifetime and energy density. Electrochemical reactions, namely, Li-ion insertion/extraction reactions, commonly occur around the nanometer-scale interfaces between the electrodes and solid electrolytes. Thus, transmission electron microscopy (TEM) is an appropriate technique to directly observe such reactions, providing important information for understanding the fundamental solid-state electrochemistry and improving battery performance. In this review, we introduce two types of TEM techniques for operando observations of battery reactions, spatially resolved electron energy-loss spectroscopy in a TEM mode for direct detection of the Li concentration profiles and electron holography for observing the electric potential changes due to Li-ion insertion/extraction reactions. We visually show how Li-ion insertion/extractions affect the crystal structures, electronic structures, and local electric potential during the charge-discharge processes in these batteries. © The Author 2016. 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.

Transmission Electron Microscopy of Cometary Residues from Micron-Sized Craters in the Stardust Al-Foils

NASA Technical Reports Server (NTRS)

Leroux, Hugues; Stroud, Rhonda M.; Dai, Zu Rong; Graham, Giles A.; Troadec, David; Bradley, John P.; Teslich, Nick; Borg, Janet; Kearsley, Anton T.; Horz, Friedrich

2008-01-01

We report Transmission Electron Microscopy (TEM) investigations of micro-craters that originated from hypervelocity impacts of comet 81P/Wild 2 dust particles on the aluminium foil of the Stardust collector. The craters were selected by Scanning Electron Microscopy (SEM) and then prepared by Focused Ion Beam (FIB) milling techniques in order to provide electron transparent cross-sections for TEM studies. The crater residues contain both amorphous and crystalline materials in varying proportions and compositions. The amorphous component is interpreted as resulting from shock melting during the impact and the crystalline phases as relict minerals. The latter show evidence for shock metamorphism. Based on the residue morphology and the compositional variation, the impacting particles are inferred to have been dominated by mixtures of submicron olivine, pyroxene and Fe-sulfide grains, in agreement with prior results of relatively coarse-grained mineral assemblages in the aerogel collector.

Towards 3D crystal orientation reconstruction using automated crystal orientation mapping transmission electron microscopy (ACOM-TEM).

PubMed

Kobler, Aaron; Kübel, Christian

2018-01-01

To relate the internal structure of a volume (crystallite and phase boundaries) to properties (electrical, magnetic, mechanical, thermal), a full 3D reconstruction in combination with in situ testing is desirable. In situ testing allows the crystallographic changes in a material to be followed by tracking and comparing the individual crystals and phases. Standard transmission electron microscopy (TEM) delivers a projection image through the 3D volume of an electron-transparent TEM sample lamella. Only with the help of a dedicated TEM tomography sample holder is an accurate 3D reconstruction of the TEM lamella currently possible. 2D crystal orientation mapping has become a standard method for crystal orientation and phase determination while 3D crystal orientation mapping have been reported only a few times. The combination of in situ testing with 3D crystal orientation mapping remains a challenge in terms of stability and accuracy. Here, we outline a method to 3D reconstruct the crystal orientation from a superimposed diffraction pattern of overlapping crystals without sample tilt. Avoiding the typically required tilt series for 3D reconstruction enables not only faster in situ tests but also opens the possibility for more stable and more accurate in situ mechanical testing. The approach laid out here should serve as an inspiration for further research and does not make a claim to be complete.

[Architectural ultrastructure of the human urinary transitional epithelium].

PubMed

Takayama, H; Konishi, T

1984-07-01

Human urinary bladder mucosa, confirmed to be normal by cystoscopic, histologic and bacteriologic examination, were obtained from four patients at prostatectomy and from two patients at an anti-VUR procedure. The luminal surface and the three dimensional architecture of the bladder mucosa were observed by scanning electron microscopy (SEM) after cryofracture of specimen and by transmission electron microscopy (TEM). The epithelium consists of superficial, intermediate and basal cells, and SEM and TEM showed that it was stratified. Intermediate cells reached the basal lamina by slender cytoplasmic processes but superficial cells were not directly in contact with the basal lamina. No pleomorphic or long microvilli were observed but short microvilli or granular protrusions were sparsely seen on the luminal surface of superficial cells. SEM of cryofractured surfaces revealed that cells from each cell layer were in contact with cellular junctions such as ridges, plicated projections and septum-like walls. Their junctions were more complicated with increasing depth of the cell layer. No pleomorphic or long microvilli were observed on any cell surface of the intermediate or basal cell layer. Under TEM, however, these junctional structures of ridges, plicated projections and septal walls appeared to be microvilli under TEM. Microvilli-like structures on TEM, therefore, have to be carefully distinguished from real microvilli. Careful observation is required when the presence of cells covered with microvilli is described as a sign of malignancy.

Multi-class segmentation of neuronal electron microscopy images using deep learning

NASA Astrophysics Data System (ADS)

Khobragade, Nivedita; Agarwal, Chirag

2018-03-01

Study of connectivity of neural circuits is an essential step towards a better understanding of functioning of the nervous system. With the recent improvement in imaging techniques, high-resolution and high-volume images are being generated requiring automated segmentation techniques. We present a pixel-wise classification method based on Bayesian SegNet architecture. We carried out multi-class segmentation on serial section Transmission Electron Microscopy (ssTEM) images of Drosophila third instar larva ventral nerve cord, labeling the four classes of neuron membranes, neuron intracellular space, mitochondria and glia / extracellular space. Bayesian SegNet was trained using 256 ssTEM images of 256 x 256 pixels and tested on 64 different ssTEM images of the same size, from the same serial stack. Due to high class imbalance, we used a class-balanced version of Bayesian SegNet by re-weighting each class based on their relative frequency. We achieved an overall accuracy of 93% and a mean class accuracy of 88% for pixel-wise segmentation using this encoder-decoder approach. On evaluating the segmentation results using similarity metrics like SSIM and Dice Coefficient, we obtained scores of 0.994 and 0.886 respectively. Additionally, we used the network trained using the 256 ssTEM images of Drosophila third instar larva for multi-class labeling of ISBI 2012 challenge ssTEM dataset.

Cross-sectional TEM specimen preparation for W/B{sub 4}C multilayer sample using FIB

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

Mondal, Puspen, E-mail: puspen@rrcat.gov.in; Pradhan, P. C.; Tiwari, Pragya

2016-05-23

A recent emergence of a cross-beam scanning electron microscopy (SEM)/focused-ion-beam (FIB) system have given choice to fabricate cross-sectional transmission electron microscopy (TEM) specimen of thin film multilayer sample. A 300 layer pair thin film multilayer sample of W/B{sub 4}C was used to demonstrate the specimen lift-out technique in very short time as compared to conventional cross-sectional sample preparation technique. To get large area electron transparent sample, sample prepared by FIB is followed by Ar{sup +} ion polishing at 2 kV with grazing incident. The prepared cross-sectional sample was characterized by transmission electron microscope.

Electron Microscopy of Ebola Virus-Infected Cells.

PubMed

Noda, Takeshi

2017-01-01

Ebola virus (EBOV) replicates in host cells, where both viral and cellular components show morphological changes during the process of viral replication from entry to budding. These steps in the replication cycle can be studied using electron microscopy (EM), including transmission electron microscopy (TEM) and scanning electron microscopy (SEM), which is one of the most useful methods for visualizing EBOV particles and EBOV-infected cells at the ultrastructural level. This chapter describes conventional methods for EM sample preparation of cultured cells infected with EBOV.

Trapping two types of particles using a double-ring-shaped radially polarized beam

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

Zhang Yaoju; Ding Biaofeng; Suyama, Taikei

An optical-trap method based on the illumination of a double-ring-shaped radially polarized beam (R-TEM{sub 11}*) is proposed. The numerical results based on the vector diffraction theory show that a highly focused R-TEM{sub 11}* beam not only can produce a bright spot but also can form an optical cage in the focal region by changing the truncation parameter {beta}, defined as the ratio of the radius of the aperture to the waist of the beam. The radiation forces acting on Rayleigh particles are calculated by using the Rayleigh scattering theory. The bright spot generated by the R-TEM{sub 11}* beam with amore » {beta} value close to 2 can three-dimensionally trap a particle with a refractive index larger than that of the ambient. An optical cage or three-dimensional dark spot generated by the R-TEM{sub 11}* beam with a {beta} value close to 1.3 can three-dimensionally trap a particle with refractive index smaller than that of the ambient. Because the adjustment of the truncation parameter can be actualized by simply changing the radius of a circular aperture inserted in the front of the lens, only one optical-trap system in the present method can be used to three-dimensionally trap two types of particles with different refractive indices.« less

Synthesis, structural, optical and morphological characterization of hematite through the precipitation method: Effect of varying the nature of the base

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

2017-08-01

Iron oxide (α-Fe2O3) nanoparticles were synthesized using the precipitation synthesis method focusing only on (FeCl3, 6H2O), NaOH, KOH and NH4OH as raw materials. The impact of varying the nature of the base on the crystalline phase, size and morphology of α-Fe2O3 products was explored. XRD spectra revealed that samples crystallize in the rhombohedral (hexagonal) system at 800 °C.The Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) were used to detect the morphology of synthesized nanoparticles and specify their sizes. However, the Fourier Transform Infra-Red (FT-IR) spectroscopy has permitted the observation of vibration band Fe-O. Raman spectroscopy was used not only to prove that we have synthesized hematite but also to identify their phonon modes. The Thermo Gravimetric Analysis (TGA) findings allow the thermal cycle determination of samples whereas Differential Thermal Analysis (DTA) findings allow the phase transition temperature identification. Besides, the optical investigation revealed that samples have an optical gap of about 2.1 eV. Findings highlight that the nature of the agent precipitant plays a significant role in the morphology of the products and the formation of the crystalline phase. Hematite synthesis with the base NH4OH brought about much stronger, sharper and wider diffraction peaks of α-Fe2O3. The morphology of samples are spherical with a size of about 61 nm while the size of the nanoparticles of hematite which we have synthesized with NaOH and KOH is respectively of the order of 82 and 79 nm.

Biomolecule-assisted hydrothermal synthesis of silver bismuth sulfide with nanostructures

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

Kaowphong, Sulawan, E-mail: sulawank@gmail.com; Materials Science Research Center, Faculty of Science, Chiang Mai University, Chiang Mai 50200

2012-05-15

Silver bismuth sulfide (AgBiS{sub 2}) nanostructures were successfully prepared via a simple biomolecule-assisted hydrothermal synthesis at 200 Degree-Sign C for 12-72 h. Silver nitrate, bismuth nitrate and L-cysteine were used as starting materials. Here, the biomolecule, L-cysteine, was served as the sulfide source and a complexing agent. The products, characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM), were cubic AgBiS{sub 2} nanoparticles with a diameter range of about 20-75 nm. It was found that their crystallinity and particle size increased with increasing reaction time. The energy dispersive X-ray spectroscopy (EDX) and inductively coupledmore » plasma optical emission spectrophotometry (ICP-OES) analyses were used to confirm the stoichiometry of AgBiS{sub 2}. The optical band gap of the AgBiS{sub 2} nanoparticles, calculated from UV-vis spectra, was 3.0 eV which indicated a strong blue shift because of the quantum confinement effect. A possible formation mechanism of the AgBiS{sub 2} nanoparticles was also discussed. - Graphical abstract: The optical band gap of the as-prepared AgBiS{sub 2} nanoparticles displays a strong blue shift comparing to the 2.46 eV of bulk AgBiS{sub 2} caused by the quantum confinement effects. Highlights: Black-Right-Pointing-Pointer A simple biomolecule-assisted hydrothermal method is developed to prepare AgBiS{sub 2}. Black-Right-Pointing-Pointer L-Cysteine is served as the sulfide source and a complexing agent. Black-Right-Pointing-Pointer Increase in band gap of the AgBiS{sub 2} nanoparticles attributes to the quantum confinement effects.« less

A sustained release formulation of chitosan modified PLCL:poloxamer blend nanoparticles loaded with optical agent for animal imaging

NASA Astrophysics Data System (ADS)

Ranjan, Amalendu P.; Zeglam, Karim; Mukerjee, Anindita; Thamake, Sanjay; Vishwanatha, Jamboor K.

2011-07-01

The objective of this study was to develop optical imaging agent loaded biodegradable nanoparticles with indocynanine green (ICG) using chitosan modified poly(L-lactide-co-epsilon-caprolactone) (PLCL):poloxamer (Pluronic F68) blended polymer. Nanoparticles were formulated with an emulsification solvent diffusion technique using PLCL and poloxamer as blend-polymers. Polyvinyl alcohol (PVA) and chitosan were used as stabilizers. The particle size, shape and zeta potential of the formulated nanoparticles and the release kinetics of ICG from these nanoparticles were determined. Further, biodistribution of these nanoparticles was studied in mice at various time points until 24 h following intravenous administration, using a non-invasive imaging system. The average particle size of the nanoparticles was found to be 146 ± 3.7 to 260 ± 4.5 nm. The zeta potential progressively increased from - 41.6 to + 25.3 mV with increasing amounts of chitosan. Particle size and shape of the nanoparticles were studied using transmission electron microscopy (TEM) which revealed the particles to be smooth and spherical in shape. These nanoparticles were efficiently delivered to the cytoplasm of the cells, as observed in prostate and breast cancer cells using confocal laser scanning microscopy. In vitro release studies indicated sustained release of ICG from the nanoparticles over a period of seven days. Nanoparticle distribution results in mice showing improved uptake and accumulation with chitosan modified nanoparticles in various organs and slower clearance at different time points over a 24 h period as compared to unmodified nanoparticles. The successful formulation of such cationically modified nanoparticles for encapsulating optical agents may lead to a potential deep tissue imaging technique for tumor detection, diagnosis and therapy.

Deformation localization and dislocation channel dynamics in neutron-irradiated austenitic stainless steels

DOE PAGES

Gussev, Maxim N.; Field, Kevin G.; Busby, Jeremy T.

2015-02-24

We investigated dynamics of deformation localization and dislocation channel formation in situ in a neutron irradiated AISI 304 austenitic stainless steel and a model 304-based austenitic alloy by combining several analytical techniques including optic microscopy and laser confocal microscopy, scanning electron microscopy, electron backscatter diffraction and transmission electron microscopy. Channel formation was observed at 70% of the formal tensile yield stress for both alloys. It was shown that triple junction points do not always serve as a source of dislocation channels; at stress levels below the yield stress, channels often formed near the middle of the grain boundary. For amore » single grain, the role of elastic stiffness value (Young modulus) in the channel formation was analyzed; it was shown that in the irradiated 304 steels the initial channels appeared in soft grains with a high Schmid factor located near stiff grains with high elastic stiffness. Moreover, the spatial organization of channels in a single grain was analyzed; it was shown that secondary channels operating in the same slip plane as primary channels often appeared at the middle or at one third of the way between primary channels. The twinning nature of dislocation channels was analyzed for grains of different orientation using TEM. Finally, it was shown that in the AISI 304 steel, channels were twin-free in grains oriented close to [001] and [101] of standard unit triangle; [111]-grains and grains oriented close to Schmid factor maximum contained deformation twins.« less

Transmission electron microscopy, fluorescence microscopy, and confocal raman microscopic analysis of ultrastructural and compositional heterogeneity of Cornus alba L. wood cell wall.

PubMed

Ma, Jianfeng; Ji, Zhe; Zhou, Xia; Zhang, Zhiheng; Xu, Feng

2013-02-01

Transmission electron microscopy (TEM), fluorescence microscopy, and confocal Raman microscopy can be used to characterize ultrastructural and compositional heterogeneity of plant cell walls. In this study, TEM observations revealed the ultrastructural characterization of Cornus alba L. fiber, vessel, axial parenchyma, ray parenchyma, and pit membrane between cells, notably with the ray parenchyma consisting of two well-defined layers. Fluorescence microscopy evidenced that cell corner middle lamella was more lignified than adjacent compound middle lamella and secondary wall with variation in lignification level from cell to cell. In situ Raman images showed that the inhomogeneity in cell wall components (cellulose and lignin) among different cells and within morphologically distinct cell wall layers. As the significant precursors of lignin biosynthesis, the pattern of coniferyl alcohol and aldehyde (joint abbreviation Lignin-CAA for both structures) distribution in fiber cell wall was also identified by Raman images, with higher concentration occurring in the fiber secondary wall where there was the highest cellulose concentration. Moreover, noteworthy was the observation that higher concentration of lignin and very minor amounts of cellulose were visualized in the pit membrane areas. These complementary microanalytical methods provide more accurate and complete information with regard to ultrastructural and compositional characterization of plant cell walls.

On the Progress of Scanning Transmission Electron Microscopy (STEM) Imaging in a Scanning Electron Microscope.

PubMed

Sun, Cheng; Müller, Erich; Meffert, Matthias; Gerthsen, Dagmar

2018-04-01

Transmission electron microscopy (TEM) with low-energy electrons has been recognized as an important addition to the family of electron microscopies as it may avoid knock-on damage and increase the contrast of weakly scattering objects. Scanning electron microscopes (SEMs) are well suited for low-energy electron microscopy with maximum electron energies of 30 keV, but they are mainly used for topography imaging of bulk samples. Implementation of a scanning transmission electron microscopy (STEM) detector and a charge-coupled-device camera for the acquisition of on-axis transmission electron diffraction (TED) patterns, in combination with recent resolution improvements, make SEMs highly interesting for structure analysis of some electron-transparent specimens which are traditionally investigated by TEM. A new aspect is correlative SEM, STEM, and TED imaging from the same specimen region in a SEM which leads to a wealth of information. Simultaneous image acquisition gives information on surface topography, inner structure including crystal defects and qualitative material contrast. Lattice-fringe resolution is obtained in bright-field STEM imaging. The benefits of correlative SEM/STEM/TED imaging in a SEM are exemplified by structure analyses from representative sample classes such as nanoparticulates and bulk materials.

Frequency dependent dielectric properties of combustion synthesized Dy2Ti2O7 pyrochlore oxide

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Synthesis of indium phosphide nanocrystals by sonochemical method and survey of optical properties

NASA Astrophysics Data System (ADS)

Trung, Ho Minh; Duy Thien, Nguyen; Van Vu, Le; Long, Nguyen Ngoc; Hieu, Truong Kim

2013-10-01

Indium phosphide semiconductor materials (InP) have various applications in the field of semiconductor optoelectronics because of its advantages. But the making of this material is difficult due to the very weak chemical activity of In element. In this report we present a simple method to synthesize InP nanocrystals from inorganic precursors such as indium chloride (InCl3), yellow phosphorus (P4), reduction agent NaBH4 at low temperature with the aid of ultrasound. Structural, morphological and optical properties of the formed InP nanocrystals were examined by transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersed X-ray analysis (EDS), Raman scattering, absorption and photoluminscence (PL) spectroscopy. After the surface treatment of InP nanocrystals with liquid hydrofluoric (HF) acid, the luminescence spectra have an enhanced intensity and consist of the peaks in the region from 500 nm to 700 nm. The intensity of these peaks strongly depends on the concentration and etching time of HF. International Workshop on Advanced Materials and Nanotechnology 2012 (IWAMN 2012).

Selective Capture of Histidine-tagged Proteins from Cell Lysates Using TEM grids Modified with NTA-Graphene Oxide

NASA Astrophysics Data System (ADS)

Benjamin, Christopher J.; Wright, Kyle J.; Bolton, Scott C.; Hyun, Seok-Hee; Krynski, Kyle; Grover, Mahima; Yu, Guimei; Guo, Fei; Kinzer-Ursem, Tamara L.; Jiang, Wen; Thompson, David H.

2016-10-01

We report the fabrication of transmission electron microscopy (TEM) grids bearing graphene oxide (GO) sheets that have been modified with Nα, Nα-dicarboxymethyllysine (NTA) and deactivating agents to block non-selective binding between GO-NTA sheets and non-target proteins. The resulting GO-NTA-coated grids with these improved antifouling properties were then used to isolate His6-T7 bacteriophage and His6-GroEL directly from cell lysates. To demonstrate the utility and simplified workflow enabled by these grids, we performed cryo-electron microscopy (cryo-EM) of His6-GroEL obtained from clarified E. coli lysates. Single particle analysis produced a 3D map with a gold standard resolution of 8.1 Å. We infer from these findings that TEM grids modified with GO-NTA are a useful tool that reduces background and improves both the speed and simplicity of biological sample preparation for high-resolution structure elucidation by cryo-EM.

Strain relaxation induced surface morphology of heterogeneous GaInNAs layers grown on GaAs substrate

NASA Astrophysics Data System (ADS)

Gelczuk, Ł.; Jóźwiak, G.; Moczała, M.; Dłużewski, P.; Dąbrowska-Szata, M.; Gotszalk, T. P.

2017-07-01

The partially-relaxed heterogeneous GaInNAs layers grown on GaAs substrate by atmospheric pressure vapor phase epitaxy (AP-MOVPE) were investigated by transmission electron microscopy (TEM) and atomic force microscopy (AFM). The planar-view TEM image shows a regular 2D network of misfit dislocations oriented in two orthogonal 〈1 1 0〉 crystallographic directions at the (0 0 1) layer interface. Moreover, the cross-sectional view TEM image reveals InAs-rich and V-shaped precipitates in the near surface region of the GaInNAs epitaxial layer. The resultant undulating surface morphology, known as a cross-hatch pattern, is formed as observed by AFM. The numerical analysis of the AFM image of the GaInNAs layer surface with the well-defined cross-hatch morphology enabled us to determine a lower bound of actual density of misfit dislocations. However, a close correspondence between the asymmetric distribution of interfacial misfit dislocations and undulating surface morphology is observed.

AAO-based nanoreservoir arrays: A quick and easy support for TEM characterization

NASA Astrophysics Data System (ADS)

Mace, M.; Sahaf, H.; Moyen, E.; Bedu, F.; Masson, L.; Hanbücken, M.

2010-12-01

Large-scale arrays of calibrated, nanometer sized reservoirs are prepared by adapting the well-established electrochemical method used so far for the preparation of anodic aluminium oxide (AAO) membranes. The bottom plane of the assembly is prepared to be transparent for high-energy electrons, enabling their use as a universal sample support for transmission electron microscopy studies of nanoparticles. The nanoreservoir substrates can be cleaned under ultra-high-vacuum conditions and filled, by evaporating different materials. Filled nanoreservoirs can locally be sealed with a thin carbon layer using focused-ion-beam-induced deposition (FIBID). Nanoparticles, grow at various adsorption places on the walls and bottom planes inside the nanoreservoirs. They can be characterized by transmission electron microscopy (TEM) without further sample preparation in different crystallographic directions. Due to the dense array-arrangement of the reservoirs, very good statistics can already be obtained on one single sample. The controlled fabrication of the nanoreservoir array and first TEM results obtained on Au nanoparticles before and after sealing of the reservoirs, are presented.

Scanning electron microscopy imaging of dislocations in bulk materials, using electron channeling contrast.

PubMed

Crimp, Martin A

2006-05-01

The imaging and characterization of dislocations is commonly carried out by thin foil transmission electron microscopy (TEM) using diffraction contrast imaging. However, the thin foil approach is limited by difficult sample preparation, thin foil artifacts, relatively small viewable areas, and constraints on carrying out in situ studies. Electron channeling imaging of electron channeling contrast imaging (ECCI) offers an alternative approach for imaging crystalline defects, including dislocations. Because ECCI is carried out with field emission gun scanning electron microscope (FEG-SEM) using bulk specimens, many of the limitations of TEM thin foil analysis are overcome. This paper outlines the development of electron channeling patterns and channeling imaging to the current state of the art. The experimental parameters and set up necessary to carry out routine channeling imaging are reviewed. A number of examples that illustrate some of the advantages of ECCI over thin foil TEM are presented along with a discussion of some of the limitations on carrying out channeling contrast analysis of defect structures. Copyright (c) 2006 Wiley-Liss, Inc.

Selective Capture of Histidine-tagged Proteins from Cell Lysates Using TEM grids Modified with NTA-Graphene Oxide.

PubMed

Benjamin, Christopher J; Wright, Kyle J; Bolton, Scott C; Hyun, Seok-Hee; Krynski, Kyle; Grover, Mahima; Yu, Guimei; Guo, Fei; Kinzer-Ursem, Tamara L; Jiang, Wen; Thompson, David H

2016-10-17

We report the fabrication of transmission electron microscopy (TEM) grids bearing graphene oxide (GO) sheets that have been modified with N α , N α -dicarboxymethyllysine (NTA) and deactivating agents to block non-selective binding between GO-NTA sheets and non-target proteins. The resulting GO-NTA-coated grids with these improved antifouling properties were then used to isolate His 6 -T7 bacteriophage and His 6 -GroEL directly from cell lysates. To demonstrate the utility and simplified workflow enabled by these grids, we performed cryo-electron microscopy (cryo-EM) of His 6 -GroEL obtained from clarified E. coli lysates. Single particle analysis produced a 3D map with a gold standard resolution of 8.1 Å. We infer from these findings that TEM grids modified with GO-NTA are a useful tool that reduces background and improves both the speed and simplicity of biological sample preparation for high-resolution structure elucidation by cryo-EM.

Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy.

PubMed

Zhu, Yihan; Ciston, Jim; Zheng, Bin; Miao, Xiaohe; Czarnik, Cory; Pan, Yichang; Sougrat, Rachid; Lai, Zhiping; Hsiung, Chia-En; Yao, Kexin; Pinnau, Ingo; Pan, Ming; Han, Yu

2017-05-01

Metal-organic frameworks (MOFs) are crystalline porous materials with designable topology, porosity and functionality, having promising applications in gas storage and separation, ion conduction and catalysis. It is challenging to observe MOFs with transmission electron microscopy (TEM) due to the extreme instability of MOFs upon electron beam irradiation. Here, we use a direct-detection electron-counting camera to acquire TEM images of the MOF ZIF-8 with an ultralow dose of 4.1 electrons per square ångström to retain the structural integrity. The obtained image involves structural information transferred up to 2.1 Å, allowing the resolution of individual atomic columns of Zn and organic linkers in the framework. Furthermore, TEM reveals important local structural features of ZIF-8 crystals that cannot be identified by diffraction techniques, including armchair-type surface terminations and coherent interfaces between assembled crystals. These observations allow us to understand how ZIF-8 crystals self-assemble and the subsequent influence of interfacial cavities on mass transport of guest molecules.

Size distribution and volume fraction of T(1) phase precipitates from TEM images: Direct measurements and related correction.

PubMed

Dorin, Thomas; Donnadieu, Patricia; Chaix, Jean-Marc; Lefebvre, Williams; Geuser, Frédéric De; Deschamps, Alexis

2015-11-01

Transmission Electron Microscopy (TEM) can be used to measure the size distribution and volume fraction of fine scale precipitates in metallic systems. However, such measurements suffer from a number of artefacts that need to be accounted for, related to the finite thickness of the TEM foil and to the projected observation in two dimensions of the microstructure. We present a correction procedure to describe the 3D distribution of disc-like particles and apply this method to the plate-like T1 precipitates in an Al-Li-Cu alloy in two ageing conditions showing different particle morphologies. The precipitates were imaged in a High-Angular Annular Dark Field Microscope (HAADF-STEM). The corrected size distribution is further used to determine the precipitate volume fraction. Atom probe tomography (APT) is finally utilised as an alternative way to measure the precipitate volume fraction and test the validity of the electron microscopy results. Copyright © 2015 Elsevier Ltd. All rights reserved.

Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy

NASA Astrophysics Data System (ADS)

Zhu, Yihan; Ciston, Jim; Zheng, Bin; Miao, Xiaohe; Czarnik, Cory; Pan, Yichang; Sougrat, Rachid; Lai, Zhiping; Hsiung, Chia-En; Yao, Kexin; Pinnau, Ingo; Pan, Ming; Han, Yu

2017-05-01

Metal-organic frameworks (MOFs) are crystalline porous materials with designable topology, porosity and functionality, having promising applications in gas storage and separation, ion conduction and catalysis. It is challenging to observe MOFs with transmission electron microscopy (TEM) due to the extreme instability of MOFs upon electron beam irradiation. Here, we use a direct-detection electron-counting camera to acquire TEM images of the MOF ZIF-8 with an ultralow dose of 4.1 electrons per square ångström to retain the structural integrity. The obtained image involves structural information transferred up to 2.1 Å, allowing the resolution of individual atomic columns of Zn and organic linkers in the framework. Furthermore, TEM reveals important local structural features of ZIF-8 crystals that cannot be identified by diffraction techniques, including armchair-type surface terminations and coherent interfaces between assembled crystals. These observations allow us to understand how ZIF-8 crystals self-assemble and the subsequent influence of interfacial cavities on mass transport of guest molecules.

Recent advances in electron tomography: TEM and HAADF-STEM tomography for materials science and semiconductor applications.

PubMed

Kübel, Christian; Voigt, Andreas; Schoenmakers, Remco; Otten, Max; Su, David; Lee, Tan-Chen; Carlsson, Anna; Bradley, John

2005-10-01

Electron tomography is a well-established technique for three-dimensional structure determination of (almost) amorphous specimens in life sciences applications. With the recent advances in nanotechnology and the semiconductor industry, there is also an increasing need for high-resolution three-dimensional (3D) structural information in physical sciences. In this article, we evaluate the capabilities and limitations of transmission electron microscopy (TEM) and high-angle-annular-dark-field scanning transmission electron microscopy (HAADF-STEM) tomography for the 3D structural characterization of partially crystalline to highly crystalline materials. Our analysis of catalysts, a hydrogen storage material, and different semiconductor devices shows that features with a diameter as small as 1-2 nm can be resolved in three dimensions by electron tomography. For partially crystalline materials with small single crystalline domains, bright-field TEM tomography provides reliable 3D structural information. HAADF-STEM tomography is more versatile and can also be used for high-resolution 3D imaging of highly crystalline materials such as semiconductor devices.

4D electron microscopy: principles and applications.

PubMed

Flannigan, David J; Zewail, Ahmed H

2012-10-16

The transmission electron microscope (TEM) is a powerful tool enabling the visualization of atoms with length scales smaller than the Bohr radius at a factor of only 20 larger than the relativistic electron wavelength of 2.5 pm at 200 keV. The ability to visualize matter at these scales in a TEM is largely due to the efforts made in correcting for the imperfections in the lens systems which introduce aberrations and ultimately limit the achievable spatial resolution. In addition to the progress made in increasing the spatial resolution, the TEM has become an all-in-one characterization tool. Indeed, most of the properties of a material can be directly mapped in the TEM, including the composition, structure, bonding, morphology, and defects. The scope of applications spans essentially all of the physical sciences and includes biology. Until recently, however, high resolution visualization of structural changes occurring on sub-millisecond time scales was not possible. In order to reach the ultrashort temporal domain within which fundamental atomic motions take place, while simultaneously retaining high spatial resolution, an entirely new approach from that of millisecond-limited TEM cameras had to be conceived. As shown below, the approach is also different from that of nanosecond-limited TEM, whose resolution cannot offer the ultrafast regimes of dynamics. For this reason "ultrafast electron microscopy" is reserved for the field which is concerned with femtosecond to picosecond resolution capability of structural dynamics. In conventional TEMs, electrons are produced by heating a source or by applying a strong extraction field. Both methods result in the stochastic emission of electrons, with no control over temporal spacing or relative arrival time at the specimen. The timing issue can be overcome by exploiting the photoelectric effect and using pulsed lasers to generate precisely timed electron packets of ultrashort duration. The spatial and temporal resolutions achievable with short intense pulses containing a large number of electrons, however, are limited to tens of nanometers and nanoseconds, respectively. This is because Coulomb repulsion is significant in such a pulse, and the electrons spread in space and time, thus limiting the beam coherence. It is therefore not possible to image the ultrafast elementary dynamics of complex transformations. The challenge was to retain the high spatial resolution of a conventional TEM while simultaneously enabling the temporal resolution required to visualize atomic-scale motions. In this Account, we discuss the development of four-dimensional ultrafast electron microscopy (4D UEM) and summarize techniques and applications that illustrate the power of the approach. In UEM, images are obtained either stroboscopically with coherent single-electron packets or with a single electron bunch. Coulomb repulsion is absent under the single-electron condition, thus permitting imaging, diffraction, and spectroscopy, all with high spatiotemporal resolution, the atomic scale (sub-nanometer and femtosecond). The time resolution is limited only by the laser pulse duration and energy carried by the electron packets; the CCD camera has no bearing on the temporal resolution. In the regime of single pulses of electrons, the temporal resolution of picoseconds can be attained when hundreds of electrons are in the bunch. The applications given here are selected to highlight phenomena of different length and time scales, from atomic motions during structural dynamics to phase transitions and nanomechanical oscillations. We conclude with a brief discussion of emerging methods, which include scanning ultrafast electron microscopy (S-UEM), scanning transmission ultrafast electron microscopy (ST-UEM) with convergent beams, and time-resolved imaging of biological structures at ambient conditions with environmental cells.

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

NASA Technical Reports Server (NTRS)

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

2012-01-01

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

Preservation of protein globules and peptidoglycan in the mineralized cell wall of nitrate-reducing, iron(II)-oxidizing bacteria: a cryo-electron microscopy study.

PubMed

Miot, J; Maclellan, K; Benzerara, K; Boisset, N

2011-11-01

Iron-oxidizing bacteria are important actors of the geochemical cycle of iron in modern environments and may have played a key role all over Earth's history. However, in order to better assess that role on the modern and the past Earth, there is a need for better understanding the mechanisms of bacterial iron oxidation and for defining potential biosignatures to be looked for in the geologic record. In this study, we investigated experimentally and at the nanometre scale the mineralization of iron-oxidizing bacteria with a combination of synchrotron-based scanning transmission X-ray microscopy (STXM), scanning transmission electron microscopy (STEM) and cryo-transmission electron microscopy (cryo-TEM). We show that the use of cryo-TEM instead of conventional microscopy provides detailed information of the successive iron biomineralization stages in anaerobic nitrate-reducing iron-oxidizing bacteria. These results suggest the existence of preferential Fe-binding and Fe-oxidizing sites on the outer face of the plasma membrane leading to the nucleation and growth of Fe minerals within the periplasm of these cells that eventually become completely encrusted. In contrast, the septa of dividing cells remain nonmineralized. In addition, the use of cryo-TEM offers a detailed view of the exceptional preservation of protein globules and the peptidoglycan within the Fe-mineralized cell walls of these bacteria. These organic molecules and ultrastructural details might be protected from further degradation by entrapment in the mineral matrix down to the nanometre scale. This is discussed in the light of previous studies on the properties of Fe-organic interactions and more generally on the fossilization of mineral-organic assemblies. © 2011 Blackwell Publishing Ltd.

Tattoo Pigments Are Observed in the Kupffer Cells of the Liver Indicating Blood-Borne Distribution of Tattoo Ink.

PubMed

Sepehri, Mitra; Sejersen, Tobias; Qvortrup, Klaus; Lerche, Catharina M; Serup, Jørgen

2017-01-01

Tattoo pigments are deposited in the skin and known to distribute to regional lymph nodes. Tattoo pigments are small particles and may be hypothesized to reach the blood stream and become distributed to peripheral organs. This has not been studied in the past. The aim of the study was to trace tattoo pigments in internal organs in mice extensively tattooed with 2 different tattoo ink products. Three groups of mice were studied, i.e., 10 tattooed black, 10 tattooed red, and 5 untreated controls. They were tattooed on the entire back with commercial tattoo inks, black and red. Mice were sacrificed after 1 year. Samples were isolated from tattooed skin, lymph nodes, liver, spleen, kidney, and lung. Samples were examined for deposits of tattoo pigments by light microscopy and transmission electron microscopy (TEM). TEM identified intracellular tattoo pigments in the skin and in lymph nodes. TEM in both groups of tattooed mice showed tattoo pigment deposits in the Kupffer cells in the liver, which is a new observation. TEM detected no pigment in other internal organs. Light microscopy showed dense pigment in the skin and in lymph nodes but not in internal organs. The study demonstrated black and red tattoo pigment deposits in the liver; thus, tattoo pigment distributed from the tattooed skin via the blood stream to this important organ of detoxification. The finding adds a new dimension to tattoo pigment distribution in the body, i.e., as observed via the blood in addition to the lymphatic pathway. © 2017 S. Karger AG, Basel.

Counting Synapses Using FIB/SEM Microscopy: A True Revolution for Ultrastructural Volume Reconstruction.

PubMed

Merchán-Pérez, Angel; Rodriguez, José-Rodrigo; Alonso-Nanclares, Lidia; Schertel, Andreas; Defelipe, Javier

2009-01-01

The advent of transmission electron microscopy (TEM) in the 1950s represented a fundamental step in the study of neuronal circuits. The application of this technique soon led to the realization that the number of synapses changes during the course of normal life, as well as under certain pathological or experimental circumstances. Since then, one of the main goals in neurosciences has been to define simple and accurate methods to estimate the magnitude of these changes. Contrary to analysing single sections, TEM reconstructions are extremely time-consuming and difficult. Therefore, most quantitative studies use stereological methods to define the three-dimensional characteristics of synaptic junctions that are studied in two dimensions. Here, to count the exact number of synapses per unit of volume we have applied a new three-dimensional reconstruction method that involves the combination of focused ion beam milling and scanning electron microscopy (FIB/SEM). We show that the images obtained with FIB/SEM are similar to those obtained with TEM, but with the advantage that FIB/SEM permits serial reconstructions of large volumes of tissue to be generated rapidly and automatically. Furthermore, we compared the estimates of the number of synapses obtained with stereological methods with the values obtained by FIB/SEM reconstructions. We concluded that FIB/SEM not only provides the actual number of synapses per volume but it is also much easier and faster to use than other currently available TEM methods. More importantly, it also avoids most of the errors introduced by stereological methods and overcomes the difficulties associated with these techniques.

Self-Healing Thermal Annealing: Surface Morphological Restructuring Control of GaN Nanorods

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

Conroy, Michele; Li, Haoning; Zubialevich, Vitaly Z.

With advances in nanolithography and dry etching, top-down methods of nanostructuring have become a widely used tool for improving the efficiency of optoelectronics. These nano dimensions can offer various benefits to the device performance in terms of light extraction and efficiency, but often at the expense of emission color quality. Broadening of the target emission peak and unwanted yellow luminescence are characteristic defect-related effects due to the ion beam etching damage, particularly for III–N based materials. In this article we focus on GaN based nanorods, showing that through thermal annealing the surface roughness and deformities of the crystal structure canmore » be “self-healed”. Correlative electron microscopy and atomic force microscopy show the change from spherical nanorods to faceted hexagonal structures, revealing the temperature-dependent surface morphology faceting evolution. The faceted nanorods were shown to be strain- and defect-free by cathodoluminescence hyperspectral imaging, micro-Raman, and transmission electron microscopy (TEM). In-situ TEM thermal annealing experiments allowed for real time observation of dislocation movements and surface restructuring observed in ex-situ annealing TEM sampling. This thermal annealing investigation gives new insight into the redistribution path of GaN material and dislocation movement post growth, allowing for improved understanding and in turn advances in optoelectronic device processing of compound semiconductors.« less

Novel synthesis and structural analysis of zinc oxide nanoparticles for the non enzymatic glucose biosensor.

PubMed

Dayakar, T; Venkateswara Rao, K; Bikshalu, K; Rajendar, V; Park, Si-Hyun

2017-06-01

A non-enzymatic glucose biosensor was developed by utilizing the zinc oxide nanoparticles (ZnO NPs) synthesized by a novel green method using the leaf extract of Ocimum tenuiflorum. The structural, optical and morphological properties of ZnO NPs characterized by means of X-ray diffraction (XRD), ultraviolet-visible (UV-vis) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy-dispersive X-ray (EDAX) spectroscopy, and transmission electron microscopy (TEM). The XRD analysis revealed that the ZnO NPs were crystalline and had a hexagonal wurtzite structure. The crystallite size measured by XRD was the same as that measured using SEM and TEM. The UV-vis absorption spectrum estimates the band gap of ZnO NPs present in the range of 2.82 to 3.45eV. The reduction and formation of ZnO NPs mainly due to the involvement of leaf extract bio-molecular compounds analyzed from the FTIR spectra. The SEM result confirms the morphology of the NPs responsible from the various concentration of leaf extract in the synthesis process. HRTEM analysis depicts the spherical structure of ZnO NPs. The synthesized NPs have the average size ranges from 10 to 20nm. The fabricated GCE/ZnO glucose sensor represents superior electro catalytic activity that has been observed for ZnO NPs with a reproducible sensitivity of 631.30μAmM -1 cm -2 , correlation coefficient of R=0.998, linear dynamic range from 1-8.6mM, low detection limit of 0.043μM (S/N=3) and response time<4s. Copyright © 2017 Elsevier B.V. All rights reserved.

Evolution mechanisms of the primary α and β phases during α/β deformation of an α/β titanium alloy TC8

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

Wang, Ke, E-mail: study_ke@cqu.edu.cn

A TC8 titanium alloy was isothermally compressed at the strain rates of 10–50 s{sup −1} in the two-phase region of 820–940 °C, and the evolution mechanisms of the primary α and β phases, including grain morphology, dynamic recovery (DRV) and dynamic recrystallization (DRX), were investigated by optical microscopy (OM) and transmission electron microscopy (TEM). OM reveals that the phase content and grain morphology are more significantly influenced by the deformation temperature than the strain rate. The β grains achieve refinement only at 940 °C due to DRX in the β phase. TEM reveals the remarkable variations of the DRX grains,more » subgrains, sub-boundaries and dislocations morphology with temperature and strain rate related to DRV and DRX in the primary α phase. The DRX in the primary α phase appears most strongly at a middle temperature of 860 °C, and DRV dominates in the primary α phase at 940 °C. While the dominant mechanism varies from DRV to DRX in the β phase as the temperature increases. Finally, the influence mechanism of deformation parameters on the primary α grain morphology is revealed based on the combined effect of DRV and DRX in the primary α phase and diffusion of the β phase. - Highlights: •The β grains achieve refinement only at 940 °C due to DRX in the β phase. •The DRX in the primary α phase is most remarkable at 860 °C. •The dominant mechanism in β phase varies from DRV to DRX with increasing temperature. •The interaction between the primary α and β phases depends on the phase content.« less

Imaging heterostructured quantum dots in cultured cells with epifluorescence and transmission electron microscopy

PubMed Central

Rivera, Erin M.; Provencio, Casilda Trujillo; Steinbruck, Andrea; Rastogi, Pawan; Dennis, Allison; Hollingsworth, Jennifer; Serrano, Elba

2011-01-01

Quantum dots (QDs) are semiconductor nanocrystals with extensive imaging and diagnostic capabilities, including the potential for single molecule tracking. Commercially available QDs offer distinct advantages over organic fluorophores, such as increased photostability and tunable emission spectra, but their cadmium selenide (CdSe) core raises toxicity concerns. For this reason, replacements for CdSe-based QDs have been sought that can offer equivalent optical properties. The spectral range, brightness and stability of InP QDs may comprise such a solution. To this end, LANL/CINT personnel fabricated moderately thick-shell novel InP QDs that retain brightness and emission over time in an aqueous environment. We are interested in evaluating how the composition and surface properties of these novel QDs affect their entry and sequestration within the cell. Here we use epifluorescence and transmission electron microscopy (TEM) to evaluate the structural properties of cultured Xenopus kidney cells (A6; ATCC) that were exposed either to commercially available CdSe QDs (Qtracker® 565, Invitrogen) or to heterostructured InP QDs (LANL). Epifluorescence imaging permitted assessment of the general morphology of cells labeled with fluorescent molecular probes (Alexa Fluor® ® phalloidin; Hoechst 33342), and the prevalence of QD association with cells. In contrast, TEM offered unique advantages for viewing electron dense QDs at higher resolution with regard to subcellular sequestration and compartmentalization. Preliminary results show that in the absence of targeting moieties, InP QDs (200 nM) can passively enter cells and sequester nonspecifically in cytosolic regions whereas commercially available targeted QDs principally associate with membranous structures within the cell. Supported by: NIH 5R01GM084702. PMID:21808662

Facile synthesis of silver nanoparticles and its antibacterial activity against Escherichia coli and unknown bacteria on mobile phone touch surfaces/computer keyboards

NASA Astrophysics Data System (ADS)

Reddy, T. Ranjeth Kumar; Kim, Hyun-Joong

2016-07-01

In recent years, there has been significant interest in the development of novel metallic nanoparticles using various top-down and bottom-up synthesis techniques. Kenaf is a huge biomass product and a potential component for industrial applications. In this work, we investigated the green synthesis of silver nanoparticles (AgNPs) by using kenaf ( Hibiscus cannabinus) cellulose extract and sucrose, which act as stabilizing and reducing agents in solution. With this method, by changing the pH of the solution as a function of time, we studied the optical, morphological and antibacterial properties of the synthesized AgNPs. In addition, these nanoparticles were characterized by Ultraviolet-visible spectroscopy, transmission electron microscopy (TEM), field-emission scanning electron microscopy, Fourier transform infrared (FTIR) spectroscopy and energy-dispersive X-ray spectroscopy (EDX). As the pH of the solution varies, the surface plasmon resonance peak also varies. A fast rate of reaction at pH 10 compared with that at pH 5 was identified. TEM micrographs confirm that the shapes of the particles are spherical and polygonal. Furthermore, the average size of the nanoparticles synthesized at pH 5, pH 8 and pH 10 is 40.26, 28.57 and 24.57 nm, respectively. The structure of the synthesized AgNPs was identified as face-centered cubic (fcc) by XRD. The compositional analysis was determined by EDX. FTIR confirms that the kenaf cellulose extract and sucrose act as stabilizing and reducing agents for the silver nanoparticles. Meanwhile, these AgNPs exhibited size-dependent antibacterial activity against Escherichia coli ( E. coli) and two other unknown bacteria from mobile phone screens and computer keyboard surfaces.

Chemical Reactions of Molecules Promoted and Simultaneously Imaged by the Electron Beam in Transmission Electron Microscopy.

PubMed

Skowron, Stephen T; Chamberlain, Thomas W; Biskupek, Johannes; Kaiser, Ute; Besley, Elena; Khlobystov, Andrei N

2017-08-15

The main objective of this Account is to assess the challenges of transmission electron microscopy (TEM) of molecules, based on over 15 years of our work in this field, and to outline the opportunities in studying chemical reactions under the electron beam (e-beam). During TEM imaging of an individual molecule adsorbed on an atomically thin substrate, such as graphene or a carbon nanotube, the e-beam transfers kinetic energy to atoms of the molecule, displacing them from equilibrium positions. Impact of the e-beam triggers bond dissociation and various chemical reactions which can be imaged concurrently with their activation by the e-beam and can be presented as stop-frame movies. This experimental approach, which we term ChemTEM, harnesses energy transferred from the e-beam to the molecule via direct interactions with the atomic nuclei, enabling accurate predictions of bond dissociation events and control of the type and rate of chemical reactions. Elemental composition and structure of the reactant molecules as well as the operating conditions of TEM (particularly the energy of the e-beam) determine the product formed in ChemTEM processes, while the e-beam dose rate controls the reaction rate. Because the e-beam of TEM acts simultaneously as a source of energy for the reaction and as an imaging tool monitoring the same reaction, ChemTEM reveals atomic-level chemical information, such as pathways of reactions imaged for individual molecules, step-by-step and in real time; structures of illusive reaction intermediates; and direct comparison of catalytic activity of different transition metals filmed with atomic resolution. Chemical transformations in ChemTEM often lead to previously unforeseen products, demonstrating the potential of this method to become not only an analytical tool for studying reactions, but also a powerful instrument for discovery of materials that can be synthesized on preparative scale.

A correlative approach for combining microCT, light and transmission electron microscopy in a single 3D scenario

PubMed Central

2013-01-01

Background In biomedical research, a huge variety of different techniques is currently available for the structural examination of small specimens, including conventional light microscopy (LM), transmission electron microscopy (TEM), confocal laser scanning microscopy (CLSM), microscopic X-ray computed tomography (microCT), and many others. Since every imaging method is physically limited by certain parameters, a correlative use of complementary methods often yields a significant broader range of information. Here we demonstrate the advantages of the correlative use of microCT, light microscopy, and transmission electron microscopy for the analysis of small biological samples. Results We used a small juvenile bivalve mollusc (Mytilus galloprovincialis, approximately 0.8 mm length) to demonstrate the workflow of a correlative examination by microCT, LM serial section analysis, and TEM-re-sectioning. Initially these three datasets were analyzed separately, and subsequently they were fused in one 3D scene. This workflow is very straightforward. The specimen was processed as usual for transmission electron microscopy including post-fixation in osmium tetroxide and embedding in epoxy resin. Subsequently it was imaged with microCT. Post-fixation in osmium tetroxide yielded sufficient X-ray contrast for microCT imaging, since the X-ray absorption of epoxy resin is low. Thereafter, the same specimen was serially sectioned for LM investigation. The serial section images were aligned and specific organ systems were reconstructed based on manual segmentation and surface rendering. According to the region of interest (ROI), specific LM sections were detached from the slides, re-mounted on resin blocks and re-sectioned (ultrathin) for TEM. For analysis, image data from the three different modalities was co-registered into a single 3D scene using the software AMIRA®. We were able to register both the LM section series volume and TEM slices neatly to the microCT dataset, with small geometric deviations occurring only in the peripheral areas of the specimen. Based on co-registered datasets the excretory organs, which were chosen as ROI for this study, could be investigated regarding both their ultrastructure as well as their position in the organism and their spatial relationship to adjacent tissues. We found structures typical for mollusc excretory systems, including ultrafiltration sites at the pericardial wall, and ducts leading from the pericardium towards the kidneys, which exhibit a typical basal infolding system. Conclusions The presented approach allows a comprehensive analysis and presentation of small objects regarding both the overall organization as well as cellular and subcellular details. Although our protocol involves a variety of different equipment and procedures, we maintain that it offers savings in both effort and cost. Co-registration of datasets from different imaging modalities can be accomplished with high-end desktop computers and offers new opportunities for understanding and communicating structural relationships within organisms and tissues. In general, the correlative use of different microscopic imaging techniques will continue to become more widespread in morphological and structural research in zoology. Classical TEM serial section investigations are extremely time consuming, and modern methods for 3D analysis of ultrastructure such as SBF-SEM and FIB-SEM are limited to very small volumes for examination. Thus the re-sectioning of LM sections is suitable for speeding up TEM examination substantially, while microCT could become a key-method for complementing ultrastructural examinations. PMID:23915384

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Thermo-optical properties of residential coals and combustion aerosols

NASA Astrophysics Data System (ADS)

Pintér, Máté; Ajtai, Tibor; Kiss-Albert, Gergely; Kiss, Diána; Utry, Noémi; Janovszky, Patrik; Palásti, Dávid; Smausz, Tomi; Kohut, Attila; Hopp, Béla; Galbács, Gábor; Kukovecz, Ákos; Kónya, Zoltán; Szabó, Gábor; Bozóki, Zoltán

2018-04-01

In this study, we present the inherent optical properties of carbonaceous aerosols generated from various coals (hard through bituminous to lignite) and their correlation with the thermochemical and energetic properties of the bulk coal samples. The nanoablation method provided a unique opportunity for the comprehensive investigation of the generated particles under well controlled laboratory circumstances. First, the wavelength dependent radiative features (optical absorption and scattering) and the size distribution (SD) of the generated particulate matter were measured in-situ in aerosol phase using in-house developed and customised state-of-the-art instrumentation. We also investigated the morphology and microstructure of the generated particles using Transmission Electron Microscopy (TEM) and Electron Diffraction (ED). The absorption spectra of the measured samples (quantified by Absorption Angström Exponent (AAE)) were observed to be distinctive. The correlation between the thermochemical features of bulk coal samples (fixed carbon (FC) to volatile matter (VM) ratio and calorific value (CV)) and the AAE of aerosol assembly were found to be (r2 = 0.97 and r2 = 0.97) respectively. Lignite was off the fitted curves in both cases most probably due to its high optically inactive volatile material content. Although more samples are necessary to be investigated to draw statistically relevant conclusion, the revealed correlation between CV and Single Scattering Albedo (SSA) implies that climatic impact of coal combusted aerosol could depend on the thermal and energetic properties of the bulk material.

Review of advanced imaging techniques

PubMed Central

Chen, Yu; Liang, Chia-Pin; Liu, Yang; Fischer, Andrew H.; Parwani, Anil V.; Pantanowitz, Liron

2012-01-01

Pathology informatics encompasses digital imaging and related applications. Several specialized microscopy techniques have emerged which permit the acquisition of digital images (“optical biopsies”) at high resolution. Coupled with fiber-optic and micro-optic components, some of these imaging techniques (e.g., optical coherence tomography) are now integrated with a wide range of imaging devices such as endoscopes, laparoscopes, catheters, and needles that enable imaging inside the body. These advanced imaging modalities have exciting diagnostic potential and introduce new opportunities in pathology. Therefore, it is important that pathology informaticists understand these advanced imaging techniques and the impact they have on pathology. This paper reviews several recently developed microscopic techniques, including diffraction-limited methods (e.g., confocal microscopy, 2-photon microscopy, 4Pi microscopy, and spatially modulated illumination microscopy) and subdiffraction techniques (e.g., photoactivated localization microscopy, stochastic optical reconstruction microscopy, and stimulated emission depletion microscopy). This article serves as a primer for pathology informaticists, highlighting the fundamentals and applications of advanced optical imaging techniques. PMID:22754737

EBIC/TEM investigations of defects in solar silicon ribbon materials

NASA Technical Reports Server (NTRS)

Ast, D. G.

1981-01-01

Transmission electron microscopy was used to investigate the defect structure of edge defined film growth (EFG) material, web dentritic ribbons (WEB), and ribbon to ribbon recrystallized material (RTR). The most common defects in all these materials are coherent first order twin boundaries. These coherent twins can be very thin, a few atomic layers. Bundles of the twins which contain odd numbers of twins will in optical images appear as a seemingly single first twin boundary. First-order coherent twin boundaries are not electrically active, except at locations where they contain intrinsic (grain boundary) dislocations. These dislocations take up small deviations from the ideal twin relation and play the same role in twin boundaries as conventional and play the some role in twin boundaries as conventional edge and screw dislocations in small angle tilt and twist boundaries.

Experimentally determined wear behavior of an Al2O3-SiC composite from 25 to 1200 C

NASA Technical Reports Server (NTRS)

Dellacorte, Christopher; Farmer, Serene C.; Book, Patricia O.

1990-01-01

The sliding wear behavior of a self-mated alumina-silicon carbide whisker toughened composite was studied using optical, scanning electron (SEM) and transmission electron (TEM) microscopy. Because of its excellent strength and toughness properties this composite material is under consideration for use in heat engine applications for sliding contacts which operate at elevated temperatures. The composite's wear behavior and especially its wear mechanisms are not well understood. Pin-on-disk specimens were slid in air at 2.7 m/s sliding velocity, under a 26.5-N load, at temperatures 25 to 1200 C. Pin wear increased with increasing temperature. Based upon the microscopic analyses, the wear mechanism seems to be loosening of the reinforcing whiskers due to frictional and bulk heating. This leads to whisker pullout and increased wear.

Growth and characterization of cubic SiC single-crystal films on Si

NASA Technical Reports Server (NTRS)

Powell, J. Anthony; Matus, L. G.; Kuczmarski, Maria A.

1987-01-01

Morphological and electrical characterization results are presented for cubic SiC films grown by chemical vapor deposition on single-crystal Si substrates. The films, up to 40 microns thick, were characterized by optical microscopy, (SEM), (TEM), electron channeling, surface profilometry, and Hall measurements. A variety of morphological features observed on the SiC films are described. Electrical measurements showed a decrease in the electron mobility with increasing electron carrier concentration, similar to that observed in Si. Room-temperature electron mobilities up to 520 sq cm/V-s (at an electron carrier concentration of 5 x 10 to the 16th/cu cm) were measured. Finally, a number of parameters believed to be important in the growth process were investigated, and some discussion is given of their possible effects on the film characteristics.

Growth and characterization of cubic SiC single-crystal films on Si

NASA Astrophysics Data System (ADS)

Powell, J. Anthony; Matus, L. G.; Kuczmarski, Maria A.

1987-06-01

Morphological and electrical characterization results are presented for cubic SiC films grown by chemical vapor deposition on single-crystal Si substrates. The films, up to 40 microns thick, were characterized by optical microscopy, (SEM), (TEM), electron channeling, surface profilometry, and Hall measurements. A variety of morphological features observed on the SiC films are described. Electrical measurements showed a decrease in the electron mobility with increasing electron carrier concentration, similar to that observed in Si. Room-temperature electron mobilities up to 520 sq cm/V-s (at an electron carrier concentration of 5 x 10 to the 16th/cu cm) were measured. Finally, a number of parameters believed to be important in the growth process were investigated, and some discussion is given of their possible effects on the film characteristics.

Growth of ZnMgTe/ZnTe waveguide structures on ZnTe (0 0 1) substrates by molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Kumagai, Y.; Imada, S.; Baba, T.; Kobayashi, M.

2011-05-01

ZnMgTe/ZnTe/ZnMgTe layered structures were grown on (0 0 1) ZnTe substrates by molecular beam epitaxy. This structure was designed to apply to waveguides in various optoelectronic devices to reduce light loss. Since the lattice mismatch between ZnTe and ZnMgTe was not negligible, the critical layer thickness (CLT) was theoretically derived. Structures with varying Mg composition and layer thickness of ZnMgTe cladding layer were grown and examined for crystal quality with respect to theoretical data. The crystal quality was investigated by means of cross sectional transmission electron microscopy (TEM) and reciprocal space mapping (RSM). Optical confinements were observed by irradiating a laser beam from one end of the sample and monitoring the transmitted light from the other end.

Three-dimensional image formation in fiber-optical second-harmonic-generation microscopy.

PubMed

Gu, Min; Fu, Ling

2006-02-06

Three-dimensional (3-D) image formation in fiber-optical second-harmonic-generation microscopy is revealed to be purely coherent and therefore can be described by a 3-D coherent transfer function (CTF) that exhibits the same spatial frequency passband as that of fiber-optical reflection-mode non-fluorescence microscopy. When the numerical aperture of the fiber is much larger than the angle of convergence of the illumination on the fiber aperture, the performance of fiber-optical second-harmonic-generation microscopy behaves as confocal second-harmonic-generation microscopy. The dependence of axial resolution on fiber coupling parameters shows an improvement of approximately 7%, compared with that in fiber-optical two-photon fluorescence microscopy.

Synthesis of carbon-encapsulated metal nanoparticles from wood char

Treesearch

Yicheng Du; Chuji Wang; Hossein Toghiani; Zhiyong Cai; Xiaojian Liu; Jilei Zhang; Qiangu Yan

2010-01-01

Carbon-encapsulated metal nanoparticles were synthesized by thermal treatment of wood char, with or without transition metal ions pre-impregnated, at 900ºC to 1,100ºC. Nanoparticles with concentric multilayer shells were observed. The nanoparticles were analyzed by scanning electron microscopy, transmission electron microscopy (TEM), X-ray diffraction...

Collaboration at the Nanoscale: Exploring Viral Genetics with Electron Microscopy

ERIC Educational Resources Information Center

Duboise, S. Monroe; Moulton, Karen D.; Jamison, Jennifer L.

2009-01-01

The Maine Science Corps is a project sponsored by the National Science Foundation's (NSF) Graduate Teaching Fellows in K-12 Education (GK-12 ) program. Through this program, the University of Southern Maine's (USM) virology and transmission electron microscopy (TEM) research group provides high school teachers and students in rural areas with…

Super-resolution atomic force photoactivated microscopy of biological samples (Conference Presentation)

NASA Astrophysics Data System (ADS)

Lee, Seunghyun; Kim, Hyemin; Shin, Seungjun; Doh, Junsang; Kim, Chulhong

2017-03-01

Optical microscopy (OM) and photoacoustic microscopy (PAM) have previously been used to image the optical absorption of intercellular features of biological cells. However, the optical diffraction limit ( 200 nm) makes it difficult for these modalities to image nanoscale inner cell structures and the distribution of internal cell components. Although super-resolution fluorescence microscopy, such as stimulated emission depletion microscopy (STED) and stochastic optical reconstruction microscopy (STORM), has successfully performed nanoscale biological imaging, these modalities require the use of exogenous fluorescence agents, which are unfavorable for biological samples. Our newly developed atomic force photoactivated microscopy (AFPM) can provide optical absorption images with nanoscale lateral resolution without any exogenous contrast agents. AFPM combines conventional atomic force microscopy (AFM) and an optical excitation system, and simultaneously provides multiple contrasts, such as the topography and magnitude of optical absorption. AFPM can detect the intrinsic optical absorption of samples with 8 nm lateral resolution, easily overcoming the diffraction limit. Using the label-free AFPM system, we have successfully imaged the optical absorption properties of a single melanoma cell (B16F10) and a rosette leaf epidermal cell of Arabidopsis (ecotype Columbia (Col-0)) with nanoscale lateral resolution. The remarkable images show the melanosome distribution of a melanoma cell and the biological structures of a plant cell. AFPM provides superior imaging of optical absorption with a nanoscale lateral resolution, and it promises to become widely used in biological and chemical research.

Characterization of Sulfur and Nanostructured Sulfur Battery Cathodes in Electron Microscopy Without Sublimation Artifacts

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

Levin, Barnaby D. A.; Zachman, Michael J.; Werner, Jörg G.

Abstract Lithium sulfur (Li–S) batteries have the potential to provide higher energy storage density at lower cost than conventional lithium ion batteries. A key challenge for Li–S batteries is the loss of sulfur to the electrolyte during cycling. This loss can be mitigated by sequestering the sulfur in nanostructured carbon–sulfur composites. The nanoscale characterization of the sulfur distribution within these complex nanostructured electrodes is normally performed by electron microscopy, but sulfur sublimates and redistributes in the high-vacuum conditions of conventional electron microscopes. The resulting sublimation artifacts render characterization of sulfur in conventional electron microscopes problematic and unreliable. Here, we demonstratemore » two techniques, cryogenic transmission electron microscopy (cryo-TEM) and scanning electron microscopy in air (airSEM), that enable the reliable characterization of sulfur across multiple length scales by suppressing sulfur sublimation. We use cryo-TEM and airSEM to examine carbon–sulfur composites synthesized for use as Li–S battery cathodes, noting several cases where the commonly employed sulfur melt infusion method is highly inefficient at infiltrating sulfur into porous carbon hosts.« less

Electron microscopy characterization of Ni-Cr-B-Si-C laser deposited coatings.

PubMed

Hemmati, I; Rao, J C; Ocelík, V; De Hosson, J Th M

2013-02-01

During laser deposition of Ni-Cr-B-Si-C alloys with high amounts of Cr and B, various microstructures and phases can be generated from the same chemical composition that results in heterogeneous properties in the clad layer. In this study, the microstructure and phase constitution of a high-alloy Ni-Cr-B-Si-C coating deposited by laser cladding were analyzed by a combination of several microscopy characterization techniques including scanning electron microscopy in secondary and backscatter imaging modes, energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM). The combination of EDS and EBSD allowed unequivocal identification of micron-sized precipitates as polycrystalline orthorhombic CrB, single crystal tetragonal Cr5B3, and single crystal hexagonal Cr7C3. In addition, TEM characterization showed various equilibrium and metastable Ni-B, Ni-Si, and Ni-Si-B eutectic products in the alloy matrix. The findings of this study can be used to explain the phase formation reactions and to tune the microstructure of Ni-Cr-B-Si-C coatings to obtain the desired properties.

Femtosecond nonlinear optical properties of laser ablated gold nanoparticles in water

NASA Astrophysics Data System (ADS)

Krishnakanth, K. N.; Bharathi, M. S. S.; Hamad, S.; Rao, S. Venugopal

2018-04-01

Femtosecond third order nonlinear optical (NLO) properties of ultrafast laser ablated gold (Au) colloidsin distilled waterare investigatedusing degenerate four wave mixing technique with 50fs pulses at 800nm wavelength. The estimated value of χ(3) obtained for Au nanoparticles is 1.93×10-14 e.s.u. The characterization of the NPs was achieved done using TEM and HR-TEM techniques. We also present the time resolved studies of Au colloids by using DFWM technique in the forward BOXCAR phase matching geometry.

Isolation and characterization of nanosheets containing few layers of the Aurivillius family of oxides and metal-organic compounds

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

Sreedhara, M.B.; Prasad, B.E.; Moirangthem, Monali

2015-04-15

Nanosheets containing few-layers of ferroelectric Aurivillius family of oxides, Bi{sub 2}A{sub n−1}B{sub n}O{sub 3n+3} (where A=Bi{sup 3+}, Ba{sup 2+} etc. and B=Ti{sup 4+}, Fe{sup 3+} etc.) with n=3, 4, 5, 6 and 7 have been prepared by reaction with n-butyllithium, followed by exfoliation in water. The few-layer samples have been characterized by Tyndall cones, atomic force microscopy, optical spectroscopy and other techniques. The few-layer species have a thickness corresponding to a fraction of the c-parameter along which axis the perovskite layers are stacked. Magnetization measurements have been carried out on the few-layer samples containing iron. Few-layer species of a fewmore » layered metal-organic compounds have been obtained by ultrasonication and characterized by Tyndall cones, atomic force microscopy, optical spectroscopy and magnetic measurements. Significant changes in the optical spectra and magnetic properties are found in the few-layer species compared to the bulk samples. Few-layer species of the Aurivillius family of oxides may find uses as thin layer dielectrics in photovoltaics and other applications. - Graphical abstract: Exfoliation of the layered Aurivillius oxides into few-layer nanosheets by chemical Li intercalation using n-BuLi followed by reaction in water. Exfoliation of the layered metal-organic compounds into few-layer nanosheets by ultrasonication. - Highlights: • Few-layer nanosheets of Aurivillius family of oxides with perovskite layers have been generated by lithium intercalation. • Few-layer nanosheets of few layered metal-organic compounds have been generated by ultrasonication. • Few-layer nanosheets of the Aurivillius oxides have been characterized by AFM, TEM and optical spectroscopy. • Aurivillius oxides containing Fe show layer dependent magnetic properties. • Exfoliated few-layer metal-organic compounds show changes in spectroscopic and magnetic properties compared with bulk materials.« less

Electron microscopy investigations of nanoparticles for cancer diagnostic applications

NASA Astrophysics Data System (ADS)

Koh, Ai Leen

This dissertation concerns electron microscopy characterization of magnetic (MNP) and surface enhanced Raman scattering (SERS) nanoparticles for in-vitro cancer diagnostic applications. Electron microscopy is an essential characterization tool owing to its (sub) nanometer spatial resolution. Structural information about the nanoparticles can be obtained using transmission electron microscopy (TEM), which can in turn be correlated to their physical characteristics. The scanning electron microscope (SEM) has excellent depth of field and can be effectively utilized to obtain high resolution information about nanoparticles binding onto cell surfaces. Part One of this thesis focuses on MNPs for bio-sensing and detection applications. As a preliminary study, chemically-synthesized, commercially-available iron oxide nanoparticles were compared against their laboratory-synthesized counterparts to assess their suitability for this application. The motivation for this initial study came about due to the lack of published data on commercially available iron oxide nanoparticles. TEM studies show that the latter are "beads" composed of multiple iron oxide cores encapsulated by a polymer shell, with large standard deviations in core diameter. Laboratory-synthesized iron oxide nanoparticles, on the other hand, are single core particles with small variations in diameter and therefore are expected to be better candidates for the required application. A key limitation in iron oxide nanoparticles is their relatively weak magnetic signals. The development of high moment Synthetic Anti-Ferromagnetic (SAF) nanoparticles aims to overcome this issue. SAFs are a novel class of MNPs fabricated using nanoimprint lithography, direct deposition of multilayer structure and final suspension into liquid medium (water). TEM analyses of cross-section specimens reveal that the SAFs possess characteristics similar to those of sputtered magnetic multilayer thin films. Their layered structure is preserved after a chemical etch. Magnetic measurements show a slight decrease in magnetic moment after ion milling. From TEM characterization, the introduction of oxygen into the copper release layer, prior the film deposition process, can effectively control the topography of the oxidized-copper grains and, consequently, lead to the production of SAF nanoparticles with flatter layers. Size distribution studies performed on SAFs fabricated using self-assembled stamps show that it is possible to produce monodisperse nanoparticles with diameters from 70 nm up. Part Two of the dissertation describes structural characterization experiments performed on Composite Organic-Inorganic Nanoparticles (COINs), which are a novel type of SERS nanoclusters formed by aggregating silver nanoparticles with Raman molecules, and then encapsulating them with an organic coating that stabilizes the aggregates and promotes subsequent functionalization with antibodies. Part Three of this dissertation focuses on the development and application of electron microscopy-based techniques to characterize the nanomaterial-biology interactions, to assess how, or indeed whether, nanoparticles are attaching to the cancer cells. The technique of negative staining was applied to simultaneously visualize inorganic nanoparticles and their biofunctionalized entities under the TEM and to verify the successful functionalization of nanoparticles with antibodies. The interpretation of the negatively-stained COINs was consistent with the EFTEM data. Next, the localization and characterization of CD54-functionalized COINs on the apicolateral portions of U937 leukemia cell lines was determined using TEM, SEM and Scanning Auger Microscopy. The analyses show that CD54 antigens are localized at a specific region on U937 leukemia cell surfaces. SEM imaging and SER spectroscopy correlation studies of different antibody-conjugated COINs attached onto different cancer cell lines show a direct correlation between the number of COINs binding to cells and the corresponding SER intensity. Finally, TEM was used to locate intra-cellularly labeled COINs and to trace the phospho-stat6 signaling pathway in U937 leukemia cells, demonstrating that COINs can be used to detect intracellular phosphorylation signaling events. These experiments demonstrate the importance of electron microscopy for analyzing the material-biology interface and for validating the attachment of nanoparticles on and in cells. Thus, electron microscope provides complementary imaging and spectroscopic information to current magnetic and SERS bio-detection technologies. (Abstract shortened by UMI.)

Cr-substitution effect on structural, optical and electrical properties of Cr{sub x}Ce{sub 1−x}PO{sub 4} (x = 0.00, 0.08, 0.10 and 0.20) nanorods

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

Fadhalaoui, Amor; Dhaouadi, Hassouna, E-mail: dhaouadihassouna@yahoo.fr; Marouani, Houda

2016-01-15

Graphical abstract: The Cr{sub x}Ce{sub 1−x}PO{sub 4} (x = 0.00, 0.08, 0.10 and 0.20) nanorods synthesized under hydrothermal conditions. - Highlights: • Cr{sub x}Ce{sub 1−x}PO{sub 4} (x = 0.00–0.20) nanorods were synthesized by hydrothermal method. • Mean crystallite size of the products decreases with Cr-content. • Obvious improvements of the electrical conductivity comparatively to CePO4. - Abstract: Cr{sub x}Ce{sub 1−x}PO{sub 4} (x = 0.00–0.20) nanorods were synthesized using the hydrothermal method. The as-prepared samples were characterized by X-ray diffraction (XRD), infrared absorption spectroscopy (IR) and transmission electron microscopy (TEM). The XRD results revealed the formation of a pure CePO{sub 4}more » hexagonal phase. TEM images confirmed the nano-size character of the as-prepared samples. Impedance spectroscopy analysis was used to analyze the electrical behavior of samples as a function of frequency at different temperatures. The increase of Cr-amount led to an increase in the total conductivities and decreased the activation energies (E{sub a} (x = 0.00) = 1.08 eV to E{sub a} (x = 0.20) = 0.80 eV). The optical properties of Cr{sub x}Ce{sub 1−x}PO{sub 4} nanomaterials were investigated using UV–vis spectroscopy. The band-gap energy values decreased with increasing Cr-content showing a red-shift trend. The improvement of the electrical conductivity and optical properties makes the Cr{sub x}Ce{sub 1−x}PO{sub 4} nanomaterials possible candidates to be used as electrolytes in solid oxide fuel cells, in photocatalytic and photovoltaic applications.« less

The 2015 super-resolution microscopy roadmap

NASA Astrophysics Data System (ADS)

Hell, Stefan W.; Sahl, Steffen J.; Bates, Mark; Zhuang, Xiaowei; Heintzmann, Rainer; Booth, Martin J.; Bewersdorf, Joerg; Shtengel, Gleb; Hess, Harald; Tinnefeld, Philip; Honigmann, Alf; Jakobs, Stefan; Testa, Ilaria; Cognet, Laurent; Lounis, Brahim; Ewers, Helge; Davis, Simon J.; Eggeling, Christian; Klenerman, David; Willig, Katrin I.; Vicidomini, Giuseppe; Castello, Marco; Diaspro, Alberto; Cordes, Thorben

2015-11-01

Far-field optical microscopy using focused light is an important tool in a number of scientific disciplines including chemical, (bio)physical and biomedical research, particularly with respect to the study of living cells and organisms. Unfortunately, the applicability of the optical microscope is limited, since the diffraction of light imposes limitations on the spatial resolution of the image. Consequently the details of, for example, cellular protein distributions, can be visualized only to a certain extent. Fortunately, recent years have witnessed the development of ‘super-resolution’ far-field optical microscopy (nanoscopy) techniques such as stimulated emission depletion (STED), ground state depletion (GSD), reversible saturated optical (fluorescence) transitions (RESOLFT), photoactivation localization microscopy (PALM), stochastic optical reconstruction microscopy (STORM), structured illumination microscopy (SIM) or saturated structured illumination microscopy (SSIM), all in one way or another addressing the problem of the limited spatial resolution of far-field optical microscopy. While SIM achieves a two-fold improvement in spatial resolution compared to conventional optical microscopy, STED, RESOLFT, PALM/STORM, or SSIM have all gone beyond, pushing the limits of optical image resolution to the nanometer scale. Consequently, all super-resolution techniques open new avenues of biomedical research. Because the field is so young, the potential capabilities of different super-resolution microscopy approaches have yet to be fully explored, and uncertainties remain when considering the best choice of methodology. Thus, even for experts, the road to the future is sometimes shrouded in mist. The super-resolution optical microscopy roadmap of Journal of Physics D: Applied Physics addresses this need for clarity. It provides guidance to the outstanding questions through a collection of short review articles from experts in the field, giving a thorough discussion on the concepts underlying super-resolution optical microscopy, the potential of different approaches, the importance of label optimization (such as reversible photoswitchable proteins) and applications in which these methods will have a significant impact. Mark Bates, Christian Eggeling

Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

Structural and optical properties of glancing angle deposited In2O3 columnar arrays and Si/In2O3 photodetector

NASA Astrophysics Data System (ADS)

Mondal, A.; Shougaijam, B.; Goswami, T.; Dhar, J. C.; Singh, N. K.; Choudhury, S.; Chattopadhay, K. K.

2014-04-01

Ordered and perpendicular columnar arrays of In2O3 were synthesized on conducting ITO electrode by a simple glancing angle deposition (GLAD) technique. The as-deposited In2O3 columns were investigated by field emission gun-scanning electron microscope (FEG-SEM). The average length and diameter of the columns were estimated ˜400 nm and ˜100 nm, respectively. The morphology of the structure was examined by transmission electron microscopy (TEM). X-ray diffraction (XRD) analysis shows the polycrystalline nature of the sample which was verified by selective area electron diffraction (SAED) analysis. The growth mechanism and optical properties of the columns were also discussed. Optical absorption shows that In2O3 columns have a high band to band transition at ˜3.75 eV. The ultraviolet and green emissions were obtained from the In2O3 columnar arrays. The P-N junction was formed between In2O3 and P-type Si substrate. The GLAD synthesized In2O3 film exhibits low current conduction compared to In2O3 TF. However, the Si/GLAD-In2O3 detector shows ˜1.5 times enhanced photoresponsivity than that of Si/In2O3 TF.

Synergistic Growth of Giant Wormlike Micelles in Ternary Mixed Surfactant Solutions: Effect of Octanoic Acid.

PubMed

Georgieva, Gergana S; Anachkov, Svetoslav E; Lieberwirth, Ingo; Koynov, Kaloian; Kralchevsky, Peter A

2016-12-06

The synergistic growth of giant wormlike micelles in ternary mixed solutions composed of an anionic surfactant (sodium laurylethersulfate, SLES), a zwitterionic surfactant (cocamidopropyl betaine, CAPB), and octanoic acid (HC8) is studied. Rheological data and their analysis in terms of Cole-Cole plots and micellar characteristic times are presented, and the micellar structures behind the observed rheological behavior are revealed by cryo-TEM micrographs. The surfactant composition is fixed near the maximal micelle size of the binary SLES + CAPB system, whereas the concentration of HC8 is varied. At a given HC8 concentration, the viscosity of the ternary micellar solutions exhibits a very high and sharp peak. Polarized-light optical microscopy indicates that all investigated solutions are isotropic rather than liquid-crystalline. The cryo-TEM imaging shows complex phase behavior: wormlike micelles to the left of the peak, giant entangled wormlike micelles at the peak, and long wormlike micelles coexisting with multiconnected micellar aggregates to the right of the peak. The formation of multiconnected micelles leads to a drop in viscosity at the higher concentrations. The results contribute to a better understanding of the structure-rheology relations in micellar surfactant solutions and could be useful for controlling the properties of formulations in personal-care and house-hold detergency.

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.

Newly recognized hosts for uranium in the Hanford Site vadose zone

USGS Publications Warehouse

Stubbs, J.E.; Veblen, L.A.; Elbert, D.C.; Zachara, J.M.; Davis, J.A.; Veblen, D.R.

2009-01-01

Uranium contaminated sediments from the U.S. Department of Energy's Hanford Site have been investigated using electron microscopy. Six classes of solid hosts for uranium were identified. Preliminary sediment characterization was carried out using optical petrography, and electron microprobe analysis (EMPA) was used to locate materials that host uranium. All of the hosts are fine-grained and intergrown with other materials at spatial scales smaller than the analytical volume of the electron microprobe. A focused ion beam (FIB) was used to prepare electron-transparent specimens of each host for the transmission electron microscope (TEM). The hosts were identified as: (1) metatorbernite [Cu(UO2)2(PO4)2??8H2O]; (2) coatings on sediment clasts comprised mainly of phyllosilicates; (3) an amorphous zirconium (oxyhydr)oxide found in clast coatings; (4) amorphous and poorly crystalline materials that line voids within basalt lithic fragments; (5) amorphous palagonite surrounding fragments of basaltic glass; and (6) Fe- and Mn-oxides. These findings demonstrate the effectiveness of combining EMPA, FIB, and TEM to identify solid-phase contaminant hosts. Furthermore, they highlight the complexity of U geochemistry in the Hanford vadose zone, and illustrate the importance of microscopic transport in controlling the fate of contaminant metals in the environment. ?? 2008 Elsevier Ltd.

Atomic layer epitaxy of Ruddlesden-Popper SrO(SrTiO{sub 3}){sub n} films by means of metalorganic aerosol deposition

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

Jungbauer, M.; Hühn, S.; Moshnyaga, V.

2014-12-22

We report an atomic layer epitaxial growth of Ruddlesden-Popper (RP) thin films of SrO(SrTiO{sub 3}){sub n} (n = ∞, 2, 3, 4) by means of metalorganic aerosol deposition (MAD). The films are grown on SrTiO{sub 3}(001) substrates by means of a sequential deposition of Sr-O/Ti-O{sub 2} atomic monolayers, monitored in-situ by optical ellipsometry. X-ray diffraction and transmission electron microscopy (TEM) reveal the RP structure with n = 2–4 in accordance with the growth recipe. RP defects, observed by TEM in a good correlation with the in-situ ellipsometry, mainly result from the excess of SrO. Being maximal at the film/substrate interface, the SrO excess rapidlymore » decreases and saturates after 5–6 repetitions of the SrO(SrTiO{sub 3}){sub 4} block at the level of 2.4%. This identifies the SrTiO{sub 3} substrate surface as a source of RP defects under oxidizing conditions within MAD. Advantages and limitations of MAD as a solution-based and vacuum-free chemical deposition route were discussed in comparison with molecular beam epitaxy.« less

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

DOE PAGES

Zhang, C.; Balachandran, S.; Eisenlohr, P.; ...

2017-10-04

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

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

Zhang, C.; Balachandran, S.; Eisenlohr, P.

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

The role of electron irradiation history in liquid cell transmission electron microscopy.

PubMed

Moser, Trevor H; Mehta, Hardeep; Park, Chiwoo; Kelly, Ryan T; Shokuhfar, Tolou; Evans, James E

2018-04-01

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC-TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role of cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. These results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides.

The role of electron irradiation history in liquid cell transmission electron microscopy

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

Moser, Trevor H.; Mehta, Hardeep; Park, Chiwoo

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC- TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the rolemore » of cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. These results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides.« less

The role of electron irradiation history in liquid cell transmission electron microscopy

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

Moser, Trevor H.; Mehta, Hardeep; Park, Chiwoo

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC-TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role ofmore » cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. Lastly, these results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides.« less

The role of electron irradiation history in liquid cell transmission electron microscopy

PubMed Central

Mehta, Hardeep

2018-01-01

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC-TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role of cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. These results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides. PMID:29725619

Transmission electron microscopy of polyhydroxybutyrate-co-valerate (PHBV)/nanocrystalline cellulose (NCC) bio-nanocomposite prepared using cryo-ultramicrotomy

NASA Astrophysics Data System (ADS)

Ismarul, N. I.; Engku, A. H. E. U.; Siti, N. K.; Tay, K. Y.

2017-12-01

Environmental issues on disposal and end-of-life for product made from synthetic petroleum-derived polymers have gained increasing attention from materials scientist to search for new materials with similar physical and mechanical properties but environmental friendly in a way that they are renewable and biodegradable as well. This work is to study the effect of nanocrystalline cellulose in improving the thermal stability of polyhydroxybutyrate-co-valerate biopolymer for high temperature processing of packaging material. 10 % w/w PHBV-NCC bio-nanocomposite feedstock pellet prepared using RONDOL minilab compounder was used as the sample for the preparation of Transmission Electron Microscopy (TEM) sample. RMC Cryo-Ultramicrotomy equipment was used to prepare the ultra-thin slice of the bio-nanocomposite pellet under liquid nitrogen at - 60 °C. Diamond knife was used to slice off about 80-100 nm ultra-thin bio-nanocomposite films and was transferred into the lacey carbon film coated grid using cooled sugar solution. A few drops of phosphotungstic acid was used as negative stain to improve the contrast during the TEM analysis. HITACHI TEM systems was used to obtain the TEM micrograph of PHBV-NCC bio-nanocomposite using 80kV accelerating voltage. A well dispersed NCC in PHBV matrix, ranging from 5 to 25 nm in width was observed.

The role of electron irradiation history in liquid cell transmission electron microscopy

DOE PAGES

Moser, Trevor H.; Mehta, Hardeep; Park, Chiwoo; ...

2018-04-20

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC-TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role ofmore » cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. Lastly, these results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides.« less

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

Sharma, Rabindar K.; Reddy, G. B.

In this work, we have successfully developed plasma assisted paste sublimation route to deposit vertically aligned MoO{sub 3} nanoflakes (NFs) on nickel coated glass substrate in oxygen plasma ambience with the assistant of Ni thin layer as a catalyst. In our case, sublimation source (Mo strip surface) is resistively heated by flowing current across it. The structural, morphological, and optical properties of NFs have been investigated systematically using x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) with selected area electron diffraction (SAED), High resolution transmission electron microscopy (HRTEM), micro-Raman spectroscopy, and Photoluminescence (PL) spectroscopy. Studies reveal thatmore » the presence of oxygen plasma and the nickel thin layer are very essential for the growth of vertically aligned NFs. The observed results divulge that α-MoO{sub 3} NFs are deposited uniformly on large scale with very high aspect (height/thickness) ratio more than 30 and well aligned along [0 k 0] crystallographic direction where k is even (2, 4, 6). Raman spectrum shows a significant size effect on the vibrational property of MoO{sub 3} nanoflakes. The PL spectrum of MoO{sub 3} NFs was recorded at room temperature and four prominent peaks at 365 nm, 395 nm, 452 nm, and 465 nm corresponding to UV-visible region were observed. In this paper, a three step growth strategy for the formation of MoO{sub 3} NFs has been proposed in detail.« less

Growth characteristics of primary M7C3 carbide in hypereutectic Fe-Cr-C alloy.

PubMed

Liu, Sha; Zhou, Yefei; Xing, Xiaolei; Wang, Jibo; Ren, Xuejun; Yang, Qingxiang

2016-09-06

The microstructure of the hypereutectic Fe-Cr-C alloy is observed by optical microscopy (OM). The initial growth morphology, the crystallographic structure, the semi-molten morphology and the stacking faults of the primary M7C3 carbide are observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The in-suit growth process of the primary M7C3 carbide was observed by confocal laser microscope (CLM). It is found that the primary M7C3 carbide in hypereutectic Fe-Cr-C alloy is irregular polygonal shape with several hollows in the center and gaps on the edge. Some primary M7C3 carbides are formed by layers of shell or/and consist of multiple parts. In the initial growth period, the primary M7C3 carbide forms protrusion parallel to {} crystal planes. The extending and revolving protrusion forms the carbide shell. The electron backscattered diffraction (EBSD) maps show that the primary M7C3 carbide consists of multiple parts. The semi-molten M7C3 carbide contains unmelted shell and several small-scale carbides inside, which further proves that the primary M7C3 carbide is not an overall block. It is believed that the coalescence of the primary M7C3 carbides is ascribed to the growing condition of the protrusion and the gap filling process.

Microstructural characteristics and aging response of Zn-containing Al-Mg-Si-Cu alloy

NASA Astrophysics Data System (ADS)

Cai, Yuan-hua; Wang, Cong; Zhang, Ji-shan

2013-07-01

Al-Mg-Si-Cu alloys with and without Zn addition were fabricated by conventional ingot metallurgy method. The microstructures and properties were investigated using optical microscopy (OM), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), tensile test, hardness test, and electrical conductivity measurement. It is found that the as-cast Al-Mg-Si-Cu-Zn alloy is composed of coarse dendritic grains, long needle-like β/δ-AlFeSi white intermetallics, and Chinese script-like α-AlFeSi compounds. During high temperature homogenization treatment, only harmful needle-like β-AlFeSi phase undergoes fragmentation and spheroidizing at its tips, and the destructive needle-like δ-phase does not show any morphological and size changes. Phase transitions from β-AlFeSi to α-AlFeSi and from δ-AlFeSi to β-AlFeSi are also not found. Zn addition improves the aging hardening response during the former aging stage and postpones the peak-aged hardness to a long aging time. In T4 condition, Zn addition does not obviously increase the yield strength and decrease the elongation, but it markedly improves paint-bake hardening response during paint-bake cycle. The addition of 0.5wt% Zn can lead to an increment of 99 MPa in yield strength compared with the value of 69 MPa for the alloy without Zn after paint-bake cycle.

Growth characteristics of primary M7C3 carbide in hypereutectic Fe-Cr-C alloy

PubMed Central

Liu, Sha; Zhou, Yefei; Xing, Xiaolei; Wang, Jibo; Ren, Xuejun; Yang, Qingxiang

2016-01-01

The microstructure of the hypereutectic Fe-Cr-C alloy is observed by optical microscopy (OM). The initial growth morphology, the crystallographic structure, the semi-molten morphology and the stacking faults of the primary M7C3 carbide are observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The in-suit growth process of the primary M7C3 carbide was observed by confocal laser microscope (CLM). It is found that the primary M7C3 carbide in hypereutectic Fe-Cr-C alloy is irregular polygonal shape with several hollows in the center and gaps on the edge. Some primary M7C3 carbides are formed by layers of shell or/and consist of multiple parts. In the initial growth period, the primary M7C3 carbide forms protrusion parallel to {} crystal planes. The extending and revolving protrusion forms the carbide shell. The electron backscattered diffraction (EBSD) maps show that the primary M7C3 carbide consists of multiple parts. The semi-molten M7C3 carbide contains unmelted shell and several small-scale carbides inside, which further proves that the primary M7C3 carbide is not an overall block. It is believed that the coalescence of the primary M7C3 carbides is ascribed to the growing condition of the protrusion and the gap filling process. PMID:27596718

Non-Cytotoxic Quantum Dot–Chitosan Nanogel Biosensing Probe for Potential Cancer Targeting Agent

PubMed Central

Maxwell, Tyler; Banu, Tahmina; Price, Edward; Tharkur, Jeremy; Campos, Maria Gabriela Nogueira; Gesquiere, Andre; Santra, Swadeshmukul

2015-01-01

Quantum dot (Qdot) biosensors have consistently provided valuable information to researchers about cellular activity due to their unique fluorescent properties. Many of the most popularly used Qdots contain cadmium, posing the risk of toxicity that could negate their attractive optical properties. The design of a non-cytotoxic probe usually involves multiple components and a complex synthesis process. In this paper, the design and synthesis of a non-cytotoxic Qdot-chitosan nanogel composite using straight-forward cyanogen bromide (CNBr) coupling is reported. The probe was characterized by spectroscopy (UV-Vis, fluorescence), microscopy (Fluorescence, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Dynamic Light Scattering. This activatable (“OFF”/“ON”) probe contains a core–shell Qdot (CdS:Mn/ZnS) capped with dopamine, which acts as a fluorescence quencher and a model drug. Dopamine capped “OFF” Qdots can undergo ligand exchange with intercellular glutathione, which turns the Qdots “ON” to restore fluorescence. These Qdots were then coated with chitosan (natural biocompatible polymer) functionalized with folic acid (targeting motif) and Fluorescein Isothiocyanate (FITC; fluorescent dye). To demonstrate cancer cell targetability, the interaction of the probe with cells that express different folate receptor levels was analyzed, and the cytotoxicity of the probe was evaluated on these cells and was shown to be nontoxic even at concentrations as high as 100 mg/L. PMID:28347126

Ezrin enhances line tension along transcellular tunnel edges via NMIIa driven actomyosin cable formation

NASA Astrophysics Data System (ADS)

Stefani, Caroline; Gonzalez-Rodriguez, David; Senju, Yosuke; Doye, Anne; Efimova, Nadia; Janel, Sébastien; Lipuma, Justine; Tsai, Meng Chen; Hamaoui, Daniel; Maddugoda, Madhavi P.; Cochet-Escartin, Olivier; Prévost, Coline; Lafont, Frank; Svitkina, Tatyana; Lappalainen, Pekka; Bassereau, Patricia; Lemichez, Emmanuel

2017-06-01

Transendothelial cell macroaperture (TEM) tunnels control endothelium barrier function and are triggered by several toxins from pathogenic bacteria that provoke vascular leakage. Cellular dewetting theory predicted that a line tension of uncharacterized origin works at TEM boundaries to limit their widening. Here, by conducting high-resolution microscopy approaches we unveil the presence of an actomyosin cable encircling TEMs. We develop a theoretical cellular dewetting framework to interpret TEM physical parameters that are quantitatively determined by laser ablation experiments. This establishes the critical role of ezrin and non-muscle myosin II (NMII) in the progressive implementation of line tension. Mechanistically, fluorescence-recovery-after-photobleaching experiments point for the upstream role of ezrin in stabilizing actin filaments at the edges of TEMs, thereby favouring their crosslinking by NMIIa. Collectively, our findings ascribe to ezrin and NMIIa a critical function of enhancing line tension at the cell boundary surrounding the TEMs by promoting the formation of an actomyosin ring.

Ezrin enhances line tension along transcellular tunnel edges via NMIIa driven actomyosin cable formation

PubMed Central

Stefani, Caroline; Gonzalez-Rodriguez, David; Senju, Yosuke; Doye, Anne; Efimova, Nadia; Janel, Sébastien; Lipuma, Justine; Tsai, Meng Chen; Hamaoui, Daniel; Maddugoda, Madhavi P.; Cochet-Escartin, Olivier; Prévost, Coline; Lafont, Frank; Svitkina, Tatyana; Lappalainen, Pekka; Bassereau, Patricia; Lemichez, Emmanuel

2017-01-01

Transendothelial cell macroaperture (TEM) tunnels control endothelium barrier function and are triggered by several toxins from pathogenic bacteria that provoke vascular leakage. Cellular dewetting theory predicted that a line tension of uncharacterized origin works at TEM boundaries to limit their widening. Here, by conducting high-resolution microscopy approaches we unveil the presence of an actomyosin cable encircling TEMs. We develop a theoretical cellular dewetting framework to interpret TEM physical parameters that are quantitatively determined by laser ablation experiments. This establishes the critical role of ezrin and non-muscle myosin II (NMII) in the progressive implementation of line tension. Mechanistically, fluorescence-recovery-after-photobleaching experiments point for the upstream role of ezrin in stabilizing actin filaments at the edges of TEMs, thereby favouring their crosslinking by NMIIa. Collectively, our findings ascribe to ezrin and NMIIa a critical function of enhancing line tension at the cell boundary surrounding the TEMs by promoting the formation of an actomyosin ring. PMID:28643776

Ezrin enhances line tension along transcellular tunnel edges via NMIIa driven actomyosin cable formation.

PubMed

Stefani, Caroline; Gonzalez-Rodriguez, David; Senju, Yosuke; Doye, Anne; Efimova, Nadia; Janel, Sébastien; Lipuma, Justine; Tsai, Meng Chen; Hamaoui, Daniel; Maddugoda, Madhavi P; Cochet-Escartin, Olivier; Prévost, Coline; Lafont, Frank; Svitkina, Tatyana; Lappalainen, Pekka; Bassereau, Patricia; Lemichez, Emmanuel

2017-06-23

Transendothelial cell macroaperture (TEM) tunnels control endothelium barrier function and are triggered by several toxins from pathogenic bacteria that provoke vascular leakage. Cellular dewetting theory predicted that a line tension of uncharacterized origin works at TEM boundaries to limit their widening. Here, by conducting high-resolution microscopy approaches we unveil the presence of an actomyosin cable encircling TEMs. We develop a theoretical cellular dewetting framework to interpret TEM physical parameters that are quantitatively determined by laser ablation experiments. This establishes the critical role of ezrin and non-muscle myosin II (NMII) in the progressive implementation of line tension. Mechanistically, fluorescence-recovery-after-photobleaching experiments point for the upstream role of ezrin in stabilizing actin filaments at the edges of TEMs, thereby favouring their crosslinking by NMIIa. Collectively, our findings ascribe to ezrin and NMIIa a critical function of enhancing line tension at the cell boundary surrounding the TEMs by promoting the formation of an actomyosin ring.

Detecting single-electron events in TEM using low-cost electronics and a silicon strip sensor.

PubMed

Gontard, Lionel C; Moldovan, Grigore; Carmona-Galán, Ricardo; Lin, Chao; Kirkland, Angus I

2014-04-01

There is great interest in developing novel position-sensitive direct detectors for transmission electron microscopy (TEM) that do not rely in the conversion of electrons into photons. Direct imaging improves contrast and efficiency and allows the operation of the microscope at lower energies and at lower doses without loss in resolution, which is especially important for studying soft materials and biological samples. We investigate the feasibility of employing a silicon strip detector as an imaging detector for TEM. This device, routinely used in high-energy particle physics, can detect small variations in electric current associated with the impact of a single charged particle. The main advantages of using this type of sensor for direct imaging in TEM are its intrinsic radiation hardness and large detection area. Here, we detail design, simulation, fabrication and tests in a TEM of the front-end electronics developed using low-cost discrete components and discuss the limitations and applications of this technology for TEM.

Direct observation of a stacking fault in Si(1 - x)Ge(x) semiconductors by spherical aberration-corrected TEM and conventional ADF-STEM.

PubMed

Yamasaki, Jun; Kawai, Tomoyuki; Tanaka, Nobuo

2004-01-01

Spherical aberration (C(S))-corrected transmission electron microscopy (TEM) and annular dark-field scanning TEM (ADF-STEM) are applied to high-resolution observation of stacking faults in Si(1 - x)Ge(x) alloy films prepared on a Si(100) buffer layer by the chemical vapor deposition method. Both of the images clarify the individual nature of stacking faults from their directly interpretable image contrast and also by using image simulation in the case of the C(S)-corrected TEM. Positions of the atomic columns obtained in the ADF-STEM images almost agree with a projection of the theoretical model studied by Chou et al. (Phys. Rev. B 32(1985): 7979). Comparison between the C(S)-corrected TEM and ADF-STEM images shows that their resolution is at a similar level, but directly interpretable image contrast is obtained in ultrathin samples for C(S)-corrected TEM and in slightly thicker samples for ADF-STEM.

Field emission scanning electron microscopy (FE-SEM) as an approach for nanoparticle detection inside cells.

PubMed

Havrdova, M; Polakova, K; Skopalik, J; Vujtek, M; Mokdad, A; Homolkova, M; Tucek, J; Nebesarova, J; Zboril, R

2014-12-01

When developing new nanoparticles for bio-applications, it is important to fully characterize the nanoparticle's behavior in biological systems. The most common techniques employed for mapping nanoparticles inside cells include transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). These techniques entail passing an electron beam through a thin specimen. STEM or TEM imaging is often used for the detection of nanoparticles inside cellular organelles. However, lengthy sample preparation is required (i.e., fixation, dehydration, drying, resin embedding, and cutting). In the present work, a new matrix (FTO glass) for biological samples was used and characterized by field emission scanning electron microscopy (FE-SEM) to generate images comparable to those obtained by TEM. Using FE-SEM, nanoparticle images were acquired inside endo/lysosomes without disruption of the cellular shape. Furthermore, the initial steps of nanoparticle incorporation into the cells were captured. In addition, the conductive FTO glass endowed the sample with high stability under the required accelerating voltage. Owing to these features of the sample, further analyses could be performed (material contrast and energy-dispersive X-ray spectroscopy (EDS)), which confirmed the presence of nanoparticles inside the cells. The results showed that FE-SEM can enable detailed characterization of nanoparticles in endosomes without the need for contrast staining or metal coating of the sample. Images showing the intracellular distribution of nanoparticles together with cellular morphology can give important information on the biocompatibility and demonstrate the potential of nanoparticle utilization in medicine. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

PubMed

Chaturvedi, Archana; Bajpai, Anil K; Bajpai, Jaya; K Singh, Sunil

2016-08-01

In this investigation cryogels composed of poly (vinyl alcohol) (PVA) were prepared by repeated freeze thaw method followed by in situ precipitation of zinc oxide nanoparticles within the cryogel networks. Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD), Energy dispersive X-ray spectroscopy (EDX) were used to characterize the nanocomposites. The morphologies of native PVA cryogels and PVA cryogel-ZnO nanocomposites were observed by scanning electron microscopy (SEM), transmission electron microscopy (TEM) techniques. The SEM analysis suggested that cryogels show a well-defined porous morphology whereas TEM micrographs revealed the presence of nearly spherical and well separated zinc oxide nanoparticles with diameter<100nm. XRD results showed all relevant Bragg's reflections for crystal structure of zinc oxide nanoparticles. Thermo gravimetric-differential thermal analysis (TG-DTA) was conducted to evaluate thermal stability of the nanocomposites. Mechanical properties of nanocomposites were determined in terms of tensile strength and percent elongation. Biocompatible nature was ascertained by anti-haemolytic activity, bovine serum albumin (blood protein) adsorption and in vitro cytotoxicity tests. The prepared nanocomposites were also investigated for swelling and deswelling behaviours. The results revealed that both the swelling and deswelling process depend on the chemical composition of the nanocomposites, number of freeze-thaw cycles, pH and temperature of the swelling medium. The developed biocompatible PVA cryogel-ZnO nanocomposites were also tested for antibacterial activities against both Gram-negative and Gram-positive bacteria. Copyright © 2016 Elsevier B.V. All rights reserved.

An Integrated Micro- and Macroarchitectural Analysis of the Drosophila Brain by Computer-Assisted Serial Section Electron Microscopy

PubMed Central

Cardona, Albert; Saalfeld, Stephan; Preibisch, Stephan; Schmid, Benjamin; Cheng, Anchi; Pulokas, Jim; Tomancak, Pavel; Hartenstein, Volker

2010-01-01

The analysis of microcircuitry (the connectivity at the level of individual neuronal processes and synapses), which is indispensable for our understanding of brain function, is based on serial transmission electron microscopy (TEM) or one of its modern variants. Due to technical limitations, most previous studies that used serial TEM recorded relatively small stacks of individual neurons. As a result, our knowledge of microcircuitry in any nervous system is very limited. We applied the software package TrakEM2 to reconstruct neuronal microcircuitry from TEM sections of a small brain, the early larval brain of Drosophila melanogaster. TrakEM2 enables us to embed the analysis of the TEM image volumes at the microcircuit level into a light microscopically derived neuro-anatomical framework, by registering confocal stacks containing sparsely labeled neural structures with the TEM image volume. We imaged two sets of serial TEM sections of the Drosophila first instar larval brain neuropile and one ventral nerve cord segment, and here report our first results pertaining to Drosophila brain microcircuitry. Terminal neurites fall into a small number of generic classes termed globular, varicose, axiform, and dendritiform. Globular and varicose neurites have large diameter segments that carry almost exclusively presynaptic sites. Dendritiform neurites are thin, highly branched processes that are almost exclusively postsynaptic. Due to the high branching density of dendritiform fibers and the fact that synapses are polyadic, neurites are highly interconnected even within small neuropile volumes. We describe the network motifs most frequently encountered in the Drosophila neuropile. Our study introduces an approach towards a comprehensive anatomical reconstruction of neuronal microcircuitry and delivers microcircuitry comparisons between vertebrate and insect neuropile. PMID:20957184

Pulsed Laser Ablation-Induced Green Synthesis of TiO2 Nanoparticles and Application of Novel Small Angle X-Ray Scattering Technique for Nanoparticle Size and Size Distribution Analysis.

PubMed

Singh, Amandeep; Vihinen, Jorma; Frankberg, Erkka; Hyvärinen, Leo; Honkanen, Mari; Levänen, Erkki

2016-12-01

This paper aims to introduce small angle X-ray scattering (SAXS) as a promising technique for measuring size and size distribution of TiO 2 nanoparticles. In this manuscript, pulsed laser ablation in liquids (PLAL) has been demonstrated as a quick and simple technique for synthesizing TiO 2 nanoparticles directly into deionized water as a suspension from titanium targets. Spherical TiO 2 nanoparticles with diameters in the range 4-35 nm were observed with transmission electron microscopy (TEM). X-ray diffraction (XRD) showed highly crystalline nanoparticles that comprised of two main photoactive phases of TiO 2 : anatase and rutile. However, presence of minor amounts of brookite was also reported. The traditional methods for nanoparticle size and size distribution analysis such as electron microscopy-based methods are time-consuming. In this study, we have proposed and validated SAXS as a promising method for characterization of laser-ablated TiO 2 nanoparticles for their size and size distribution by comparing SAXS- and TEM-measured nanoparticle size and size distribution. SAXS- and TEM-measured size distributions closely followed each other for each sample, and size distributions in both showed maxima at the same nanoparticle size. The SAXS-measured nanoparticle diameters were slightly larger than the respective diameters measured by TEM. This was because SAXS measures an agglomerate consisting of several particles as one big particle which slightly increased the mean diameter. TEM- and SAXS-measured mean diameters when plotted together showed similar trend in the variation in the size as the laser power was changed which along with extremely similar size distributions for TEM and SAXS validated the application of SAXS for size distribution measurement of the synthesized TiO 2 nanoparticles.

Direct observation of morphological evolution of a catalyst during carbon nanotube forest growth: new insights into growth and growth termination

NASA Astrophysics Data System (ADS)

Jeong, Seojeong; Lee, Jaegeun; Kim, Hwan-Chul; Hwang, Jun Yeon; Ku, Bon-Cheol; Zakharov, Dmitri N.; Maruyama, Benji; Stach, Eric A.; Kim, Seung Min

2016-01-01

In this study, we develop a new methodology for transmission electron microscopy (TEM) analysis that enables us to directly investigate the interface between carbon nanotube (CNT) arrays and the catalyst and support layers for CNT forest growth without any damage induced by a post-growth TEM sample preparation. Using this methodology, we perform in situ and ex situ TEM investigations on the evolution of the morphology of the catalyst particles and observe the catalyst particles to climb up through CNT arrays during CNT forest growth. We speculate that the lifted catalysts significantly affect the growth and growth termination of CNT forests along with Ostwald ripening and sub-surface diffusion. Thus, we propose a modified growth termination model which better explains various phenomena related to the growth and growth termination of CNT forests.In this study, we develop a new methodology for transmission electron microscopy (TEM) analysis that enables us to directly investigate the interface between carbon nanotube (CNT) arrays and the catalyst and support layers for CNT forest growth without any damage induced by a post-growth TEM sample preparation. Using this methodology, we perform in situ and ex situ TEM investigations on the evolution of the morphology of the catalyst particles and observe the catalyst particles to climb up through CNT arrays during CNT forest growth. We speculate that the lifted catalysts significantly affect the growth and growth termination of CNT forests along with Ostwald ripening and sub-surface diffusion. Thus, we propose a modified growth termination model which better explains various phenomena related to the growth and growth termination of CNT forests. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr05547d

Cryo-electron microscopy and cryo-electron tomography of nanoparticles.

PubMed

Stewart, Phoebe L

2017-03-01

Cryo-transmission electron microscopy (cryo-TEM or cryo-EM) and cryo-electron tomography (cryo-ET) offer robust and powerful ways to visualize nanoparticles. These techniques involve imaging of the sample in a frozen-hydrated state, allowing visualization of nanoparticles essentially as they exist in solution. Cryo-TEM grid preparation can be performed with the sample in aqueous solvents or in various organic and ionic solvents. Two-dimensional (2D) cryo-TEM provides a direct way to visualize the polydispersity within a nanoparticle preparation. Fourier transforms of cryo-TEM images can confirm the structural periodicity within a sample. While measurement of specimen parameters can be performed with 2D TEM images, determination of a three-dimensional (3D) structure often facilitates more spatially accurate quantization. 3D structures can be determined in one of two ways. If the nanoparticle has a homogeneous structure, then 2D projection images of different particles can be averaged using a computational process referred to as single particle reconstruction. Alternatively, if the nanoparticle has a heterogeneous structure, then a structure can be generated by cryo-ET. This involves collecting a tilt-series of 2D projection images for a defined region of the grid, which can be used to generate a 3D tomogram. Occasionally it is advantageous to calculate both a single particle reconstruction, to reveal the regular portions of a nanoparticle structure, and a cryo-electron tomogram, to reveal the irregular features. A sampling of 2D cryo-TEM images and 3D structures are presented for protein based, DNA based, lipid based, and polymer based nanoparticles. WIREs Nanomed Nanobiotechnol 2017, 9:e1417. doi: 10.1002/wnan.1417 For further resources related to this article, please visit the WIREs website. © 2016 Wiley Periodicals, Inc.

A facile method for synthesis of graphene-coated hexagonal ZnO photocatalyst with enhanced photodegradation activity

NASA Astrophysics Data System (ADS)

Zhang, Yunlong; Zhang, Yuzhi

2017-12-01

A kind of hexagonal ZnO (HZO) was synthesized in N-methyl-2-pyrrolidone (NMP)/H2O mixed solvent for a high exposure of polar ±(0001) facets to get a high-efficiency photocatalyst. The amine-functionalized HZO particles were coated with graphene oxide (GO) by electrostatic force-induced self-assemby and thermal reduction to form HZO@Gr core/shell structure. The as-prepared HZO and HZO@Gr were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and UV-visible diffuse reflectance spectroscopy (UV-vis/DRS). The results indicate that the graphene on HZO@Gr remains high quality and the optical properties of the composite change a lot with sunlight absorption improving, bandgap and photoluminescence (PL) intensity decreasing. The obtained HZO photocatalyst shows good photocatalytic activity for methylene blue (MB) under UV-visible irradiation. Furthermore, the HZO@Gr photocatalyst exhibits the best photodegradation rate of MB reaching up to 98.2% within 50 minutes. The graphene-coated HZO structure could offer new directions which would further extend the scope for synthesis of various ZnO/graphene composites with improved properties useful for various applications.

Explosive Shock-Wave Consolidation of Aluminum Powder/Carbon Nanotube Aggregate Mixtures: Optical and Electron Metallography

NASA Astrophysics Data System (ADS)

Salas, W.; Alba-Baena, N. G.; Murr, L. E.

2007-12-01

The formation of conventional metal-matrix composites reinforced with carbon nanotubes (CNTs) has proven difficult because of the agglomeration and inability of CNTs to disperse. We have explored the explosive consolidation of 150- μm aluminum powder/multiwalled carbon nanotube (MWCNT) aggregates (including multiconcentric fullerenes) at volume percentages of 2 and 5 pct. These consolidated mixtures formed two-phase, monolithic systems (TPSs) with the MWCNT aggregate material spreading along the Al grains and forming carbon phases mainly at the Al particle triple points. The Al powder particle (or grain) hardness increased from HRE 22 to HRE 40 for the consolidated Al, while the two-phase system hardness dropped from HRE 40 to HRE 39 and 33, respectively, for 2 and 5 vol pct MWCNT aggregate additions. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) observations illustrate a laminate-like structure of the consolidated MWCNT aggregate material, which is easily delaminated, causing intergranular (Al) failure. The Al grains exhibited a shock-induced dislocation substructure (0.5 to 3 μm) and recrystallized subgrains, which increased the individual particle/grain Vickers hardness from 24 to 43 HV.

Switchable nanoassembly from an azobenzene-containing dye.

PubMed

Wang, Jing; Ha, Chang-Sik

2011-07-01

In this work, we investigated optical properties and the morphology of the amphiphilic azobenzene dye 1 containing hydroxyl azobenzene and C10 alkyl chains. Since the hydroxyl group on 1 has a pKa of 9.38, the deprotonation of the hydroxyl group occurs at pH > pKa (9.38) and thus the 1 nanoparticles are negatively charged. The deprotonated hydroxyl group is hydrophilic relative to the long alkyl chain that is hydrophobic, while the hydrophobic and hydrophilic parts are connected by covalent bonds. When such an azobenzene molecule 1 with both hydrophobic and hydrophilic groups exists in solution, "self-aggregation" may occur due to the hydrophobic interaction between the long alkyl chains. The scattered morphology at pH 7.0 (neutral state) and the aggregated morphology at pH 10.5 (anionic state) of 1 were demostrated by transmission electron microscopy (TEM) and atomic force microscopy (AFM) images. Formation of supramolecular aggregation-induced vesicular-like structures are highly interesting due to the ability to respond to external triggers, pH. The pH value can be reversed by adding acid or base to the system, that is, switching the aggregation "on" and "off" can be repeated.

Electrochemical synthesis of MoS2 quantum dots embedded nanostructured porous silicon with enhanced electroluminescence property

NASA Astrophysics Data System (ADS)

Shrivastava, Megha; Kumari, Reeta; Parra, Mohammad Ramzan; Pandey, Padmini; Siddiqui, Hafsa; Haque, Fozia Z.

2017-11-01

In this report we present the successful enhancement in electroluminescence (EL) in nanostructured n-type porous silicon (PS) with an idea of embedding luminophorous Molybdenum disulfide (MoS2) quantum dots (QD's). Electrochemical anodization technique was used for the formation of PS surface and MoS2 QD's were prepared using the electrochemical route. Spin coating technique was employed for the proper incorporation of MoS2 QD's within the PS nanostructures. The crystallographic analysis was performed using X-ray diffraction (XRD), Raman and Fourier transform infrared (FT-IR) spectroscopy techniques. However, surface morphology was determined using Transmission electron microscopy (TEM) and Atomic force microscopy (AFM). The optical measurements were performed on photoluminescence (PL) spectrophotometer; additionally for electroluminescence (EL) study special arrangement of instrumental setup was made at laboratory level which provides novelty to this work. A diode prototype was made comprising Ag/MoS2:PS/Silicon/Ag for EL study. The MoS2:PS shows a remarkable concentration dependent enhancement in PL as well as in EL intensities, which paves a way to better utilize this strategy in optoelectronic device applications.

Preparation and characterization of nanostructured Pt/TiO2 thin films treated using electron beam.

PubMed

Shin, Joong-Hyeok; Woo, Hee-Gweon; Kim, Bo-Hye; Lee, Byung Cheol; Jun, Jin

2010-05-01

Pt nanoparticle-doped titanium dioxide (Pt/TiO2) thin films were prepared on a silicon wafer substrate by sol-gel spin coating process. The prepared thin films were treated with electron beam (EB at 1.1 MeV, 100, 200, 300 kGy) at air atmosphere. The effect of EB-irradiation on the composition of the treated thin films, optical properties and morphology of thin films were investigated by various analytical techniques such as X-ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The crystal structure of the TiO2 layer was found to be an anatase phase and the size of TiO2 particles was determined to be about 13 nm. Pt nanoparticles with diameter of 5 nm were observed on surface of the films. A new layer (presumed to be Pt-Ti complex and/or PtO2 compound) was created in the Pt/TiO2 thin film treated with EB (300 kGy). The transmittance of thin film decreased with EB treatment whereas the refractive index increased.

Fabrication of CaFe2O4 nanofibers via electrospinning method with enhanced visible light photocatalytic activity

NASA Astrophysics Data System (ADS)

Wang, Jianmin; Wang, Yunan; Liu, Yinglei; Li, Song; Cao, Feng; Qin, Gaowu

CaFe2O4 nanofibers with diameters of about 130nm have been fabricated via a facile electrospinning method. The structures, morphologies and optical properties of the obtained CaF2O4 nanofibers have been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and UV-Visible UV-Vis diffuse reflectance spectrum. The photocatalytic activities of the CaFe2O4 nanofibers are evaluated by the photo-degradation of Methyl orange (MO). The results show that the CaFe2O4 nanofibers (72%) exhibit much higher photocatalytic performance than the CaFe2O4 powders (27%) prepared by conventional method under visible light irradiation. The enhanced photocatalytic performance of CaFe2O4 nanofibers could be attributed to the large surface area, high photogenerated charge carriers density and low charge transfer resistance, as revealed by photoelectrochemical measurement. And fundamentally, it could be attributed to the decreased particle size and the fibrous nanostructure. This work not only provides an efficient way to improve the photocatalytic activity of CaFe2O4, but also provides a new method for preparing materials with nanofibrous structure.

Effects of periplocoside X on midgut cells and digestive enzymes activity of the soldiers of red imported fire ant.

PubMed

Li, Yan; Zeng, Xin-Nian

2013-07-01

The pathological effects of ingested periplocoside X, an insecticidal component isolated from the root of Periploca sepium Bunge, on the midgut epithelial cells of the soldiers of red imported fire ant were studied and the symptom was described. The results showed that periplocoside X could induce a severe, time-dependent cytotoxicity in the midgut epithelial cells. An optical microscopy showed that epithelial cells swelled firstly and then lysed. Transmission electron microscopy (TEM) showed that numerous swollen lysosomes were appeared, microvilli were disrupted and sloughed off, and the numbers of the rough endoplasmic reticulum and the mitochondria decreased sharply in earlier stage. Numerous vacuoles were observed in the later stage. Finally, periplocoside X resulted in cell death by cytolysis. Assay of main three digestive enzymes activity indicated that amylase activity was significantly inhibited, but no significant changes were seen for lipase activity and total protease activity. So it is suggested that periplocoside X induced mainly to organic damage of midgut epithelium cells of insect. In all, insect midgut is one of targets for periplocoside X. Copyright © 2013 Elsevier Inc. All rights reserved.

Creep fatigue life prediction for engine hot section materials (isotropic)

NASA Technical Reports Server (NTRS)

Nelson, R. S.; Levan, G. W.; Harvey, P. R.

1992-01-01

This Final Report covers the activities completed under the optional program of the NASA HOST Contract, NAS3-23288. The initial effort of the optional program was report-in NASA CR189221, which consisted of high temperature strain controlled fatigue tests to study the effects of thermomechanical fatigue, multiaxial loading, reactive environments, and imposed stresses. The baseline alloy used in the tests included B1900+Hf (with or without coating) and wrought INCO 718. Tests conducted on B1900+Hf included environmental tests using various atmospheres (75 psig oxygen, purified argon, or block exposures) and specimen tests of wrought INCO 718 included tensile, creep, stress rupture, TMF, multiaxial, and mean stress tests. Results of these testings were used to calibrate a CDA model for INCO 718 alloy and to develop modifications or corrections to the CDA model to handle additional failure mechanisms. The Socie parameter was found to provide the best correlation for INCO multiaxial loading. Microstructural evaluations consisting of optical, Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM) techniques, and surface replication techniques to determine crack initiation lives provided data which were used to develop life prediction models.

Non-covalent attachment of silver nanoclusters onto single-walled carbon nanotubes with human serum albumin as linking molecule

NASA Astrophysics Data System (ADS)

Rodríguez-Galván, Andrés; Heredia, Alejandro; Amelines-Sarria, Oscar; Rivera, Margarita; Medina, Luis A.; Basiuk, Vladimir A.

2015-03-01

The attachment of silver nanoclusters (AgNCs) onto single-walled carbon nanotubes (SWNTs) for the formation of integrated fluorescence sites has attracted much attention due their potential applications as biological probes and nanovectors in theragnosis. Here, we report the preparation through assembly of fluorescent quasi 1-D nanomaterial based on SWNTs and silver nanoclusters (AgNCs) non-covalently attached to human serum albumin as biological linker. The fluorescent SWNT-AgNCs-HSA conjugates were characterized by atomic force microscopy, high-resolution transmission electron microscopy (HRTEM), high angle annular dark field scanning TEM (HAADF-STEM), fluorescent and UV-vis spectroscopy. The above techniques confirmed that AgNCs were non-covalently attached onto the external surface of SWNTs. In addition, it was observed that the modification did not affect the optical properties of the synthesized AgNCs since the absorption spectra and fluorescence under UV irradiation (λ = 365 nm) remain the same. The effect of the functionalized systems was tested on mammal red blood cells (RBCs) and it was found that their structural integrity was compromised by the conjugates, limiting their biological and medical applications.

Dispersion of single-wall carbon nanotubes with supramolecular Congo red - properties of the complexes and mechanism of the interaction.

PubMed

Jagusiak, Anna; Piekarska, Barbara; Pańczyk, Tomasz; Jemioła-Rzemińska, Małgorzata; Bielańska, Elżbieta; Stopa, Barbara; Zemanek, Grzegorz; Rybarska, Janina; Roterman, Irena; Konieczny, Leszek

2017-01-01

A method of dispersion of single-wall carbon nanotubes (SWNTs) in aqueous media using Congo red (CR) is proposed. Nanotubes covered with CR constitute the high capacity system that provides the possibility of binding and targeted delivery of different drugs, which can intercalate into the supramolecular, ribbon-like CR structure. The study revealed the presence of strong interactions between CR and the surface of SWNTs. The aim of the study was to explain the mechanism of this interaction. The interaction of CR and carbon nanotubes was studied using spectral analysis of the SWNT-CR complex, dynamic light scattering (DLS), differential scanning calorimetry (DSC) and microscopic methods: atomic force microscopy (AFM), transmission (TEM), scanning (SEM) and optical microscopy. The results indicate that the binding of supramolecular CR structures to the surface of the nanotubes is based on the "face to face stacking". CR molecules attached directly to the surface of the nanotubes can bind further, parallel-oriented molecules and form supramolecular and protruding structures. This explains the high CR binding capacity of carbon nanotubes. The presented system - containing SWNTs covered with CR - offers a wide range of biomedical applications.

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

Silicon nitride grids are compatible with correlative negative staining electron microscopy and tip-enhanced Raman spectroscopy for use in the detection of micro-organisms.

PubMed

Lausch, V; Hermann, P; Laue, M; Bannert, N

2014-06-01

Successive application of negative staining transmission electron microscopy (TEM) and tip-enhanced Raman spectroscopy (TERS) is a new correlative approach that could be used to rapidly and specifically detect and identify single pathogens including bioterrorism-relevant viruses in complex samples. Our objective is to evaluate the TERS-compatibility of commonly used electron microscopy (EM) grids (sample supports), chemicals and negative staining techniques and, if required, to devise appropriate alternatives. While phosphortungstic acid (PTA) is suitable as a heavy metal stain, uranyl acetate, paraformaldehyde in HEPES buffer and alcian blue are unsuitable due to their relatively high Raman scattering. Moreover, the low thermal stability of the carbon-coated pioloform film on copper grids (pioloform grids) negates their utilization. The silicon in the cantilever of the silver-coated atomic force microscope tip used to record TERS spectra suggested that Si-based grids might be employed as alternatives. From all evaluated Si-based TEM grids, the silicon nitride (SiN) grid was found to be best suited, with almost no background Raman signals in the relevant spectral range, a low surface roughness and good particle adhesion properties that could be further improved by glow discharge. Charged SiN grids have excellent particle adhesion properties. The use of these grids in combination with PTA for contrast in the TEM is suitable for subsequent analysis by TERS. The study reports fundamental modifications and optimizations of the negative staining EM method that allows a combination with near-field Raman spectroscopy to acquire a spectroscopic signature from nanoscale biological structures. This should facilitate a more precise diagnosis of single viral particles and other micro-organisms previously localized and visualized in the TEM. © 2014 The Society for Applied Microbiology.