Optical and vibrational properties of PbSe nanoparticles synthesized in clinoptilolite

NASA Astrophysics Data System (ADS)

Flores-Valenzuela, J.; Cortez-Valadez, M.; Ramírez-Bon, R.; Arizpe-Chavez, H.; Román-Zamorano, J. F.; Flores-Acosta, M.

2015-08-01

In this work, the optical and vibrational properties of composites based on PbSe semiconductor immersed in a zeolite matrix are reported. The natural zeolite, (clinoptilolite) was used as the host material of PbSe nanoparticles. The method for obtaining these particles is also reported here, which is based on ion exchange processes inside the natural zeolite in alkaline aqueous solution that contains the precursor ions Pb2+ and Se2-. The process of synthesis was conducted temperature, volume, concentration and reaction time of the precursors. The samples were studied by powder X-ray diffraction, TEM (transmission electron microscopy), diffuse reflectance and Raman spectroscopy. The experimental results demonstrate that with this method, the particles with nanometric PbSe sizes were synthesized in the zeolite matrix. Vibrational Raman bands at low wave numbers were detected in these particles by the presence of a shoulder located at 135 cm-1 and a band at around 149 cm-1. The vibrational calculations for small clusters of PbSe at LSDA (Local Spin Density Approximation) level combined with the basis set LANDL2DZ (Los Alamos National Laboratory 2 double ζ), were considered through DFT (Density Functionl Theory). The "breathing" Raman modes located at 119-152 cm-1 were detected for this level of theory.

Investigation of structural, optical, magnetic and electrical properties of tungsten doped Nisbnd Zn nano-ferrites

NASA Astrophysics Data System (ADS)

Pathania, Abhilash; Bhardwaj, Sanjay; Thakur, Shyam Singh; Mattei, Jean-Luc; Queffelec, Patrick; Panina, Larissa V.; Thakur, Preeti; Thakur, Atul

2018-02-01

Tungsten substituted nickel-zinc ferrite nanoparticles with chemical composition of Ni0.5Zn0.5WxFe2-xO4 (x = 0.0, 0.2, 0.4, 0.6, 0.8 & 1.0) were successfully synthesized by a chemical co-precipitation method. The prepared ferrites were pre sintered at 850 °C and then annealed at 1000 °C in a muffle furnace for 3 h each. This sintered powder was inspected by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and vibrating sample magnetometer (VSM) to study the structural, optical, and magnetic properties. XRD measurement revealed the phase purity of all the nanoferrite samples with cubic spinel structure. The estimated crystallite size by X-ray line broadening is found in the range of 49-62 nm. FTIR spectra of all the samples have observed two prominent absorption bands in the range 400-700 cm-1 arising due to tetrahedral and octahedral stretching vibrations. Vibrating sample magnetometer experiments showed that the saturation magnetizations (MS) decreased with an increase in non-magnetic tungsten ion doping. The electrical resistivity of tungsten doped Nisbnd Zn nano ferrites were examined extensively as a function of temperature. With an increase in tungsten composition, resistivity was found to decrease from 2.2 × 105 Ω cm to 1.9 × 105 Ω cm which indicates the semiconducting behavior of the ferrite samples. The activation energy also decreased from 0.0264 to 0.0221 eV at x = 0.0 to x = 1.0. These low coercive field tungsten doped Nisbnd Zn ferrites are suitable for hyperthermia and sensor applications. These observations are explained in detail on the basis of various models and theories.

Synthesis, characterization, bioactivity and antibacterial studies of silver doped calcium borosilicate glass-ceramics

NASA Astrophysics Data System (ADS)

Kumar, Alesh; Mariappan, C. R.

2018-04-01

Bioactive glass-ceramics 45.8 mol% SiO- 45.8 CaO - 8.4 B2O3 doped with Ag2O were synthesized by sol-gel method. The glass-ceramic nature of samples was confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM) analysis. Fourier transform infrared (FT-IR) spectra reveal the probable stretching and bending vibration modes of silicate and borate groups. UV-Visible spectra reveal the presence of Ag+ ions and metallic Ag in the glass matrix for Ag2O doped ceramic sample. Biocompatibility of the glass nature of samples was studied by soaking of samples in Dulbecco's Modified Eagle's Medium (DMEM) with subsequent XRD studies. It was found that bone-like apatite formation on the glasses after soaked in DMEM. Antibacterial studies of glass ceramics powder against gram positive and negative microorganisms were carried out.

FC and ZFC magnetic properties of ferro-spinels (MFe2O4) prepared by solution-combustion method

NASA Astrophysics Data System (ADS)

Aravind, G.; Kumar, R. Vijaya; Nathaniyal, V.; Rambabu, T.; Ravinder, D.

2017-07-01

Magnetic ferro-spinels MFe2O4 (M= Co and Ni) prepared by citrate-gel solution combustion method using metal nitrates with low sintering temperature (500°C). From the XRD and TEM studies confirm that a nano crystalline nature of the prepared samples. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetic studies of the prepared ferro-spinels are measured by using vibrating sample magnetometer (VSM). The resultant magnetization of the prepared samples as a function of an applied magnetic field 10 T was measured at two different temperatures 5 K and 310 K. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetization measurements under an applied field of 100 Oe and 1000 Oe in the temperature range of 5-375 K were carried out, which shows the blocking temperature of these two samples at around 350 K.

Structural, microstructural and vibrational analyses of the monoclinic tungstate BiLuWO6

NASA Astrophysics Data System (ADS)

Ait Ahsaine, H.; Taoufyq, A.; Patout, L.; Ezahri, M.; Benlhachemi, A.; Bakiz, B.; Villain, S.; Guinneton, F.; Gavarri, J.-R.

2014-10-01

The bismuth lutetium tungstate phase BiLuWO6 has been prepared using a solid state route with stoichiometric mixtures of oxide precursors. The obtained polycrystalline phase has been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy. In the first step, the crystal structure has been refined using Rietveld method: the crystal cell was resolved using monoclinic system (parameters a, b, c, β) with space group A2/m. SEM images showed the presence of large crystallites with a constant local nominal composition (BiLuW). TEM analyses showed that the actual local structure could be better represented by a superlattice (a, 2b, c, β) associated with space groups P2 or P2/m. The Raman spectroscopy showed the presence of vibrational bands similar to those observed in the compounds BiREWO6 with RE=Y, Gd, Nd. However, these vibrational bands were characterized by large full width at half maximum, probably resulting from the long range Bi/Lu disorder and local WO6 octahedron distortions in the structure.

Incredible antibacterial activity of noble metal functionalized magnetic core-zeolitic shell nanostructures.

PubMed

Padervand, M; Janatrostami, S; Karanji, A Kiani; Gholami, M R

2014-02-01

Functionalized magnetic core-zeolitic shell nanostructures were prepared by hydrothermal and coprecipitation methods. The products were characterized by Vibrating Sample Magnetometer (VSM), X-ray powder diffraction (XRD), Fourier Transform Infrared (FTIR) spectra, nitrogen adsorption-desorption isotherms, and Transmission Electron Microscopy (TEM). The growth of mordenite nanoparticles on the surface of silica coated nickel ferrite nanoparticles in the presence of organic templates was also confirmed. Antibacterial activity of the prepared nanostructures was investigated by the inactivation of Escherichia coli as a gram negative bacterium. A new mechanism was proposed for inactivation of E. coli over the prepared samples. In addition, the Minimum Inhibitory Concentration (MIC) and reuse ability were studied. TEM images of the destroyed cell wall after the treatment time were performed to illustrate the inactivation mechanism. According to the experimental results, the core-shell nanostructures which were modified by organic agents and then functionalized with noble metal nanoparticles were the most active. The interaction of the noble metals with the organic components on the surface of nanostructures was studied theoretically and the obtained results were used to interpret the experimental results. © 2013. Published by Elsevier B.V. All rights reserved.

Combinatorial investigation of Fe–B thin-film nanocomposites

PubMed Central

Brunken, Hayo; Grochla, Dario; Savan, Alan; Kieschnick, Michael; Meijer, Jan D; Ludwig, Alfred

2011-01-01

Combinatorial magnetron sputter deposition from elemental targets was used to create Fe–B composition spread type thin film materials libraries on thermally oxidized 4-in. Si wafers. The materials libraries consisting of wedge-type multilayer thin films were annealed at 500 or 700 °C to transform the multilayers into multiphase alloys. The libraries were characterized by nuclear reaction analysis, Rutherford backscattering, nanoindentation, vibrating sample magnetometry, x-ray diffraction (XRD) and transmission electron microscopy (TEM). Young's modulus and hardness values were related to the annealing parameters, structure and composition of the films. The magnetic properties of the films were improved by annealing in a H2 atmosphere, showing a more than tenfold decrease in the coercive field values in comparison to those of the vacuum-annealed films. The hardness values increased from 8 to 18 GPa when the annealing temperature was increased from 500 to 700 °C. The appearance of Fe2B phases, as revealed by XRD and TEM, had a significant effect on the mechanical properties of the films. PMID:27877435

Fabrication of bifunctional core-shell Fe3O4 particles coated with ultrathin phosphor layer

PubMed Central

2013-01-01

Bifunctional monodispersed Fe3O4 particles coated with an ultrathin Y2O3:Tb3+ shell layer were fabricated using a facile urea-based homogeneous precipitation method. The obtained composite particles were characterized by powder X-ray diffraction, transmission electron microscopy (TEM), quantum design vibrating sample magnetometry, and photoluminescence (PL) spectroscopy. TEM revealed uniform spherical core-shell-structured composites ranging in size from 306 to 330 nm with a shell thickness of approximately 25 nm. PL spectroscopy confirmed that the synthesized composites displayed a strong eye-visible green light emission. Magnetic measurements indicated that the composite particles obtained also exhibited strong superparamagnetic behavior at room temperature. Therefore, the inner Fe3O4 core and outer Y2O3:Tb3+ shell layer endow the composites with both robust magnetic properties and strong eye-visible luminescent properties. These composite materials have potential use in magnetic targeting and bioseparation, simultaneously coupled with luminescent imaging. PMID:23962025

Fabrication of bifunctional core-shell Fe3O4 particles coated with ultrathin phosphor layer

NASA Astrophysics Data System (ADS)

Atabaev, Timur Sh; Kim, Hyung-Kook; Hwang, Yoon-Hwae

2013-08-01

Bifunctional monodispersed Fe3O4 particles coated with an ultrathin Y2O3:Tb3+ shell layer were fabricated using a facile urea-based homogeneous precipitation method. The obtained composite particles were characterized by powder X-ray diffraction, transmission electron microscopy (TEM), quantum design vibrating sample magnetometry, and photoluminescence (PL) spectroscopy. TEM revealed uniform spherical core-shell-structured composites ranging in size from 306 to 330 nm with a shell thickness of approximately 25 nm. PL spectroscopy confirmed that the synthesized composites displayed a strong eye-visible green light emission. Magnetic measurements indicated that the composite particles obtained also exhibited strong superparamagnetic behavior at room temperature. Therefore, the inner Fe3O4 core and outer Y2O3:Tb3+ shell layer endow the composites with both robust magnetic properties and strong eye-visible luminescent properties. These composite materials have potential use in magnetic targeting and bioseparation, simultaneously coupled with luminescent imaging.

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.

TEA controllable preparation of magnetite nanoparticles (Fe3O4 NPs) with excellent magnetic properties

NASA Astrophysics Data System (ADS)

Han, Chengliang; Zhu, Dejie; Wu, Hanzhao; Li, Yao; Cheng, Lu; Hu, Kunhong

2016-06-01

A fast and controllable synthesis method for superparamagnetic magnetite nanoparticles (Fe3O4 NPs) was developed in Fe(III)-triethanolamine (TEA) solution. The phase structure, morphology and particle size of the as-synthesized samples were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results showed that the magnetic particles were pure Fe3O4 with mean sizes of approximately 10 nm. The used TEA has key effects on the formation of well dispersing Fe3O4 NPs. Vibrating sample magnetometer (VSM) result indicated that the as-obtained Fe3O4 NPs exhibited superparamagnetic behavior and the saturation magnetization (Ms) was about 70 emu/g, which had potential applications in magnetic science and technology.

Synthesis, electrical and magnetic properties of sodium borosilicate glasses containing Co-ferrites nanoparticles

NASA Astrophysics Data System (ADS)

Othman, H. A.; Eltabey, M. M.; Ibrahim, Samia. E.; El-Deen, L. M. Sharaf; Elkholy, M. M.

2017-02-01

Co-ferrites nanoparticles that have been prepared by the co-precipitation method were added to sodium borosilicate (Na2O-B2O3-SiO2) glass matrix by the solid solution method and they were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) and magnetization measurements. (XRD) revealed the formation of the Co-ferrite magnetic crystalline phase embedded in an amorphous matrix in all the samples. The investigated samples by (TEM) showed the formation of the cobalt ferrite nanoparticles with a spherical shape and highly monodispersed with an average size about 13 nm. IR data revealed that the BO3 and BO4 are the main structural units of these samples network. IR spectra of the investigated samples showed the characteristic vibration bands of Co-ferrite. Composition and frequency dependent dielectric properties of the prepared samples were measured at room temperature in the frequency range 100-100 kHz. The conductivity was found to increase with increasing cobalt ferrite content. The variations of conductivity and dielectric properties with frequency and composition were discussed. Magnetic hysteresis loops were traced at room temperature using VSM and values of saturation magnetization MS and coercive field HC were determined. The obtained results revealed that a ferrimagnetic behavior were observed and as Co-ferrite concentration increases the values of MS and HC increase from 2.84 to 8.79 (emu/g) and from 88.4 to 736.3 Oe, respectively.

Vibration testing of the JE-M-604-4-IUE rocket motor (Thiokol P/N E 28639-03)

NASA Technical Reports Server (NTRS)

Alt, R. E.; Tosh, J. T.

1976-01-01

The NASA International Ultraviolet Explorer (IUE) rocket motor (TE-M-604-4), a solid fuel, spherical rocket motor, was vibration tested in the Impact, Vibration, and Acceleration (IVA) Test Unit of the von Karman Gas Dynamics Facility (VKF). The objective of the test program was to subject the motor to qualification levels of sinusoidal and random vibration prior to the altitude firing of the motor in the Propulsion Development Test Cell (T-3), Engine Test Facility (ETF), AEDC. The vibration testing consisted of a low level sine survey from 5 to 2,000 Hz, followed by a qualification level sine sweep and qualification level random vibration. A second low level sine survey followed the qualification level testing. This sequence of testing was accomplished in each of three orthogonal axes. No motor problems were observed due to the imposition of these dynamic environments.

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

PubMed

Wang, Jun; Zhang, Kai; Zhu, Yuejin

2005-05-01

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

Magnetite Nanoparticles Coated with Rifampicin and Chlortetracycline for Drug Delivery Applications

NASA Astrophysics Data System (ADS)

Nǎdejde, Claudia; Ciurlicǎ, Ecaterina Foca-nici; Creangǎ, Dorina; Cârlescu, Aurelian; Bǎdescu, Vasile

2010-12-01

Four types of biocompatible magnetic fluids based on superparamagnetic nanoparticles with Fe3O4 cores were functionalized with antibiotics (rifampicin or chlortetracycline) as potential candidates for in vivo biomedical applications, such as magnetically controlled drug delivery. The synthesis consisted in coprecipitation of iron oxide in basic, as well as in acid medium, followed by the dispersion of the resulted magnetite nanoparticles in aqueous solution containing the antibiotic. The chosen method to prepare the magnetite-core/drug-shell systems avoided intermediate organic coating of the magnetic nanoparticles. Comparative analysis of the rheological features of the aqueous magnetic fluid samples was performed. The structural features of the coated magnetic particles were investigated by X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM) and Vibrating Sample Magnetometry (VSM). Good crystallinity and adequate stability in time were evidenced. Drug delivery curves were spectrophotometrically provided.

Microwave assisted scalable synthesis of titanium ferrite nanomaterials

NASA Astrophysics Data System (ADS)

Shukla, Abhishek; Bhardwaj, Abhishek K.; Singh, S. C.; Uttam, K. N.; Gautam, Nisha; Himanshu, A. K.; Shah, Jyoti; Kotnala, R. K.; Gopal, R.

2018-04-01

Titanium ferrite magnetic nanomaterials are synthesized by one-step, one pot, and scalable method assisted by microwave radiation. Effects of titanium content and microwave exposure time on size, shape, morphology, yield, bonding nature, crystalline structure, and magnetic properties of titanium ferrite nanomaterials are studied. As-synthesized nanomaterials are characterized by X-ray diffraction (XRD), ultraviolet-visible absorption spectroscopy (UV-Vis), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), Raman spectroscopy, transmission electron microscopy (TEM), and vibrating sample magnetometer measurements. XRD measurements depict the presence of two phases of titanium ferrite into the same sample, where crystallite size increases from ˜33 nm to 37 nm with the increase in titanium concentration. UV-Vis measurement showed broad spectrum in the spectral range of 250-600 nm which reveals that its characteristic peaks lie between ultraviolet and visible region; ATR-FTIR and Raman measurements predict iron-titanium oxide structures that are consistent with XRD results. The micrographs of TEM and selected area electron diffraction patterns show formation of hexagonal shaped particles with a high degree of crystallinity and presence of multi-phase. Energy dispersive spectroscopy measurements confirm that Ti:Fe compositional mass ratio can be controlled by tuning synthesis conditions. Increase of Ti defects into titanium ferrite lattice, either by increasing titanium precursor or by increasing exposure time, enhances its magnetic properties.

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

NASA Astrophysics Data System (ADS)

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

2016-05-01

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

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.

Synthesis and magnetic properties of NiFe2-xSmxO4 nanopowder

NASA Astrophysics Data System (ADS)

Hassanzadeh-Tabrizi, S. A.; Behbahanian, Shahrzad; Amighian, Jamshid

2016-07-01

NiFe2-xSmxO4 (x=0.00, 0.05, 0.10 and 0.15) nanopowders were synthesized via a sol-gel combustion route. The structural studies were carried out by X-ray diffractometer, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. The XRD results confirmed the formation of single-phase spinel cubic structure. The crystallite size decreased with an increase of samarium ion concentration, while lattice parameter and lattice strain increased with samarium substitution. TEM micrographs showed that agglomerated nanoparticles with particle sizes ranging from 35 to 90 nm were obtained. The magnetic studies were carried out using vibrating sample magnetometer. Magnetic measurements revealed that the saturation magnetization (Ms) of NiFe2-xSmxO4 nanoparticles decreases with increasing Sm3+substitution. The reduction of saturation magnetization is attributed to the dilution of the magnetic interaction. The coercivity (Hc) of samples increases by adding samarium.

Measurement of the Elastic Modulus of a Single Boron Nitride Nanotube

NASA Astrophysics Data System (ADS)

Chopra, Nasreen G.; Cohen, Marvin L.; Louie, Steven G.; Zettl, A.

1997-03-01

In situ transmission electron microscope (TEM) measurements of thermally-excited vibrational characteristics of boron nitride (BN) nanotubes are used to extract the elastic modulus. We find BN nanotubes to have a higher axial Young's modulus, 1.2 TPa, than any other insulating fiber. This value is consistent with theoretical predictions and confirms previous TEM observations of the high degree of crystallinity of these structures. This work was supported by the U. S. Department of Energy under contract No. DE-AC03-76-SF00098 and the Office of Naval Research, Order No. N00014-95-F-0099

Superparamagnetic iron oxide-reduced graphene oxide nanohybrid-a vehicle for targeted drug delivery and hyperthermia treatment of cancer

NASA Astrophysics Data System (ADS)

Gupta, Jagriti; Prakash, Anand; Jaiswal, Manish K.; Agarrwal, Atanuu; Bahadur, D.

2018-02-01

In this work, an efficient superparamagnetic iron oxide-reduced graphene oxide (Fe3O4-RGO) nanohybrid has been synthesized following one-step co-precipitation method. The phase identification, microstructure and magnetic behavior of nanohybrid were characterized by X-ray diffraction, transmission electron microscopy (TEM), raman spectroscopy and vibrating sample magnetometer (VSM), respectively. TEM micrograph confirms the presence of well-segregated Fe3O4 nanoparticles in RGO layers. The layered RGO minimizes the agglomeration in Fe3O4 nanoparticles with slight reduction in magnetic behavior. Doxorubicin (DOX) has been used as a model drug to investigate the loading efficiency of nanohybrid and chemo-thermo therapeutic effect on human cervical cancer (HeLa cells). The DOX loaded nanohybrid (DOX-Fe3O4-RGO) shows maximum inhibition of human cervical cancer cell lines during magnetic field assisted hyperthermia treatment. The synergistic effect of nanohybrid demonstrated the potential for cancer cell proliferation prevention up to 90% when treated at the concentration of 2 mg mL-1 for one million cells and exposed to AC field of 335 Oe at a fixed frequency of 265 kHz for 35 min.

Self-cleaning superhydrophobic epoxy coating based on fibrous silica-coated iron oxide magnetic nanoparticles.

PubMed

Alamri, Haleema; Al-Shahrani, Abdullah; Bovero, Enrico; Khaldi, Turki; Alabedi, Gasan; Obaid, Waleed; Al-Taie, Ihsan; Fihri, Aziz

2018-03-01

Inspired by the self-cleaning lotus leaf, a facile method of fabricating superhydrophobic silica coated magnetite nanoparticles using a cost-effective process is presented in this work. The structural characterizations and magnetic properties of the obtained core-shell magnetic nanoparticles were characterized by means of X-ray diffraction (XRD), thermal gravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). TEM analysis revealed that the particles present flower-like dendrimeric fibers morphology. The particles were uniformly dispersed on the surface of an epoxy resin coating with the purpose to increase the roughness and reduce the surface energy of the surface. The resulting superhydrophobic surface provides robust water-repellent surface under harsh conditions, thanks to its self-cleaning characteristic. The superhydrophobicity of this surface was confirmed based on the measurements of a water contact angle around 175°, which surpasses the theoretical limit of the superhydrophobicity. The simplicity and the cost-effectiveness of the process developed in this study appears to be a promising route for the preparation of other magnetic superhydrophobic organic-inorganic hybrid materials that would be beneficial in a wide variety of applications. Copyright © 2017 Elsevier Inc. All rights reserved.

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.

Multiple functionalities of Ni nanoparticles embedded in carboxymethyl guar gum polymer: catalytic activity and superparamagnetism

NASA Astrophysics Data System (ADS)

Sardar, Debasmita; Sengupta, Manideepa; Bordoloi, Ankur; Ahmed, Md. A.; Neogi, S. K.; Bandyopadhyay, Sudipta; Jain, Ruchi; Gopinath, Chinnakonda S.; Bala, Tanushree

2017-05-01

Composites comprising of metallic nanoparticles in polymer matrices have allured significant importance due to multifunctionalities. Here a simple protocol has been described to embed Ni nanoparticles in carboxymethyl guar gum (CMGG) polymer. The composite formation helps in the stabilization of Ni nanoparticles which are otherwise prone towards aerial oxidation. Further the nanoparticles retain their superparamagnetic nature and catalytic capacity. Ni-Polymer composite catalyses the reduction of 4-Nitrophenol to 4-Aminophenol very efficiently in presence of NaBH4, attaining a complete conversion under some experimental conditions. Ni-Polymer composite is well characterized using UV-vis spectroscopy, FTIR, XPS, powder XRD, TGA, SEM and TEM. A detailed magnetic measurement using superconducting quantum interference device-vibrating sample magnetometer (SQUID-VSM) reveals superparamagnetic behaviour of the composite.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Effects of Phonation Time and Magnitude Dose on Vocal Fold Epithelial Genes, Barrier Integrity, and Function

PubMed Central

Kojima, Tsuyoshi; Valenzuela, Carla V.; Novaleski, Carolyn K.; Van Deusen, Mark; Mitchell, Joshua R.; Garrett, C. Gaelyn; Sivasankar, M. Preeti; Rousseau, Bernard

2014-01-01

Objective To investigate the effects of increasing time and magnitude doses of vibration exposure on transcription of the vocal fold's junctional proteins, structural alterations, and functional tissue outcomes. Study Design Animal study. Methods 100 New Zealand White breeder rabbits were studied. Dependent variables were measured in response to increasing time doses (30, 60, or 120 minutes) and magnitude doses (control, modal intensity, and raised intensity) of vibration exposure. Messenger RNA expression of occludin, zonula occluden-1 (ZO-1), E-cadherin, β-catenin, interleukin 1β (IL-1β), cyclooxygenase-2 (COX-2), transforming growth factor β-1 (TGFβ1), and fibronectin were measured. Tissue structural alterations were assessed using transmission electron microscopy (TEM). Transepithelial resistance was used to measure functional tissue outcomes. Results Occludin gene expression was downregulated in vocal folds exposed to 120 minute time doses of raised intensity phonation, relative to control, and modal intensity phonation. ZO-1 gene expression was upregulated following a 120 minute time dose of modal intensity phonation, compared to control, and downregulated after a 120 minute time dose of raised intensity phonation, compared to modal intensity phonation. E-cadherin gene expression was downregulated after a120 minute time dose of raised intensity phonation, compared to control and modal intensity phonation. TEM revealed extensive desquamation of the stratified squamous epithelial cells with increasing time and magnitude doses of vibration exposure. A general observation of lower transepithelial resistance measures was made in tissues exposed to raised intensity phonation, compared to all other groups. Conclusions This study provides evidence of vocal fold tissue responses to varying time and magnitude doses of vibration exposure. Level of Evidence N/A PMID:25073715

The synthesis of Fe3O4/MWCNT nanocomposites from local iron sands for electrochemical sensors

NASA Astrophysics Data System (ADS)

Rahmawati, Retno; Taufiq, Ahmad; Sunaryono, Yuliarto, Brian; Suyatman, Nugraha, Noviandri, Indra; Setyorini, Dian Ayu; Kurniadi, Deddy

2018-05-01

The aim of this research is producing the electrochemical sensor, especially for working electrodes based on the nanocomposites of multi-walled carbon nanotube (MWCNT) and magnetite (Fe3O4) nanoparticles from iron sands. The sonochemical method by ultrasonic horn was successfully used for the synthesis of the nanocomposites. The characterizations of the sample were conducted via X-Ray Diffractometer (XRD), Fourier Transform Infra-Red (FTIR) Spectrometer, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Brunauer-Emmett-Teller (BET) method for surface area, Vibrating Sample Magnetometer (VSM) and Cyclic Voltammetry (CV). The analysis of X-Ray Diffraction (XRD) pattern showed two phases of crystalline, namely MWCNT and Fe3O4, peak of MWCNT comes from (002) plan while peaks of Fe3O4 come from (2 2 0), (3 1 1), (4 0 0), (4 2 2), (5 1 1), and (4 4 0) plans. From XRD data, MWCNT has a hexagonal structure and Fe3O4 has inverse spinel cubic structure, respectively. The FTIR spectra revealed that the functionalization process of MWCNT successfully generated carboxyl and carbonyl groups to bind Fe3O4 on MWCNT surfaces. Moreover, the functional groups of Fe-O bonding that showed the existence of Fe3O4 in the nanocomposites were also detected in those spectra. Meanwhile, the SEM and TEM images showed that the nanoparticles of Fe3O4 attached on the MWCNT surface and formed agglomeration between particles due to magnetic forces. Through Brunauer-Emmett-Teller (BET) method, it is identified that the nanocomposite has a large surface area 318 m2/g that makes this material very suitable for electrochemical sensor applications. Moreover, the characterization of magnetic properties via Vibrating Sample Magnetometer (VSM) showed that the nanocomposites have superparamagnetic behavior at room temperature and the presence of the MWCNT reduced the magnetic properties of Fe3O4. Lastly, the electrochemical characterization with Cyclic Voltammetry (CV) proved that Fe3O4/MWCNT nanocomposites with iron sands as the starting materials have high sensitivity and serve as excellent electron transfer materials. Based on the results of the research, the Fe3O4/MWCNT nanocomposites from iron sands are much recommended for electrochemical sensor.

Effect of pulsed and continuous ultrasound on structural and magnetic properties of nano-sized Ni0.4Cu0.2Zn0.4Fe2O4 ferrite

NASA Astrophysics Data System (ADS)

Hassen, Harzali; Adel, Megriche; Arbi, Mgaidi

2018-03-01

Ultrasound-assisted co-precipitation has been used to prepare nano-sized Ni0.4Cu0.2Zn0.4Fe2O4 ferrite. Continuous (C-US) and pulsed (P-US) ultrasound modes are used at constant frequency = 20 kHz, reaction time = 2 h and pulse durations of 10 s on and 10 s off. All experiments were conducted at two temperatures 90 and 100°C. Samples were characterized by X-ray diffraction (XRD), Fourier transform spectroscopy (FT-IR), N2 adsorption isotherms at 77 k analysis (BET), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM) techniques. A nanocrystalline single-phase with particle size in the range 12-18 nm is obtained in both modes: continuous and pulsed ultrasound mode. FT-IR measurements show two absorption bands assigned to the tetrahedral and octahedral vibrations (ν1 and ν2) characteristics of cubic spinel ferrite. The specific surface area (S BET) is in the range of 110-140 m2 g-1 and an average pore size between 5.5 and 6.5 nm. The lowest values are obtained in pulsed mode. Finally, this work shows that the magnetic properties are affected by the ultrasound conditions, without affecting the particle shape. The saturation magnetization (Ms) values obtained for all samples are comparable. In P-US mode, the saturation magnetization (Ms) increases as temperature increases. Moreover, P-US mode opens a new avenue for synthesis of NiCuZn ferrites.

Preparation and characterization of polyol assisted ultrafine Cu-Ni-Mg-Ca mixed ferrite via co-precipitation method

NASA Astrophysics Data System (ADS)

Boobalan, T.; Pavithradevi, S.; Suriyanarayanan, N.; Manivel Raja, M.; Ranjith Kumar, E.

2017-04-01

Nanocrystalline spinel ferrite of composition Cu0.2Ni0.2Mg0.2Ca0.4Fe2O4 is synthesized by wet hydroxyl co-precipitation method in ethylene glycol as chelating agent and sodium hydroxide as precipitator at pH 8. Ethylene glycol is utilized as the medium which serves as the dissolvable and in addition a complexing specialist. The synthesized particles are annealed at various temperatures. Thermogravimetric investigation affirms that at 280 °C ethylene glycol is dissipated totally and stable phase arrangement happens over 680 °C. FTIR spectra of as synthesized and annealed at 1050 °C recorded between 400 cm-1 and 4000 cm-1. Structural characterizations of all the samples are carried out by X-ray diffraction (XRD) technique. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) affirm that the particles are spherical and cubic shape with the crystallite size of 12 nm to 32 nm. Magnetic measurements are performed utilizing vibrating sample magnetometer at room temperature.

Fabrication of Fe3O4@CuO core-shell from MOF based materials and its antibacterial activity

NASA Astrophysics Data System (ADS)

Rajabi, S. K.; Sohrabnezhad, Sh.; Ghafourian, S.

2016-12-01

Magnetic Fe3O4@CuO nanocomposite with a core/shell structure was successfully synthesized via direct calcinations of magnetic Fe3O4@HKUST-1 in air atmosphere. The morphology, structure, magnetic and porous properties of the as-synthesized nano composites were characterized by using scanning electron microscope (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (PXRD), and vibration sample magnetometer (VSM). The results showed that the nanocomposite material included a Fe3O4 core and a CuO shell. The Fe3O4@CuO core-shell can be separated easily from the medium by a small magnet. The antibacterial activity of Fe3O4-CuO core-shell was investigated against gram-positive and gram-negative bacteria. A new mechanism was proposed for inactivation of bacteria over the prepared sample. It was demonstrated that the core-shell exhibit recyclable antibacterial activity, acting as an ideal long-acting antibacterial agent.

Preparation and evaluation of magnetic core-shell mesoporous molecularly imprinted polymers for selective adsorption of tetrabromobisphenol S.

PubMed

Wang, Xuemei; Huang, Pengfei; Ma, Xiaomin; Wang, Huan; Lu, Xiaoquan; Du, Xinzhen

2017-05-01

Novel magnetic mesoporous molecularly imprinted polymers (MMIPs) with core-shell structure were prepared by simple surface molecular imprinting polymerization using tetrabromobisphenol-S (TBBPS) as the template. The MMIPs-TBBPS were characterized by fourier-transform infrared spectrometry (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), N 2 adsorption-desorption transmission, and vibrating sample magnetometry. The resultant MMIPs-TBBPS were successfully applied magnetic solid-phase extraction (MSPE) coupled with HPLC determination of TBBPS in spiked real water samples with recoveries of 77.8-88.9%. The adsorption experiments showed that the binding capacity of MMIPs-TBBPS to TBBPS and six structural analogs were significantly higher than that of the magnetic nonimprinted polymers (MNIPs). Meanwhile, the MMIPs-TBBPS possessed rapid binding affinity, excellent magnetic response, specific selectivity and high adsorption capacity toward TBBPS with a maximum adsorption capacity of 1626.8µgg -1 . The analytical results indicate that the MMIPs-TBBPS are promising materials for selective separation and fast enrichment of TBBPS from complicated enviromental samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Optical, Magnetic and Photocatalytic Activity Studies of Li, Mg and Sr Doped and Undoped Zinc Oxide Nanoparticles.

PubMed

Shanthi, S I; Poovaragan, S; Arularasu, M V; Nithya, S; Sundaram, R; Magdalane, C Maria; Kaviyarasu, K; Maaza, M

2018-08-01

Nanoparticles of Li, Mg and Sr doped and undoped zinc oxide was prepared by simple precipitation method. The structural, optical, and magnetic properties of the samples were investigated by the Powder X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Fourier Transform Infrared (FTIR) spectroscopy, Ultra-violet Visible spectroscopy (UV-vis) spectra, Photoluminescence (PL) and Vibrational Sample Magnetometer (VSM). The Powder X-ray diffraction data confirm the formation of hexagonal wurtzite structure of all doped and undoped ZnO. The SEM photograph reveals that the pores availability and particles size in the range of 10 nm-50 nm. FTIR and UV-Visible spectra results confirm the incorporation of the dopant into the ZnO lattice nanostructure. The UV-Visible spectra indicate that the shift of blue region (lower wavelength) due to bandgap widening. Photoluminescence intensity varies with doping due to the increase of oxygen vacancies in prepared ZnO. The pure ZnO exist paramagnetic while doped (Li, Mg and Sr) ZnO exist ferromagnetic property. The photocatalytic activity of the prepared sample also carried out in detail.

Clinical and psychopathological features associated with treatment-emergent mania in bipolar-II depressed outpatients exposed to antidepressants.

PubMed

Fornaro, Michele; Anastasia, Annalisa; Monaco, Francesco; Novello, Stefano; Fusco, Andrea; Iasevoli, Felice; De Berardis, Domenico; Veronese, Nicola; Solmi, Marco; de Bartolomeis, Andrea

2018-07-01

Treatment-emergent affective switch (TEAS), including treatment-emergent mania (TEM), carry significant burden in the clinical management of bipolar depression, whereas the use of antidepressants raises both efficacy, safety and tolerability concerns. The present study assesses the prevalence and clinical correlates of TEM in selected sample of Bipolar Disorder (BD) Type-II (BD-II) acute depression outpatients. Post-hoc analysis of the clinical and psychopathological features associated with TEM among 91 BD-II depressed outpatients exposed to antidepressants. Second-generation antipsychotics (SGA) (p = .005), lithium (≤ .001), cyclothymic/irritable/hyperthymic temperaments (p = ≤ .001; p = .001; p = .003, respectively), rapid-cycling (p = .005) and depressive mixed features (p = .003) differed between TEM + cases vs. TEM - controls. Upon multinomial logistic regression, the accounted psychopathological features correctly classified as much as 88.6% of TEM + cases (35/91 overall sample, or 38.46% of the sample), yet not statistically significantly [Exp(B) = .032; p = ns]. Specifically, lithium [B = - 2.385; p = .001], SGAs [B = - 2.354; p = .002] predicted lower rates of TEM + in contrast to the number of lifetime previous psychiatric hospitalizations [B = 2.380; p = .002], whereas mixed features did not [B = 1.267; p = ns]. Post-hoc analysis. Lack of systematic pharmacological history record; chance of recall bias and Berkson's biases. Permissive operational criterion for TEM. Relatively small sample size. Cyclothymic temperament and mixed depression discriminated TEM + between TEM - cases, although only lithium and the SGAs reliably predicted TEM +/- grouping. Larger-sampled/powered longitudinal replication studies are warranted to allow firm conclusions on the matter, ideally contributing to the identification of clear-cut sub-phenotypes of BD towards patient-tailored-pharmacotherapy. Copyright © 2018 Elsevier B.V. All rights reserved.

Shape control of the magnetic iron oxide nanoparticles under different chain length of reducing agents

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

Ngoi, Kuan Hoon; Chia, Chin-Hua, E-mail: chia@ukm.edu.my; Zakaria, Sarani

2015-09-25

We report on the effect of using reducing agents with different chain-length on the synthesis of iron oxide nanoparticles by thermal decomposition of iron (III) acetylacetonate in 1-octadecene. This modification allows us to control the shape of nanoparticles into spherical and cubic iron oxide nanoparticles. The highly monodisperse 14 nm spherical nanoparticles are obtained under 1,2-dodecanediol and average 14 nm edge-length cubic iron oxide nanoparticles are obtained under 1,2-tetradecanediol. The structural characterization such as transmission electron microscope (TEM) and X-ray diffraction (XRD) shows similar properties between two particles with different shapes. The vibrating sample magnetometer (VSM) shows no significant difference between sphericalmore » and cubic nanoparticles, which are 36 emu/g and 37 emu/g respectively and superparamagnetic in nature.« less

High frequency electromagnetic reflection loss performance of substituted Sr-hexaferrite nanoparticles/SWCNTs/epoxy nanocomposite

NASA Astrophysics Data System (ADS)

Gordani, Gholam Reza; Ghasemi, Ali; saidi, Ali

2015-10-01

In this study, the electromagnetic properties of a novel nanocomposite material made of substituted Sr-hexaferrite nanoparticles and different percentage of single walled carbon nanotube have been studied. The structural, magnetic and electromagnetic properties of samples were studied as a function of volume percentage of SWCNTs by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, vibrating sample magnetometer and vector network analysis. Well suitable crystallinity of hexaferrite nanoparticles was confirmed by XRD patterns. TEM and FESEM micrographs were shown the good homogenity and high level of dispersivity of SWCNTs and Sr-hexaferrite nanoparticles in nanocomposite samples. The VSM results shown that with increasing in amount of CNTs (0-6 vol%), the saturation of magnetization decreased up to 11 emu/g for nanocomposite sample contains of 6 vol% of SWCNTs. The vector network analysis results show that the maximum value of reflection loss was -36.4 dB at the frequency of 11 GHz with an absorption bandwidth of more than 4 GHz (<-20 dB). The results indicate that, this nanocomposite material with appropriate amount of SWCNTs hold great promise for microwave device applications.

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.

A novel green synthesis of Fe3O4-Ag core shell recyclable nanoparticles using Vitis vinifera stem extract and its enhanced antibacterial performance

NASA Astrophysics Data System (ADS)

Venkateswarlu, Sada; Natesh Kumar, B.; Prathima, B.; Anitha, K.; Jyothi, N. V. V.

2015-01-01

We described a novel and eco-friendly method for preparing Fe3O4-Ag core shell nanoparticles (CSNPs) with high magnetism and potent antibacterial activity. The Fe3O4-Ag CSNPs were obtained using waste material of Vitis vinifera (grape) stem extract as the green solvent, reducing and capping agent. The result recorded from X-ray powder diffraction (XRD), UV-vis spectrum, energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR) supports the biosynthesis and characterization of Fe3O4-Ag CSNPs. From transmission electron microscopy (TEM) the size of the Fe3O4-Ag nanoparticles was measured below 50 nm; high-resolution TEM (HRTEM) indicates the core shell structure; and selected area electron diffraction (SAED) has revealed polycrystalline nature. Vibrating sample magnetometer (VSM) shows the ferromagnetic nature of Fe3O4-Ag CSNPs at room temperature with saturation magnetization of 15.74 emu/g. Further, these biogenic nanoparticles were highly hazardous to microorganisms. The antibacterial activity of biogenic Fe3O4-Ag CSNPs showed potent inhibitory activity against both Gram-positive and Gram-negative pathogens. These nanoparticles may also be reusable because of its excellent ferromagnetic property.

Effect of magnetic and thermal properties of iron oxide nanoparticles (IONs) in nitrile butadiene rubber (NBR) latex

NASA Astrophysics Data System (ADS)

Ong, Hun Tiar; Julkapli, Nurhidayatullaili Muhd; Hamid, Sharifah Bee Abd; Boondamnoen, O.; Tai, Mun Foong

2015-12-01

Nitrile butadiene rubber (NBR) gloves are one of the most important personal protective equipments but they are possible to tear off and contaminate food or pharmaceutical and healthcare products during manufacturing and packaging process. High tendency of torn glove remaining in food or products due to white or light flesh-coloured glove is not easy to be detected by naked eyes. In this paper, iron oxide nanoparticles (IONs) selected as additive for NBR to improve its detectability by mean of magnetic properties. IONs synthesized via precipitation method and compounded with NBR latex before casting on petri dish. The properties of IONs were investigated by X-ray Diffractometry (XRD), Transmission Electron Microscope (TEM), Raman Spectroscopy and Vibrating Sample Magnetometer (VSM). Meanwhile NBR/IONs composites were studied by Thermogravimetry Analysis (TGA), Differential Scanning Calorimetry (DSC) and Vibrating Sample Magnetometer (VSM). It observed that, synthesized IONs shows of 25.28 nm crystallite with 25.86 nm semipherical (changed as) shape. Meanwhile, Magnetite and maghemite phase are found in range of 670 cm-1 and 700 cm-1 respectively, which it contributes magnetization saturation of 73.96 emu/g at 10,000 G by VSM. Thermal stability and magnetic properties were increased with incorporating IONs into NBR latex up to 20 phr. NBR/IONs 5 phr has the optimum thermal stability, lowest glass transition temperature (-14.83 °C) and acceptable range of magnetization saturation (3.83 emu/g at 10,000 G) to form NBR gloves with magnetic detectability.

Efficient photocatalytic degradation of rhodamine-B by Fe doped CuS diluted magnetic semiconductor nanoparticles under the simulated sunlight irradiation

NASA Astrophysics Data System (ADS)

Sreelekha, N.; Subramanyam, K.; Amaranatha Reddy, D.; Murali, G.; Rahul Varma, K.; Vijayalakshmi, R. P.

2016-12-01

The present work is planned for a simple, inexpensive and efficient approach for the synthesis of Cu1-xFexS (x = 0.00, 0.01, 0.03, 0.05 and 0.07) nanoparticles via simplistic chemical co-precipitation route by using ethylene diamine tetra acetic acid (EDTA) as a capping molecules. As synthesized nanoparticles were used as competent catalysts for degradation of rhodamine-B organic dye pollutant. The properties of prepared samples were analyzed with energy dispersive analysis of X-rays (EDAX), X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-visible optical absorption spectroscopy, Fourier transform infrared (FTIR) spectra, Raman spectra and vibrating sample magnetometer (VSM). EDAX spectra corroborated the existence of Fe in prepared nanoparticles within close proximity to stoichiometric ratio. XRD, FTIR and Raman patterns affirmed that configuration of single phase hexagonal crystal structure as that of (P63/mmc) CuS, without impurity crystals. The average particle size estimated by TEM scrutiny is in the assortment of 5-10 nm. UV-visible optical absorption measurements showed that band gap narrowing with increasing the Fe doping concentration. VSM measurements revealed that 3% Fe doped CuS nanoparticles exhibited strong ferromagnetism at room temperature and changeover of magnetic signs from ferromagnetic to the paramagnetic nature with increasing the Fe doping concentration in CuS host lattice. Among all Fe doped CuS nanoparticles, 3% Fe inclusion CuS sample shows better photocatalytic performance in decomposition of RhB compared with the pristine CuS. Thus as synthesized Cu0·97Fe0·03S nanocatalysts are tremendously realistic compounds for photocatalytic fictionalization in the direction of organic dye degradation under visible light.

New Generation Materials and Structures for Nanophotonics and Nanoelectronics

DTIC Science & Technology

2006-04-30

been investigated using thermogravimetric analysis and FTIR spectroscopy. The nanoparticles appear to have excess surfactants on their surface, but...processes. We continued analysis of the vibrational modes of the InP/II- VI core-shell nanoparticles determined by IR and Raman studies, and initiated...photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), BET surface area analysis , transmission electron microscopy (TEM), and SQUID magnetometry. In

An efficient and cost-effective method for preparing transmission electron microscopy samples from powders

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

Wen, Haiming; Lin, Yaojun; Seidman, David N.

The preparation of transmission electron microcopy (TEM) samples from powders with particle sizes larger than ~100 nm poses a challenge. The existing methods are complicated and expensive, or have a low probability of success. Herein, we report a modified methodology for preparation of TEM samples from powders, which is efficient, cost-effective, and easy to perform. This method involves mixing powders with an epoxy on a piece of weighing paper, curing the powder–epoxy mixture to form a bulk material, grinding the bulk to obtain a thin foil, punching TEM discs from the foil, dimpling the discs, and ion milling the dimpledmore » discs to electron transparency. Compared with the well established and robust grinding–dimpling–ion-milling method for TEM sample preparation for bulk materials, our modified approach for preparing TEM samples from powders only requires two additional simple steps. In this article, step-by-step procedures for our methodology are described in detail, and important strategies to ensure success are elucidated. Furthermore, our methodology has been applied successfully for preparing TEM samples with large thin areas and high quality for many different mechanically milled metallic powders.« less

An efficient and cost-effective method for preparing transmission electron microscopy samples from powders

DOE PAGES

Wen, Haiming; Lin, Yaojun; Seidman, David N.; ...

2015-09-09

The preparation of transmission electron microcopy (TEM) samples from powders with particle sizes larger than ~100 nm poses a challenge. The existing methods are complicated and expensive, or have a low probability of success. Herein, we report a modified methodology for preparation of TEM samples from powders, which is efficient, cost-effective, and easy to perform. This method involves mixing powders with an epoxy on a piece of weighing paper, curing the powder–epoxy mixture to form a bulk material, grinding the bulk to obtain a thin foil, punching TEM discs from the foil, dimpling the discs, and ion milling the dimpledmore » discs to electron transparency. Compared with the well established and robust grinding–dimpling–ion-milling method for TEM sample preparation for bulk materials, our modified approach for preparing TEM samples from powders only requires two additional simple steps. In this article, step-by-step procedures for our methodology are described in detail, and important strategies to ensure success are elucidated. Furthermore, our methodology has been applied successfully for preparing TEM samples with large thin areas and high quality for many different mechanically milled metallic powders.« less

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

NASA Astrophysics Data System (ADS)

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

2001-01-01

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

Synthesis and characterization of struvite nano particles

NASA Astrophysics Data System (ADS)

Rathod, K. R.; Jogiya, B. V.; Chauhan, C. K.; Joshi, M. J.

2015-06-01

Struvite, Ammonium Magnesium Phosphate Hexahydrate [(AMPH) - (NH4)MgPO4.6(H2O)], is one of the fascinating inorganic phosphate minerals. Struvite is one of the components of the urinary stones. Struvite occurs as crystallites in urine and grows as a type of kidney stone. In this study, struvite nano particles were synthesized by wet chemical technique. The aqueous solutions containing dissolved Mg(CH3COO)2.4H2O and (NH4)H2PO4 mixed at the Mg/P molar ratio of 1.00. The synthesized struvite nano particles were characterized by XRD, FT-IR, Thermal Analysis and TEM. From XRD, crystal structure of the nano particle was found to be orthorhombic and crystalline size was found to be within 11 to 26 nm. The FT-IR spectrum for the struvite nano particles confirmed the presence of a water molecule and metal-oxygen stretching vibration, O-H stretching and bending, N-H bending and stretching, P-O bending and stretching vibrations. The Thermal Analysis was carried out from room temperature to 900°C. From TEM analysis, particle size was 23 to 30 nm. All the results were compared with bulk struvite.

Phonon shift in chemically exfoliated WS2 nanosheet

NASA Astrophysics Data System (ADS)

Sarkar, Abdus Salam; Pal, Suman Kalyan

2018-04-01

We have synthesized few layer WS2 nanosheets in a low boiling point solvent. Few layer of WS2 sheets are characterized by various techniques such as UV-visible and Raman spectroscopy, transmission electron microscopy (TEM), atomic force microscopy (AFM) and scanning electron microscopy (SEM). UV-Vis absorption spectra confirm the well dispersed in isopropyl alcohol. SEM and TEM images indicate the sheet like morphology of WS2. Atomic force microscopy image and room temperature Raman spectroscopy confirm the exfoliation of few layer (4-5 layer) of WS2. Further, Raman spectroscopy was used as a meteorology tool to determine the temperature co-efficient. We have systematically investigated the temperature dependent Raman spectroscopic behavior of few layer WS2. Our results depict the softening of the Raman modes E12g in plane vibration and A1g out of plane vibration with increasing the temperature from 77 K to 300 K. Softening of the Raman modes could be explained in terms of the double resonance which is active in the layered materials. The observed temperature coefficients for two Raman peaks E12g and A1g, are - 0.022 cm-1 and -0.009 cm-1, respectively.

Determining the vibrations between sensor and sample in SQUID microscopy

NASA Astrophysics Data System (ADS)

Schiessl, Daniel; Kirtley, John R.; Paulius, Lisa; Rosenberg, Aaron J.; Palmstrom, Johanna C.; Ullah, Rahim R.; Holland, Connor M.; Fung, Y.-K.-K.; Ketchen, Mark B.; Gibson, Gerald W.; Moler, Kathryn A.

2016-12-01

Vibrations can cause noise in scanning probe microscopies. Relative vibrations between the scanning sensor and the sample are important but can be more difficult to determine than absolute vibrations or vibrations relative to the laboratory. We measure the noise spectral density in a scanning SQUID microscope as a function of position near a localized source of magnetic field and show that we can determine the spectra of all three components of the relative sensor-sample vibrations. This method is a powerful tool for diagnosing vibrational noise in scanning microscopies.

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.

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.

Vibrational Spectroscopic Studies on the Formation of Ion-exchangeable Titania Nanotubes

NASA Astrophysics Data System (ADS)

Hodos, Mária; Haspel, Henrik; Horváth, Endre; Kukovecz, Ákos; Kónya, Zoltán; Kiricsi, Imre

2005-09-01

Ion-exchangeable titanium-oxide nanotubes have commanded considerable interest from the materials science community in the past five years. Synthesized under hydrothermal conditions from TiO2, typical nanotubes are 150-200 nm long and 8-20 nm wide. High resolution TEM images revealed that unlike multiwall carbon nanotubes which are made of coaxial single-wall nanotubes, the titania tubes possess a spiral cross-section. An interesting feature of the titania tubes is their considerable ion-exchange capacity which could be utilized e.g. for enhancing their photocatalytic activity by doping the titania tubes with CdS nanoparticles. In this contribution we present a comprehensive TEM, FT-Raman and FT-farIR characterization study of the formation process.

Design assurance test of the Thiokol Te-M-521-5 apogee kick motor tested in the spin mode at simulated altitude conditions

NASA Technical Reports Server (NTRS)

Cimino, A. A.

1973-01-01

One Thiokol Chemical Corporation TE-M-521-5 solid-propellant apogee rocket motor was successfully fired at an average simulated altitude of about 108,000 ft while spinning at 46 rpm. The general program objectives were to verify compliance of motor performance with the manufacturer's specifications. Specific primary objectives were to determine vacuum ballistic performance of the motor after prefire vibration conditioning and temperature conditioning at 40F, altitude ignition characteristics, motor structural integrity, and motor temperature-time history during and after motor operation. Additional objectives were to measure the lateral (nonaxial) thrust component during motor operation and to measure radiation heat flux in the vicinity of the nozzle exit plane.

Synthesis and Characterization Materials M-Barium Hexaferrite Doping Ions Co-Mn Nano Particle

NASA Astrophysics Data System (ADS)

Susilawati; Doyan, A.; Sahlam

2017-05-01

This research has been success in the synthesis of M-Barium hexaferrite (BaM) doping Co-Mn ions using coprecipitation method are expected to be applied as a base material in the coating RADAR. M-Barium hexaferrite (BaM) are BaFe12-2xCoxMnxO19 synthesized with various concentrations (x = 0.0, 0.1, 0.2, 0.3) and the calcinations temperature (T = 400°C, 600°C, 800°C). The materials characterization using a X-Ray Diffraction (XRD), Transmission Electron Microscope (TEM), Inductance Capacitance and resistance (LCR) meter, and Vibrating Sample Magnetometer (VSM) Instruments. The measurement results using XRD shows the material has a hexagonal crystalline structure. The measurement results using a TEM show a sample of nano crystal materials with grain diameters up to 40 nm and spacing of the crystal lattice. The measurement results using a LCR-meter shows the electric conductivity of 1.15 × 10-6 S/cm to BaM without doping, 3.75 × 10-6 S/cm to 0.1 doping concentration calcination temperature of 400 °C, and 1,23 × 10-5 S/cm to 0.3 doping concentration calcination temperature of 800 °C, thus including semiconductor materials. The magnetic properties of materials using a VSM test results show the value of coercivity of 0.1 T; remanence value of 0.06 emu/g; and the saturation value of 0.42 emu/g. The results above show BaM Co-Mn metal doping potential as anti-radar material.

Synthesis of carbon nanoparticles from commercially available liquified petroleum gas

NASA Astrophysics Data System (ADS)

Nandiyanto, A. B. D.; Fadhlulloh, M. A.; Rahman, T.; Mudzakir, A.

2016-04-01

The aim of this study was to synthesize carbon nanoparticles (CNPs) from commercially available liquefied petroleum gas (LPG). In the research procedure, LPG was reacted with air to construct CNPs. To confirm the successful synthesis of CNPs, we conducted several sample analyses: Gas Chromatography-Mass Spectrometry (GC-MS), Transmission Electron Microscope (TEM), X-ray Diffraction (XRD), and Infrared Spectra (FTIR). We also varied LPG and oxygen mole ratios at 0.8; 2.4; 4.8; and 7.2. The GC-MS results indicated the composition of LPG was propane (58.90%), isobutane (18.35%), butane (22.26%), and butane, 2-methyl (0.48%). The TEM results showed that the particles were spheres with sizes of between 25 and 35 nm. The sizes of particles were controllable, depending on the mole ratio. The XRD results showed mole ratios of LPG and oxygen of 0.80 and 2.40 were natural graphite, whereas the mole ratios of 4.80 and 7.20 were hexagonal graphite. FT-IR results showed CNPs have absorption peaks at wave number (i) 752 (C-H bend sp2); (ii) 835 (C=C); (iii) 1274 (C-O-C vibration); (iv) 1400 and 1600 (C-C stretch aromatic); (v) 2800 (C-H sp2); (vi) 2900 (CH sp3); (vii) 3100 (C-H aromatic); and (viii) 3400 cm-1 (O-H). From the FTIR analysis results, the sample contained allotrope graphite due to detection of peaks at 1400 and 1600 cm-1 (C-C stretch aromatic) and 3100 cm-1 (C-H aromatic).

Dopant mapping in thin FIB prepared silicon samples by Off-Axis Electron Holography.

PubMed

Pantzer, Adi; Vakahy, Atsmon; Eliyahou, Zohar; Levi, George; Horvitz, Dror; Kohn, Amit

2014-03-01

Modern semiconductor devices function due to accurate dopant distribution. Off-Axis Electron Holography (OAEH) in the transmission electron microscope (TEM) can map quantitatively the electrostatic potential in semiconductors with high spatial resolution. For the microelectronics industry, ongoing reduction of device dimensions, 3D device geometry, and failure analysis of specific devices require preparation of thin TEM samples, under 70 nm thick, by focused ion beam (FIB). Such thicknesses, which are considerably thinner than the values reported to date in the literature, are challenging due to FIB induced damage and surface depletion effects. Here, we report on preparation of TEM samples of silicon PN junctions in the FIB completed by low-energy (5 keV) ion milling, which reduced amorphization of the silicon to 10nm thick. Additional perpendicular FIB sectioning enabled a direct measurement of the TEM sample thickness in order to determine accurately the crystalline thickness of the sample. Consequently, we find that the low-energy milling also resulted in a negligible thickness of electrically inactive regions, approximately 4nm thick. The influence of TEM sample thickness, FIB induced damage and doping concentrations on the accuracy of the OAEH measurements were examined by comparison to secondary ion mass spectrometry measurements as well as to 1D and 3D simulations of the electrostatic potentials. We conclude that for TEM samples down to 100 nm thick, OAEH measurements of Si-based PN junctions, for the doping levels examined here, resulted in quantitative mapping of potential variations, within ~0.1 V. For thinner TEM samples, down to 20 nm thick, mapping of potential variations is qualitative, due to a reduced accuracy of ~0.3 V. This article is dedicated to the memory of Zohar Eliyahou. Copyright © 2014 Elsevier B.V. All rights reserved.

Comparative study of structural and magnetic properties of nano-crystalline Li 0.5Fe 2.5O 4 prepared by various methods

NASA Astrophysics Data System (ADS)

Verma, Vivek; Pandey, Vibhav; Singh, Sukhveer; Aloysius, R. P.; Annapoorni, S.; Kotanala, R. K.

2009-08-01

Lithium ferrite has been considered as one of the highly strategic magnetic material. Nano-crystalline Li 0.5Fe 2.5O 4 was prepared by four different techniques and characterized by X-ray diffraction, vibrating sample magnetometer (VSM), transmission electron microscope (TEM) and Fourier transform infrareds (FTIR). The effect of annealing temperature (700, 900 and 1050 °C) on microstructure has been correlated to the magnetic properties. From X-ray diffraction patterns, it is confirmed that the pure phase of lithium ferrite began to form at 900 °C annealing. The particle size of as-prepared lithium ferrite was observed around 40, 31, 22 and 93 nm prepared by flash combustion, sol-gel, citrate precursor and standard ceramic technique, respectively. Lithium ferrite prepared by citrate precursor method shows a maximum saturation magnetization 67.6 emu/g at 5 KOe.

Polyethyleneimine-modified superparamagnetic Fe3O4 nanoparticles: An efficient, reusable and water tolerance nanocatalyst

NASA Astrophysics Data System (ADS)

Khoobi, Mehdi; Delshad, Tayebeh Modiri; Vosooghi, Mohsen; Alipour, Masoumeh; Hamadi, Hosein; Alipour, Eskandar; Hamedani, Majid Pirali; Sadat ebrahimi, Seyed Esmaeil; Safaei, Zahra; Foroumadi, Alireza; Shafiee, Abbas

2015-02-01

A novel magnetically separable catalyst was prepared based on surface modification of Fe3O4 magnetic nanoparticle (MNPs) with polyethyleneimine (PEI) via covalent bonding. [3-(2,3-Epoxypropoxy)propyl]trimethoxysilane (EPO) was used as cross linker to bond PEI on the surface of MNPs with permanent stability in contrast to PEI coating via electrostatic interactions. The synthesized catalyst was characterized by Fourier transform infrared (FT-IR), thermogravimetric analysis (TGA), X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). The catalyst show high efficiency for one-pot synthesis of 2-amino-3-cyano-4H-pyran derivatives via multi-component reaction (MCR). This procedure offers the advantages of green reaction media, high yield, short reaction time, easy purification of the products and simple recovery and reuse of the catalyst by simple magnetic decantation without significant loss of catalytic activity.

Cysteine-Functionalized Chitosan Magnetic Nano-Based Particles for the Recovery of Light and Heavy Rare Earth Metals: Uptake Kinetics and Sorption Isotherms

PubMed Central

Galhoum, Ahmed A.; Mafhouz, Mohammad G.; Abdel-Rehem, Sayed T.; Gomaa, Nabawia A.; Atia, Asem A.; Vincent, Thierry; Guibal, Eric

2015-01-01

Cysteine-functionalized chitosan magnetic nano-based particles were synthesized for the sorption of light and heavy rare earth (RE) metal ions (La(III), Nd(III) and Yb(III)). The structural, surface, and magnetic properties of nano-sized sorbent were investigated by elemental analysis, FTIR, XRD, TEM and VSM (vibrating sample magnetometry). Experimental data show that the pseudo second-order rate equation fits the kinetic profiles well, while sorption isotherms are described by the Langmuir model. Thermodynamic constants (ΔG°, ΔH°) demonstrate the spontaneous and endothermic nature of sorption. Yb(III) (heavy RE) was selectively sorbed while light RE metal ions La(III) and Nd(III) were concentrated/enriched in the solution. Cationic species RE(III) in aqueous solution can be adsorbed by the combination of chelating and anion-exchange mechanisms. The sorbent can be efficiently regenerated using acidified thiourea. PMID:28347004

Amine-functionalized magnetic mesoporous silica nanoparticles for DNA separation

NASA Astrophysics Data System (ADS)

Sheng, Wei; Wei, Wei; Li, Junjian; Qi, Xiaoliang; Zuo, Gancheng; Chen, Qi; Pan, Xihao; Dong, Wei

2016-11-01

We report a modified approach for the functionalized magnetic mesoporous silica nanoparticles (MMSN) using polymer microspheres incorporated with magnetic nanoparticles in the presence of cetyltrimethylammonium bromide (CTAB) and the core-shell magnetic silica nanoparticles (MSN). These particles were functionalized with amino groups via the addition of aminosilane directly to the particle sol. We then evaluate their DNA separation abilities and find the capacity of DNA binding significantly increased (210.22 μg/mg) compared with normal magnetic silica spheres (138.44 μg/mg) by using an ultraviolet and visible spectrophotometer (UV). The morphologies, magnetic properties, particle size, pore size, core-shell structure and Zeta potential are characterized by Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM), Transmission electron microscopy (TEM), Powder X-ray diffraction (XRD), and dynamic light scattering (DLS). This work demonstrates that our MMSN own an excellent potential application in bioseparation and drug delivery.

Simulation and experimental results of optical and thermal modeling of gold nanoshells.

PubMed

Ghazanfari, Lida; Khosroshahi, Mohammad E

2014-09-01

This paper proposes a generalized method for optical and thermal modeling of synthesized magneto-optical nanoshells (MNSs) for biomedical applications. Superparamagnetic magnetite nanoparticles with diameter of 9.5 ± 1.4 nm are fabricated using co-precipitation method and subsequently covered by a thin layer of gold to obtain 15.8 ± 3.5 nm MNSs. In this paper, simulations and detailed analysis are carried out for different nanoshell geometry to achieve a maximum heat power. Structural, magnetic and optical properties of MNSs are assessed using vibrating sample magnetometer (VSM), X-ray diffraction (XRD), UV-VIS spectrophotometer, dynamic light scattering (DLS), and transmission electron microscope (TEM). Magnetic saturation of synthesized magnetite nanoparticles are reduced from 46.94 to 11.98 emu/g after coating with gold. The performance of the proposed optical-thermal modeling technique is verified by simulation and experimental results. Copyright © 2014 Elsevier B.V. All rights reserved.

Microstructural, Magnetic, and Optical Properties of Pr-Doped Perovskite Manganite La0.67Ca0.33MnO3 Nanoparticles Synthesized via Sol-Gel Process

NASA Astrophysics Data System (ADS)

Xia, Weiren; Wu, Heng; Xue, Piaojie; Zhu, Xinhua

2018-05-01

We report on microstructural, magnetic, and optical properties of Pr-doped perovskite manganite (La1 - xPrx)0.67Ca0.33MnO3 (LPCMO, x = 0.0-0.5) nanoparticles synthesized via sol-gel process. Structural characterizations (X-ray and electron diffraction patterns, (high resolution) TEM images) provide information regarding the phase formation and the single-crystalline nature of the LPCMO systems. X-ray and electron diffraction patterns reveal that all the LPCMO samples crystallize in perovskite crystallography with an orthorhombic structure ( Pnma space group), where the MnO6 octahedron is elongated along the b axis due to the Jahn-Teller effect. That is confirmed by Raman spectra. Crystallite sizes and grain sizes were calculated from XRD and TEM respectively, and the lattice fringes resolved in the high-resolution TEM images of individual LPCMO nanoparticle confirmed its single-crystalline nature. FTIR spectra identify the characteristic Mn-O bond stretching vibration mode near 600 cm- 1, which shifts towards high wavenumbers with increasing post-annealing temperature or Pr-doping concentration, resulting in further distortion of the MnO6 octahedron. XPS revealed dual oxidation states of Mn3+ and Mn4+ in the LPCMO nanoparticles. UV-vis absorption spectra confirm the semiconducting nature of the LPCMO nanoparticles with optical bandgaps of 2.55-2.71 eV. Magnetic measurements as a function of temperature and magnetic field at field cooling and zero-field cooling modes, provided a Curie temperature around 230 K, saturation magnetization of about 81 emu/g, and coercive field of 390 Oe at 10 K. Such magnetic properties and the semiconducting nature of the LPCMO nanoparticles will make them as suitable candidate for magnetic semiconductor spintronics.

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.

In vitro effects of 6 % hydroxyethyl starch 130/0.42 solution on feline whole blood coagulation measured by rotational thromboelastometry.

PubMed

Albrecht, Nathalie A; Howard, Judith; Kovacevic, Alan; Adamik, Katja N

2016-07-26

The artificial colloid, hydroxyethyl starch (HES), is recommended for intravascular volume expansion and colloid-osmotic pressure enhancement in dogs and cats. A well-known side effect of HES solutions in humans and dogs is coagulopathy. However, HES-associated coagulopathy has thus far not been investigated in cats. The goal of this study was to assess the in vitro effects of 6 % HES 130/0.42 on feline whole blood samples using rotational thromboelastometry (ROTEM). A further goal was to develop feline reference intervals for ROTEM at our institution. In this in vitro experimental study, blood samples of 24 adult healthy cats were collected by atraumatic jugular phlebotomy following intramuscular sedation. Baseline ROTEM analyses (using ex-tem, in-tem and fib-tem assays) were performed in duplicate. Additionally, ROTEM analyses were performed on blood samples after dilution with either Ringer's acetate (RA) or 6 % HES 130/0.42 (HES) in a 1:6 dilution (i.e. 1 part solution and 6 parts blood). Coefficients of variation of duplicate measures were below 12 % in all ex-tem assays, 3 of 4 in-tem assays but only 1 of 3 fib-tem assays. Reference intervals were similar albeit somewhat narrower than those previously published. Dilution with both solutions lead to significantly prolonged CT (in-tem), CFT (ex-tem and in-tem), and reduced MCF (ex-tem, in-tem, and fib-tem) and alpha (ex-tem and in-tem). Compared to RA, dilution with HES caused a significant prolongation of CT in fib-tem (P = 0.016), CFT in ex-tem (P = 0.017) and in-tem (P = 0.019), as well as a reduction in MCF in in-tem (P = 0.032) and fib-tem (P = 0.020), and alpha in ex-tem (P = 0.014). However, only a single parameter (CFT in ex-tem) was outside of the established reference interval after dilution with HES. In vitro hemodilution of feline blood with RA and HES causes a small but significant impairment of whole blood coagulation, with HES leading to a significantly greater effect on coagulation than RA. Further studies are necessary to evaluate the in vivo effects and the clinical significance of these findings.

Influence of nickel substitution on crystal structure and magnetic properties of strontium ferrite preparation via sol-gel auto-combustion route

NASA Astrophysics Data System (ADS)

Roohani, Ebrahim; Arabi, Hadi; Sarhaddi, Reza

2018-01-01

In this research, SrFe12-xNixO19 (x = 0 - 1) hexagonal ferrites were prepared by sol-gel auto-combustion method. Effect of Ni substitution on structural, morphological and magnetic properties of nanoparticles was investigated by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM), respectively. The XRD results confirmed that all samples with x ≤ 0.5 have single phase M-type strontium ferrite structure, whereas for the SrFe12-xNixO19 samples with x > 0.5, the spinel NiFe2O4 phase has also appeared. The lattice parameters and crystallite sizes of the powders were concluded from the XRD data and Williamson-Hall method. Magnetic analyses showed that the coercivity of powders decreased from 5672 Oe to 639 Oe while the saturation magnetization increased from 74 emu/g to 81 emu/g with nickel substitution. The results of this study suggest that the strontium hexaferrites doped with Ni are suitable for applications in high density magnetic recording media as well as microwave devices because of their promising magnetic properties.

Prevalence of β-lactam (blaTEM) and Metronidazole (nim) Resistance Genes in the Oral Cavity of Greek Subjects

PubMed Central

Koukos, Georgios; Konstantinidis, Antonios; Tsalikis, Lazaros; Arsenakis, Minas; Slini, Theodora; Sakellari, Dimitra

2016-01-01

Objectives: The aim of this study is to investigate the prevalence of blaTEM and nim genes that encode resistance to β-lactams and nitroimidazoles, respectively, in the oral cavity of systemically healthy Greek subjects. Materials and Methodology: After screening 720 potentially eligible subjects, 154 subjects were recruited for the study, including 50 periodontally healthy patients, 52 cases of gingivitis and 52 cases of chronic periodontitis. The clinical parameters were assessed with an automated probe. Various samples were collected from the tongue, first molars and pockets >6mm, and analysed by polymerase chain reaction-amplification of the blaTEM and nim genes, using primers and conditions previously described in the literature. Results: There was a high rate of detection of blaTEM in plaque and tongue samples alike in all periodontal conditions (37% of plaque and 60% of tongue samples, and 71% of participants). The blaTEM gene was detected more frequently in the tongue samples of the periodontally healthy (56%) and chronic periodontitis (62%) groups compared to the plaque samples from the same groups (36% and 29%, respectively; z-test with Bonferroni corrections-tests, P<0.05). The nim gene was not detected in any of the 343 samples analysed. Conclusion: The oral cavity of Greek subjects often harbours blaTEM but not nim genes, and therefore the antimicrobial activity of β-lactams might be compromised. PMID:27099637

Nonlinear Interactions for Broadband Energy Harvesting

DTIC Science & Technology

2015-04-22

harvesting ,” Journal of Sound and Vibration , V. 331, No. 4, pp. 922– 937. 12. Sah, S.M., Mann, B.P., 2012, “Potential well metamorphosis of a pivoting...Nonlinear non- conservative behavior and modeling of piezoelectric energy harvesters including proof mass effects,” Journal of Intelligent Material...Experimental investigation of a post-buckled piezoelectric beam with an attached central mass used to harvest energy,” Journal of Sys- tems and Control

Probing influence of rare earth ions (Er3+, Dy3+ and Gd3+) on structural, magnetic and optical properties of magnetite nanoparticles

NASA Astrophysics Data System (ADS)

Jain, Richa; Luthra, Vandna; Gokhale, Shubha

2018-06-01

Fe3-xRExO4 (RE = Er, Dy and Gd) nanoparticles with x varying from 0 to 0.1 were synthesized using co-precipitation method. The synthesized nanoparticles were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM) and UV-Vis spectroscopy techniques. TEM images reveal round shaped particles of ∼8-14 nm diameter in case of undoped magnetite (Fe3O4) nanoparticles whereas there is evolution of rod like structures by the doping of RE ions with aspect ratio in the range of 6-16. The room temperature saturation magnetization (Ms) values show gradual increase with doping till a critical doping level which is found to depend on the ionic radius of dopant ion (x = 0.01 for Er, 0.03 for Dy and 0.04 for Gd). There is a variation in the maximum value of saturation magnetization which is directly proportional to the number of unpaired 4f electrons in the dopant element. Low temperature magnetization study, carried out at 5 K and 120 K reveal an increase in the value of Ms as well as coercivity. The direct bandgaps calculated from UV-Visible data are found to decrease with increasing number of unpaired electrons in the dopant ions.

Self-Assembly of Large-Scale Shape-Controlled DNA Nano-Structures

DTIC Science & Technology

2014-12-16

discharged carbon-coated TEM grids for 4 min and then stained for 1 min using a 2% aqueous uranyl formate solution containing 25 mM NaOH. Imaging was...temperature for 3 h in the dark. TEM imaging. For imaging, 2,5 pi annealed sample was adsorbed for 2 min onto glow- discharged , carbon-coated TEM grids...Imaging. For ’I’EM imaging, a 3.S //L sample (l—5 nM) was adsorbed onto glow discharged carbon-coated TEM grids for 4 min and then stained for 1 min or a

Breaking through the bandwidth barrier in distributed fiber vibration sensing by sub-Nyquist randomized sampling

NASA Astrophysics Data System (ADS)

Zhang, Jingdong; Zhu, Tao; Zheng, Hua; Kuang, Yang; Liu, Min; Huang, Wei

2017-04-01

The round trip time of the light pulse limits the maximum detectable frequency response range of vibration in phase-sensitive optical time domain reflectometry (φ-OTDR). We propose a method to break the frequency response range restriction of φ-OTDR system by modulating the light pulse interval randomly which enables a random sampling for every vibration point in a long sensing fiber. This sub-Nyquist randomized sampling method is suits for detecting sparse-wideband- frequency vibration signals. Up to MHz resonance vibration signal with over dozens of frequency components and 1.153MHz single frequency vibration signal are clearly identified for a sensing range of 9.6km with 10kHz maximum sampling rate.

Transmission Electron Microscopy of Vacuum Sensitive, Radiation Sensitive, and Structurally Delicate Materials

NASA Astrophysics Data System (ADS)

Levin, Barnaby

The transmission electron microscope (TEM) is a powerful tool for characterizing the nanoscale and atomic structure of materials, offering insights into their fundamental physical properties. However, TEM characterization requires very thin samples of material to be placed in a high vacuum environment, and exposed to electron radiation. The high vacuum will induce some materials to evaporate or sublimate, preventing them from being accurately characterized, radiation may damage the sample, causing mass loss, or altering its structure, and structurally delicate samples may collapse and break apart when they are thinned for TEM imaging. This dissertation discusses three different projects in which each of these three difficulties pose challenges to TEM characterization of samples. Firstly, we outline strategies for minimizing radiation damage when characterizing materials in TEM at atomic resolution. We consider types of radiation damage, such as vacancy enhanced displacement, that are not included in some previous discussions of beam damage, and we consider how to minimize damage when using new imaging techniques such as annular bright-field scanning TEM. Our methodology emphasizes the general principle that variation of both signal strength and damage cross section must be considered when choosing an experimental electron beam voltage to minimize damage. Secondly, we consider samples containing sulfur, which is prone to sublimation in high vacuum. TEM is routinely used to attempt to characterize the sulfur distribution in lithium-sulfur battery electrodes, but sublimation artifacts can give misleading results. We demonstrate that sulfur sublimation can be suppressed by using cryogenic TEM to characterize sulfur at very low temperatures, or by using the recently developed airSEM to characterize sulfur without exposing it to vacuum. Finally, we discuss the characterization of aging cadmium yellow paint from early 20th century art masterpieces. The binding medium holding paint particles together bends and curls as sample thickness is reduced to 100 nm, making high resolution characterization challenging. We acquire lattice resolution images of the pigment particles through the binder using high voltage zero-loss energy filtered TEM, allowing us to measure the pigment particle size and determine the pigment crystal structure, providing insight into why the paint is aging and how it was synthesized.

High-pressure freezing for scanning transmission electron tomography analysis of cellular organelles.

PubMed

Walther, Paul; Schmid, Eberhard; Höhn, Katharina

2013-01-01

Using an electron microscope's scanning transmission mode (STEM) for collection of tomographic datasets is advantageous compared to bright field transmission electron microscopic (TEM). For image formation, inelastic scattering does not cause chromatic aberration, since in STEM mode no image forming lenses are used after the beam has passed the sample, in contrast to regular TEM. Therefore, thicker samples can be imaged. It has been experimentally demonstrated that STEM is superior to TEM and energy filtered TEM for tomography of samples as thick as 1 μm. Even when using the best electron microscope, adequate sample preparation is the key for interpretable results. We adapted protocols for high-pressure freezing of cultivated cells from a physiological state. In this chapter, we describe optimized high-pressure freezing and freeze substitution protocols for STEM tomography in order to obtain high membrane contrast.

A non-uniformly under-sampled blade tip-timing signal reconstruction method for blade vibration monitoring.

PubMed

Hu, Zheng; Lin, Jun; Chen, Zhong-Sheng; Yang, Yong-Min; Li, Xue-Jun

2015-01-22

High-speed blades are often prone to fatigue due to severe blade vibrations. In particular, synchronous vibrations can cause irreversible damages to the blade. Blade tip-timing methods (BTT) have become a promising way to monitor blade vibrations. However, synchronous vibrations are unsuitably monitored by uniform BTT sampling. Therefore, non-equally mounted probes have been used, which will result in the non-uniformity of the sampling signal. Since under-sampling is an intrinsic drawback of BTT methods, how to analyze non-uniformly under-sampled BTT signals is a big challenge. In this paper, a novel reconstruction method for non-uniformly under-sampled BTT data is presented. The method is based on the periodically non-uniform sampling theorem. Firstly, a mathematical model of a non-uniform BTT sampling process is built. It can be treated as the sum of certain uniform sample streams. For each stream, an interpolating function is required to prevent aliasing in the reconstructed signal. Secondly, simultaneous equations of all interpolating functions in each sub-band are built and corresponding solutions are ultimately derived to remove unwanted replicas of the original signal caused by the sampling, which may overlay the original signal. In the end, numerical simulations and experiments are carried out to validate the feasibility of the proposed method. The results demonstrate the accuracy of the reconstructed signal depends on the sampling frequency, the blade vibration frequency, the blade vibration bandwidth, the probe static offset and the number of samples. In practice, both types of blade vibration signals can be particularly reconstructed by non-uniform BTT data acquired from only two probes.

A Non-Uniformly Under-Sampled Blade Tip-Timing Signal Reconstruction Method for Blade Vibration Monitoring

PubMed Central

Hu, Zheng; Lin, Jun; Chen, Zhong-Sheng; Yang, Yong-Min; Li, Xue-Jun

2015-01-01

High-speed blades are often prone to fatigue due to severe blade vibrations. In particular, synchronous vibrations can cause irreversible damages to the blade. Blade tip-timing methods (BTT) have become a promising way to monitor blade vibrations. However, synchronous vibrations are unsuitably monitored by uniform BTT sampling. Therefore, non-equally mounted probes have been used, which will result in the non-uniformity of the sampling signal. Since under-sampling is an intrinsic drawback of BTT methods, how to analyze non-uniformly under-sampled BTT signals is a big challenge. In this paper, a novel reconstruction method for non-uniformly under-sampled BTT data is presented. The method is based on the periodically non-uniform sampling theorem. Firstly, a mathematical model of a non-uniform BTT sampling process is built. It can be treated as the sum of certain uniform sample streams. For each stream, an interpolating function is required to prevent aliasing in the reconstructed signal. Secondly, simultaneous equations of all interpolating functions in each sub-band are built and corresponding solutions are ultimately derived to remove unwanted replicas of the original signal caused by the sampling, which may overlay the original signal. In the end, numerical simulations and experiments are carried out to validate the feasibility of the proposed method. The results demonstrate the accuracy of the reconstructed signal depends on the sampling frequency, the blade vibration frequency, the blade vibration bandwidth, the probe static offset and the number of samples. In practice, both types of blade vibration signals can be particularly reconstructed by non-uniform BTT data acquired from only two probes. PMID:25621612

Sub-nano tesla magnetic imaging based on room-temperature magnetic flux sensors with vibrating sample magnetometry

NASA Astrophysics Data System (ADS)

Adachi, Yoshiaki; Oyama, Daisuke

2017-05-01

We developed a two-dimensional imaging method for weak magnetic charge distribution using a commercially available magnetic impedance sensor whose magnetic field resolution is 10 pT/Hz1/2 at 10 Hz. When we applied the vibrating sample magnetometry, giving a minute mechanical vibration to the sample and detecting magnetic signals modulated by the vibration frequency, the effects of 1/f noise and the environmental low-frequency band noise were suppressed, and a weak magnetic charge distribution was obtained without magnetic shielding. Furthermore, improvement in the spatial resolution was also expected when the signals were demodulated at the second harmonic frequency of the vibration. In this paper, a preliminary magnetic charge imaging using the vibrating sample magnetometry and its results are demonstrated.

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

NASA Technical Reports Server (NTRS)

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

2016-01-01

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

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

NASA Technical Reports Server (NTRS)

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

2017-01-01

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

Electric shielding films for biased TEM samples and their application to in situ electron holography.

PubMed

Nomura, Yuki; Yamamoto, Kazuo; Hirayama, Tsukasa; Saitoh, Koh

2018-06-01

We developed a novel sample preparation method for transmission electron microscopy (TEM) to suppress superfluous electric fields leaked from biased TEM samples. In this method, a thin TEM sample is first coated with an insulating amorphous aluminum oxide (AlOx) film with a thickness of about 20 nm. Then, the sample is coated with a conductive amorphous carbon film with a thickness of about 10 nm, and the film is grounded. This technique was applied to a model sample of a metal electrode/Li-ion-conductive-solid-electrolyte/metal electrode for biasing electron holography. We found that AlOx film with a thickness of 10 nm has a large withstand voltage of about 8 V and that double layers of AlOx and carbon act as a 'nano-shield' to suppress 99% of the electric fields outside of the sample. We also found an asymmetry potential distribution between high and low potential electrodes in biased solid-electrolyte, indicating different accumulation behaviors of lithium-ions (Li+) and lithium-ion vacancies (VLi-) in the biased solid-electrolyte.

Studies on magnetic properties of chemically synthesized crystalline calcium ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Debnath, A.; Bera, A.; Chattopadhyay, K. K.; Saha, B.

2016-05-01

Spinel-type ferrites have taken a very important role for modern electronic industry. Most of these ferrites exhibit low-loss dielectric properties, high resistivity, low eddy current and also high temperature ferromagnetism. Calcium ferrite is one such important metal oxide which is environmentally safe, chemically stable, low cost and greatly abundant. This outstanding material of calcium ferrite is synthesized by a simple chemical precipitation method using NaOH as the precipitating agent. Ferric chloride anhydrous (FeCl3) and Calcium chloride dihydrate (CaCl2.2H2O) were used as iron and calcium sources respectively. The samples were heated at 200°C for 8h to obtain homogeneous powder of Calcium ferrite. The powders were characterized by using X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), Transmission electrical microscopy (TEM), and Fourier transform infrared spectroscopic (FTIR) measurements. The polycrystalline nature of the sample was confirmed by X-ray diffraction study. The magnetic properties of the sample were investigated by vibrating sample magnetometer (VSM) measurements. Magnetization curve of the prepared sample depicts that as synthesized calcium ferrite nanoparticles have saturation magnetic moment of 1.74 emu/g and the coercivity of 35.08 Oe with superparamagnetic behavior. The synthesized calcium ferrite nanoparticles with such magnetic properties will be a candidate material for different applications in electronics and exploring its functionality in the field of recently developing semiconductor device physics and spintronics.

Frontiers of in situ electron microscopy

DOE PAGES

Zheng, Haimei; Zhu, Yimei; Meng, Shirley Ying

2015-01-01

In situ transmission electron microscopy (TEM) has become an increasingly important tool for materials characterization. It provides key information on the structural dynamics of a material during transformations and the correlation between structure and properties of materials. With the recent advances in instrumentation, including aberration corrected optics, sample environment control, the sample stage, and fast and sensitive data acquisition, in situ TEM characterization has become more and more powerful. In this article, a brief review of the current status and future opportunities of in situ TEM is included. It also provides an introduction to the six articles covered by inmore » this issue of MRS Bulletin explore the frontiers of in situ electron microscopy, including liquid and gas environmental TEM, dynamic four-dimensional TEM, nanomechanics, ferroelectric domain switching studied by in situ TEM, and state-of-the-art atomic imaging of light elements (i.e., carbon atoms) and individual defects.« less

Preparation and magnetic properties of nano size nickel ferrite particles using hydrothermal method

PubMed Central

2012-01-01

Background Nickel ferrite, a kind of soft magnetic materials is one of the most attracting class of materials due to its interesting and important properties and has many technical applications, such as in catalysis, sensors and so on. In this paper the synthesis of NiFe2O4 nanoparticles by the hydrothermal method is reported and the inhibition of surfactant (Glycerol or Sodium dodecyl sulfate) on the particles growth is investigated. Methods For investigation of the inhibition effect of surfactant on NiFe2O4 particles growth, the samples were prepared in presence of Glycerol and Sodium dodecyl sulfate. The X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM) and inductively coupled plasma atomic emission spectrometer (ICP-AES) techniques were used to characterize the samples. Results The results of XRD and ICP-AES show that the products were pure NiFe2O4 and also nanoparticles grow with increasing the temperature, while surfactant prevents the particle growth under the same condition. The average particle size was determined from the Scherrer's equation and TEM micrographs and found to be in the range of 50-60 nm that decreased up to 10-15 nm in presence of surfactant. The FT-IR results show two absorption bands near to 603 and 490 cm-1 for the tetrahedral and octahedral sites respectively. Furthermore, the saturated magnetization and coercivity of NiFe2O4 nanoparticles were in the range of 39.60 emu/g and 15.67 Qe that decreased for samples prepared in presence of surfactant. As well as, the nanoparticles exhibited a superparamagnetic behavior at room temperature. Conclusions Nanosized nickel ferrite particles were synthesized with and without surfactant assisted hydrothermal methods. The results show that with increasing of temperature, the crystallinity of nanoparticles is increased. In the presence of surfactants, the crystallinity of NiFe2O4 nanoparticles decreased in comparison with surfactant- free prepared samples. All of the nickel ferrite nanoparticles were superparamagnetic at room temperature. Graphical abstract PMID:22462726

Preparation and magnetic properties of nano size nickel ferrite particles using hydrothermal method.

PubMed

Nejati, Kamellia; Zabihi, Rezvanh

2012-03-30

Nickel ferrite, a kind of soft magnetic materials is one of the most attracting class of materials due to its interesting and important properties and has many technical applications, such as in catalysis, sensors and so on. In this paper the synthesis of NiFe2O4 nanoparticles by the hydrothermal method is reported and the inhibition of surfactant (Glycerol or Sodium dodecyl sulfate) on the particles growth is investigated. For investigation of the inhibition effect of surfactant on NiFe2O4 particles growth, the samples were prepared in presence of Glycerol and Sodium dodecyl sulfate. The X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM) and inductively coupled plasma atomic emission spectrometer (ICP-AES) techniques were used to characterize the samples. The results of XRD and ICP-AES show that the products were pure NiFe2O4 and also nanoparticles grow with increasing the temperature, while surfactant prevents the particle growth under the same condition. The average particle size was determined from the Scherrer's equation and TEM micrographs and found to be in the range of 50-60 nm that decreased up to 10-15 nm in presence of surfactant. The FT-IR results show two absorption bands near to 603 and 490 cm-1 for the tetrahedral and octahedral sites respectively. Furthermore, the saturated magnetization and coercivity of NiFe2O4 nanoparticles were in the range of 39.60 emu/g and 15.67 Qe that decreased for samples prepared in presence of surfactant. As well as, the nanoparticles exhibited a superparamagnetic behavior at room temperature. Nanosized nickel ferrite particles were synthesized with and without surfactant assisted hydrothermal methods. The results show that with increasing of temperature, the crystallinity of nanoparticles is increased. In the presence of surfactants, the crystallinity of NiFe2O4 nanoparticles decreased in comparison with surfactant- free prepared samples. All of the nickel ferrite nanoparticles were superparamagnetic at room temperature. GRAPHICAL

RECENT DEVELOPMENT IN TEM CHARACTERIZATION OF IRRADIATED RERTR FUELS

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

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

2011-10-01

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

Effect of Ca substitution on some physical properties of nano-structured and bulk Ni-ferrite samples

NASA Astrophysics Data System (ADS)

Assar, S. T.; Abosheiasha, H. F.

2015-01-01

Nanoparticles of Ni1-xCaxFe2O4 (x=0.0, 0.02, 0.04, 0.06 and 0.10) were prepared by citrate precursor method. A part of these samples was sintered at 600 °C for 2 h in order to keep the particles within the nano-size while the other part was sintered at 1000 °C to let the particles to grow to the bulk size. The effect of Ca2+ ion substitution in nickel ferrite on some structural, magnetic, electrical and thermal properties was investigated. All samples were characterized by using X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer (VSM). A two probe method was used to measure the dc electrical conductivity whereas the photoacoustic (PA) technique was used to determine the thermal diffusivity of the samples. To interpret different experimental results for nano and bulk samples some cation distributions were assumed based on the VSM and XRD data. These suggested cation distributions give logical explanations for other experimental results such as the observed values of the absorption bands in FTIR spectra and the dc conductivity results. Finally, in the thermal measurements it was found that increasing the Ca2+ ion content causes a decrease in the thermal diffusivity of both nano and bulk samples. The explanation of this behavior is ascribed to the phonon-phonon scattering.

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

Prevalence and characteristics of vibrator use among women who have sex with women.

PubMed

Schick, Vanessa; Herbenick, Debby; Rosenberger, Joshua G; Reece, Michael

2011-12-01

Research suggests that vibrator use may be more prevalent among lesbian/bisexual-identified women. However, previous research has been limited by small samples of lesbian- and bisexual-identified women and has not focused specifically on the characteristics of vibrator use between women. The present study was designed in order to develop a comprehensive understanding of women's use of vibrators with their female sexual partners and to understand the extent to which vibrator use is related to their sexual experiences. Data were collected via a cross-sectional web-based survey from 2,192 women living in the United States and the United Kingdom. All participants reported engaging in sexual behavior with only women in the previous year. Sociodemographic characteristics, vibrator use history, vibrator use perceptions, and the Female Sexual Function Index (FSFI). Over three-quarters of women in the sample reported a history of vibrator use during solo masturbation/with a female partner and over a quarter of the sample reported use in the previous month. Participants who were older, white, and in a long-term relationship were the most likely to use a vibrator with a female partner in the previous year. Vibrator use lifetime history was unrelated to all FSFI subscales with the exception of pain for lesbian and queer-identified women. In contrast to lifetime use, participants who used a vibrator with a female sexual partner in the previous month scored higher on several of the FSFI domains than women who reported no vibrator use or vibrator use only during solo masturbation in the past month. Vibrator use was common among this sample of women who have sex with women. Women who reported recent vibrator use with other women had higher mean sexual functioning scores than women who reported no vibrator use or vibrator use only during masturbation. Implications for health-care providers are discussed. © 2011 International Society for Sexual Medicine.

Characterization of Friction Joints Subjected to High Levels of Random Vibration

NASA Technical Reports Server (NTRS)

deSantos, Omar; MacNeal, Paul

2012-01-01

This paper describes the test program in detail including test sample description, test procedures, and vibration test results of multiple test samples. The material pairs used in the experiment were Aluminum-Aluminum, Aluminum- Dicronite coated Aluminum, and Aluminum-Plasmadize coated Aluminum. Levels of vibration for each set of twelve samples of each material pairing were gradually increased until all samples experienced substantial displacement. Data was collected on 1) acceleration in all three axes, 2) relative static displacement between vibration runs utilizing photogrammetry techniques, and 3) surface galling and contaminant generation. This data was used to estimate the values of static friction during random vibratory motion when "stick-slip" occurs and compare these to static friction coefficients measured before and after vibration testing.

Electrical, structural and thermal studies of carbon nanotubes from natural legume seeds: kala chana

NASA Astrophysics Data System (ADS)

Ranu, Rachana; Chauhan, Yatishwar; Singh, Pramod K.; Bhattacharya, B.; Tomar, S. K.

2016-12-01

Carbon nanotubes (CNTs) are the carbon materials measured at nanoscale level and they are defined in two types according to the number of concentric layers, i.e. single-layer tube is single-walled nanotubes, while multi-layer tube structure is called multi-walled nanotubes. The green method synthesis for the preparation of CNTs begins with the smashing of legume seeds kala chana, and then they form complex with cobalt salt. Desiccation of the complex compound forms cobalt salt and seed protein. The complex is then decomposed at 625 °C in muffle furnace for 20 min. Purification of the decomposed sample is done through acid wash treatment and dried in vacuum oven. The confirmations of CNTs are done by nuclear magnetic resonance and Fourier transform infrared, which analyzes the denatured protein, reacted to the metal salt. X-Ray diffraction determines the MWNTs with transmission electron microscope (TEM) reports the network structure of CNTs. thermal gravimetric analysis (TGA)-differential thermal analysis (DTA)-thermogravimetric analysis (DTG) tests the amount of sample under thermal treatment. Vibrating sample magnetometer determines the paramagnetic nature of CNTs. CNTs thus prepared can be used in mechanical fields, in solar cells, in electronics fields, etc. because of their multidisciplinary properties. The synthesized CNTs are eco-friendly in nature, prepared by the legume seed natural precursor.

Functionalization of SBA-15 mesoporous silica by Cu-phosphonate units: Probing of synthesis route

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

Laskowski, Lukasz, E-mail: lukasz.laskowski@kik.pcz.pl; Czestochowa University of Technology, Institute of Physics, Al. Armii Krajowej 19, 42-201 Czestochowa; Laskowska, Magdalena, E-mail: magdalena.laskowska@onet.pl

2014-12-15

Mesoporous silica SBA-15 containing propyl-copper phosphonate units was investigated. The structure of mesoporous samples was tested by N{sub 2} isothermal sorption (BET and BHJ analysis), TEM microscopy and X-Ray scattering. Quantitative analysis EDX has given information about proportions between component atoms in the sample. Quantitative elemental analysis has been carried out to support EDX. To examine bounding between copper atoms and phosphonic units the Raman spectroscopy was carried out. As a support of Raman scattering, the theoretical calculations were made based on density functional theory, with the B3LYP method. By comparison of the calculated vibrational spectra of the molecule withmore » experimental results, distribution of the active units inside silica matrix has been determined. - Graphical abstract: The present study is devoted to mesoporous silica SBA-15 containing propyl-copper phosphonate units. The species were investigated to confirm of synthesis procedure correctness by the micro-Raman technique combined with DFT numerical simulations. Complementary research was carried out to test the structure of mesoporous samples. - Highlights: • SBA-15 silica functionalized with propyl-copper phosphonate units was synthesized. • Synthesis efficiency probed by Raman study supported with DFT simulations. • Homogenous distribution of active units was proved. • Synthesis route enables precise control of distance between copper ions.« less

Preparation and characterization of magnetic Wells-Dawson heteropoly acid nanoparticles for magnetic solid-phase extraction of aromatic amines in water samples.

PubMed

Amiri, Amirhassan; Saadati-Moshtaghin, Hamid Reza; Zonoz, Farokhzad Mohammadi; Targhoo, Azadeh

2017-02-03

In this work, aminopropyl modified silica-coated magnetite nanoparticles with Wells-Dawson heteropoly acid (P 2 W 17 Fe@APSCMNPs) was first synthesized and underwent highly efficient magnetic solid-phase extraction (MSPE) of aromatic amines from aqueous samples. The resulted nanomaterials were characterized with different physicochemical techniques such as Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). Aniline, N,N-dimethylaniline, o-toluidine and 3-chloroaniline were selected as target compounds. The sample quantification was carried out using gas chromatography-flame ionization detector (GC-FID). Under optimal working conditions, the developed method showed good linearity (R>0.9912) in the range of 0.01-100ngmL -1 . The method displays detection limits (at an S/N ration of 3) in the range from 0.003 to 0.01ngmL -1 , and the limits of quantification (at an S/N ratio of 10) are between 0.01 and 0.04ngmL -1 . The enrichment factors (EFs) were in the range of 75-113. Relative standard deviations (RSDs) are 4.8-8.3%. The applicability of the developed method was examined by analyzing different water samples (river water, tap water, well water and wastewater) and the relative recovery values for the spiked water samples were found to be in the range of 90.7-99.8%. Copyright © 2016 Elsevier B.V. All rights reserved.

Immobilization of Magnetic Nanoparticles onto Amine-Modified Nano-Silica Gel for Copper Ions Remediation

PubMed Central

Elkady, Marwa; Hassan, Hassan Shokry; Hashim, Aly

2016-01-01

A novel nano-hybrid was synthesized through immobilization of amine-functionalized silica gel nanoparticles with nanomagnetite via a co-precipitation technique. The parameters, such as reagent concentrations, reaction temperature and time, were optimized to accomplish the nano-silica gel chelating matrix. The most proper amine-modified silica gel nanoparticles were immobilized with magnetic nanoparticles. The synthesized magnetic amine nano-silica gel (MANSG) was established and characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared (FTIR), thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC) and vibrating sample magnetometry (VSM). The feasibility of MANSG for copper ions’ remediation from wastewater was examined. MANSG achieves a 98% copper decontamination from polluted water within 90 min. Equilibrium sorption of copper ions onto MANSG nanoparticles obeyed the Langmuir equation compared to the Freundlich, Temkin, Elovich and Dubinin-Radushkevich (D-R) equilibrium isotherm models. The pseudo-second-order rate kinetics is appropriate to describe the copper sorption process onto the fabricated MANSG. PMID:28773583

Synthesis, Characterization and Cytotoxicity of Novel Multifunctional Fe3O4@SiO2@GdVO4:Dy3+ Core-Shell Nanocomposite as a Drug Carrier

PubMed Central

Li, Bo; Fan, Huitao; Zhao, Qiang; Wang, Congcong

2016-01-01

In this study, multifunctional Fe3O4@SiO2@GdVO4:Dy3+ nanocomposites were successfully synthesized via a two-step method. Their structure, luminescence and magnetic properties were characterized by X-ray diffraction (XRD), scanning electronic microscope (SEM), transmission electron microscopy (TEM), photoluminescence (PL) spectra and vibrating sample magnetometer (VSM). The results indicated that the as-prepared multifunctional composites displayed a well-defined core-shell structure. The composites show spherical morphology with a size distribution of around 360 nm. Additionally, the composites exhibit high saturation magnetization (20.40 emu/g) and excellent luminescence properties. The inner Fe3O4 cores and the outer GdVO4:Dy3+ layers endow the composites with good responsive magnetic properties and strong fluorescent properties, which endow the nanoparticles with great potential applications in drug delivery, magnetic resonance imaging, and marking and separating of cells in vitro. PMID:28773275

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.

Synthesis, characterization and microwave characteristics of ATP/BaFe12O19/PANI ternary composites

NASA Astrophysics Data System (ADS)

Bai, Dezhong; Feng, Huixia; Chen, Nali; Tan, Lin; Qiu, Jianhui

2018-07-01

In this paper, we introduced attapulgite (ATP) into the system of ferrite composites for the first time. By sol-gel self-propagating combustion method, attapulgite/barium ferrite (ATP/BaFe12O19) was prepared, and then ternary composites of attapulgite/barium ferrite/polyaniline (ATP/BaFe12O19/PANI) were obtained by in-situ oxidative polymerization of aniline on ATP/BaFe12O19 mixture. The phase composition, morphology and electromagnetic properties of the as-prepared composites were characterized by X-ray diffraction (XRD), Transmission election microscope (TEM), Fourier transform infrared (FTIR), vibrating sample magnetometer (VSM) and vector network analyzer (VNA). We found that the ATP/BaFe12O19/PANI composites at a thickness of 2 mm have the minimum reflection loss of -11.89 dB at 11.28 GHz, besides the effective absorption bandwidth (less than -5 dB) reached 6.39 GHz (from 8.42 GHz to 14.81 GHz).

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.

Synthesis and characterization of barium hexaferrite with manganese (Mn) doping material as anti-radar

NASA Astrophysics Data System (ADS)

Susilawati, Doyan, Aris; Khalilurrahman

2017-01-01

Have been successfully synthesized barium powder doping Manganese hexaferrite with the expected potential as anti-radar material. Synthesis was done by using the co-precipitation method, the variation of the variable x concentrations used were 0; 0.2; 0.4; and 0.6 and calcined at temperatures of 400, 600 and 800°C. Characterization powders of hexaferrite have used XRD (X-Ray Diffraction), SEM (Scanning Electron Microscopy), TEM (Transmission Electron Microscopy), LCR (inductance, capacitance, and resistance) meter, and VSM (Vibrating Sample Magnetometer). The higher the concentration and temperature of calcinations given affect the color of the powder. The test results using XRD indicates that it has formed barium hexaferrite phase with a hexagonal crystal structure. Tests using SEM showed that all the constituent elements barium powder hexaferrite by doping Manganese powders have been spread evenly. XRD test results were confirmed by a test using a TEM showing the crystal structure and the powder was sized nano particles. The results from the LCR meter showed that the barium powder hexaferrite by doping Manganese that has been synthesized classified in semiconductor materials. The result from VSM showed that the value of coercivity magnetic powder doped barium hexaferrite Manganese is smaller when compared with barium hexaferrite without doping and belong to the soft magnetic. Based on the results of the synthesis and characterization, we can conclude that the barium powder heksaferrite by doping Manganese potential as a material anti-radar.

Synthesis and characterization of arsenic-doped cysteine-capped thoria-based nanoparticles

NASA Astrophysics Data System (ADS)

Pereira, F. J.; Díez, M. T.; Aller, A. J.

2013-09-01

Thoria materials have been largely used in the nuclear industry. Nonetheless, fluorescent thoria-based nanoparticles provide additional properties to be applied in other fields. Thoria-based nanoparticles, with and without arsenic and cysteine, were prepared in 1,2-ethanediol aqueous solutions by a simple precipitation procedure. The synthesized thoria-based nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (ED-XRS), Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy and fluorescence microscopy. The presence of arsenic and cysteine, as well as the use of a thermal treatment facilitated fluorescence emission of the thoria-based nanoparticles. Arsenic-doped and cysteine-capped thoria-based nanoparticles prepared in 2.5 M 1,2-ethanediol solutions and treated at 348 K showed small crystallite sizes and strong fluorescence. However, thoria nanoparticles subjected to a thermal treatment at 873 K also produced strong fluorescence with a very narrow size distribution and much smaller crystallite sizes, 5 nm being the average size as shown by XRD and TEM. The XRD data indicated that, even after doping of arsenic in the crystal lattice of ThO2, the samples treated at 873 K were phase pure with the fluorite cubic structure. The Raman and FT-IR spectra shown the most characteristics vibrational peaks of cysteine together with other peaks related to the bonds of this molecule to thoria and arsenic when present.

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.

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.

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.

Synthesis and characterization of Cu0.3Zn0.5Mg0.2Fe2O4 nanoparticles as a magnetic drug delivery system

NASA Astrophysics Data System (ADS)

Ansari, Mohammad; Bigham, Ashkan; Hassanzadeh-Tabrizi, S. A.; Abbastabar Ahangar, H.

2017-10-01

Mixed spinel ferrite nanoparticles are being applied in biomedical applications due to their biocompatibility, antibacterial activity, particular magnetic and electronic properties with chemical and thermal stabilities. The Cu0.3Zn0.5Mg0.2Fe2O4 nanoparticles are synthesized through the thermal treatment method. Polyvinyl alcohol (PVA) is used as the capping agent to stabilize the particles and prevent their agglomeration. The synthesized nanoparticles are characterized through X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), N2 adsorption-desorption, field emission scanning electron microscopy (FESEM), and transmission electron microscope (TEM). The magnetic characterization is made on a vibrating sample magnetometer (VSM), which displayed super-paramagnetic behavior of the synthesized sample. Potential application of the Cu0.3Zn0.5Mg0.2Fe2O4 nanoparticles as a drug delivery agent is assessed in vitro by estimating their release properties. The obtained results indicate that the amount of ibuprofen (IBU) adsorbed into the nanocarrier of Cu0.3Zn0.5Mg0.2Fe2O4 is 104 mg/g and the drug release is sustained up to 72 h.

Enhanced sonocatalytic degradation of organic dyes from aqueous solutions by novel synthesis of mesoporous Fe3O4-graphene/ZnO@SiO2 nanocomposites.

PubMed

Areerob, Yonrapach; Cho, Ju Yong; Jang, Won Kweon; Oh, Won-Chun

2018-03-01

Fe 3 O 4 -graphene/ZnO@mesoporous-SiO 2 (MGZ@SiO 2 ) nanocomposites was synthesized via a simple one pot hydrothermal method. The as-obtained samples were investigated using various techniques, as follows: scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and specific surface area (BET) vibrating sample magnetometer (VSM), among others. The sonocatalytic activities of the catalysts were tested according to the oxidation for the removal of methylene blue (MB), methyl orange (MO), and rhodamine B (RhB) under ultrasonic irradiation. The optimal conditions including the irradiation time, pH, dye concentration, catalyst dosage, and ultrasonic intensity are 60min, 11, 50mg/L, 1.00g/L, and 40W/m 2 , respectively. The MGZ@SiO 2 showed the higher enhanced sonocatalytic degradation from among the three dyes; furthermore, the sonocatalytic-degradation mechanism is discussed. This study shows that the MGZ@SiO 2 can be applied asa novel-design catalyst for the removal of organic pollutants from aqueous solutions. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis and characterization of polyvinylimidazole-grafted superparamagnetic iron oxide nanoparticles (Si-PVIm-grafted SPION)

NASA Astrophysics Data System (ADS)

Erdemi, H.; Sözeri, H.; Şenel, M.; Baykal, A.

2012-08-01

Polyvinylimidazole (PVIm)-grafted superparamagnetic iron oxide nanoparticles (SPION) (Si-PVIm-grafted Fe3O4 NPs) were prepared by grafting of telomere of PVIm on the SPION. The product identified as magnetite, which has an average crystallite size of 9 ± 2 nm as estimated from X-ray line profile fitting. Particle size was estimated as 10.0 ± 0.5 nm from TEM micrographs. Mean particle size is found as 8.4 ± 1.0 nm which agrees well with the values calculated from XRD patterns (9 ± 2 nm). Vibrating Sample Magnetometer (VSM) analysis explained the superparamagnetic nature of the nanocomposite. Thermogravimetric analysis showed that the Si-Imi is 25 % of the Si-PVIm-grafted SPION, which means an inorganic content is about 75 %. Detailed electrical and dielectric properties of the properties of the product are also presented. The conductivity of the sample increases significantly with temperature and has the value in the range of 1.14 × 10-7-1.78 × 10-4 S cm-1. Analysis of the real and imaginary parts of the permittivities indicated temperature and frequency dependency representing interfacial polarization and temperature-assisted reorganization effects.

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.

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

Yashchuk, Valeriy V; Conley, Raymond; Anderson, Erik H.

We discuss the results of SEM and TEM measurements with the BPRML test samples fabricated from a BPRML (WSi2/Si with fundamental layer thickness of 3 nm) with a Dual Beam FIB (focused ion beam)/SEM technique. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML test samples can be used to characterize x-raymore » microscopes. Corresponding work with x-ray microscopes is in progress.« less

The Shock and Vibration Digest. Volume 18, Number 10

DTIC Science & Technology

1986-10-01

STRUCTURAL SYSTEMS BRIDGES 86-1882 Analysis of the Observed Seismic Response of a Highway Bridge J.C. Wilson 34 ■>:--;■- fWVW^VWUiWlWWI...3), pp 339-354 (May-June 1986) 10 fig«, 6 table«, 24 ref« KEY WORDS; Bridge «, Seumic re»pon«e, Sy«tem identification techniques...Strong-motion accelerograms obtained on separa- tion bridge during a 19 79 California earthquake are used to examine the response of this multi- ple

Unusual structural transition of antimicrobial VP1 peptide.

PubMed

Shanmugam, Ganesh; Phambu, Nsoki; Polavarapu, Prasad L

2011-05-01

VP1 peptide, an active domain of m-calpain enzyme with antimicrobial activity is found to undergo an unusual conformational transition in trifluoroethanol (TFE) solvent. The nature of, and time dependent variations in, circular dichroism associated with the amide I vibrations, suggest that VP1 undergoes self-aggregation forming anti-parallel β-sheet structure in TFE. Transmission electron micrograph (TEM) images revealed that β-sheet aggregates formed by VP1 possess fibril-like assemblies. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

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

PubMed

Sáfrán, György

2018-04-01

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

Microstructural, Magnetic, and Optical Properties of Pr-Doped Perovskite Manganite La0.67Ca0.33MnO3 Nanoparticles Synthesized via Sol-Gel Process.

PubMed

Xia, Weiren; Wu, Heng; Xue, Piaojie; Zhu, Xinhua

2018-05-04

We report on microstructural, magnetic, and optical properties of Pr-doped perovskite manganite (La 1 - x Pr x ) 0.67 Ca 0.33 MnO 3 (LPCMO, x = 0.0-0.5) nanoparticles synthesized via sol-gel process. Structural characterizations (X-ray and electron diffraction patterns, (high resolution) TEM images) provide information regarding the phase formation and the single-crystalline nature of the LPCMO systems. X-ray and electron diffraction patterns reveal that all the LPCMO samples crystallize in perovskite crystallography with an orthorhombic structure (Pnma space group), where the MnO 6 octahedron is elongated along the b axis due to the Jahn-Teller effect. That is confirmed by Raman spectra. Crystallite sizes and grain sizes were calculated from XRD and TEM respectively, and the lattice fringes resolved in the high-resolution TEM images of individual LPCMO nanoparticle confirmed its single-crystalline nature. FTIR spectra identify the characteristic Mn-O bond stretching vibration mode near 600 cm - 1 , which shifts towards high wavenumbers with increasing post-annealing temperature or Pr-doping concentration, resulting in further distortion of the MnO 6 octahedron. XPS revealed dual oxidation states of Mn 3+ and Mn 4+ in the LPCMO nanoparticles. UV-vis absorption spectra confirm the semiconducting nature of the LPCMO nanoparticles with optical bandgaps of 2.55-2.71 eV. Magnetic measurements as a function of temperature and magnetic field at field cooling and zero-field cooling modes, provided a Curie temperature around 230 K, saturation magnetization of about 81 emu/g, and coercive field of 390 Oe at 10 K. Such magnetic properties and the semiconducting nature of the LPCMO nanoparticles will make them as suitable candidate for magnetic semiconductor spintronics.

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.

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.

A novel multi-scale adaptive sampling-based approach for energy saving in leak detection for WSN-based water pipelines

NASA Astrophysics Data System (ADS)

Saqib, Najam us; Faizan Mysorewala, Muhammad; Cheded, Lahouari

2017-12-01

In this paper, we propose a novel monitoring strategy for a wireless sensor networks (WSNs)-based water pipeline network. Our strategy uses a multi-pronged approach to reduce energy consumption based on the use of two types of vibration sensors and pressure sensors, all having different energy levels, and a hierarchical adaptive sampling mechanism to determine the sampling frequency. The sampling rate of the sensors is adjusted according to the bandwidth of the vibration signal being monitored by using a wavelet-based adaptive thresholding scheme that calculates the new sampling frequency for the following cycle. In this multimodal sensing scheme, the duty-cycling approach is used for all sensors to reduce the sampling instances, such that the high-energy, high-precision (HE-HP) vibration sensors have low duty cycles, and the low-energy, low-precision (LE-LP) vibration sensors have high duty cycles. The low duty-cycling (HE-HP) vibration sensor adjusts the sampling frequency of the high duty-cycling (LE-LP) vibration sensor. The simulated test bed considered here consists of a water pipeline network which uses pressure and vibration sensors, with the latter having different energy consumptions and precision levels, at various locations in the network. This is all the more useful for energy conservation for extended monitoring. It is shown that by using the novel features of our proposed scheme, a significant reduction in energy consumption is achieved and the leak is effectively detected by the sensor node that is closest to it. Finally, both the total energy consumed by monitoring as well as the time to detect the leak by a WSN node are computed, and show the superiority of our proposed hierarchical adaptive sampling algorithm over a non-adaptive sampling approach.

Studies on magnetic properties of chemically synthesized crystalline calcium ferrite nanoparticles

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

Debnath, A., E-mail: debnathanimesh@gmail.com; Bera, A.; Saha, B.

Spinel-type ferrites have taken a very important role for modern electronic industry. Most of these ferrites exhibit low-loss dielectric properties, high resistivity, low eddy current and also high temperature ferromagnetism. Calcium ferrite is one such important metal oxide which is environmentally safe, chemically stable, low cost and greatly abundant. This outstanding material of calcium ferrite is synthesized by a simple chemical precipitation method using NaOH as the precipitating agent. Ferric chloride anhydrous (FeCl{sub 3}) and Calcium chloride dihydrate (CaCl{sub 2}.2H{sub 2}O) were used as iron and calcium sources respectively. The samples were heated at 200°C for 8h to obtain homogeneousmore » powder of Calcium ferrite. The powders were characterized by using X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), Transmission electrical microscopy (TEM), and Fourier transform infrared spectroscopic (FTIR) measurements. The polycrystalline nature of the sample was confirmed by X-ray diffraction study. The magnetic properties of the sample were investigated by vibrating sample magnetometer (VSM) measurements. Magnetization curve of the prepared sample depicts that as synthesized calcium ferrite nanoparticles have saturation magnetic moment of 1.74 emu/g and the coercivity of 35.08 Oe with superparamagnetic behavior. The synthesized calcium ferrite nanoparticles with such magnetic properties will be a candidate material for different applications in electronics and exploring its functionality in the field of recently developing semiconductor device physics and spintronics.« less

Structural, microstructural and vibrational analyses of the monoclinic tungstate BiLuWO{sub 6}

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

Ait Ahsaine, H.; Taoufyq, A.; Institut Matériaux Microélectronique et Nanosciences de Provence, IM2NP, UMR CNRS 7334, Université de Toulon, BP 20132, 83957 La Garde Cedex

2014-10-15

The bismuth lutetium tungstate phase BiLuWO{sub 6} has been prepared using a solid state route with stoichiometric mixtures of oxide precursors. The obtained polycrystalline phase has been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy. In the first step, the crystal structure has been refined using Rietveld method: the crystal cell was resolved using monoclinic system (parameters a, b, c, β) with space group A2/m. SEM images showed the presence of large crystallites with a constant local nominal composition (BiLuW). TEM analyses showed that the actual local structure could be better representedmore » by a superlattice (a, 2b, c, β) associated with space groups P2 or P2/m. The Raman spectroscopy showed the presence of vibrational bands similar to those observed in the compounds BiREWO{sub 6} with RE=Y, Gd, Nd. However, these vibrational bands were characterized by large full width at half maximum, probably resulting from the long range Bi/Lu disorder and local WO{sub 6} octahedron distortions in the structure. - Graphical abstract: The average structure of BiLuWO{sub 6} determined from X-ray diffraction data can be represented by A2/m space group. Experimental Electron Diffraction patterns along the [0vw] zone axes of the monoclinic structure and associated simulated patterns show the existence of a monoclinic superstructure with space group P2 or P2/m. - Highlights: • A new monoclinic BiLuWO{sub 6} phase has been elaborated from solid-state reaction. • The space group of the monoclinic disordered average structure should be A2/m. • Transmission electron microscopy leads to a superlattice with P2/m space group. • Raman spectroscopy suggests existence of local disorder.« less

Ni-CeO2 spherical nanostructures for magnetic and electrochemical supercapacitor applications.

PubMed

Murugan, Ramachandran; Ravi, Ganesan; Vijayaprasath, Gandhi; Rajendran, Somasundharam; Thaiyan, Mahalingam; Nallappan, Maheswari; Gopalan, Muralidharan; Hayakawa, Yasuhiro

2017-02-08

The synthesis of nanoparticles has great control over the structural and functional characteristics of materials. In this study, CeO 2 and Ni-CeO 2 spherical nanoparticles were prepared using a microwave-assisted method. The prepared nanoparticles were characterized via thermogravimetry, X-ray diffraction (XRD), Raman, FTIR, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), vibrating sample magnetometry (VSM) and cyclic voltammetry (CV). The pure CeO 2 sample exhibited a flake-like morphology, whereas Ni-doped CeO 2 showed spherical morphology with uniform shapes. Spherical morphologies for the Ni-doped samples were further confirmed via TEM micrographs. Thermogravimetric analyses revealed that decomposition varies with Ni-doping in CeO 2 . XRD revealed that the peak shifts towards lower angles for the Ni-doped samples. Furthermore, a diamagnetic to ferromagnetic transition was observed in Ni-doped CeO 2 . The ferromagnetic property was attributed to the introduction of oxygen vacancies in the CeO 2 lattice upon doping with Ni, which were confirmed by Raman and XPS. The pseudo-capacitive properties of pure and Ni-doped CeO 2 samples were evaluated via cyclic voltammetry and galvanostatic charge-discharge studies, wherein 1 M KOH was used as the electrolyte. The specific capacitances were 235, 351, 382, 577 and 417 F g -1 corresponding to the pure 1%, 3%, 5% and 7% of Ni doped samples at the current density of 2 A g -1 , respectively. The 5% Ni-doped sample showed an excellent cyclic stability and maintained 94% of its maximum specific capacitance after 1000 cycles.

Balanced mechanical resonator for powder handling device

NASA Technical Reports Server (NTRS)

Sarrazin, Philippe C. (Inventor); Brunner, Will M. (Inventor)

2012-01-01

A system incorporating a balanced mechanical resonator and a method for vibration of a sample composed of granular material to generate motion of a powder sample inside the sample holder for obtaining improved analysis statistics, without imparting vibration to the sample holder support.

(Project 13-5292) Correlating thermal and mechanical coupling based multiphysics behavior of nuclear materials through in-situ measurements

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

Tomar, Vikas

Irradiations and post characterization experiments were performed first on Zr samples. This step will help understand the effect of the 2.5% alloying elements on the behavior of Zircaloy-4 (PWR cladding material) when compared to pure Zr. Irradiation flux measurements and sample temperature calibrations were performed at different energies prior to the irradiation experiments. Irradiations were performed with two different energy regimes1: non-displacment energies and displacement energies. Time was also dedicated to optimize transmission electron microscopy (TEM) sample preparation conditions via electropolishing technique. This step is crucial to prepare TEM samples for the in-situ TEM/irradiation experiments (Year 2). In addition, Zircaloy-4more » samples are being prepared for irradiation, and a setup is built by one of our collaborators (Dr. Mert Efe) to prepare ultrafine (UF) and nanocrystalline (NC) Zircaloy-4 samples for comparison with the commercial Zircaloy-4 samples.« less

Sparse Representation Based Frequency Detection and Uncertainty Reduction in Blade Tip Timing Measurement for Multi-Mode Blade Vibration Monitoring

PubMed Central

Pan, Minghao; Yang, Yongmin; Guan, Fengjiao; Hu, Haifeng; Xu, Hailong

2017-01-01

The accurate monitoring of blade vibration under operating conditions is essential in turbo-machinery testing. Blade tip timing (BTT) is a promising non-contact technique for the measurement of blade vibrations. However, the BTT sampling data are inherently under-sampled and contaminated with several measurement uncertainties. How to recover frequency spectra of blade vibrations though processing these under-sampled biased signals is a bottleneck problem. A novel method of BTT signal processing for alleviating measurement uncertainties in recovery of multi-mode blade vibration frequency spectrum is proposed in this paper. The method can be divided into four phases. First, a single measurement vector model is built by exploiting that the blade vibration signals are sparse in frequency spectra. Secondly, the uniqueness of the nonnegative sparse solution is studied to achieve the vibration frequency spectrum. Thirdly, typical sources of BTT measurement uncertainties are quantitatively analyzed. Finally, an improved vibration frequency spectra recovery method is proposed to get a guaranteed level of sparse solution when measurement results are biased. Simulations and experiments are performed to prove the feasibility of the proposed method. The most outstanding advantage is that this method can prevent the recovered multi-mode vibration spectra from being affected by BTT measurement uncertainties without increasing the probe number. PMID:28758952

Effects of Axial Vibration on Needle Insertion into the Tail Veins of Rats and Subsequent Serial Blood Corticosterone Levels

PubMed Central

Clement, Ryan S; Unger, Erica L; Ocón-Grove, Olga M; Cronin, Thomas L; Mulvihill, Maureen L

2016-01-01

Blood collection is commonplace in biomedical research. Obtaining sufficient sample while minimizing animal stress requires significant skill and practice. Repeated needle punctures can cause discomfort and lead to variable release of stress hormones, potentially confounding analysis. We designed a handheld device to reduce the force necessary for needle insertion by using low-frequency, axial (forward and backward) micromotions (that is, vibration) delivered to the needle during venipuncture. Tests with cadaver rat-tail segments (n = 18) confirmed that peak insertion forces were reduced by 73% on average with needle vibration. A serial blood-sampling study was then conducted by using Sprague–Dawley rats divided into 2 groups based on needle condition used to cause bleeds: vibration on (n = 10) and vibration off (n = 9). On 3 days (1 wk apart), 3 tail-vein blood collections were performed in each subject at 1-h intervals. To evaluate associated stress levels, plasma corticosterone concentration was quantified by radioimmunoassay and behavior (that is, movement and vocalization) was scored by blinded review of blood-sampling videos. After the initial trial, average corticosterone was lower (46% difference), the mean intrasubject variance trended lower (72%), and behavioral indications of stress were rated lower for the vibration-on group compared with the vibration-off group. Adding controlled vibrations to needles during insertion may decrease the stress associated with blood sampling from rats—an important methodologic advance for investigators studying and assessing stress processes and a refinement over current blood sampling techniques. PMID:27025813

Gearbox Tooth Cut Fault Diagnostics Using Acoustic Emission and Vibration Sensors — A Comparative Study

PubMed Central

Qu, Yongzhi; He, David; Yoon, Jae; Van Hecke, Brandon; Bechhoefer, Eric; Zhu, Junda

2014-01-01

In recent years, acoustic emission (AE) sensors and AE-based techniques have been developed and tested for gearbox fault diagnosis. In general, AE-based techniques require much higher sampling rates than vibration analysis-based techniques for gearbox fault diagnosis. Therefore, it is questionable whether an AE-based technique would give a better or at least the same performance as the vibration analysis-based techniques using the same sampling rate. To answer the question, this paper presents a comparative study for gearbox tooth damage level diagnostics using AE and vibration measurements, the first known attempt to compare the gearbox fault diagnostic performance of AE- and vibration analysis-based approaches using the same sampling rate. Partial tooth cut faults are seeded in a gearbox test rig and experimentally tested in a laboratory. Results have shown that the AE-based approach has the potential to differentiate gear tooth damage levels in comparison with the vibration-based approach. While vibration signals are easily affected by mechanical resonance, the AE signals show more stable performance. PMID:24424467

Post Irradiation TEM Investigation of ZrN Coated U(Mo) Particles Prepared with FIB

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

Van Renterghem, W.; Leenaers, A.; Van den Berghe, S.

2015-10-01

In the framework of the Selenium project, two dispersion fuel plates were fabricated with Si and ZrN coated fuel particles and irradiated in the Br2 reactor of SCK•CEN to high burn-up. The first analysis of the irradiated plate proved the reduced swelling of the fuel plate and interaction layer growth up to 70% burn-up. The question was raised how the structure of the interaction layer had been affected by the irradiation and how the structure of the fuel particles had evolved. Hereto, samples from the ZrN coated UMo particles were prepared for transmission electron microscopy (TEM) using focused ion beammore » milling (FIB) at INL. The FIB technique allowed to precisely select the area of the interaction layer and/or fuel to produce a sample that is TEM transparent over an area of 20 by 20 µm. In this contribution, the first TEM results will be presented from the 66% burn-up sample.« less

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.

49 CFR 178.819 - Vibration test.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 49 Transportation 2 2010-10-01 2010-10-01 false Vibration test. 178.819 Section 178.819... Testing of IBCs § 178.819 Vibration test. (a) General. The vibration test must be conducted for the... vibration test. (b) Test method. (1) A sample IBC, selected at random, must be filled and closed as for...

Copper, gold, and silver decorated magnetic core-polymeric shell nanostructures for destruction of pathogenic bacteria

NASA Astrophysics Data System (ADS)

Padervand, Mohsen; Karanji, Ahmad Kiani; Elahifard, Mohammad Reza

2017-05-01

Fe3O4 magnetic nanoparticles (MNPs) were prepared by co-precipitation method. The nanoparticles were silica coated using TEOS, and then modified by the polymeric layers of polypropylene glycol (PPG) and polyethylene glycol (PEG). Finally, the core-shell samples were decorated with Ag, Au, and Cu nanoparticles. The products were characterized by vibrating sample magnetometry (VSM), TGA, SEM, XRD, and FTIR methods. The antibacterial activity of the prepared samples was evaluated in inactivation of E. coli and S. aureus microorganisms, representing the Gram-negative and Gram-positive species, respectively. The effect of solid dosage, bacteria concentration and type of polymeric modifier on the antibacterial activity was investigated. TEM images of the bacteria were recorded after the treatment time and according to the observed changes in the cell wall, the mechanism of antibacterial action was discussed. The prepared nanostructures showed high antibacterial activity against both Gram-negative and Gram-positive bacteria. This was due to the leaching of metal ions which subsequently led to the lysis of bacteria. A theoretical investigation was also done by studying the interaction of loaded metals with the nucleotide components of the microorganism DNA, and the obtained results were used to explain the experimental data. Finally, based on the observed inactivation curves, we explain the antibacterial behavior of the prepared nanostructures mathematically.

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

PubMed

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

2013-12-01

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

A comprehensive overview on the structure and comparison of magnetic properties of nanocrystalline synthesized by a thermal treatment method

NASA Astrophysics Data System (ADS)

Naseri, Mahmoud Goodarz; Halimah, M. K.; Dehzangi, Arash; Kamalianfar, Ahmad; Saion, Elias B.; Majlis, Burhanuddin Y.

2014-03-01

This study reports the simple synthesis of MFe2O4 (where M=Zn, Mn and Co) nanostructures by a thermal treatment method, followed by calcination at various temperatures from 723 to 873 K. Poly(vinyl pyrrolidon) (PVP) was used as a capping agent to stabilize the particles and prevent them from agglomeration. The pyrolytic behaviors of the polymeric precursor were analyzed by use of simultaneous thermo-gravimetry analyses (TGA) and derivative thermo-gravimetry (DTG) analyses. The characterization studies were conducted by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Fourier transform infrared spectroscopy (FT-IR) confirmed the presence of metal oxide bands for all the calcined samples. Magnetic properties were demonstrated by a vibrating sample magnetometer (VSM), which displayed that the calcined samples exhibited different types of magnetic behavior. The present study also substantiated that magnetic properties of ferrite nanoparticles prepared by the thermal treatment method, from viewing microstructures of them, can be explained as the results of the two important factors: cation distribution and impurity phase of α-Fe2O3. These two factors are subcategory of the preparation method which is related to macrostructure of ferrite. Electron paramagnetic resonance (EPR) spectroscopy showed the existence of unpaired electrons ZnFe2O4 and MnFe2O4 nanoparticles while it did not exhibit resonance signal for CoFe2O4 nanoparticles.

Strength and Dislocation Structure Evolution of Small Metals under Vibrations

NASA Astrophysics Data System (ADS)

Ngan, Alfonso

2015-03-01

It is well-known that ultrasonic vibration can soften metals, and this phenomenon has been widely exploited in industrial applications concerning metal forming and bonding. In this work, we explore the effects of a superimposed small oscillatory load on metal plasticity, from the nano- to macro-size range, and from audible to ultrasonic frequency ranges. Macroscopic and nano-indentation were performed on aluminum, copper and molybdenum, and the results show that the simultaneous application of oscillatory stresses can lower the hardness of these samples. More interestingly, EBSD and TEM observations show that subgrain formation and reduction in dislocation density generally occurred when stress oscillations were applied. These findings point to an important knowledge gap in metal plasticity - the existing understanding of ultrasound softening in terms of the vibrations either imposing additional stress waves to augment the quasi-static applied load, or heating up the metal, whereas the metal's intrinsic deformation resistance or dislocation interactive processes are assumed unaltered by the ultrasound, is proven wrong by the present results. Furthermore, in the case of nanoindentation, the Continuous Stiffness Measurement technique for contact stiffness measurement assumes that the imposed signal-carrier oscillations do not intrinsically alter the material properties of the specimen, and again, the present results prove that this can be wrong. To understand the enhanced subgrain formation and dislocation annihilation, Discrete Dislocation Dynamics (DDD) simulations were carried out and these show that when an oscillatory stress is superimposed on a quasi-static applied stress, reversals of motion of dislocations may occur, and these allow the dislocations to revisit repeatedly suitable configurations for annihilation. DDD, however, was unable to predict the observed subgrain formation presumably because the number of dislocations that can be handled is not large enough. Subgrain formation was directly predicted by a new simulation method of dislocation plasticity based on the dynamics of dislocation density functions.

Compressive Sensing of Roller Bearing Faults via Harmonic Detection from Under-Sampled Vibration Signals

PubMed Central

Tang, Gang; Hou, Wei; Wang, Huaqing; Luo, Ganggang; Ma, Jianwei

2015-01-01

The Shannon sampling principle requires substantial amounts of data to ensure the accuracy of on-line monitoring of roller bearing fault signals. Challenges are often encountered as a result of the cumbersome data monitoring, thus a novel method focused on compressed vibration signals for detecting roller bearing faults is developed in this study. Considering that harmonics often represent the fault characteristic frequencies in vibration signals, a compressive sensing frame of characteristic harmonics is proposed to detect bearing faults. A compressed vibration signal is first acquired from a sensing matrix with information preserved through a well-designed sampling strategy. A reconstruction process of the under-sampled vibration signal is then pursued as attempts are conducted to detect the characteristic harmonics from sparse measurements through a compressive matching pursuit strategy. In the proposed method bearing fault features depend on the existence of characteristic harmonics, as typically detected directly from compressed data far before reconstruction completion. The process of sampling and detection may then be performed simultaneously without complete recovery of the under-sampled signals. The effectiveness of the proposed method is validated by simulations and experiments. PMID:26473858

Fast removal of malachite green dye using novel superparamagnetic sodium alginate-coated Fe3O4 nanoparticles.

PubMed

Mohammadi, Abbas; Daemi, Hamed; Barikani, Mehdi

2014-08-01

In this study, superparamagnetic sodium alginate-coated Fe3O4 nanoparticles (Alg-Fe3O4) as a novel magnetic adsorbent were prepared by in situ coprecipitation method, in which Fe3O4 nanoparticles were precipitated from FeCl3 and FeCl2 under alkaline medium in the presence of sodium alginate. The Alg-Fe3O4 nanoparticles were used for removal of malachite green (MG) from aqueous solutions using batch adsorption technique. The characterization of synthesized nanoparticles was performed using XRD, FTIR, TEM, TGA and vibrating sample magnetometer (VSM) techniques. FTIR analysis of synthesized nanoparticles provided the evidence that sodium alginate was successfully coated on the surface of Fe3O4 nanoparticles. The FT-IR and TGA characterization showed that the Alg-Fe3O4 nanoparticles contained about 14% (w/w) of sodium alginate. Moreover, TEM analysis indicated that the average diameter of the Alg-Fe3O4 nanoparticles was about 12nm. The effects of adsorbent dosage, pH and temperature were investigated on the adsorption properties of MG onto Alg-Fe3O4 nanoparticles. The equilibrium adsorption data were modeled using the Langmuir and Freundlich isotherms. The maximum adsorption capacity obtained from Langmuir isotherm equation was 47.84mg/g. The kinetics of adsorption of MG onto Alg-Fe3O4 nanoparticles were investigated using the pseudo-first-order and pseudo-second-order kinetic models. The results showed that the adsorption of MG onto nanoparticles followed pseudo-second-order kinetic model. Copyright © 2014 Elsevier B.V. All rights reserved.

International Conference on Defects in Insulating Crystals Held at Parma, Italy on August 29th September 2nd, 1988

DTIC Science & Technology

1988-09-01

transmission electron microscopy(TEM) as a main tool. Here we present some case studies from work done by our research group in Solid State Physics in Nanjing...complete order of this composition. A group theory study shows that all Raman peaks are due, in principle, to the movement of the three sorts of ions...and 1I) is the intensity of the exciting Ehght beam. T is the Ramiian tenisor of the studied vibrational niode. For a totally symmnetric A, mode four

Multiple double cross-section transmission electron microscope sample preparation of specific sub-10 nm diameter Si nanowire devices.

PubMed

Gignac, Lynne M; Mittal, Surbhi; Bangsaruntip, Sarunya; Cohen, Guy M; Sleight, Jeffrey W

2011-12-01

The ability to prepare multiple cross-section transmission electron microscope (XTEM) samples from one XTEM sample of specific sub-10 nm features was demonstrated. Sub-10 nm diameter Si nanowire (NW) devices were initially cross-sectioned using a dual-beam focused ion beam system in a direction running parallel to the device channel. From this XTEM sample, both low- and high-resolution transmission electron microscope (TEM) images were obtained from six separate, specific site Si NW devices. The XTEM sample was then re-sectioned in four separate locations in a direction perpendicular to the device channel: 90° from the original XTEM sample direction. Three of the four XTEM samples were successfully sectioned in the gate region of the device. From these three samples, low- and high-resolution TEM images of the Si NW were taken and measurements of the NW diameters were obtained. This technique demonstrated the ability to obtain high-resolution TEM images in directions 90° from one another of multiple, specific sub-10 nm features that were spaced 1.1 μm apart.

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.

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

NASA Technical Reports Server (NTRS)

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

2017-01-01

SiC fiber-bonded ceramics (SA-Tyrannohex: SA-THX) diffusion-bonded with TiCu metallic interlayers were investigated. Thin samples of the ceramics were prepared with a focused ion beam (FIB) and the interfacial microstructure of the prepared samples was studied by transmission electron microscopy (TEM) and scanning TEM (STEM). In addition to conventional microstructure observation, for detailed analysis of reaction compounds in diffusion-bonded area, we performed STEM-EDS measurements and selected area electron diffraction (SAD) experiments. The TEM and STEM experiments revealed the diffusion-bonded area was composed of only one reaction layer, which was characterized by TiC precipitates in Cu-Si compound matrix. This reaction layer was in good contact with the SA-THX substrates, and it is concluded that the joint structure led to the excellent bonding strength.

Measurement of food texture by an acoustic vibration method

NASA Astrophysics Data System (ADS)

Sakurai, Naoki; Taniwaki, Mitsuru; Iwatani, Shin-ichiro; Akimoto, Hidemi

2011-09-01

Food texture was measured by a new acoustic vibration method. A piezoelectric sensor sandwiched between a probe and piston was inserted into a food sample by delivery of silicon oil to a cylinder by a pump. Vibration emitted from the food sample on insertion of the probe was monitored by voltage outputs of the sensor. The voltage signals were passed through 19 half octave bands to calculate texture index for each band. The texture index was defined as vibration energy of the probe caused by the food rupture and/or breakage per unit time.

Ferromagnetic Mn-Implanted GaP: Microstructures vs Magnetic Properties.

PubMed

Yuan, Ye; Hübner, René; Liu, Fang; Sawicki, Maciej; Gordan, Ovidiu; Salvan, G; Zahn, D R T; Banerjee, D; Baehtz, Carsten; Helm, Manfred; Zhou, Shengqiang

2016-02-17

Ferromagnetic GaMnP layers were prepared by ion implantation and pulsed laser annealing (PLA). We present a systematic investigation on the evolution of microstructure and magnetic properties depending on the pulsed laser annealing energy. The sample microstructure was analyzed by high-resolution X-ray diffraction (HR-XRD), transmission electron microscopy (TEM), Rutherford backscattering spectrometry (RBS), ultraviolet Raman spectroscopy (UV-RS), and extended X-ray absorption fine structure (EXAFS) spectroscopy. The presence of X-ray Pendellösung fringes around GaP (004) and RBS channeling prove the epitaxial structure of the GaMnP layer annealed at the optimized laser energy density (0.40 J/cm(2)). However, a forbidden TO vibrational mode of GaP appears and increases with annealing energy, suggesting the formation of defective domains inside the layer. These domains mainly appear in the sample surface region and extend to almost the whole layer with increasing annealing energy. The reduction of the Curie temperature (TC) and of the uniaxial magnetic anisotropy gradually happens when more defects and the domains appear as increasing the annealing energy density. This fact univocally points to the decisive role of the PLA parameters on the resulting magnetic characteristics in the processed layers, which eventually determine the magnetic (or spintronics) figure of merit.

Harman Measurements for Thermoelectric Materials and Modules under Non-Adiabatic Conditions

NASA Astrophysics Data System (ADS)

Roh, Im-Jun; Lee, Yun Goo; Kang, Min-Su; Lee, Jae-Uk; Baek, Seung-Hyub; Kim, Seong Keun; Ju, Byeong-Kwon; Hyun, Dow-Bin; Kim, Jin-Sang; Kwon, Beomjin

2016-12-01

Accuracy of the Harman measurement largely depends on the heat transfer between the sample and its surroundings, so-called parasitic thermal effects (PTEs). Similar to the material evaluations, measuring thermoelectric modules (TEMs) is also affected by the PTEs especially when measuring under atmospheric condition. Here, we study the correction methods for the Harman measurements with systematically varied samples (both bulk materials and TEMs) at various conditions. Among several PTEs, the heat transfer via electric wires is critical. Thus, we estimate the thermal conductance of the electric wires, and correct the measured properties for a certain sample shape and measuring temperature. The PTEs are responsible for the underestimation of the TEM properties especially under atmospheric conditions (10-35%). This study will be useful to accurately characterize the thermoelectric properties of materials and modules.

Synthesis of CeO2 nanoparticles: Photocatalytic and antibacterial activities

NASA Astrophysics Data System (ADS)

Reddy Yadav, L. S.; Lingaraju, K.; Daruka Prasad, B.; Kavitha, C.; Banuprakash, G.; Nagaraju, G.

2017-05-01

We have successfully synthesized CeO2 nanoparticles (Nps) via the solution combustion method using sugarcane juice as a novel combustible fuel. The structural features, optical properties and morphology of the nanoparticles were characterized using XRD, FTIR, and Raman spectroscopy, UV-Vis, SEM and TEM. Structural characterization of the product shows cubic phase CeO2 . FTIR and Raman spectrum show characteristic peaks due to the presence of Ce-O vibration. SEM images show a porous structure and, from TEM images, the size of the nanoparticles were found to be ˜ 50 nm. The photocatalytic degradation of the methylene blue (MB) dye was examined using CeO2 Nps under solar irradiation as well as UV light irradiation and we studied the effect of p H, catalytic load and concentration on the degradation of the MB dye. Furthermore, the antibacterial properties of CeO2 Nps were investigated against Gram+ve and Gram- ve pathogenic bacterial strains using the agar well diffusion method.

Phase diagram of germanium telluride encapsulated in carbon nanotubes from first-principles searches

NASA Astrophysics Data System (ADS)

Wynn, Jamie M.; Medeiros, Paulo V. C.; Vasylenko, Andrij; Sloan, Jeremy; Quigley, David; Morris, Andrew J.

2017-12-01

Germanium telluride has attracted great research interest, primarily because of its phase-change properties. We have developed a general scheme, based on the ab initio random structure searching (AIRSS) method, for predicting the structures of encapsulated nanowires, and using this we predict a number of thermodynamically stable structures of GeTe nanowires encapsulated inside carbon nanotubes of radii under 9 Å . We construct the phase diagram of encapsulated GeTe, which provides quantitative predictions about the energetic favorability of different filling structures as a function of the nanotube radius, such as the formation of a quasi-one-dimensional rock-salt-like phase inside nanotubes of radii between 5.4 and 7.9 Å . Simulated TEM images of our structures show excellent agreement between our results and experimental TEM imagery. We show that, for some nanotubes, the nanowires undergo temperature-induced phase transitions from one crystalline structure to another due to vibrational contributions to the free energy, which is a first step toward nano-phase-change memory devices.

Near-field infrared vibrational dynamics and tip-enhanced decoherence.

PubMed

Xu, Xiaoji G; Raschke, Markus B

2013-04-10

Ultrafast infrared spectroscopy can reveal the dynamics of vibrational excitations in matter. In its conventional far-field implementation, however, it provides only limited insight into nanoscale sample volumes due to insufficient spatial resolution and sensitivity. Here, we combine scattering-scanning near-field optical microscopy (s-SNOM) with femtosecond infrared vibrational spectroscopy to characterize the coherent vibrational dynamics of a nanoscopic ensemble of C-F vibrational oscillators of polytetrafluoroethylene (PTFE). The near-field mode transfer between the induced vibrational molecular coherence and the metallic scanning probe tip gives rise to a tip-mediated radiative IR emission of the vibrational free-induction decay (FID). By increasing the tip–sample coupling, we can enhance the vibrational dephasing of the induced coherent vibrational polarization and associated IR emission, with dephasing times up to T2(NF) is approximately equal to 370 fs in competition against the intrinsic far-field lifetime of T2(FF) is approximately equal to 680 fs as dominated by nonradiative damping. Near-field antenna-coupling thus provides for a new way to modify vibrational decoherence. This approach of ultrafast s-SNOM enables the investigation of spatiotemporal dynamics and correlations with nanometer spatial and femtosecond temporal resolution.

Effect of the dispersing agent on the structural and magnetic properties of CoFe2O4 /SiO2 nanocomposites

NASA Astrophysics Data System (ADS)

Daboin, Viviana; Briceño, Sarah; Suárez, Jorge; Gonzalez, Gema

2018-04-01

Cobalt ferrite nanoparticles CoFe2O4 were synthesized using the thermal decomposition method; subsequently the NPs were functionalized using poli vinyl pyrrolidone (PVP) cetyl trimethyl ammonium bromide (CTAB) and polyethylene glycol (PEG) as dispersing agent. Surface modification with silica SiO2 was made using the Stöber method and tetraethyl orthosilicate (TEOS) as precursor. The purpose of this study is to investigate the influence of the different dispersing agents on the structure and therefore on the magnetic properties of the CoFe2O4 /SiO2 nanocomposites. Structural characterization was carried out using: X-ray diffraction (XRD), infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Magnetic properties were evaluated using a vibrating sample magnetometer (VSM) at room temperature. Our results revealed that the structural and magnetic properties of the CoFe2O4 /SiO2 nanocomposites were significantly different depending of the type of dispersing agents used before the surface modification with silica SiO2 .

Coupling of transient near infrared photonic with magnetic nanoparticle for potential dissipation-free biomedical application in brain

PubMed Central

Sagar, Vidya; Atluri, V. S. R.; Tomitaka, A.; Shah, P.; Nagasetti, A.; Pilakka-Kanthikeel, S.; El-Hage, N.; McGoron, A.; Takemura, Y.; Nair, M.

2016-01-01

Combined treatment strategies based on magnetic nanoparticles (MNPs) with near infrared ray (NIR) biophotonic possess tremendous potential for non-invasive therapeutic approach. Nonetheless, investigations in this direction have been limited to peripheral body region and little is known about the potential biomedical application of this approach for brain. Here we report that transient NIR exposure is dissipation-free and has no adverse effect on the viability and plasticity of major brain cells in the presence or absence superparamagnetic nanoparticles. The 808 nm NIR laser module with thermocouple was employed for functional studies upon NIR exposure to brain cells. Magnetic nanoparticles were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), dynamic laser scattering (DLS), and vibrating sample magnetometer (VSM). Brain cells viability and plasticity were analyzed using electric cell-substrate impedance sensing system, cytotoxicity evaluation, and confocal microscopy. When efficacious non-invasive photobiomodulation and neuro-therapeutical targeting and monitoring to brain remain a formidable task, the discovery of this dissipation-free, transient NIR photonic approach for brain cells possesses remarkable potential to add new dimension. PMID:27465276

Structural and magnetic properties of Ni1-xZnxFe2O4 synthesized through the sol-gel method

NASA Astrophysics Data System (ADS)

Guan, Beh Hoe; Zahari, Muhammad Hanif; Chuan, Lee Kean

2016-11-01

Modification of crystal structure by means of substitution would result in the modification of the overall physical properties of crystallite materials especially in ferrites. This study aims to investigate the effect of non-magnetic Zn substitution in spinel NiFe2O4 and its direct effect towards its microstructural and magnetic properties. Magnetic nanoparticles of Nickel-Zinc ferrite with the chemical formula, Ni1-xZnxFe2O4 (x=0.00, 0.25, 0.50, 0.75) were synthesized through the sol-gel route. Phase formation and structural properties of the synthesized ferrite were identified through X-ray diffraction (XRD) analysis and transmission electron microscopy (TEM). Magnetic properties such as the magnetic saturation, coercivity and remanence were measured by a vibrating sample magnetometer (VSM). XRD measurements reveals successful synthesis of single-phased Nickel ferrite and Nickel—Zinc ferrite. Both crystallite and grain size shows fluctuation with increasing Zn content. The ferrites were found to be ferrimagnetic in nature and show differing values with different x values.

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

NASA Astrophysics Data System (ADS)

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

2016-11-01

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

Synthesis of magnetic activated carbon/α-Fe2O3 nanocomposite and its application in the removal of acid yellow 17 dye from water.

PubMed

Ranjithkumar, V; Sangeetha, S; Vairam, S

2014-05-30

The adsorption of acid yellow 17 dye on activated carbon/α-Fe2O3 nanocomposite prepared by simple pyrolytic method using iron(II) gluconate was investigated by batch technique. The composite was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), and vibrating sample magnetometry (VSM). The size of iron oxide nanoparticles formed from iron(II) gluconate precursor is in the range 5-17nm. The saturation magnetization (Ms), remanence (Mr) and coercivity (Hc) of the magnetic carbon nanocomposite is 5.6emu/g, 1.14emu/g and 448Oe, respectively. The adsorption data are found to fit well with Langmuir and, fairly well with Freundlich and Tempkin isotherms at higher concentration of dye (40-100mg/L). Kinetics data indicate that the adsorption of dye follows pseudo-second order kinetics model. Copyright © 2014 Elsevier B.V. All rights reserved.

Nitrogen Doped Graphene Nickel Ferrite Magnetic Photocatalyst for the Visible Light Degradation of Methylene Blue.

PubMed

Singh, Rajinder; Ladol, Jigmet; Khajuria, Heena; Sheikh, Haq Nawaz

2017-01-01

A facile approach has been devised for the preparation of magnetic NiFe2O4 photocatalyst (NiFe2O4-NG) supported on nitrogen doped graphene (NG). The NiFe2O4-NG composite was synthesized by one step hydrothermal method. The nanocomposite catalyst was characterized by Powder X-ray diffraction (PXRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), Ultraviolet-visible spectroscopy (UV-Vis) and Vibrating sample magnetometry (VSM). It is found that the combination of NiFe2O4 nanoparticles with nitrogen-doped graphene sheets converts NiFe2O4 into a good catalyst for methylene blue (MB) dye degradation by irradiation of visible light. The catalytic activity under visible light irradiation is assigned to extensive movement of photogenerated electron from NiFe2O4 to the conduction band of the reduced NG, effectively blocking direct recombination of electrons and holes. The NiFe2O4 nanoparticles alone have efficient magnetic property, so can be used for magnetic separation in the solution without additional magnetic support.

Focused Heavy Ion Nuclear Microprobe facility at the University of North Texas

NASA Astrophysics Data System (ADS)

Guo, B. N.; Yang, C.; El Bouanani, M.; Duggan, J. L.; McDaniel, F. D.

1999-10-01

A Focused Heavy Ion Nuclear Microprobe facility has been constructed at the University of North Texas. The microprobe utilizes two separated Russian magnetic quadrupole quadruplets. The two identical magnetic quadrupole doublet lenses are separated by 2.61 meters. The lens system with ~ 80 times demagnification has the ability to focus proton, alpha particle, or heavier ions down to a spot size of ~ 1 μm. The microprobe components rest on a 7 meter steel beam support with vibration isolation. A computer provides control for the lens power supplies and also the parameters for a post-lens scanning coil to raster-scan the beam across the sample. Up to four detection channels can be used for simultaneous data acquisition under VME control. A RISC workstation is used to collect, display and analyze the data. The data is transferred via ethernet. A detailed description of the facility and data acquisition system along with preliminary testing results on TEM grids with Rutherford Backscattering Spectrometry and the Ion Beam Induced Charge Collection techniques will be presented.

Improving the catalytic activity of magnetic Fe3O4/ZnO-CdO/reduced graphene oxide for ultrasonic degradation of the organic pollutants and the green oxidation of olefins

NASA Astrophysics Data System (ADS)

Mirzazadeh, Hoda; Lashanizadegan, Maryam

2018-05-01

Magnetic Fe3O4/ZnO-CdO/reduced graphene oxide (MFZC/RGO) has been synthesized by simple hydrothermal method. The structure and morphology were investigated by X-ray diffraction (XRD), Transmission electron microscopy (TEM), Scanning electron microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDS), Diffuse reflectance spectroscopy (DRS), Vibrating sample magnetometer (VSM), Raman and Fourier-transform infrared spectroscopy (FTIR). MFZC/RGO was applied as catalyst in degradation of methylene blue (MB), rhodamin B (RhB) and methylorange (MO) under ultrasonic irradiation. Based on the results, excellent degradation efficiencies of MB, RhB and MO (>99%) were achieved within 10, 20 and 20 min, respectively under oxygen flow. Moreover the catalytic property of MFZC/RGO was investigated in oxidation of styrene, α-methyl styrene, cyclohexene and cyclooctene under oxygen flow. In addition, MFZC/RGO can be easily collected and separated by an external magnet. The catalyst displayed negligible loss in activity and selectivity within several successive runs due to super paramagnetism.

Coupling of transient near infrared photonic with magnetic nanoparticle for potential dissipation-free biomedical application in brain.

PubMed

Sagar, Vidya; Atluri, V S R; Tomitaka, A; Shah, P; Nagasetti, A; Pilakka-Kanthikeel, S; El-Hage, N; McGoron, A; Takemura, Y; Nair, M

2016-07-28

Combined treatment strategies based on magnetic nanoparticles (MNPs) with near infrared ray (NIR) biophotonic possess tremendous potential for non-invasive therapeutic approach. Nonetheless, investigations in this direction have been limited to peripheral body region and little is known about the potential biomedical application of this approach for brain. Here we report that transient NIR exposure is dissipation-free and has no adverse effect on the viability and plasticity of major brain cells in the presence or absence superparamagnetic nanoparticles. The 808 nm NIR laser module with thermocouple was employed for functional studies upon NIR exposure to brain cells. Magnetic nanoparticles were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), dynamic laser scattering (DLS), and vibrating sample magnetometer (VSM). Brain cells viability and plasticity were analyzed using electric cell-substrate impedance sensing system, cytotoxicity evaluation, and confocal microscopy. When efficacious non-invasive photobiomodulation and neuro-therapeutical targeting and monitoring to brain remain a formidable task, the discovery of this dissipation-free, transient NIR photonic approach for brain cells possesses remarkable potential to add new dimension.

Coupling of transient near infrared photonic with magnetic nanoparticle for potential dissipation-free biomedical application in brain

NASA Astrophysics Data System (ADS)

Sagar, Vidya; Atluri, V. S. R.; Tomitaka, A.; Shah, P.; Nagasetti, A.; Pilakka-Kanthikeel, S.; El-Hage, N.; McGoron, A.; Takemura, Y.; Nair, M.

2016-07-01

Combined treatment strategies based on magnetic nanoparticles (MNPs) with near infrared ray (NIR) biophotonic possess tremendous potential for non-invasive therapeutic approach. Nonetheless, investigations in this direction have been limited to peripheral body region and little is known about the potential biomedical application of this approach for brain. Here we report that transient NIR exposure is dissipation-free and has no adverse effect on the viability and plasticity of major brain cells in the presence or absence superparamagnetic nanoparticles. The 808 nm NIR laser module with thermocouple was employed for functional studies upon NIR exposure to brain cells. Magnetic nanoparticles were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), dynamic laser scattering (DLS), and vibrating sample magnetometer (VSM). Brain cells viability and plasticity were analyzed using electric cell-substrate impedance sensing system, cytotoxicity evaluation, and confocal microscopy. When efficacious non-invasive photobiomodulation and neuro-therapeutical targeting and monitoring to brain remain a formidable task, the discovery of this dissipation-free, transient NIR photonic approach for brain cells possesses remarkable potential to add new dimension.

Modulation in magnetic exchange interaction, core shell structure and Hopkinson's peak with chromium substitution into Ni0.75Co0.25Fe2O4 nano particles

NASA Astrophysics Data System (ADS)

Uday Bhasker, S.; Choudary, G. S. V. R. K.; Reddy, M. V. Ramana

2018-05-01

The ever growing applications and ever evolving challenges of magnetic nano particles has been motivating the researchers from various disciplines towards this area of magnetic nano particles. Cation substitutional effect on the magnetic structure of the nanoparticles forms a crucial aspect in their applications. Here the environmentally benign auto combustion method was employed to synthesize chromium substituted nickel cobalt ferrite (Ni0.75Co0.25Fe2-xCrxO4; x = 0, 0.10, 0.15) nano particles, from aqueous metal nitrate solutions. Chromium substitution has shown its effect on the structural, magnetic and electrical properties of Ni0.75Co0.25Fe2O4. Structural and phase analysis of the prepared samples show increased phase purity of ferrite sample with increasing Cr substitution. The TEM (Transmission Electron Microscope) image confirms the nano size of the particles, EDS (Energy dispersive X-ray Spectroscopy) has supported the stoichiometry of the prepared samples and FTIR (Fourier-transform infrared spectroscopic) analysis confirms the spinel structure and also suggests cation redistributions with chromium substitution. VSM (Vibrational Sample Magnetometer) is used to study the magnetic properties through magnetic hysteresis (M-H) loop and magnetic Hopkinson effect. All samples show hysteresis and show reduction in magnetic properties with increase in chromium content. The thermo magnetic study shows Hopkinson peak(s) in the magnetization vs. temperature (M-T) graph and also shows variation in the nature of Hopkinson peak with chromium substitution. Possible reasons for the changes in the nature of the peak are discussed.

49 CFR 178.985 - Vibration test.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 49 Transportation 3 2013-10-01 2013-10-01 false Vibration test. 178.985 Section 178.985... Packagings § 178.985 Vibration test. (a) General. All rigid Large Packaging and flexible Large Packaging design types must be capable of withstanding the vibration test. (b) Test method. (1) A sample Large...

49 CFR 178.985 - Vibration test.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 49 Transportation 3 2014-10-01 2014-10-01 false Vibration test. 178.985 Section 178.985... Packagings § 178.985 Vibration test. (a) General. All rigid Large Packaging and flexible Large Packaging design types must be capable of withstanding the vibration test. (b) Test method. (1) A sample Large...

49 CFR 178.985 - Vibration test.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 49 Transportation 3 2012-10-01 2012-10-01 false Vibration test. 178.985 Section 178.985... Packagings § 178.985 Vibration test. (a) General. All rigid Large Packaging and flexible Large Packaging design types must be capable of withstanding the vibration test. (b) Test method. (1) A sample Large...

49 CFR 178.985 - Vibration test.

Code of Federal Regulations, 2011 CFR

2011-10-01

... 49 Transportation 3 2011-10-01 2011-10-01 false Vibration test. 178.985 Section 178.985... Packagings § 178.985 Vibration test. (a) General. All rigid Large Packaging and flexible Large Packaging design types must be capable of withstanding the vibration test. (b) Test method. (1) A sample Large...

Thinning of Large Biological Cells for Cryo-TEM Characterization by Cryo-FIB Milling

PubMed Central

Strunk, Korrinn M.; Ke, Danxia; Gray, Jennifer L.; Zhang, Peijun

2013-01-01

SUMMARY Focused ion beam milling at cryogenic temperatures (cryo-FIB) is a valuable tool that can be used to thin vitreous biological specimens for subsequent imaging and analysis in a cryo-transmission electron microscope (cryo-TEM) in their frozen-hydrated state. This technique offers the potential benefit of eliminating the mechanical artifacts that are typically found with cryo-ultramicrotomy. However, due to the additional complexity in transferring samples in and out of the FIB, contamination and devitrification of the amorphous ice is commonly encountered. In order to address these problems, we have designed a new sample cryo-shuttle that specifically accepts Polara TEM cartridges directly in order to simplify the transfer process between the FIB and TEM. We used the quality of the ice in the sample as an indicator to test various parameters used the process, and demonstrated with successful milling of large mammalian cells. By comparing the results from larger HeLa cells to those from E. coli cells, we discuss some of the artifacts and challenges we have encountered using this technique. PMID:22906009

Comments on ”Evidence of the hydrogen release mechanism in bulk MgH2”

NASA Astrophysics Data System (ADS)

Surrey, Alexander; Nielsch, Kornelius; Rellinghaus, Bernd

2017-04-01

The effect of an electron beam induced dehydrogenation of MgH2 in the transmission electron microscope (TEM) is largely underestimated by Nogita et al., and led the authors to a misinterpretation of their TEM observations. Firstly, the selected area diffraction (SAD) pattern is falsely interpreted. A re-evaluation of the SAD pattern reveals that no MgH2 is present in the sample, but that it rather consists of Mg and MgO only. Secondly, the transformation of the sample upon in-situ heating in the TEM cannot be ascribed to dehydrogenation, but is rather to be explained by the (nanoscale) Kirkendall effect, which leads to the formation of hollow MgO shells without any metallic Mg in their cores. Hence, the conclusions drawn from the TEM investigation are invalid, as the authors apparently have never studied MgH2.

Tandem High-pressure Freezing and Quick Freeze Substitution of Plant Tissues for Transmission Electron Microscopy

PubMed Central

Bobik, Krzysztof; Dunlap, John R.; Burch-Smith, Tessa M.

2014-01-01

Since the 1940s transmission electron microscopy (TEM) has been providing biologists with ultra-high resolution images of biological materials. Yet, because of laborious and time-consuming protocols that also demand experience in preparation of artifact-free samples, TEM is not considered a user-friendly technique. Traditional sample preparation for TEM used chemical fixatives to preserve cellular structures. High-pressure freezing is the cryofixation of biological samples under high pressures to produce very fast cooling rates, thereby restricting ice formation, which is detrimental to the integrity of cellular ultrastructure. High-pressure freezing and freeze substitution are currently the methods of choice for producing the highest quality morphology in resin sections for TEM. These methods minimize the artifacts normally associated with conventional processing for TEM of thin sections. After cryofixation the frozen water in the sample is replaced with liquid organic solvent at low temperatures, a process called freeze substitution. Freeze substitution is typically carried out over several days in dedicated, costly equipment. A recent innovation allows the process to be completed in three hours, instead of the usual two days. This is typically followed by several more days of sample preparation that includes infiltration and embedding in epoxy resins before sectioning. Here we present a protocol combining high-pressure freezing and quick freeze substitution that enables plant sample fixation to be accomplished within hours. The protocol can readily be adapted for working with other tissues or organisms. Plant tissues are of special concern because of the presence of aerated spaces and water-filled vacuoles that impede ice-free freezing of water. In addition, the process of chemical fixation is especially long in plants due to cell walls impeding the penetration of the chemicals to deep within the tissues. Plant tissues are therefore particularly challenging, but this protocol is reliable and produces samples of the highest quality. PMID:25350384

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.

Improved Technique for Finding Vibration Parameters

NASA Technical Reports Server (NTRS)

Andrew, L. V.; Park, C. C.

1986-01-01

Filtering and sample manipulation reduce noise effects. Analysis technique improves extraction of vibrational frequencies and damping rates from measurements of vibrations of complicated structure. Structural vibrations measured by accelerometers. Outputs digitized at frequency high enough to cover all modes of interest. Use of method on set of vibrational measurements from Space Shuttle, raised level of coherence from previous values below 50 percent to values between 90 and 99 percent

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).

Detection of magnetic moment in thin films with a home-made vibrating sample magnetometer

NASA Astrophysics Data System (ADS)

Jordán, D.; González-Chávez, D.; Laura, D.; León Hilario, L. M.; Monteblanco, E.; Gutarra, A.; Avilés-Félix, L.

2018-06-01

This paper explores the optimization of an array of pick-up coils in a home-made vibrating sample magnetometer for the detection of magnetic moment in thin films. Sensitivity function of a 4-coils Mallinson configuration was numerically studied for the determination of the physical dimensions that enhance the sensitivity of the magnetometer. By performing numerical simulations using the Biot-Savart law combined with the principle of reciprocity we were able to determine the maximum values of sensitivity and the influence of the separation of the coils on the sensitivity function. After the optimization of the pick-up coils, the vibrating sample magnetometer was able to detect the magnetic moment of a 100 nm-thickness Fe19 Ni81 magnetic thin film along and perpendicular to the in-plane anisotropy easy axis. The implemented vibrating sample magnetometer is able to detect changes in the magnetic moment of ∼ 2 × 10-4 emu.

Systematic approach on the fabrication of Co doped ZnO semiconducting nanoparticles by mixture of fuel approach for Antibacterial applications

NASA Astrophysics Data System (ADS)

Rajendar, V.; Dayakar, T.; Shobhan, K.; Srikanth, I.; Venkateswara Rao, K.

2014-11-01

Zinc oxide (ZnO) is a wide band gap semiconductor (3.2 eV) with a high exciton binding energy (60 meV), where it has wide applications in advanced spintronic devices. The theoretical prediction of room temperature ferromagnetism and also antibacterial activity will be possible through the investigation of diluted magnetic semiconductors (DMS), such as transition metal doped ZnO, especially Cobalt doped ZnO. The aim of the work is the synthesis of Cobalt (Co) doped ZnO nanopowders were prepared Zn1-xCoxO (0 ⩽ x ⩾ 0.09) nanopowders from Sol-Gel auto combustion method have been synthesized with precursors such as Zinc and Cobalt nitrates with the assistance Ammonium acetate & Urea as fuel by increasing the cobalt concentration in zinc oxide and their structural, morphological, optical, Thermal, magnetic and antibacterial properties were studied by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), Transmission Electron microscope (TEM), UV-visible spectroscopy, thermo gravimetric/differential thermal analysis (TG/DTA) and vibrating sample magneto meter (VSM). From the antibacterial studies, against gram positive Bacillus subtilis bacteria is most abundant bacteria in soil and indoor atmosphere, which affects the stored spintronic devices so that the devices should be made with antibacterial activity of DMS like Co doped ZnO. In this article is found that ZnO:Co nanopowders with higher Co doping level (0.07 and 0.09 wt%) exhibit good antibacterial efficiency. The magnetization curves obtained using vibrating sample magnetometer (VSM) show a sign of strong room temperature ferromagnetic behavior when the Co doping level is 0.05 wt% and a weak room temperature ferromagnetic behavior Co doping level is below 0.07 wt%, and also they found to exhibit antiferromagnetic and paramagnetic properties, when the Co doping levels are 0.07 and 0.09 wt%, respectively, to enhance and increase the special magnetic and antibacterial property for sophisticated devices for the sustainable technologies.

Vibrational Micro-Spectroscopy of Human Tissues Analysis: Review.

PubMed

Bunaciu, Andrei A; Hoang, Vu Dang; Aboul-Enein, Hassan Y

2017-05-04

Vibrational spectroscopy (Infrared (IR) and Raman) and, in particular, micro-spectroscopy and micro-spectroscopic imaging have been used to characterize developmental changes in tissues, to monitor these changes in cell cultures and to detect disease and drug-induced modifications. The conventional methods for biochemical and histophatological tissue characterization necessitate complex and "time-consuming" sample manipulations and the results are rarely quantifiable. The spectroscopy of molecular vibrations using mid-IR or Raman techniques has been applied to samples of human tissue. This article reviews the application of these vibrational spectroscopic techniques for analysis of biological tissue published between 2005 and 2015.

Experimental determination of damping of plate vibrations in a viscous fluid

NASA Astrophysics Data System (ADS)

Egorov, A. G.; Kamalutdinov, A. M.; Nuriev, A. N.; Paimushin, V. N.

2017-05-01

A method of determining the aerodynamic-drag coefficient of flat vibrating plates from the vibrogram of free damping vibrations of cantilever-fixed duralumin samples has been developed. From the results of our experiments, simple approximating formulas determining the decrement of damping vibrations and the aerodynamic-drag coefficient through the dimensionless vibration amplitude and the Stokes parameter are proposed. The approach developed in this study for determining the aerodynamic-drag coefficient of a vibrating plate can be a useful alternative to purely hydrodynamic methods of finding the drag of vibrating solids.

Advanced Engine Health Management Applications of the SSME Real-Time Vibration Monitoring System

NASA Technical Reports Server (NTRS)

Fiorucci, Tony R.; Lakin, David R., II; Reynolds, Tracy D.; Turner, James E. (Technical Monitor)

2000-01-01

The Real Time Vibration Monitoring System (RTVMS) is a 32-channel high speed vibration data acquisition and processing system developed at Marshall Space Flight Center (MSFC). It Delivers sample rates as high as 51,200 samples/second per channel and performs Fast Fourier Transform (FFT) processing via on-board digital signal processing (DSP) chips in a real-time format. Advanced engine health assessment is achieved by utilizing the vibration spectra to provide accurate sensor validation and enhanced engine vibration redlines. Discrete spectral signatures (such as synchronous) that are indicators of imminent failure can be assessed and utilized to mitigate catastrophic engine failures- a first in rocket engine health assessment. This paper is presented in viewgraph form.

Harman Measurements for Thermoelectric Materials and Modules under Non-Adiabatic Conditions

PubMed Central

Roh, Im-Jun; Lee, Yun Goo; Kang, Min-Su; Lee, Jae-Uk; Baek, Seung-Hyub; Kim, Seong Keun; Ju, Byeong-Kwon; Hyun, Dow-Bin; Kim, Jin-Sang; Kwon, Beomjin

2016-01-01

Accuracy of the Harman measurement largely depends on the heat transfer between the sample and its surroundings, so-called parasitic thermal effects (PTEs). Similar to the material evaluations, measuring thermoelectric modules (TEMs) is also affected by the PTEs especially when measuring under atmospheric condition. Here, we study the correction methods for the Harman measurements with systematically varied samples (both bulk materials and TEMs) at various conditions. Among several PTEs, the heat transfer via electric wires is critical. Thus, we estimate the thermal conductance of the electric wires, and correct the measured properties for a certain sample shape and measuring temperature. The PTEs are responsible for the underestimation of the TEM properties especially under atmospheric conditions (10–35%). This study will be useful to accurately characterize the thermoelectric properties of materials and modules. PMID:27966622

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

V Yashchuk; R Conley; E Anderson

Verification of the reliability of metrology data from high quality X-ray optics requires that adequate methods for test and calibration of the instruments be developed. For such verification for optical surface profilometers in the spatial frequency domain, a modulation transfer function (MTF) calibration method based on binary pseudo-random (BPR) gratings and arrays has been suggested [1] and [2] and proven to be an effective calibration method for a number of interferometric microscopes, a phase shifting Fizeau interferometer, and a scatterometer [5]. Here we describe the details of development of binary pseudo-random multilayer (BPRML) test samples suitable for characterization of scanningmore » (SEM) and transmission (TEM) electron microscopes. We discuss the results of TEM measurements with the BPRML test samples fabricated from a WiSi2/Si multilayer coating with pseudo-randomly distributed layers. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML test samples can be used to characterize X-ray microscopes. Corresponding work with X-ray microscopes is in progress.« 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

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

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.

Soil chemical insights provided through vibrational spectroscopy

USDA-ARS?s Scientific Manuscript database

Vibrational spectroscopy techniques provide a powerful approach to study environmental materials and processes. These multifunctional analysis tools can be used to probe molecular vibrations of solid, liquid, and gaseous samples for characterizing materials, elucidating reaction mechanisms, and exam...

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.

Synthesis, surface modification and characterisation of biocompatible magnetic iron oxide nanoparticles for biomedical applications.

PubMed

Mahdavi, Mahnaz; Ahmad, Mansor Bin; Haron, Md Jelas; Namvar, Farideh; Nadi, Behzad; Rahman, Mohamad Zaki Ab; Amin, Jamileh

2013-06-27

Superparamagnetic iron oxide nanoparticles (MNPs) with appropriate surface chemistry exhibit many interesting properties that can be exploited in a variety of biomedical applications such as magnetic resonance imaging contrast enhancement, tissue repair, hyperthermia, drug delivery and in cell separation. These applications required that the MNPs such as iron oxide Fe₃O₄ magnetic nanoparticles (Fe₃O₄ MNPs) having high magnetization values and particle size smaller than 100 nm. This paper reports the experimental detail for preparation of monodisperse oleic acid (OA)-coated Fe₃O₄ MNPs by chemical co-precipitation method to determine the optimum pH, initial temperature and stirring speed in order to obtain the MNPs with small particle size and size distribution that is needed for biomedical applications. The obtained nanoparticles were characterized by Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray fluorescence spectrometry (EDXRF), thermogravimetric analysis (TGA), X-ray powder diffraction (XRD), and vibrating sample magnetometer (VSM). The results show that the particle size as well as the magnetization of the MNPs was very much dependent on pH, initial temperature of Fe²⁺ and Fe³⁺ solutions and steering speed. The monodisperse Fe₃O₄ MNPs coated with oleic acid with size of 7.8 ± 1.9 nm were successfully prepared at optimum pH 11, initial temperature of 45°C and at stirring rate of 800 rpm. FTIR and XRD data reveal that the oleic acid molecules were adsorbed on the magnetic nanoparticles by chemisorption. Analyses of TEM show the oleic acid provided the Fe₃O₄ particles with better dispersibility. The synthesized Fe₃O₄ nanoparticles exhibited superparamagnetic behavior and the saturation magnetization of the Fe₃O₄ nanoparticles increased with the particle size.

Improvement on controllable fabrication of streptavidin-modified three-layer core-shell Fe3O4@SiO2@Au magnetic nanocomposites with low fluorescence background.

PubMed

Jiang, Hongrong; Zeng, Xin; Xi, Zhijiang; Liu, Ming; Li, Chuanyan; Li, Zhiyang; Jin, Lian; Wang, Zhifei; Deng, Yan; He, Nongyue

2013-04-01

In present study, we put forward an approach to prepare three-layer core-shell Fe3O4@SiO2@Au magnetic nanocomposites via the combination of self-assembling, seed-mediated growing and multi-step chemical reduction. The Fe3O4@SiO2@Au magnetic nanocomposites were analyzed and characterized by transmission electron microscope (TEM), scanning electronic microscope (SEM), energy dispersive spectrometer analysis (EDS), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM), and ultraviolet and visible spectrophotometer (UV-Vis). TEM and SEM characterizations showed that the FeO4@SiO2@Au nanocomposites were obtained successfully with three-layer structures, especially a layer of thin, smooth and continuous gold shell. The average diameter of Fe3O4@SiO2@Au nanocomposites was about 600 nm and an excellent dispersity was observed for the as-prepared nanoparticles. EDS characterizations demonstrated that the nanocomposites contained three elements of the precursors, Fe, Si, and Au. Furthermore, FT-IR showed that the silica and gold shell were coated successfully. UV-Vis and VSM characterizations showed that the Fe3O4@SiO2@Au nanocomposites exhibited good optical and magnetic property, and the saturation magnetization was 25.76 emu/g. In conclusion, the Fe3O4@SiO2@Au magnetic nanocomposites with three-layer core-shell structures were prepared. Furthermore, Fe3O4@SiO2@Au magnetic nanocomposites were modified with streptavidin (SA) successfully, and it was validated that they performed low fluorescence background, suggesting that they should have good applications especially in bioassay based on fluorescence detection through bonding the biotinylated fluorescent probes.

Blind identification of full-field vibration modes of output-only structures from uniformly-sampled, possibly temporally-aliased (sub-Nyquist), video measurements

NASA Astrophysics Data System (ADS)

Yang, Yongchao; Dorn, Charles; Mancini, Tyler; Talken, Zachary; Nagarajaiah, Satish; Kenyon, Garrett; Farrar, Charles; Mascareñas, David

2017-03-01

Enhancing the spatial and temporal resolution of vibration measurements and modal analysis could significantly benefit dynamic modelling, analysis, and health monitoring of structures. For example, spatially high-density mode shapes are critical for accurate vibration-based damage localization. In experimental or operational modal analysis, higher (frequency) modes, which may be outside the frequency range of the measurement, contain local structural features that can improve damage localization as well as the construction and updating of the modal-based dynamic model of the structure. In general, the resolution of vibration measurements can be increased by enhanced hardware. Traditional vibration measurement sensors such as accelerometers have high-frequency sampling capacity; however, they are discrete point-wise sensors only providing sparse, low spatial sensing resolution measurements, while dense deployment to achieve high spatial resolution is expensive and results in the mass-loading effect and modification of structure's surface. Non-contact measurement methods such as scanning laser vibrometers provide high spatial and temporal resolution sensing capacity; however, they make measurements sequentially that requires considerable acquisition time. As an alternative non-contact method, digital video cameras are relatively low-cost, agile, and provide high spatial resolution, simultaneous, measurements. Combined with vision based algorithms (e.g., image correlation or template matching, optical flow, etc.), video camera based measurements have been successfully used for experimental and operational vibration measurement and subsequent modal analysis. However, the sampling frequency of most affordable digital cameras is limited to 30-60 Hz, while high-speed cameras for higher frequency vibration measurements are extremely costly. This work develops a computational algorithm capable of performing vibration measurement at a uniform sampling frequency lower than what is required by the Shannon-Nyquist sampling theorem for output-only modal analysis. In particular, the spatio-temporal uncoupling property of the modal expansion of structural vibration responses enables a direct modal decoupling of the temporally-aliased vibration measurements by existing output-only modal analysis methods, yielding (full-field) mode shapes estimation directly. Then the signal aliasing properties in modal analysis is exploited to estimate the modal frequencies and damping ratios. The proposed method is validated by laboratory experiments where output-only modal identification is conducted on temporally-aliased acceleration responses and particularly the temporally-aliased video measurements of bench-scale structures, including a three-story building structure and a cantilever beam.

Evaluation of Argon ion irradiation hardening of ferritic/martensitic steel-T91 using nanoindentation, X-ray diffraction and TEM techniques

NASA Astrophysics Data System (ADS)

Naveen Kumar, N.; Tewari, R.; Mukherjee, P.; Gayathri, N.; Durgaprasad, P. V.; Taki, G. S.; Krishna, J. B. M.; Sinha, A. K.; Pant, P.; Revally, A. K.; Dutta, B. K.; Dey, G. K.

2017-08-01

In the present study, microstructures of Ferritic-martensitic T-91 steel irradiated at room temperature for 5, 10 and 20 dpa using 315 KeV Ar+9 ions have been characterized by grazing incident X-ray diffraction (GIXRD) and by transmission electron microscopy (TEM). Line profiles of GIXRD patterns have shown that the size of domain continuously reduced with increasing dose of radiation. TEM investigations of irradiated samples have shown the presence of black dots, the number density of which decreases with increasing dose. Microstructures of irradiated samples have also revealed the presence of point defect clusters, such as dislocation loops and bubbles. In addition, dissolution of precipitates due to irradiation was also observed. Nano-indentation studies on the irradiated samples have shown saturation behavior in hardness as a function of dose which could be correlated with the changes in the yield strength of the alloy.

GHz laser-free time-resolved transmission electron microscopy: A stroboscopic high-duty-cycle method.

PubMed

Qiu, Jiaqi; Ha, Gwanghui; Jing, Chunguang; Baryshev, Sergey V; Reed, Bryan W; Lau, June W; Zhu, Yimei

2016-02-01

A device and a method for producing ultrashort electron pulses with GHz repetition rates via pulsing an input direct current (dc) electron beam are provided. The device and the method are based on an electromagnetic-mechanical pulser (EMMP) that consists of a series of transverse deflecting cavities and magnetic quadrupoles. The EMMP modulates and chops the incoming dc electron beam and converts it into pico- and sub-pico-second electron pulse sequences (pulse trains) at >1GHz repetition rates, as well as controllably manipulates the resulting pulses. Ultimately, it leads to negligible electron pulse phase-space degradation compared to the incoming dc beam parameters. The temporal pulse length and repetition rate for the EMMP can be continuously tunable over wide ranges. Applying the EMMP to a transmission electron microscope (TEM) with any dc electron source (e.g. thermionic, Schottky, or field-emission source), a GHz stroboscopic high-duty-cycle TEM can be realized. Unlike in many recent developments in time-resolved TEM that rely on a sample pumping laser paired with a laser launching electrons from a photocathode to probe the sample, there is no laser in the presented experimental set-up. This is expected to be a significant relief for electron microscopists who are not familiar with laser systems. The EMMP and the sample are externally driven by a radiofrequency (RF) source synchronized through a delay line. With no laser pumping the sample, the problem of the pump laser induced residual heating/damaging the sample is eliminated. As many RF-driven processes can be cycled indefinitely, sampling rates of 1-50GHz become accessible. Such a GHz stroboscopic TEM would open up a new paradigm for in situ and in operando experiments to study samples externally driven electromagnetically. Complementary to the lower (MHz) repetition rates experiments enabled by laser photocathode TEM, new experiments in the multi-GHz regime will be enabled by the proposed RF design. Because TEM is also a platform for various analytical methods, there are infinite application opportunities in energy and electronics to resolve charge (electronic and ionic) transport, and magnetic, plasmonic and excitonic dynamics in advanced functional materials. In addition, because the beam duty-cycle can be as high as ~10(-1) (or 10%), detection can be accomplished by commercially available detectors. In this article, we report an optimal design of the EMMP. The optimal design was found using an analytical generalized matrix approach in the thin lens approximation along with detailed beam dynamics taking actual realistic dc beam parameters in a TEM operating at 200keV. Copyright © 2015 Elsevier B.V. All rights reserved.

Sol-gel route approach and improvisation in physico-chemical, structural, magnetic and electrical properties of BaCox/2Znx/2ZrxFe(12-2x)O19 ferrites

NASA Astrophysics Data System (ADS)

Kaur Jassal, Amanpreet; Mudsainiyan, R. K.; Chawla, S. K.; Anu; Bindra Narang, Sukhleen; Pubby, Kunal

2018-02-01

The structural and magnetic properties of Zn, Co and Zr cations doped barium hexaferrite [Ba(Znx/2Cox/2)xZrxFe(12-2x)O19] nanoparticles synthesized by sol-gel method have been investigated. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM) were employed to investigate the physico-chemical properties of the obtained ferrite samples. XRD studies reveal that the magnetoplumbite structure for all sample (up to x = 0.8) have been formed and the crystallite size of nanoparticles lies in the range of 34-46 nm. At higher dopant concentration, other impurities (α-Fe2O3 and BaFe2O4 etc.) have been observed. Magnetic studies indicate that site occupancy and nature of dopant ions greatly affect the behavior of magnetic properties. The results of VSM and LCR analysis show that magnetic and electrical parameters vary with an increase in dopant concentration. The results of BET surface area of samples indicate that these types of materials could be used for catalytic properties. Dielectric constant, dielectric loss tangent and A.C. conductivity weremeasured using impedance analyzer over wide frequency range 20 Hz-120 MHz. All the three parameters increase significantly with increase in doping. Increase in dielectric constant proposes these materials for fabrication of microwave devices, while increase in dielectric loss tangent proposes these for applications such as attenuator, absorber etc.

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.

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

Yashchuk, V.V.; Conley, R.; Anderson, E.H.

Verification of the reliability of metrology data from high quality X-ray optics requires that adequate methods for test and calibration of the instruments be developed. For such verification for optical surface profilometers in the spatial frequency domain, a modulation transfer function (MTF) calibration method based on binarypseudo-random (BPR) gratings and arrays has been suggested and and proven to be an effective calibration method for a number of interferometric microscopes, a phase shifting Fizeau interferometer, and a scatterometer. Here we describe the details of development of binarypseudo-random multilayer (BPRML) test samples suitable for characterization of scanning (SEM) and transmission (TEM) electronmore » microscopes. We discuss the results of TEM measurements with the BPRML test samples fabricated from a WiSi{sub 2}/Si multilayer coating with pseudo-randomly distributed layers. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML testsamples can be used to characterize X-ray microscopes. Corresponding work with X-ray microscopes is in progress.« 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.

Terahertz thickness determination with interferometric vibration correction for industrial applications.

PubMed

Pfeiffer, Tobias; Weber, Stefan; Klier, Jens; Bachtler, Sebastian; Molter, Daniel; Jonuscheit, Joachim; Von Freymann, Georg

2018-05-14

In many industrial fields, like automotive and painting industry, the thickness of thin layers is a crucial parameter for quality control. Hence, the demand for thickness measurement techniques continuously grows. In particular, non-destructive and contact-free terahertz techniques access a wide range of thickness determination applications. However, terahertz time-domain spectroscopy based systems perform the measurement in a sampling manner, requiring fixed distances between measurement head and sample. In harsh industrial environments vibrations of sample and measurement head distort the time-base and decrease measurement accuracy. We present an interferometer-based vibration correction for terahertz time-domain measurements, able to reduce thickness distortion by one order of magnitude for vibrations with frequencies up to 100 Hz and amplitudes up to 100 µm. We further verify the experimental results by numerical calculations and find very good agreement.

Rate constants and mechanisms for the crystallization of Al nano-goethite under environmentally relevant conditions

NASA Astrophysics Data System (ADS)

Bazilevskaya, Ekaterina; Archibald, Douglas D.; Martínez, Carmen Enid

2012-07-01

Mobile inorganic and organic nanocolloidal particles originate-from and interact-with bulk solid phases in soil and sediment environments, and as such, they contribute to the dynamic properties of environmental systems. In particular, ferrihydrite and (nano)goethite are the most abundant of nanocolloidal Fe oxy(hydr)oxides in these environments. We therefore investigated the ferrihydrite to goethite phase transformation using experimental reaction conditions that mimicked environmental conditions where the formation of nanocolloidal Fe oxy(hydr)oxides may occur: slow titration of dilute solutions to pH 5 at 25 °C with and without 2 mol% Al. Subsequently, the rate constants from 54-d nano-goethite aging/crystallization experiments at 50 °C were determined using aliquots pulled for vibrational spectroscopy (including multivariate curve resolution, MCR, analyses of infrared spectra) and synchrotron-based X-ray diffraction (XRD). We also present a mechanistic model that accounts for the nano-goethite crystallization observed by the aforementioned techniques, and particle structural characteristics observed by dynamic light scattering (DLS) and transmission electron microscopy (TEM). In contrast to the common assumption that metastable ferrihydrite precipitates first, before it transforms to goethite, the presence of characteristic infrared bands in freshly synthesized nanoparticle suspensions indicate goethite can precipitate directly from solution under environmentally relevant conditions: low Fe concentration, ambient temperature, and pH maintained at 5. However, the presence of 2 mol% Al prevented direct goethite precipitation. Rate constants obtained by fitting the contributions from the MCR-derived goethite-like component to the OH-stretching region were (7.4 ± 1.1) × 10-7 s-1 for 0% Al and (4.2 ± 0.4) × 10-7 s-1 for 2 mol% Al suspensions. Rate constants derived from intensities of OH-bending infrared vibrations (795 and 895 cm-1) showed similar values, within error, for both 0 and 2 mol% Al nanoparticle suspensions. Thus, the presence of 2 mol% Al decreased the rate constants determined from analyses of infrared OH-stretching and OH-bending vibrations by 43-57%. We postulate that dissolution re-precipitation reactions are accelerated in aggregate microenvironments by locally increased supersaturation, yielding the dominant mechanism for transformation of ferrihydrite to goethite and goethite crystal growth when bulk ion concentrations are low. Although we did observe growth of a population of prismatic goethite single crystals by TEM, there was more substantial growth of a population of polycrystalline goethite needles that appeared to retain some defects from a preceding aggregation step that we detected with DLS. Since the presence of Al hinders the dissolution of ferrihydrite, it too reduces the rate of crystallization to goethite and its crystal growth. As exemplified in this nano-particle crystallization study, the combination of advanced spectral-curve-resolution algorithms and sensitive and quantitative infrared sampling techniques opens future opportunities for the quantification of mineral phase dynamics in nanocolloidal suspensions, which is important for many aspects of environmental studies.

Vibrational Action Spectroscopy of Solids: New Surface-Sensitive Technique

NASA Astrophysics Data System (ADS)

Wu, Zongfang; Płucienik, Agata; Feiten, Felix E.; Naschitzki, Matthias; Wachsmann, Walter; Gewinner, Sandy; Schöllkopf, Wieland; Staemmler, Volker; Kuhlenbeck, Helmut; Freund, Hans-Joachim

2017-09-01

Vibrational action spectroscopy employing infrared radiation from a free-electron laser has been successfully used for many years to study the vibrational and structural properties of gas phase aggregates. Despite the high sensitivity of this method no relevant studies have yet been conducted for solid sample surfaces. We have set up an experiment for the application of this method to such targets, using infrared light from the free-electron laser of the Fritz Haber Institute. In this Letter, we present first results of this technique with adsorbed argon and neon atoms as messengers. We were able to detect surface-located vibrations of a thin V2O3(0 0 0 1 ) film on Au(111) as well as adsorbate vibrations, demonstrating that this method is highly surface sensitive. We consider that the dominant channel for desorption of the messenger atoms is direct inharmonic vibrational coupling, which is essentially insensitive to subsurface or bulk vibrations. Another channel is thermal desorption due to sample heating by absorption of infrared light. The high surface sensitivity of the nonthermal channel and its insensitivity to subsurface modes makes this technique an ideal tool for the study of surface-located vibrations.

Vibrational Action Spectroscopy of Solids: New Surface-Sensitive Technique.

PubMed

Wu, Zongfang; Płucienik, Agata; Feiten, Felix E; Naschitzki, Matthias; Wachsmann, Walter; Gewinner, Sandy; Schöllkopf, Wieland; Staemmler, Volker; Kuhlenbeck, Helmut; Freund, Hans-Joachim

2017-09-29

Vibrational action spectroscopy employing infrared radiation from a free-electron laser has been successfully used for many years to study the vibrational and structural properties of gas phase aggregates. Despite the high sensitivity of this method no relevant studies have yet been conducted for solid sample surfaces. We have set up an experiment for the application of this method to such targets, using infrared light from the free-electron laser of the Fritz Haber Institute. In this Letter, we present first results of this technique with adsorbed argon and neon atoms as messengers. We were able to detect surface-located vibrations of a thin V_{2}O_{3}(0001) film on Au(111) as well as adsorbate vibrations, demonstrating that this method is highly surface sensitive. We consider that the dominant channel for desorption of the messenger atoms is direct inharmonic vibrational coupling, which is essentially insensitive to subsurface or bulk vibrations. Another channel is thermal desorption due to sample heating by absorption of infrared light. The high surface sensitivity of the nonthermal channel and its insensitivity to subsurface modes makes this technique an ideal tool for the study of surface-located vibrations.

Atomic force microscopy capable of vibration isolation with low-stiffness Z-axis actuation.

PubMed

Ito, Shingo; Schitter, Georg

2018-03-01

For high-resolution imaging without bulky external vibration isolation, this paper presents an atomic force microscope (AFM) capable of vibration isolation with its internal Z-axis (vertical) actuators moving the AFM probe. Lorentz actuators (voice coil actuators) are used for the Z-axis actuation, and flexures guiding the motion are designed to have a low stiffness between the mover and the base. The low stiffness enables a large Z-axis actuation of more than 700 µm and mechanically isolates the probe from floor vibrations at high frequencies. To reject the residual vibrations, the probe tracks the sample by using a displacement sensor for feedback control. Unlike conventional AFMs, the Z-axis actuation attains a closed-loop control bandwidth that is 35 times higher than the first mechanical resonant frequency. The closed-loop AFM system has robustness against the flexures' nonlinearity and uses the first resonance for better sample tracking. For further improvement, feedforward control with a vibration sensor is combined, and the resulting system rejects 98.4% of vibrations by turning on the controllers. The AFM system is demonstrated by successful AFM imaging in a vibrational environment. Copyright © 2017 Elsevier B.V. All rights reserved.

EBSD and TEM characterization of high burn-up mixed oxide fuel

NASA Astrophysics Data System (ADS)

Teague, Melissa; Gorman, Brian; Miller, Brandon; King, Jeffrey

2014-01-01

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

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

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

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

2014-01-01

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

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

TEM-187, a new extended-spectrum β-lactamase with weak activity in a Proteus mirabilis clinical strain.

PubMed

Corvec, Stéphane; Beyrouthy, Racha; Crémet, Lise; Aubin, Guillaume Ghislain; Robin, Frédéric; Bonnet, Richard; Reynaud, Alain

2013-05-01

A Proteus mirabilis clinical strain (7001324) was isolated from urine sample of a patient hospitalized in a long-term-care facility. PCR and cloning experiments performed with this strain identified a novel TEM-type β-lactamase (TEM-187) differing by four amino acid substitutions (Leu21Phe, Arg164His, Ala184Val, and Thr265Met) from TEM-1. This characterization provides further evidence for the diversity of extended-spectrum β-lactamases (ESBL) produced by P. mirabilis and for their potential spread to other Enterobacteriaceae due to a lack of sensitive detection methods used in daily practice.

Focused Ion Beam (FIB) combined with SEM (FIB/SEM) and TEM: Advanced tools for nano-analysis in Geosciences

NASA Astrophysics Data System (ADS)

Wirth, R.; Morales, L. G.

2011-12-01

Focused ion beam (FIB) techniques have been successfully applied to the preparation of site-specific electron transparent membranes for transmission electron microscopy (TEM) investigations in Geosciences since several years. For example, systematic TEM studies of nano-inclusions in diamond foils prepared with FIB have improved our knowledge on diamond formation. However, FIB is not exclusively used for sample preparation for TEM application because it has been proved that one and the same TEM foil can also be used for Synchrotron IR, Synchrotron X-Ray fluorescence (XRF), scanning transmission X-Ray microscopy (STXM) and NanoSIMS analysis. In addition, FIB milling turned out to be very useful for sample preparation of Brillouin scattering experiments and has a strong potential for preparation of highly-polished, micrometer-scale samples. However, a real break through in FIB application was achieved combining a Ga-ion source of the FIB with an electron source of a scanning electron microscope (SEM) in one single instrument. The combination of FIB/SEM renders access to the third dimension of the sample possible. A cavity normal to the sample surface is sputtered with Ga-ions and this newly created inner surface is imaged with the electron beam. Alternating slicing and viewing along these cavities allow the acquisition of a sequence of images that allows the observation in 3 dimensions. Recently, this technique has been successfully applied to image the structure of grain or phase boundaries in metamorphic rocks as well as micro- and nanoporosity in shales, but its applicability goes far beyond these few examples. Combining slicing and viewing with X-Ray and electron backscatter diffraction (EBSD) analysis can provide 3D elemental mapping and 3D crystallographic orientation mapping of crystalline materials. Combined FIB/SEM devices also facilitate the preparation of substantially thinner and cleaner TEM foils (approximately 30 nm) because electron beam imaging controls the progress of the sputtering process without sputtering the sample during imaging. Electron induce sputtering is substantially smaller than ion induced sputtering. Finally, the amorphous layers created by Ga-ion sputtering and Ga-ion implantation can be removed from the foil surfaces by subsequent argon ion bombardment under a low angle of incidence and low acceleration voltage thus permitting TEM high-resolution imaging and electron energy-loss spectroscopy (EELS). Additionally, ultra-thin foils have the advantage that they are electron transparent even at 30 keV, the common operational voltage of a SEM. Therefore the electron column of the FIB/SEM system can be used as a TEM at low voltage and images can be made either in bright-field, dark field and through a high-angle annular dark field (HAADF) detector. The HAADF detector provides information about the chemical composition of the specimen with high spatial resolution because it is Z-contrast sensitive.

Effect of vibration duration of high ultrasound applied to bio-composite while gelatinized on its properties.

PubMed

Abral, Hairul; Putra, Genda J; Asrofi, Mohammad; Park, Ji-Won; Kim, Hyun-Joong

2018-01-01

This article reports effect of vibration duration of high ultrasound applied to bio-composite while gelatinized on its properties. The bio-composite consists of mixing of both the tapioca starch based bioplastic and oil palm empty fruit bunch (OPEFB) fibers with high volume fraction. Gelatinization of the bio-composite sample was poured into a rectangular glass mold placed then in an ultrasonic bath with 40kHz, and 250watt in different duration for 0, 15, 30, 60min respectively. The results show that vibration during gelatinization has changed the characterisation of the bio-composite. SEM photograph displayed different fracture surface of tensile sample. For vibration duration of 60min, tensile strength (TM), and tensile modulus (TM) was improved to 64.4, 277.4%, respectively, meanwhile strain was decreased to 35.1% in comparison without vibration. Fourier Transform Infrared Spectroscopy (FTIR), and XRD diffraction of the bio-composite has changed due to various vibration duration. Moisture absorption of the vibrated bio-composite was lower than that of the untreated one. Copyright © 2017 Elsevier B.V. All rights reserved.

On the fractal morphology of combustion-generated soot aggregates

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

Koylu, U.O.

1995-12-31

The fractal properties of soot aggregates were investigated using ex-situ and in-situ experimental methods as well as computer simulations. Ex-situ experiments involved thermophoretic sampling and analysis by transmission electron microscopy (TEM), while in-situ measurements employed angular static light scattering and data inversion based on Rayleigh-Debye-Gans (RDG) approximation. Computer simulations used a sequential algorithm which mimics mass fractal-like structures. So from a variety of hydrocarbon-fueled laminar and turbulent nonpremixed flame environments were considered in the present study. The TEM analysis of projected soot images sampled from fuel-rich conditions of buoyant and weakly-buoyant laminar flames indicated that the fractal dimension of sootmore » was relatively independent of position in flames, fuel type and flame condition. These measurements yielded an average fractal dimension of 1.8, although other structure parameters such as the primary particle diameters and number of primary particles in aggregates had wide range of values. Fractal prefactor (lacunarity) was also measured for soot sampled from the fuel-lean conditions of turbulent flames, considering the actual morphology by tilting the samples during TEM analysis. These measurements yielded a fractal dimension of 1.65 and a lacunarity of 8.5, with experimental uncertainties (95% confidence) of 0.08 and 0.5, respectively. Relationships between the actual and projected structure properties of soot were also developed by combining TEM observations with numerical simulations. Practical approximate formulae were suggested to find radius of gyration of an aggregate from its maximum dimension, and number of primary particles in an aggregate from projected area. Finally, the fractal dimension and lacunarity of soot were obtained using light scattering for the same conditions of the above TEM measurements.« less

Vibrational Profiling of Brain Tumors and Cells

PubMed Central

Nelson, Sultan L; Proctor, Dustin T; Ghasemloonia, Ahmad; Lama, Sanju; Zareinia, Kourosh; Ahn, Younghee; Al-Saiedy, Mustafa R; Green, Francis HY; Amrein, Matthias W; Sutherland, Garnette R

2017-01-01

This study reports vibration profiles of neuronal cells and tissues as well as brain tumor and neocortical specimens. A contact-free method and analysis protocol was designed to convert an atomic force microscope into an ultra-sensitive microphone with capacity to record and listen to live biological samples. A frequency of 3.4 Hz was observed for both cultured rat hippocampal neurons and tissues and vibration could be modulated pharmacologically. Malignant astrocytoma tissue samples obtained from operating room, transported in artificial cerebrospinal fluid, and tested within an hour, vibrated with a much different frequency profile and amplitude, compared to meningioma or lateral temporal cortex providing a quantifiable measurement to accurately distinguish the three tissues in real-time. Vibration signals were converted to audible sound waves by frequency modulation, thus demonstrating, acoustic patterns unique to meningioma, malignant astrocytoma and neocortex. PMID:28744324

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

Yashchuk, Valeriy V; Conley, Raymond; Anderson, Erik H

Verification of the reliability of metrology data from high quality x-ray optics requires that adequate methods for test and calibration of the instruments be developed. For such verification for optical surface profilometers in the spatial frequency domain, a modulation transfer function (MTF) calibration method based on binary pseudo-random (BPR) gratings and arrays has been suggested [Proc. SPIE 7077-7 (2007), Opt. Eng. 47(7), 073602-1-5 (2008)} and proven to be an effective calibration method for a number of interferometric microscopes, a phase shifting Fizeau interferometer, and a scatterometer [Nucl. Instr. and Meth. A 616, 172-82 (2010)]. Here we describe the details ofmore » development of binary pseudo-random multilayer (BPRML) test samples suitable for characterization of scanning (SEM) and transmission (TEM) electron microscopes. We discuss the results of TEM measurements with the BPRML test samples fabricated from a WiSi2/Si multilayer coating with pseudo randomly distributed layers. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML test samples can be used to characterize x-ray microscopes. Corresponding work with x-ray microscopes is in progress.« less

Spectroscopy investigation of nanostructured nickel–zinc ferrite obtained by mechanochemical synthesis

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

Lazarević, Zorica Ž., E-mail: lzorica@yahoo.com; Milutinović, Aleksandra N.; Jovalekić, Čedomir D.

2015-03-15

Highlights: • Nano powder of Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} prepared by a soft mechanochemicaly after 10 h milling. • Phase formation controlled by XRD, Raman and IR spectroscopy. • Spectroscopy measurements indicate that the prepared samples have spinel structure. • The average particles size are found to be around 20 nm. • The degree of inversion is δ = 0.36 for NZF obtained from hydroxides for 10 h. - Abstract: Nano crystalline samples of nickel–zinc ferrite, Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} were prepared by mechanochemical route in a planetary ball mill starting from two mixtures of the appropriate quantitiesmore » of the powders: case (1) oxide powders: NiO, ZnO and α-Fe{sub 2}O{sub 3} in one case, and in the second case (2) hydroxide powders: Ni(OH){sub 2}, Zn(OH){sub 2} and Fe(OH){sub 3}. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman, IR and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.« less

Synthesis, structural, dielectric and magnetic properties of polyol assisted copper ferrite nano particles

NASA Astrophysics Data System (ADS)

Pavithradevi, S.; Suriyanarayanan, N.; Boobalan, T.

2017-03-01

Nanocrystalline copper ferrite CuFe2O4 is synthesized by co-precipitation method in ethylene glycol as chelating agent, using sodium Hydroxide as precipitator at pH 8. The as synthesized CuFe2O4 is annealed at temperatures of 350 °C, 700 °C, and 1050 °C for 2 h respectively. The thermal analysis of the synthesized sample is done by TG technique. It is shown that at 260 °C ethylene glycol has evaporated completely and after 715 °C, spinel ferrite is formed with a cubic structure. The calculated lattice parameters are in agreement with the reported values. FTIR spectra of CuFe2O4 nano particles are as synthesized and annealed at 1050 °C and recorded between 400 cm-1 and 4000 cm-1. It shows that when the temperature increases ethylene glycol gradually evaporates. Finally, nano crystalline single phase spinel ferrite is obtained. X-ray diffraction (XRD) and electron diffraction (EDS) studies show that the sample is indexed as the face centered cubic spinel structure. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated that the particles are flaky and spherical with the crystallite size in the range of 25-34 nm. From the dielectric studies, the dielectric constant decreases as the frequency increases. Low value of dielectric loss at higher frequencies suggests that the material is suitable for high frequency applications. AC conductivity increases with frequency. The magnetic properties of the samples are measured using a vibrating sample magnetometer (VSM) at room temperature, which shows that the sample exhibited a typical super paramagnetic behavior at low temperature. The saturation magnetization, remanant magnetism, and coercivity increases with applied field.

Damage-free vibrational spectroscopy of biological materials in the electron microscope

PubMed Central

Rez, Peter; Aoki, Toshihiro; March, Katia; Gur, Dvir; Krivanek, Ondrej L.; Dellby, Niklas; Lovejoy, Tracy C.; Wolf, Sharon G.; Cohen, Hagai

2016-01-01

Vibrational spectroscopy in the electron microscope would be transformative in the study of biological samples, provided that radiation damage could be prevented. However, electron beams typically create high-energy excitations that severely accelerate sample degradation. Here this major difficulty is overcome using an ‘aloof' electron beam, positioned tens of nanometres away from the sample: high-energy excitations are suppressed, while vibrational modes of energies <1 eV can be ‘safely' investigated. To demonstrate the potential of aloof spectroscopy, we record electron energy loss spectra from biogenic guanine crystals in their native state, resolving their characteristic C–H, N–H and C=O vibrational signatures with no observable radiation damage. The technique opens up the possibility of non-damaging compositional analyses of organic functional groups, including non-crystalline biological materials, at a spatial resolution of ∼10 nm, simultaneously combined with imaging in the electron microscope. PMID:26961578

Damage-free vibrational spectroscopy of biological materials in the electron microscope.

PubMed

Rez, Peter; Aoki, Toshihiro; March, Katia; Gur, Dvir; Krivanek, Ondrej L; Dellby, Niklas; Lovejoy, Tracy C; Wolf, Sharon G; Cohen, Hagai

2016-03-10

Vibrational spectroscopy in the electron microscope would be transformative in the study of biological samples, provided that radiation damage could be prevented. However, electron beams typically create high-energy excitations that severely accelerate sample degradation. Here this major difficulty is overcome using an 'aloof' electron beam, positioned tens of nanometres away from the sample: high-energy excitations are suppressed, while vibrational modes of energies <1 eV can be 'safely' investigated. To demonstrate the potential of aloof spectroscopy, we record electron energy loss spectra from biogenic guanine crystals in their native state, resolving their characteristic C-H, N-H and C=O vibrational signatures with no observable radiation damage. The technique opens up the possibility of non-damaging compositional analyses of organic functional groups, including non-crystalline biological materials, at a spatial resolution of ∼10 nm, simultaneously combined with imaging in the electron microscope.

Damage-free vibrational spectroscopy of biological materials in the electron microscope

DOE PAGES

Rez, Peter; Aoki, Toshihiro; March, Katia; ...

2016-03-10

Vibrational spectroscopy in the electron microscope would be transformative in the study of biological samples, provided that radiation damage could be prevented. However, electron beams typically create high-energy excitations that severely accelerate sample degradation. Here this major difficulty is overcome using an ‘aloof’ electron beam, positioned tens of nanometres away from the sample: high-energy excitations are suppressed, while vibrational modes of energies o1 eV can be ‘safely’ investigated. To demonstrate the potential of aloof spectroscopy, we record electron energy loss spectra from biogenic guanine crystals in their native state, resolving their characteristic C–H, N–H and C=O vibrational signatures with nomore » observable radiation damage. Furthermore, the technique opens up the possibility of non-damaging compositional analyses of organic functional groups, including non-crystalline biological materials, at a spatial resolution of ~10nm, simultaneously combined with imaging in the electron microscope.« less

Damage-free vibrational spectroscopy of biological materials in the electron microscope

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

Rez, Peter; Aoki, Toshihiro; March, Katia

Vibrational spectroscopy in the electron microscope would be transformative in the study of biological samples, provided that radiation damage could be prevented. However, electron beams typically create high-energy excitations that severely accelerate sample degradation. Here this major difficulty is overcome using an ‘aloof’ electron beam, positioned tens of nanometres away from the sample: high-energy excitations are suppressed, while vibrational modes of energies o1 eV can be ‘safely’ investigated. To demonstrate the potential of aloof spectroscopy, we record electron energy loss spectra from biogenic guanine crystals in their native state, resolving their characteristic C–H, N–H and C=O vibrational signatures with nomore » observable radiation damage. Furthermore, the technique opens up the possibility of non-damaging compositional analyses of organic functional groups, including non-crystalline biological materials, at a spatial resolution of ~10nm, simultaneously combined with imaging in the electron microscope.« less

Spectroscopic attributes of Sm3+ doped magnesium zinc sulfophosphate glass: Effects of silver nanoparticles inclusion

NASA Astrophysics Data System (ADS)

Ahmadi, F.; Hussin, R.; Ghoshal, S. K.

2017-11-01

We report the modified optical properties of Sm3+ doped magnesium zinc sulfophosphate glass system with silver nanoparticles (Ag NPs) inclusion. Three glass samples were prepared using melt quenching method and characterized. TEM images revealed the nucleation of Ag NPs with average diameter ≈12.50 nm. The UV-Vis-NIR spectra showed thirteen absorption bands. The surface plasmon resonance (SPR) band of Ag NPs was manifested at 446 nm. FTIR spectra disclosed the bonding vibrations for P-O bonds, P-O-P linkages, and PO2 units. Ag NPs concentration dependent bonding parameters and Judd-Ofelt (JO) intensity parameters were calculated. The JO parameter Ω2 was reduced with the increase of Ag NPs contents, indicating the ionicity and symmetry enhancement between Sm3+ ions with their surrounding ligands. The emission spectra of all samples under the excitation wavelength of 402 nm exhibited four significant peaks centered at 562, 599, 644 and 702 nm which are allocated to 4G5/2 →6H5/2, 6H7/2, 6H9/2 and 6H11/2 transitions, respectively. Inclusion of Ag NPs was discerned to augment the luminescence intensity by a factor of two, which was majorly ascribed to the local field effect of Ag NPs and subsequent energy transfer from the NPs to Sm3+ ions.

Detection, identification, and differentiation of sheep pox virus and goat pox virus from clinical cases in Giza Governorate, Egypt

PubMed Central

Mahmoud, M. A.; Khafagi, M. H.

2016-01-01

Aim: To isolate, identify, and differentiate Capripoxviruses (CaPV) (sheep pox virus and goat pox virus) infections by egg inoculation, transmission electron microscopy (TEM), and 30 kDa RNA polymerase subunit gene-based polymerase chain reaction (PCR) (RPO30) in clinically affected animals in Hawamdia township of Giza Governorate, Egypt. Materials and Methods: A total of 37 scab samples were collected from clinically suspected field cases of sheep pox and goat pox. These samples were collected during (2014-2015) during different outbreaks of sheep pox and goat pox from Hawamdia township of Giza Governorate, Egypt. The samples were subjected to egg inoculation, TEM, and (RPO30) gene-based PCR. By using the egg inoculation: Previously prepared 37 scab samples (n=23 sheep and n=14 goats) were inoculated on the chorioallantoic membrane of specific pathogen free (SPF) embryonated chicken eggs (12 days old age). In the presence of the suitable percentage of humidity and candling, the inoculated eggs were incubated at 37°C. By using the TEM: Samples showed positive pock lesions on the chorioallantoic membranes, were fixed in glutaraldehyde, then processed and sectioned for TEM. Using the (RPO30) gene-based PCR assay, 30 of positive samples after egg inoculation (n=19 sheep and n=11 goats) were screened. Results: Using the egg inoculation, a characteristic pock lesions for poxviruses were seen in 30/37 (n=19 sheep and n=11 goats) (81.08%). Using the TEM, examination of the positive samples after egg inoculation revealed positive result in 23/30 (n=15 sheep and n=8 goats) (76.66%). The positive results represented by the presence of negatively stained oval-shape virus particles. Using the (RPO30) gene-based PCR assay, out of 30 total of positive samples after egg inoculation (n=19 sheep and n=11 goats) were screened, 27 (90%) samples (n=17 sheep and n=10 goats) were positive. The given band sizes of sheep and goats were 172 and 152 bp, respectively. Conclusion: PCR assay depended on RPO30 gene can be used lonely for the detection, identification, and differentiation of CaPVs. RPO30 gene-based PCR assay in combination with gene sequencing helps in molecular epidemiological studies of CaPV infection. PMID:28096619

Detection, identification, and differentiation of sheep pox virus and goat pox virus from clinical cases in Giza Governorate, Egypt.

PubMed

Mahmoud, M A; Khafagi, M H

2016-12-01

To isolate, identify, and differentiate Capripoxviruses (CaPV) (sheep pox virus and goat pox virus) infections by egg inoculation, transmission electron microscopy (TEM), and 30 kDa RNA polymerase subunit gene-based polymerase chain reaction (PCR) (RPO30) in clinically affected animals in Hawamdia township of Giza Governorate, Egypt. A total of 37 scab samples were collected from clinically suspected field cases of sheep pox and goat pox. These samples were collected during (2014-2015) during different outbreaks of sheep pox and goat pox from Hawamdia township of Giza Governorate, Egypt. The samples were subjected to egg inoculation, TEM, and (RPO30) gene-based PCR. By using the egg inoculation: Previously prepared 37 scab samples (n=23 sheep and n=14 goats) were inoculated on the chorioallantoic membrane of specific pathogen free (SPF) embryonated chicken eggs (12 days old age). In the presence of the suitable percentage of humidity and candling, the inoculated eggs were incubated at 37°C. By using the TEM: Samples showed positive pock lesions on the chorioallantoic membranes, were fixed in glutaraldehyde, then processed and sectioned for TEM. Using the (RPO30) gene-based PCR assay, 30 of positive samples after egg inoculation (n=19 sheep and n=11 goats) were screened. Using the egg inoculation, a characteristic pock lesions for poxviruses were seen in 30/37 (n=19 sheep and n=11 goats) (81.08%). Using the TEM, examination of the positive samples after egg inoculation revealed positive result in 23/30 (n=15 sheep and n=8 goats) (76.66%). The positive results represented by the presence of negatively stained oval-shape virus particles. Using the (RPO30) gene-based PCR assay, out of 30 total of positive samples after egg inoculation (n=19 sheep and n=11 goats) were screened, 27 (90%) samples (n=17 sheep and n=10 goats) were positive. The given band sizes of sheep and goats were 172 and 152 bp, respectively. PCR assay depended on RPO30 gene can be used lonely for the detection, identification, and differentiation of CaPVs. RPO30 gene-based PCR assay in combination with gene sequencing helps in molecular epidemiological studies of CaPV infection.

Dynamics of Functionalized Surface Molecular Monolayers Studied with Ultrafast Infrared Vibrational Spectroscopy

PubMed Central

Rosenfeld, Daniel E.; Nishida, Jun; Yan, Chang; Gengeliczki, Zsolt; Smith, Brian J.; Fayer, Michael D.

2012-01-01

The structural dynamics of thin films consisting of tricarbonyl (1,10-phenanthroline)rhenium chloride (RePhen(CO)3Cl) linked to an alkyl silane monolayer through a triazole linker synthesized on silica-on-calcium-fluoride substrates are investigated using ultrafast infrared (IR) techniques. Ultrafast 2D IR vibrational echo experiments and polarization selective heterodyne detected transient grating (HDTG) measurements, as well as polarization dependent FT-IR and AFM experiments are employed to study the samples. The vibrational echo experiments measure spectral diffusion, while the HDTG experiments measure the vibrational excited state population relaxation and investigate the vibrational transition dipole orientational anisotropy decay. To investigate the anticipated impact of vibrational excitation transfer, which can be caused by the high concentration of RePhen(CO)3Cl in the monolayer, a concentration dependence of the spectral diffusion is measured. To generate a range of concentrations, mixed monolayers consisting of both hydrogen terminated and triazole/RePhen(CO)3Cl terminated alkyl silanes are synthesized. It is found that the measured rate of spectral diffusion is independent of concentration, with all samples showing spectral diffusion of 37 ± 6 ps. To definitively test for vibrational excitation transfer, polarization selective HDTG experiments are conducted. Excitation transfer will cause anisotropy decay. Polarization resolved heterodyne detected transient grating spectroscopy is sensitive to anisotropy decay (depolarization) caused by excitation transfer and molecular reorientation. The HDTG experiments show no evidence of anisotropy decay on the appropriate time scale, demonstrating the absence of excitation transfer the RePhen(CO)3Cl. Therefore the influence of excitation transfer on spectral diffusion is inconsequential in these samples, and the vibrational echo measurements of spectral diffusion report solely on structural dynamics. A small amount of very fast (~2 ps time scale) anisotropy decay is observed. The decay is concentration independent, and is assigned to wobbling-in-a-cone orientational motions of the RePhen(CO)3Cl. Theoretical calculations reported previously for experiments on a single concentration of the same type of sample suggested the presence of some vibrational excitation transfer and excitation transfer induced spectral diffusion. Possible reasons for the experimentally observed lack of excitation transfer in these high concentration samples are discussed. PMID:23259027

Nonlinear vibrational microscopy

DOEpatents

Holtom, Gary R.; Xie, Xiaoliang Sunney; Zumbusch, Andreas

2000-01-01

The present invention is a method and apparatus for microscopic vibrational imaging using coherent Anti-Stokes Raman Scattering or Sum Frequency Generation. Microscopic imaging with a vibrational spectroscopic contrast is achieved by generating signals in a nonlinear optical process and spatially resolved detection of the signals. The spatial resolution is attained by minimizing the spot size of the optical interrogation beams on the sample. Minimizing the spot size relies upon a. directing at least two substantially co-axial laser beams (interrogation beams) through a microscope objective providing a focal spot on the sample; b. collecting a signal beam together with a residual beam from the at least two co-axial laser beams after passing through the sample; c. removing the residual beam; and d. detecting the signal beam thereby creating said pixel. The method has significantly higher spatial resolution then IR microscopy and higher sensitivity than spontaneous Raman microscopy with much lower average excitation powers. CARS and SFG microscopy does not rely on the presence of fluorophores, but retains the resolution and three-dimensional sectioning capability of confocal and two-photon fluorescence microscopy. Complementary to these techniques, CARS and SFG microscopy provides a contrast mechanism based on vibrational spectroscopy. This vibrational contrast mechanism, combined with an unprecedented high sensitivity at a tolerable laser power level, provides a new approach for microscopic investigations of chemical and biological samples.

Blind identification of full-field vibration modes of output-only structures from uniformly-sampled, possibly temporally-aliased (sub-Nyquist), video measurements

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

Yang, Yongchao; Dorn, Charles; Mancini, Tyler

Enhancing the spatial and temporal resolution of vibration measurements and modal analysis could significantly benefit dynamic modelling, analysis, and health monitoring of structures. For example, spatially high-density mode shapes are critical for accurate vibration-based damage localization. In experimental or operational modal analysis, higher (frequency) modes, which may be outside the frequency range of the measurement, contain local structural features that can improve damage localization as well as the construction and updating of the modal-based dynamic model of the structure. In general, the resolution of vibration measurements can be increased by enhanced hardware. Traditional vibration measurement sensors such as accelerometers havemore » high-frequency sampling capacity; however, they are discrete point-wise sensors only providing sparse, low spatial sensing resolution measurements, while dense deployment to achieve high spatial resolution is expensive and results in the mass-loading effect and modification of structure's surface. Non-contact measurement methods such as scanning laser vibrometers provide high spatial and temporal resolution sensing capacity; however, they make measurements sequentially that requires considerable acquisition time. As an alternative non-contact method, digital video cameras are relatively low-cost, agile, and provide high spatial resolution, simultaneous, measurements. Combined with vision based algorithms (e.g., image correlation or template matching, optical flow, etc.), video camera based measurements have been successfully used for experimental and operational vibration measurement and subsequent modal analysis. However, the sampling frequency of most affordable digital cameras is limited to 30–60 Hz, while high-speed cameras for higher frequency vibration measurements are extremely costly. This work develops a computational algorithm capable of performing vibration measurement at a uniform sampling frequency lower than what is required by the Shannon-Nyquist sampling theorem for output-only modal analysis. In particular, the spatio-temporal uncoupling property of the modal expansion of structural vibration responses enables a direct modal decoupling of the temporally-aliased vibration measurements by existing output-only modal analysis methods, yielding (full-field) mode shapes estimation directly. Then the signal aliasing properties in modal analysis is exploited to estimate the modal frequencies and damping ratios. Furthermore, the proposed method is validated by laboratory experiments where output-only modal identification is conducted on temporally-aliased acceleration responses and particularly the temporally-aliased video measurements of bench-scale structures, including a three-story building structure and a cantilever beam.« less

Blind identification of full-field vibration modes of output-only structures from uniformly-sampled, possibly temporally-aliased (sub-Nyquist), video measurements

DOE PAGES

Yang, Yongchao; Dorn, Charles; Mancini, Tyler; ...

2016-12-05

Enhancing the spatial and temporal resolution of vibration measurements and modal analysis could significantly benefit dynamic modelling, analysis, and health monitoring of structures. For example, spatially high-density mode shapes are critical for accurate vibration-based damage localization. In experimental or operational modal analysis, higher (frequency) modes, which may be outside the frequency range of the measurement, contain local structural features that can improve damage localization as well as the construction and updating of the modal-based dynamic model of the structure. In general, the resolution of vibration measurements can be increased by enhanced hardware. Traditional vibration measurement sensors such as accelerometers havemore » high-frequency sampling capacity; however, they are discrete point-wise sensors only providing sparse, low spatial sensing resolution measurements, while dense deployment to achieve high spatial resolution is expensive and results in the mass-loading effect and modification of structure's surface. Non-contact measurement methods such as scanning laser vibrometers provide high spatial and temporal resolution sensing capacity; however, they make measurements sequentially that requires considerable acquisition time. As an alternative non-contact method, digital video cameras are relatively low-cost, agile, and provide high spatial resolution, simultaneous, measurements. Combined with vision based algorithms (e.g., image correlation or template matching, optical flow, etc.), video camera based measurements have been successfully used for experimental and operational vibration measurement and subsequent modal analysis. However, the sampling frequency of most affordable digital cameras is limited to 30–60 Hz, while high-speed cameras for higher frequency vibration measurements are extremely costly. This work develops a computational algorithm capable of performing vibration measurement at a uniform sampling frequency lower than what is required by the Shannon-Nyquist sampling theorem for output-only modal analysis. In particular, the spatio-temporal uncoupling property of the modal expansion of structural vibration responses enables a direct modal decoupling of the temporally-aliased vibration measurements by existing output-only modal analysis methods, yielding (full-field) mode shapes estimation directly. Then the signal aliasing properties in modal analysis is exploited to estimate the modal frequencies and damping ratios. Furthermore, the proposed method is validated by laboratory experiments where output-only modal identification is conducted on temporally-aliased acceleration responses and particularly the temporally-aliased video measurements of bench-scale structures, including a three-story building structure and a cantilever beam.« less

Micromechanical and in situ shear testing of Al–SiC nanolaminate composites in a transmission electron microscope (TEM)

DOE PAGES

Mayer, Carl; Li, Nan; Mara, Nathan Allan; ...

2014-11-07

Nanolaminate composites show promise as high strength and toughness materials. Still, due to the limited volume of these materials, micron scale mechanical testing methods must be used to determine the properties of these films. To this end, a novel approach combining a double notch shear testing geometry and compression with a flat punch in a nanoindenter was developed to determine the mechanical properties of these films under shear loading. To further elucidate the failure mechanisms under shear loading, in situ TEM experiments were performed using a double notch geometry cut into the TEM foil. Aluminum layer thicknesses of 50nm andmore » 100nm were used to show the effect of constraint on the deformation. Higher shear strength was observed in the 50 nm sample (690±54 MPa) compared to the 100 nm sample (423±28.7 MPa). Additionally, failure occurred along the Al-SiC interface in the 50 nm sample as opposed to failure within the Al layer in the 100 nm sample.« less

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

Vibrational Spectroscopy on Photoexcited Dye-Sensitized Films via Pump-Degenerate Four-Wave Mixing.

PubMed

Abraham, Baxter; Fan, Hao; Galoppini, Elena; Gundlach, Lars

2018-03-01

Molecular sensitization of semiconductor films is an important technology for energy and environmental applications including solar energy conversion, photocatalytic hydrogen production, and water purification. Dye-sensitized films are also scientifically complex and interesting systems with a long history of research. In most applications, photoinduced heterogeneous electron transfer (HET) at the molecule/semiconductor interface is of critical importance, and while great progress has been made in understanding HET, many open questions remain. Of particular interest is the role of combined electronic and vibrational effects and coherence of the dye during HET. The ultrafast nature of the process, the rapid intramolecular vibrational energy redistribution, and vibrational cooling present complications in the study of vibronic coupling in HET. We present the application of a time domain vibrational spectroscopy-pump-degenerate four-wave mixing (pump-DFWM)-to dye-sensitized solid-state semiconductor films. Pump-DFWM can measure Raman-active vibrational modes that are triggered by excitation of the sample with an actinic pump pulse. Modifications to the instrument for solid-state samples and its application to an anatase TiO 2 film sensitized by a Zn-porphyrin dye are discussed. We show an effective combination of experimental techniques to overcome typical challenges in measuring solid-state samples with laser spectroscopy and observe molecular vibrations following HET in a picosecond time window. The cation spectrum of the dye shows modes that can be assigned to the linker group and a mode that is localized on the Zn-phorphyrin chromophore and that is connected to photoexcitation.

Helicopter TEM parameters analysis and system optimization based on time constant

NASA Astrophysics Data System (ADS)

Xiao, Pan; Wu, Xin; Shi, Zongyang; Li, Jutao; Liu, Lihua; Fang, Guangyou

2018-03-01

Helicopter transient electromagnetic (TEM) method is a kind of common geophysical prospecting method, widely used in mineral detection, underground water exploration and environment investigation. In order to develop an efficient helicopter TEM system, it is necessary to analyze and optimize the system parameters. In this paper, a simple and quantitative method is proposed to analyze the system parameters, such as waveform, power, base frequency, measured field and sampling time. A wire loop model is used to define a comprehensive 'time constant domain' that shows a range of time constant, analogous to a range of conductance, after which the characteristics of the system parameters in this domain is obtained. It is found that the distortion caused by the transmitting base frequency is less than 5% when the ratio of the transmitting period to the target time constant is greater than 6. When the sampling time window is less than the target time constant, the distortion caused by the sampling time window is less than 5%. According to this method, a helicopter TEM system, called CASHTEM, is designed, and flight test has been carried out in the known mining area. The test results show that the system has good detection performance, verifying the effectiveness of the method.

"Rinse and trickle": a protocol for TEM preparation and investigation of inorganic fibers from biological material.

PubMed

Vigliaturo, Ruggero; Capella, Silvana; Rinaudo, Caterina; Belluso, Elena

2016-07-01

The purpose of this work is to define a sample preparation protocol that allows inorganic fibers and particulate matter extracted from different biological samples to be characterized morphologically, crystallographically and chemically by transmission electron microscopy-energy dispersive spectroscopy (TEM-EDS). The method does not damage or create artifacts through chemical attacks of the target material. A fairly rapid specimen preparation is applied with the aim of performing as few steps as possible to transfer the withdrawn inorganic matter onto the TEM grid. The biological sample is previously digested chemically by NaClO. The salt is then removed through a series of centrifugation and rinse cycles in deionized water, thus drastically reducing the digestive power of the NaClO and concentrating the fibers for TEM analysis. The concept of equivalent hydrodynamic diameter is introduced to calculate the settling velocity during the centrifugation cycles. This technique is applicable to lung tissues and can be extended to a wide range of organic materials. The procedure does not appear to cause morphological damage to the fibers or modify their chemistry or degree of crystallinity. The extrapolated data can be used in interdisciplinary studies to understand the pathological effects caused by inorganic materials.

Experiment on the concrete slab for floor vibration evaluation of deteriorated building

NASA Astrophysics Data System (ADS)

Hong, S. U.; Na, J. H.; Kim, S. H.; Lee, Y. T.

2014-08-01

Damages from noise and vibration are increasing every year, and most of which are noises between floors in deteriorated building caused by floor impact sound. In this study, the floor vibration of the deteriorated buildings constructed with the concrete slabs of thickness no more than 150 mm was evaluated by the vibration impact sound. This highly reliable study was conducted to assess floor vibration according with the serviceability evaluation standard of Reiher / Meister and Koch and vibration evaluation standard of ISO and AIJ. Designed pressure for the concrete slab sample of floor vibration assessment was 24MPa, and the sample was manufactured pursuant to KS F 2865 and JIS A 1440-2 with size of 3200 mm × 3200 mm × 140 mm. Tests were conducted twice with accelerometers, and Fast Fourier Transform was performed for comparative analysis by the vibration assessment criteria. The peak displacement from Test 1 was in the range of 0.00869 - 0.02540 mm; the value of peak frequency ranged from 18 to 27 Hz, and the average value was 22Hz. The peak acceleration value from Test 2 was in the range of 0.47 - 1.07 % g; the value of peak frequency was 18.5 - 22.57 Hz, and the average was 21Hz. The vibration was apparently recognizable in most cases according to the Reiher/Meister standard. In case of Koch graph for the damage assessment of the structure, the vibration was at the medium level and causes no damage to the building structure. The measured vibration results did not exceed the damage limit or serviceability limit of building according to the vibration assessment criteria of ISO and residential assessment guidelines provided by Architectural Institute of Japan (AIJ).

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.

Atmospheric tar balls from biomass burning in Mexico

NASA Astrophysics Data System (ADS)

Adachi, K.; Buseck, P. R.

2009-12-01

Tar balls are spherical, organic aerosol particles that result from biofuel or biomass burning. They absorb sunlight and cause warming of the atmosphere. Although distinctive when viewed with a transmission electron microscope (TEM) because of their spherical shape, much remains to be determined about details of their compositions, occurrences, and generation. Here we aim to characterize the occurrences of tar balls using individual-particle analyses with a TEM and to study their formation in young biomass-burning smoke. The samples were collected using the U.S. Forest Service Twin Otter aircraft during the MILAGRO (Megacity Initiative: Local and Global Research Observations) campaign conducted in March 2006. We analyzed 84 TEM grid samples from ~30 biomass-burning events near Mexico City and over Yucatan. Sixty samples were from young smoke (less than an hour old), and others were from haze that mainly occurred from biomass burning. Tar balls have neither an evident nucleus nor are they normally attached to other particles. They are almost perfectly spherical on TEM grids, indicating that they were solid when collected. It appears as if tar balls consist of lower volatility organic matter than many other organic aerosol particles. On average, 9% by number of biomass-burning aerosol particles were tar balls in samples collected between a few minutes to an hour after emission. On the other hand, samples collected within a few minutes after emission included few or no tar balls. The occurrences and abundances of atmospheric tar balls are important when evaluating the effects of smoke on local and regional climate.

Hydrothermal green synthesis of magnetic Fe3O4-carbon dots by lemon and grape fruit extracts and as a photoluminescence sensor for detecting of E. coli bacteria.

PubMed

Ahmadian-Fard-Fini, Shahla; Salavati-Niasari, Masoud; Ghanbari, Davood

2018-10-05

The aim of this work is preparing of a photoluminescence nanostructures for rapid detection of bacterial pathogens. Firstly, carbon dots (CDs) were synthesized by grape fruit, lemon, turmeric extracts and hydrothermal method. Then Fe 3 O 4 (magnetite) nanoparticles was achieved using these bio-compatible capping agents. Finally, magnetite-carbon dots were synthesized as a novel magnetic and photoluminescence nanocomposite. X-ray diffraction (XRD) confirms the crystallinity and phase of the products, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigate the morphology, shape and size of the magnetite, carbon dot and nanocomposites. Fourier transform infrared (FT-IR) spectroscopy shows the purity of the nanostructures. Ultraviolet-visible (UV-Vis) absorption and photo-luminescence (PL) spectroscopy show suitable photo-luminescence under ultraviolet irradiation. Vibrating sample magnetometer (VSM) shows super paramagnetic property of the product. Interestingly carbon dots were used as a non-toxic photoluminescence sensor for detecting of Escherichia coli (E. coli) bacteria. Results show quenching of photoluminescence of the CDs nanocomposite by increasing amount of E. coli bacteria. Copyright © 2018 Elsevier B.V. All rights reserved.

Synthesis of FeCo magnetic nanoalloys and investigation of heating properties for magnetic fluid hyperthermia

NASA Astrophysics Data System (ADS)

Çelik, Özer; Fırat, Tezer

2018-06-01

In this study, size controlled FeCo colloidal magnetic nanoalloys in the range of 11.5-37.2 nm were synthesized by surfactant assistant ball milling method. Magnetic separation technique was performed subsequent to synthesis process so as to obtain magnetic nanoalloy fluid with narrow size distribution. Particle distribution was determined by transmission electron microscope (TEM) while X-ray diffraction (XRD) measurements verified FeCo alloy formation as BCC structure. Vibrating sample magnetometer (VSM) method was used to investigate magnetic properties of nanoalloys. Maximum saturation magnetization and maximum coercivity were obtained as 172 Am2/kg for nanoparticles with the mean size of 37.2 nm and 19.4 mT for nanoparticles with the mean size of 13.3 nm, respectively. The heating ability of FeCo magnetic nanoalloys was determined through calorimetrical measurements for magnetic fluid hyperthermia (MFH) applications. Heat generation mechanisms were investigated by using linear response theory and Stoner-Wohlfarth (S-W) model. Specific absorption rate (SAR) values were obtained in the range of 2-15 W/g for magnetic field frequency of 171 kHz and magnetic field strength in between 6 and 14 mT.

Development of new magnetic nanoparticles: Oligochitosan obtained by γ-rays and -coated Fe3O4 nanoparticles

NASA Astrophysics Data System (ADS)

Le Thi, Thao Nguyen; Nguyen, Thi Hiep; Hoang, Dong Quy; Tran, Tuong, Vi; Nguyen, Ngoc Thuy; Nguyen, Dai Hai

2017-11-01

Oligochitosan (OCS) have been utilized as a potential bioactive material for improving food quality and human health. In this study, superparamagnetic iron oxide (Fe3O4) nanoparticles were originally coated with OCS irradiated by gamma rays for their possible biomedical applications. The formation of Fe3O4@OCS was characterized by Fourier transform infrared (FT-IR), X-ray diffraction patterns (XRD), energy dispersive X-ray spectroscopy (EDS) and thermogravimetric analysis (TGA). In addition, the superparamagnetic properties and sizes and morphologies of Fe3O4 and Fe3O4@OCS nanoparticles were demonstrated by vibrating sample magnetometer (VSM) and transmission electron microscopy (TEM), respectively. These results indicated that Fe3O4@OCS nanoparticles still maintained their superparamagnetic properties after polymeric coating, and were nearly spherical in shape with average diameter of 14.4 ± 0.31 nm, compared with 11.8 ± 0.52 nm of bare Fe3O4 nanoparticles, respectively. As a result, Fe3O4@OCS nanoparticles may serve as a promising platform for the development of new magnetic materials, which could be useful for biomedical applications.

Elaboration of nano titania-magnetic reduced graphene oxide for degradation of tartrazine dye in aqueous solution

NASA Astrophysics Data System (ADS)

Nada, Amr A.; Tantawy, Hesham R.; Elsayed, Mohamed A.; Bechelany, Mikhael; Elmowafy, Mohamed E.

2018-04-01

In this paper, magnetic nanocomposites are synthesized by loading reduced graphene oxide (RG) with two components of nanoparticles consisting of titanium dioxide (TiO2) and magnetite (Fe3O4) with varying amounts. The structural and magnetic features of the prepared composite photocatalysts were investigated by powder X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), transmission electron microscopy (TEM), UV-vis diffuse reflectance spectra (UV-vis/DRS), Raman and vibrating sample magnetometer (VSM). The resulting TiO2/magnetite reduced graphene oxide (MRGT) composite demonstrated intrinsic visible light photocatalytic activity, on degradation of tartrazine (TZ) dye from a synthetic aqueous solution. Specifically, it exhibits higher photocatalytic activity than magnetite reduced graphene oxide (MRG) and TiO2 nanoparticles. The photocatalytic degradation of TZ dye when using MRG and TiO2 for 3 h under visible light was 35% and 10% respectively, whereas for MRGT it was more than 95%. The higher photocatalytic efficiency of MRGT is due to the existence of reduced graphene oxide and magnetite which enhances the photocatalytic efficiency of the composite in visible light towards the degradation of harmful soluble azo dye (tartrazine).

Synthesis of MnxGa1-xFe2O4 magnetic nanoparticles by thermal decomposition method for medical diagnosis applications

NASA Astrophysics Data System (ADS)

Sánchez, Javier; Cortés-Hernández, Dora Alicia; Escobedo-Bocardo, José Concepción; Almanza-Robles, José Manuel; Reyes-Rodríguez, Pamela Yajaira; Jasso-Terán, Rosario Argentina; Bartolo-Pérez, Pascual; De-León-Prado, Laura Elena

2017-04-01

In this work, the synthesis of MnxGa1-xFe2O4 (x=0-1) nanosized particles by thermal decomposition method, using tetraethylene glycol (TEG) as a reaction medium, has been performed. The crystalline structure of the inverse spinel obtained in all the cases was identified by X-ray diffraction (XRD). Vibration sample magnetometry (VSM) was used to evaluate the magnetic properties of ferrites and to demonstrate their superparamagnetic behavior and the increase of magnetization values due to the Mn2+ ions incorporation into the FeGa2O4 structure. Transmission electron microscopy, energy dispersive spectroscopy (TEM-EDS) and X-ray photoelectron spectroscopy (XPS) were used to characterize the obtained magnetic nanoparticles (MNPs). These MNPs showed a near spherical morphology, an average particle size of 5.6±1.5 nm and a TEG coating layer on their surface. In all the cases MNPs showed no response when submitted to an alternating magnetic field (AMF, 10.2 kA/m, 354 kHz) using magnetic induction tests. These results suggest that the synthesized nanoparticles can be potential candidates for their use in biomedical areas.

Fabrication of Co0.5Ni0.5CrxFe2-xO4 materials via sol-gel method and their characterizations

NASA Astrophysics Data System (ADS)

Kadam, R. H.; Birajdar, A. P.; Alone, Suresh T.; Shirsath, Sagar E.

2013-02-01

Co0.5Ni0.5CrxFe2-xO4 nanoparticles have been designed by the sol-gel auto combustion method, using nitrates of the respective metal ions, and citric acid as the starting materials. The process takes only a few minutes to obtain as-received Cr-substituted Co-Ni ferrite powders. X-ray diffraction (XRD), vibrational sample magnetometer (VSM), transmission electron microscopy (TEM) are utilized in order to study the effect of variation in the Cr3+ substitution and its impact on particle size, lattice constant, specific surface area, cation distribution and magnetic properties. Lattice parameter, particle size found to decrease with increasing Cr3+ content, whereas specific surface area showed increasing trend with the Cr3+ substitution. Cation distribution indicates that the Cr, Co and Ni ions show preference toward octahedral [B] site, whereas Fe occupies both tetrahedral (A) and octahedral [B] sites. Saturation magnetization (MS) decreased from 65.1 to 40.6 emu/g with the increase in Cr3+ substitution. However, Coercivity increased from 198 to 365 Oe with the Cr3+ substitution.

One-pot synthesis of powder-form β-Ni(OH)2 monolayer nanosheets with high electrochemical performance

NASA Astrophysics Data System (ADS)

Wang, Minmin; Ren, Wanzhong; Zhao, Yunan; Liu, Yan; Cui, Hongtao

2013-08-01

In this work, β-Ni(OH)2 monolayer nanosheets, which had been thought to be unachievable, were successfully prepared for the first time by a one-pot strategy using epoxide as precipitation agent and sodium dodecyl sulfate (SDS) as surfactant. The characterization results indicate that the formation of monolayer morphology depends on the mediation of SDS molecules. The XRD patterns demonstrate the loose and defective packing of Ni(OH)2 layers in the SDS intercalated samples. The disappearing of vibration band of free hydroxyl groups in the FTIR spectra suggests the interlayer separation resulted by SDS. The TEM and AFM images further confirm the formation of monolayer nanosheets. It is proposed that the in situ modification of the secondary growth unit of β-Ni(OH)2 by SDS allows its two-dimensional anisotropic growth through steric hindrance of SDS molecules. In addition, this effect allows isolation of β-Ni(OH)2 from solvent with keeping of monolayer nanosheet state in dry powder. The electrochemical measurement results indicate that β-Ni(OH)2 monolayer nanosheets own much higher urea electrolysis performance than their corresponding multilayer structure.

From the iron boring scraps to superparamagnetic nanoparticles through an aerobic biological route.

PubMed

Daneshvar, Majid; Hosseini, Mohammad Raouf

2018-06-15

A straightforward, highly efficient, and low-cost biological route was introduced for the synthesis of magnetic nanoparticles. Three urease-positive bacteria namely, Bacillus subtilis, B. pasteurii, and B. licheniformis were used to biosynthesize ammonia and biosurfactants required for the nanoparticle production. Also, the features of the applied biological approach was compared with a chemical co-precipitation method. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), dynamic light scattering (DLS), vibrating-sample magnetometer (VSM), and Fourier transform infrared spectroscopy (FTIR) were applied to characterize the synthesized nanoparticles. Results indicated that the biologically fabricated powders had a single domain structure, and their mean particle size was in the range of 37 to 97 nm. The production capacity of the biological processes was double the chemical method, and the biosynthesized superparamagnetic nanoparticles had higher saturation magnetization up to 132 emu/g. Finally, the removal of Cr(VI) from a synthetic solution was investigated using the four products. The maximum elimination of chromium (over 99%) was achieved by the particles synthesized by B. pasteurii, with the adsorption capacity of 190 mg/g. Copyright © 2018 Elsevier B.V. All rights reserved.

Structural, magnetic and hyperfine characterization of ZnxFe3-xO4 nanoparticles prepared by sol-gel approach via inorganic precursors

NASA Astrophysics Data System (ADS)

Kotsikau, Dzmitry; Pankov, Vladimir; Petrova, Elena; Natarov, Valentin; Filimonov, Dmitry; Pokholok, Konstantin

2018-03-01

Structural characteristics and magnetic properties of ZnxFe3-xO4 (where x = 0; 0.09; 0.18; 0.45; 1) nanoparticles were studied with X-ray diffraction (XRD), transmission electron microscopy (TEM), infrared spectroscopy (IR) and vibrating sample magnetometry (VSM). Oxidation of Fe2+ ions, redistribution of Zn2+ and Fe3+ ions between octahedral and tetrahedral sites, and the formation of cation vacancies in spinel-type cubic structure of the obtained ZnxFe3-x-y□yO4 substitutional solid solutions were revealed by 57Fe Mössbauer spectroscopy. The nanoparticles synthesized via a modified sol-gel method using inorganic precursors have a size of 4-10 nm, single-phase composition, superparamagnetic behavior at room temperature (300 K) and a relatively hydrophilic surface to form stable aqueous suspensions. The maximum magnetization of 59 emu/g at 300 K corresponds to Zn0.18Fe2.82O4 composition. The listed features make the materials promising candidates for various biological and medical applications such as contrast-enhanced magnetic resonance imaging, hyperthermia of pathological tissues, controlled drug release, and separation of nucleic acids.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

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.

Improved design for a low temperature scanning tunneling microscope with an in situ tip treatment stage.

PubMed

Kim, J-J; Joo, S H; Lee, K S; Yoo, J H; Park, M S; Kwak, J S; Lee, Jinho

2017-04-01

The Low Temperature Scanning Tunneling Microscope (LT-STM) is an extremely valuable tool not only in surface science but also in condensed matter physics. For years, numerous new ideas have been adopted to perfect LT-STM performances-Ultra-Low Vibration (ULV) laboratory and the rigid STM head design are among them. Here, we present three improvements for the design of the ULV laboratory and the LT-STM: tip treatment stage, sample cleaving stage, and vibration isolation system. The improved tip treatment stage enables us to perform field emission for the purpose of tip treatment in situ without exchanging samples, while our enhanced sample cleaving stage allows us to cleave samples at low temperature in a vacuum without optical access by a simple pressing motion. Our newly designed vibration isolation system provides efficient space usage while maintaining vibration isolation capability. These improvements enhance the quality of spectroscopic imaging experiments that can last for many days and provide increased data yield, which we expect can be indispensable elements in future LT-STM designs.

Fabrication and vibration characterization of curcumin extracted from turmeric (Curcuma longa) rhizomes of the northern Vietnam.

PubMed

Van Nong, Hoang; Hung, Le Xuan; Thang, Pham Nam; Chinh, Vu Duc; Vu, Le Van; Dung, Phan Tien; Van Trung, Tran; Nga, Pham Thu

2016-01-01

In this report, we present the research results on using the conventional method and microwave technology to extract curcuminoid from turmeric roots originated in different regions of Northern Vietnam. This method is simple, yet economical, non-toxic and still able to achieve high extraction performance to get curcuminoid from turmeric roots. The detailed results on the Raman vibration spectra combined with X-ray powder diffraction and high-performance liquid chromatography/mass spectrometry allowed the evaluation of each batch of curcumin crystalline powder sample received, under the conditions of applied fabrication technology. Also, the absorption and fluorescence spectroscopies of the samples are presented in the paper. The information to be presented in this paper: absorption and fluorescence spectroscopies of the samples; new experimental study results on applied technology to mass-produce curcumin from turmeric rhizomes; comparative study results between fabricated samples and marketing curcumin products-to state the complexity of co-existing crystalline phase in curcumin powder samples. We noticed that, it is possible to use the vibration line at ~959 cm(-1)-characteristic of the ν C=O vibration, and the ~1625 cm(-1) line-characteristic of the ν C=O and ν C=C vibration in curcumin molecules, for preliminary quality assessment of naturally originated curcumin crystalline powder samples. Data on these new optical spectra will contribute to the bringing of detailed information on natural curcumin in Vietnam, serving research purposes and applications of natural curcumin powder and nanocurcumin in Vietnam, as well as being initial materials for the pharmaceutical, cosmetics or functional food industries.

Assessment of microcrystal quality by transmission electron microscopy for efficient serial femtosecond crystallography.

PubMed

Barnes, Christopher O; Kovaleva, Elena G; Fu, Xiaofeng; Stevenson, Hilary P; Brewster, Aaron S; DePonte, Daniel P; Baxter, Elizabeth L; Cohen, Aina E; Calero, Guillermo

2016-07-15

Serial femtosecond crystallography (SFX) employing high-intensity X-ray free-electron laser (XFEL) sources has enabled structural studies on microcrystalline protein samples at non-cryogenic temperatures. However, the identification and optimization of conditions that produce well diffracting microcrystals remains an experimental challenge. Here, we report parallel SFX and transmission electron microscopy (TEM) experiments using fragmented microcrystals of wild type (WT) homoprotocatechuate 2,3-dioxygenase (HPCD) and an active site variant (H200Q). Despite identical crystallization conditions and morphology, as well as similar crystal size and density, the indexing efficiency of the diffraction data collected using the H200Q variant sample was over 7-fold higher compared to the diffraction results obtained using the WT sample. TEM analysis revealed an abundance of protein aggregates, crystal conglomerates and a smaller population of highly ordered lattices in the WT sample as compared to the H200Q variant sample. While not reported herein, the 1.75 Å resolution structure of the H200Q variant was determined from ∼16 min of beam time, demonstrating the utility of TEM analysis in evaluating sample monodispersity and lattice quality, parameters critical to the efficiency of SFX experiments. Copyright © 2016 Elsevier Inc. All rights reserved.

Real-time vibration measurement by a spatial phase-shifting technique with a tilted holographic interferogram.

PubMed

Nakadate, S; Isshiki, M

1997-01-01

Real-time vibration measurement by a tilted holographic interferogram is presented that utilizes the real-time digital fringe processor of a video signal. Three intensity data sampled at every one-third of the fringe spacing of the tilted fringes are used to calculate the modulation term of the fringe that is a function of a vibration amplitude. A three-dimensional lookup table performs the calculation in a TV repetition rate to give a new fringe profile that contours the vibration amplitude. Vibration modes at the resonant frequencies of a flat speaker were displayed on a monitor as changing the exciting frequency of vibration.

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.

A simple vibrating sample magnetometer for macroscopic samples

NASA Astrophysics Data System (ADS)

Lopez-Dominguez, V.; Quesada, A.; Guzmán-Mínguez, J. C.; Moreno, L.; Lere, M.; Spottorno, J.; Giacomone, F.; Fernández, J. F.; Hernando, A.; García, M. A.

2018-03-01

We here present a simple model of a vibrating sample magnetometer (VSM). The system allows recording magnetization curves at room temperature with a resolution of the order of 0.01 emu and is appropriated for macroscopic samples. The setup can be mounted with different configurations depending on the requirements of the sample to be measured (mass, saturation magnetization, saturation field, etc.). We also include here examples of curves obtained with our setup and comparison curves measured with a standard commercial VSM that confirms the reliability of our device.

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.

Formation of the YBa2Cu2NbOy Phase in Thin Films (POSTPRINT)

DTIC Science & Technology

2010-03-01

protective layer was deposited on the top of YBCNO film by dc sputtering . A 200 nm 200 nm area film was selected and cut with a Ga ion beam (30 kV...200 TEM at 200 kV. Samples for TEM were prepared using a focused ion beam (FIB (Eindhoven, The Netherlands)) microscope. For TEM examination, a thin Pt...by dc magnetron sputtering deposition of Ag with 93 mm thickness. Transport current measurements were made in liquid nitrogen with the 4-probe method

Disc Antenna Enhanced Infrared Spectroscopy: From Self-Assembled Monolayers to Membrane Proteins.

PubMed

Pfitzner, Emanuel; Seki, Hirofumi; Schlesinger, Ramona; Ataka, Kenichi; Heberle, Joachim

2018-05-25

Plasmonic surfaces have emerged as a powerful platform for biomolecular sensing applications and can be designed to optimize the plasmonic resonance for probing molecular vibrations at utmost sensitivity. Here, we present a facile procedure to generate metallic microdisc antenna arrays that are employed in surface-enhanced infrared absorption (SEIRA) spectroscopy of biomolecules. Transmission electron microscopy (TEM) grids are used as shadow mask deployed during physical vapor deposition of gold. The resulting disc-shaped antennas exhibit enhancement factors of the vibrational bands of 4 × 10 4 giving rise to a detection limit <1 femtomol (10 -15 mol) of molecules. Surface-bound monolayers of 4-mercaptobenzoic acid show polyelectrolyte behavior when titrated with cations in the aqueous medium. Conformational rigidity of the self-assembled monolayer is validated by density functional theory calculations. The membrane protein sensory rhodopsin II is tethered to the disc antenna arrays and is fully functional as inferred from the light-induced SEIRA difference spectra. As an advance to previous studies, the accessible frequency range is improved and extended into the fingerprint region.

eV-TEM: Transmission electron microscopy in a low energy cathode lens instrument.

PubMed

Geelen, Daniël; Thete, Aniket; Schaff, Oliver; Kaiser, Alexander; van der Molen, Sense Jan; Tromp, Rudolf

2015-12-01

We are developing a transmission electron microscope that operates at extremely low electron energies, 0-40 eV. We call this technique eV-TEM. Its feasibility is based on the fact that at very low electron energies the number of energy loss pathways decreases. Hence, the electron inelastic mean free path increases dramatically. eV-TEM will enable us to study elastic and inelastic interactions of electrons with thin samples. With the recent development of aberration correction in cathode lens instruments, a spatial resolution of a few nm appears within range, even for these very low electron energies. Such resolution will be highly relevant to study biological samples such as proteins and cell membranes. The low electron energies minimize adverse effects due to radiation damage. Copyright © 2015. Published by Elsevier B.V.

TEM observations of radiation damage in tungsten irradiated by 20 MeV W ions

NASA Astrophysics Data System (ADS)

Ciupiński, Ł.; Ogorodnikova, O. V.; Płociński, T.; Andrzejczuk, M.; Rasiński, M.; Mayer, M.; Kurzydłowski, K. J.

2013-12-01

Polycrystalline, recrystallized W targets were subjected to implantation with 20 MeV W6+ ions in order to simulate radiation damage caused by fusion neutrons. Three samples with cumulative damage of 0.01, 0.1 and 0.89 dpa were produced. The near-surface zone of each sample has been analyzed by transmission electron microscopy (TEM). To this end, lamellae oriented perpendicularly to the targets implanted surface were milled out using focused ion beam (FIB). A reference lamella from non-irradiated, recrystallized W target was also prepared to estimate the damage introduced during FIB processing. TEM studies revealed a complex microstructure of the damaged zones as well as its evolution with cumulative damage level. The experimentally observed damage depth agrees very well with the one calculated using the Stopping and Range of Ions in Matter (SRIM) software.

Quantification of the effects of audible rattle and source type on the human response to environmental vibration.

PubMed

Woodcock, J; Sica, G; Peris, E; Sharp, C; Moorhouse, A T; Waddington, D C

2016-03-01

The present research quantifies the influence of source type and the presence of audible vibration-induced rattle on annoyance caused by vibration in residential environments. The sources of vibration considered are railway and the construction of a light rail system. Data were measured in the United Kingdom using a socio-vibration survey (N = 1281). These data are analyzed using ordinal logit models to produce exposure-response relationships describing community annoyance as a function of vibration exposure. The influence of source type and the presence of audible vibration-induced rattle on annoyance are investigated using dummy variable analysis, and quantified using odds-ratios and community tolerance levels. It is concluded that the sample population is more likely to express higher levels of annoyance if the vibration source is construction compared to railway, and if vibration-induced rattle is audible.

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.

Synthesis and optical properties of Co2+-doped ZnO Network prepared by new precursors

NASA Astrophysics Data System (ADS)

Akhtari, Fereshteh; Zorriasatein, Suzan; Farahmandjou, Majid; Elahi, Seyed Mohammad

2018-06-01

Pure ZnO nanoparticles (NPs) and Co/ZnO alloy NPs were synthesized with different percentages of cobalt impurity (1%, 3%, 5%, and 25%) with new precursors through the coprecipitation method. The structural results of the XRD analysis indicated that the pure and impure samples have a wurtzite hexagonal structure such that with an elevation of Co impurity up to 1%, the size of the nanocrystals declines by up to 30 nm. Furthermore, the FESEM analysis results suggest the homogeneity of the NPs such that with increased cobalt impurity, its level declines. The TEM analysis results revealed that the NPs with 5% impurity have a mean size of 32 nm in spherical form. The FTIR optical analysis results suggest a very sharp absorption peak within the wavelength ranges of 434–448 cm‑1, belonging to the Zn-O vibration bond. In addition, the absorption peak developed at the wavelength of 3428 cm‑1 is related to the activation of the OH radicals, whose absorption value grows with the addition of an impurity, thereby, causing enhanced photocatalytic activity. The UV-DRS optical analysis indicated that the absorption wavelength grows with increased impurity, causing the development of redshift and a reduction of the energy band gap. In this regard, for the pure sample, the band gap value was 3.18 eV, while for the sample with 5% impurity, the band gap was obtained as 2.68 eV. The VSM magnetic analysis suggests ferromagnetic development in the impure sample, with a saturation magnetism of 16 memu g‑1 and a coercivity field of 342 G.

Synthesis of a smart pH-responsive magnetic nanocomposite as high loading carrier of pharmaceutical agents.

PubMed

Berah, Razieh; Ghorbani, Mohsen; Moghadamnia, Ali Akbar

2017-06-01

To create facile external controlled drug delivery system, a magnetic porous carrier based on Tin oxide nanoparticles was synthesized by an inexpensive and versatile hydrothermal strategy and used for in-vitro process. Magnetic nanocomposites were qualified by Fourier Transform Infrared (FTIR), Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), Vibrational Sample Magnetometer (VSM) and Transmission Electron Microscopy (TEM). Results showed that nanoparticles were synthesized successfully with good dispersion of magnetic nanoparticles in cavity, uniform particle size distribution with average size of 65nm and high magnetization of 33.75 emu/mg. Furthermore, the nano-porosity and magnetism allowed high efficiency and remote controlled drug release. In this study, anti-migraine Sumatriptan was used as drug sample and the effect of drug concentration, Fe/Sn ratio and loading time on drug absorption were investigated. The best result was checked for stability at body temperature and different body pH. The sample with drug concentration of 0.25(mg/ml), Fe/Sn=0.22 and loading time of 1.5h had the highest drug efficiency (70%). Finally, in order to simulate the in vivo process for in-vitro step, Amnion was used and drug diffusion rate was measured in different intervals and different pH values. The result illustrated that after 25h, diffusion reached 65% at pH=2 and 56% at pH=7, and then became constant. Based on the above mentioned results, the carrier has an acceptable in vitro yield and therefore could be chosen for future in vivo researches. Copyright © 2017 Elsevier B.V. All rights reserved.

A sensitive label-free immunosensor for detection α-Fetoprotein in whole blood based on anticoagulating magnetic nanoparticles.

PubMed

Xu, Tingting; Chi, Bo; Wu, Fan; Ma, Shangshang; Zhan, Shuyue; Yi, Meihui; Xu, Hong; Mao, Chun

2017-09-15

Accurate values of tumor markers in blood play an especially important role in the diagnosis of illness. Here, based on the combination of three techniques include anticoagulant technology, nanotechnology and biosensing technology, a sensitive label-free immunosensor with anti-biofouling electrode for detection α-Fetoprotein (AFP) in whole blood was developed by anticoagulating magnetic nanoparticles. The obtained products of Fe 3 O 4 -ɛ-PL-Hep nanoparticles were characterized by fourier transform infrared (FT-IR) spectra, transmission electron microscopy (TEM), ζ-potential and vibrating sample magnetometry (VSM). Moreover, the blood compatibility of anticoagulating magnetic nanoparticles was characterized by in vitro coagulation tests, hemolysis assay and whole blood adhesion tests. Combining the anticoagulant property of heparin (Hep) and the good magnetism of Fe 3 O 4 , the Fe 3 O 4 -ɛ-PL-Hep nanoparticles could improve not only the anti-biofouling property of the electrode surface when they contact with whole blood, but also the stability and reproducibility of the proposed immunosensor. Thus, the prepared anticoagulating magnetic nanoparticles modified immunosensor for the detection of AFP showed excellent electrochemical properties with a wide concentration range from 0.1 to 100ng/mL and a low detection limit of 0.072ng/mL. Furthermore, five blood samples were assayed using the developed immunosensor. The results showed satisfactory accuracy with low relative errors. It indicated that our developed immunoassay was competitive and could be potentially used for the detection of whole blood samples directly. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis and calibration of stage axial vibration for synchrotron radiation nanoscale computed tomography.

PubMed

Fu, Jian; Li, Chen; Liu, Zhenzhong

2015-10-01

Synchrotron radiation nanoscale computed tomography (SR nano-CT) is a powerful analysis tool and can be used to perform chemical identification, mapping, or speciation of carbon and other elements together with X-ray fluorescence and X-ray absorption near edge structure (XANES) imaging. In practical applications, there are often challenges for SR nano-CT due to the misaligned geometry caused by the sample stage axial vibration. It occurs quite frequently because of experimental constraints from the mechanical error of manufacturing and assembly and the thermal expansion during the time-consuming scanning. The axial vibration will lead to the structure overlap among neighboring layers and degrade imaging results by imposing artifacts into the nano-CT images. It becomes worse for samples with complicated axial structure. In this work, we analyze the influence of axial vibration on nano-CT image by partial derivative. Then, an axial vibration calibration method for SR nano-CT is developed and investigated. It is based on the cross correlation of plane integral curves of the sample at different view angles. This work comprises a numerical study of the method and its experimental verification using a dataset measured with the full-field transmission X-ray microscope nano-CT setup at the beamline 4W1A of the Beijing Synchrotron Radiation Facility. The results demonstrate that the presented method can handle the stage axial vibration. It can work for random axial vibration and needs neither calibration phantom nor additional calibration scanning. It will be helpful for the development and application of synchrotron radiation nano-CT systems.

Growth of GaN- and ZnO-Based Nanorod Compound Structures

DTIC Science & Technology

2013-08-16

parallel with or forming a 60o tilted angle with respect to the two parallel lateral sides of individual NRs. In the edge-to-edge pattern, the shortest...kV and a probe forming lens of Cs = 1.2 mm. 3. SEM and TEM Observations Figures 2(a)-2(f) show the plan-view SEM images of samples I-VI... angle annular dark field (HAADF) image in TEM observation of an InGaN/GaN QW NR of sample I. In this image, the three almost vertical bright lines

Chrysotile in water

PubMed Central

Speil, Sidney

1974-01-01

The problems of quantitating chrysotile in water by fiber count techniques are reviewed briefly and the use of mass quantitation is suggested as a preferable measure. Chrysotile fiber has been found in almost every sample of natural water examined, but generally transmission electron miscroscopy (TEM) is required because of the small diameters involved. The extreme extrapolation required in mathematically converting a few fibers or fiber fragments under the TEM to the fiber content of a liquid sample casts considerable doubt on the validity of numbers used to compare chrysotile contents of different liquids. PMID:4470930

Nanoscale chromatin structure characterization for optical applications: a transmission electron microscopy study (Conference Presentation)

NASA Astrophysics Data System (ADS)

Li, Yue; Cherkezyan, Lusik; Zhang, Di; Almassalha, Luay; Roth, Eric; Chandler, John; Bleher, Reiner; Subramanian, Hariharan; Dravid, Vinayak P.; Backman, Vadim

2017-02-01

Structural and biological origins of light scattering in cells and tissue are still poorly understood. We demonstrate how this problem might be addressed through the use of transmission electron microscopy (TEM). For biological samples, TEM image intensity is proportional to mass-density, and thus proportional to refractive index (RI). By calculating the autocorrelation function (ACF) of TEM image intensity of a thin-section of cells, we essentially maintain the nanoscale ACF of the 3D cellular RI distribution, given that the RI distribution is statistically isotropic. Using this nanoscale 3D RI ACF, we can simulate light scattering through biological samples, and thus guiding many optical techniques to quantify specific structures. In this work, we chose to use Partial Wave Spectroscopy (PWS) microscopy as a one of the nanoscale-sensitive optical techniques. Hela cells were prepared using standard protocol to preserve nanoscale ultrastructure, and a 50-nm slice was sectioned for TEM imaging at 6 nm resolution. The ACF was calculated for chromatin, and the PWS mean sigma was calculated by summing over the power spectral density in the visible light frequency of a random medium generated to match the ACF. A 1-µm slice adjacent to the 50-nm slice was sectioned for PWS measurement to guarantee identical chromatin structure. For 33 cells, we compared the calculated PWS mean sigma from TEM and the value measured directly, and obtained a strong correlation of 0.69. This example indicates the great potential of using TEM measured RI distribution to better understand the quantification of cellular nanostructure by optical methods.

Significant characteristics of social response to noise and vibration

NASA Technical Reports Server (NTRS)

Nishinomiya, G.

1979-01-01

Several surveys made since 1971 to investigate annoyance resulting from noise and vibration, from various sources were studied in order to quantify the relation between annoyance response to noise or vibration and properties of the respondent including factors such as noise exposure, etc. Samples collected by the social surveys and physical measurements were analyzed by multi-dimensional analysis.

Detection and Monitoring of Neurotransmitters - a Spectroscopic Analysis

NASA Astrophysics Data System (ADS)

Manciu, Felicia; Lee, Kendall; Durrer, William; Bennet, Kevin

2012-10-01

In this work we demonstrate the capability of confocal Raman mapping spectroscopy for simultaneously and locally detecting important compounds in neuroscience such as dopamine, serotonin, and adenosine. The Raman results show shifting of the characteristic vibrations of the compounds, observations consistent with previous spectroscopic studies. Although some vibrations are common in these neurotransmitters, Raman mapping was achieved by detecting non-overlapping characteristic spectral signatures of the compounds, as follows: for dopamine the vibration attributed to C-O stretching, for serotonin the indole ring stretching vibration, and for adenosine the adenine ring vibrations. Without damage, dyeing, or preferential sample preparation, confocal Raman mapping provided positive detection of each neurotransmitter, allowing association of the high-resolution spectra with specific micro-scale image regions. Such information is particularly important for complex, heterogeneous samples, where modification of the chemical or physical composition can influence the neurotransmission processes. We also report an estimated dopamine diffusion coefficient two orders of magnitude smaller than that calculated by the flow-injection method.

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.

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

PubMed

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

2014-12-01

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

Subgrain boundary analyses in deformed orthopyroxene by TEM/STEM with EBSD-FIB sample preparation technique

NASA Astrophysics Data System (ADS)

Kogure, Toshihiro; Raimbourg, Hugues; Kumamoto, Akihito; Fujii, Eiko; Ikuhara, Yuichi

2014-12-01

High-resolution structure analyses using electron beam techniques have been performed for the investigation of subgrain boundaries (SGBs) in deformed orthopyroxene (Opx) in mylonite from Hidaka Metamorphic Belt, Hokkaido, Japan, to understand ductile deformation mechanism of silicate minerals in shear zones. Scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) analysis of Opx porphyroclasts in the mylonitic rock indicated that the crystal orientation inside the Opx crystals gradually changes by rotation about the b-axis by SGBs and crystal folding. In order to observe the SGBs along the b-axis by transmission electron microscopy (TEM) or scanning TEM (STEM), the following sample preparation protocol was adopted. First, petrographic thin sections were slightly etched with hydrofluoric acid to identify SGBs in SEM. The Opx crystals whose b-axes were oriented close to the normal of the surface were identified by EBSD, and the areas containing SGBs were picked and thinned for (S) TEM analysis with a focused ion beam instrument with micro-sampling system. High-resolution TEM imaging of the SGBs in Opx revealed various boundary structures from a periodic array of dissociated (100) [001] edge dislocations to partially or completely incoherent crystals, depending on the misorientation angle. Atomic-resolution STEM imaging clearly confirmed the formation of clinopyroxene (Cpx) structure between the dissociated partial dislocations. Moreover, X-ray microanalysis in STEM revealed that the Cpx contains a considerable amount of calcium replacing iron. Such chemical inhomogeneity may limit glide motion of the dislocation and eventually the plastic deformation of the Opx porphyroclasts at a low temperature. Chemical profiles across the high-angle incoherent SGB also showed an enrichment of the latter in calcium at the boundary, suggesting that SGBs are an efficient diffusion pathway of calcium out of host Opx grain during cooling.

In vitro effects of 3% hypertonic saline and 20% mannitol on canine whole blood coagulation and platelet function.

PubMed

Adamik, Katja-Nicole; Butty, Emmanuelle; Howard, Judith

2015-09-24

Hyperosmolar therapy, using either mannitol or hypertonic saline (HTS), is considered the treatment of choice for intracranial hypertension. However, hyperosmolar agents may impair coagulation and platelet function, limiting their use in patients at risk for hemorrhage. Despite this, studies evaluating the effects of mannitol compared to other hyperosmolar agents in dogs are largely lacking. The aim of this study was to compare the in vitro effects on global hemostasis and platelet function of 20% mannitol and 3% HTS on canine blood. Citrated whole blood from 15 healthy dogs was diluted with 0.9% saline, 20% mannitol and 3% HTS in ratios of 1:16 and 1:8. Rotational thromboelastometry (ROTEM) was used to assess clotting time (CT), clot formation time (CFT) and maximal clot firmness (MCF) following extrinsic activation (Ex-tem) and after platelet inhibition (Fib-tem). A platelet function analyzer (PFA-100) was used to assess closure time (Ct(PFA)). No significant differences were observed between untreated whole blood and samples diluted with saline. Samples diluted with both mannitol and HTS were hypocoagulable compared to untreated whole blood samples. At a dilution of 1:16, no significant differences were found between any measured parameter in samples diluted with saline compared to mannitol or HTS. At a 1:8 dilution, Ct(PFA) was prolonged in samples diluted with mannitol and HTS compared to saline, and Ct(PFA) was prolonged more with mannitol than HTS. Ex-tem CT was increased at a 1:8 dilution with mannitol compared to HTS. Ex-tem CFT was prolonged at a 1:8 dilution with both agents compared to saline, and was prolonged more with mannitol than HTS. Ex-tem MCF was reduced at a 1:8 dilution with both agents compared to saline. Data in this study indicate that both mannitol and HTS affect canine platelet function and whole blood coagulation in vitro in a dose-dependent fashion. The most pronounced effects were observed after high dilutions with mannitol, which impaired platelet aggregation, clot formation time, clot strength, and fibrin formation significantly more than HTS. Further in vivo studies are necessary before recommendations can be made.

Low- Z polymer sample supports for fixed-target serial femtosecond X-ray crystallography

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

Feld, Geoffrey K.; Heymann, Michael; Benner, W. Henry

X-ray free-electron lasers (XFELs) offer a new avenue to the structural probing of complex materials, including biomolecules. Delivery of precious sample to the XFEL beam is a key consideration, as the sample of interest must be serially replaced after each destructive pulse. The fixed-target approach to sample delivery involves depositing samples on a thin-film support and subsequent serial introduction via a translating stage. Some classes of biological materials, including two-dimensional protein crystals, must be introduced on fixed-target supports, as they require a flat surface to prevent sample wrinkling. A series of wafer and transmission electron microscopy (TEM)-style grid supports constructedmore » of low- Z plastic have been custom-designed and produced. Aluminium TEM grid holders were engineered, capable of delivering up to 20 different conventional or plastic TEM grids using fixed-target stages available at the Linac Coherent Light Source (LCLS). As proof-of-principle, X-ray diffraction has been demonstrated from two-dimensional crystals of bacteriorhodopsin and three-dimensional crystals of anthrax toxin protective antigen mounted on these supports at the LCLS. In conclusion, the benefits and limitations of these low- Z fixed-target supports are discussed; it is the authors' belief that they represent a viable and efficient alternative to previously reported fixed-target supports for conducting diffraction studies with XFELs.« less

Exposure to whole-body vibration and seat transmissibility in a large sample of earth scrapers.

PubMed

Salmoni, Alan; Cann, Adam; Gillin, Kent

2010-01-01

It is often difficult to access a large sample of vehicles in various work environments to evaluate worker exposure to vibration such as in construction and mining. Thus the main purpose of the present research was to test vibration exposure in a relatively large number of earth scrapers. The second aim was to assess vibration exposure values on seat transmissibility. 33earth scrapers were assessed for both exposure to whole-body vibration and seat transmissibility. Two triaxial accelerometers, one placed on the seat and one on the floor directly below the seat, were used to gather whole-body vibration values (a(w)). Each machine was tested for a minimum of three complete work cycles: idling, scraping, travelling full, dumping, travelling empty back to the scrape site. Results showed that idling and scraping produced low levels of vibration when compared to travelling and dumping. Second, when the a(w) values were compared to the EU safety standards for an eight hour work day, the data (z axis) exceeded the exposure action value (0.5 m/s2) in all machines, and the exposure limit value (1.15 m/s2) in some. Implications; Operators of the scrapers were being exposed to unsafe levels of whole-body vibration. When the seats were assessed to see whether they were attenuating operator exposure to vibration, many of the seat effective amplitude transmissibility (SEAT) values exceeded 1.0. This meant that some of the seats were actually amplifying the vibration present at the floor, particularly in the y axis. Travelways should be kept smooth, operating speeds reduced, and new seats, effective in all three axes, designed.

Soot Precursor Material: Spatial Location via Simultaneous LIF-LII Imaging and Characterization via TEM

NASA Technical Reports Server (NTRS)

VanderWal, Randall L.

1996-01-01

The chemical and physical transformation between gaseous fuel pyrolysis products and solid carbonaceous soot represents a critical step in soot formation. In this paper, simultaneous two-dimensional LIF-LII (laser-induced fluorescence - laser-induced incandescence) images identify the spatial location where the earliest identifiable chemical and physical transformation of material towards solid carbonaceous soot occurs along the axial streamline in a normal diffusion flame. The identification of the individual LIF and LII signals is achieved by examining both the excitation wavelength dependence and characteristic temporal decay of each signal. Spatially precise thermophoretic sampling measurements are guided by the LIF-LII images with characterization of the sampled material accomplished via both bright and dark field TEM. Both bright and dark field TEM measurements support the observed changes in photophysical properties which account for conversion of fluorescence to incandescence as fuel pyrolysis products evolve towards solid carbonaceous soot.

Automated grain mapping using wide angle convergent beam electron diffraction in transmission electron microscope for nanomaterials.

PubMed

Kumar, Vineet

2011-12-01

The grain size statistics, commonly derived from the grain map of a material sample, are important microstructure characteristics that greatly influence its properties. The grain map for nanomaterials is usually obtained manually by visual inspection of the transmission electron microscope (TEM) micrographs because automated methods do not perform satisfactorily. While the visual inspection method provides reliable results, it is a labor intensive process and is often prone to human errors. In this article, an automated grain mapping method is developed using TEM diffraction patterns. The presented method uses wide angle convergent beam diffraction in the TEM. The automated technique was applied on a platinum thin film sample to obtain the grain map and subsequently derive grain size statistics from it. The grain size statistics obtained with the automated method were found in good agreement with the visual inspection method.

Making the practically impossible "Merely difficult"--Cryogenic FIB lift-out for "Damage free" soft matter imaging.

PubMed

Parmenter, Christopher D J; Fay, Michael W; Hartfield, Cheryl; Eltaher, Hoda M

2016-04-01

The preparation of thinned lamellae from bulk samples for transmission electron microscopy (TEM) analysis has been possible in the focussed ion beam scanning electron microscope (FIB-SEM) for over 20 years via the in situ lift-out method. Lift-out offers a fast and site specific preparation method for TEM analysis, typically in the field of materials science. More recently it has been applied to a low-water content biological sample (Rubino 2012). This work presents the successful lift-out of high-water content lamellae, under cryogenic conditions (cryo-FIB lift-out) and using a nanomanipulator retaining its full range of motion, which are advances on the work previously done by Rubino (2012). Strategies are explored for maintaining cryogenic conditions, grid attachment using cryo-condensation of water and protection of the lamella when transferring to the TEM. © 2016 Wiley Periodicals, Inc.

Microdefects and self-interstitial diffusion in crystalline silicon

NASA Astrophysics Data System (ADS)

Knowlton, William Barthelemy

In this thesis, a study is presented of D-defects and self-interstitial diffusion in silicon using Li ion (Lisp+) drifting in an electric field and transmission electron microscopy (TEM). Obstruction of Lisp+ drifting has been found in wafers from certain but not all FZ p-type Si. Incomplete Lisp+ drifting always occurs in the central region of the wafers. This work established that interstitial oxygen is not responsible for hindering Lisp+ drifting. The Osb i concentration was measured ({˜}2× 10sp{15}\\ cmsp{-3}) by local vibrational mode Fourier transform infrared spectroscopy and did not vary radially across the wafer. TEM was performed on a samples from the partially Lisp+ drifted area and compared to regions without D-defects. Precipitates were found only in the region containing D-defects that had partially Lisp+ drifted. This result indicates D-defects are responsible for the precipitation that halts the Lisp+ drift process. The precipitates were characterized using selected area diffraction (SAD) and image contrast analysis. The results suggested that the precipitates may cause stacking faults and their identity may be lithium silicides such as Lisb{21}Sisb5\\ and\\ Lisb{13}Sisb4. TEM revealed a decreasing distribution of Li precipitates as a function of Lisp+ drift depth along the growth direction. A preliminary model is presented that simulates Lisp+ drifting. The objective of the model is to incorporate the Li precipitate density distribution and Lisp+ drift depth to extract the size and capture cross-section of the D-defects. Nitrogen (N) doping has been shown to eliminate D-defects as measured by conventional techniques. However, Lisp+ drifting has shown that D-defects are indeed still present. Lisp+ drifting is able to detect D-defects at concentrations lower than conventional techniques. Lisp+ drifting and D-defects provide a useful means to study Si self-interstitial diffusion. The process modeling program SUPREM-IV was used to simulate the results of Si self-interstitial diffusion obtained from Lisp+ drifting experiments. Anomalous results from the Si self-interstitial diffusion experiments forced a re-examination of the possibility of thermal dissociation of D-defects. Thermal annealing experiments that were performed support this possibility. A review of the current literature illustrates the need for more research on the effects of thermal processing on FZ Si to understand the dissolution kinetics of D-defects.

Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation.

PubMed

Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

2016-06-01

A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa.

Distributed fiber sparse-wideband vibration sensing by sub-Nyquist additive random sampling

NASA Astrophysics Data System (ADS)

Zhang, Jingdong; Zheng, Hua; Zhu, Tao; Yin, Guolu; Liu, Min; Bai, Yongzhong; Qu, Dingrong; Qiu, Feng; Huang, Xianbing

2018-05-01

The round trip time of the light pulse limits the maximum detectable vibration frequency response range of phase-sensitive optical time domain reflectometry ({\\phi}-OTDR). Unlike the uniform laser pulse interval in conventional {\\phi}-OTDR, we randomly modulate the pulse interval, so that an equivalent sub-Nyquist additive random sampling (sNARS) is realized for every sensing point of the long interrogation fiber. For an {\\phi}-OTDR system with 10 km sensing length, the sNARS method is optimized by theoretical analysis and Monte Carlo simulation, and the experimental results verify that a wide-band spars signal can be identified and reconstructed. Such a method can broaden the vibration frequency response range of {\\phi}-OTDR, which is of great significance in sparse-wideband-frequency vibration signal detection, such as rail track monitoring and metal defect detection.

Vibration and acoustic frequency spectra for industrial process modeling using selective fusion multi-condition samples and multi-source features

NASA Astrophysics Data System (ADS)

Tang, Jian; Qiao, Junfei; Wu, ZhiWei; Chai, Tianyou; Zhang, Jian; Yu, Wen

2018-01-01

Frequency spectral data of mechanical vibration and acoustic signals relate to difficult-to-measure production quality and quantity parameters of complex industrial processes. A selective ensemble (SEN) algorithm can be used to build a soft sensor model of these process parameters by fusing valued information selectively from different perspectives. However, a combination of several optimized ensemble sub-models with SEN cannot guarantee the best prediction model. In this study, we use several techniques to construct mechanical vibration and acoustic frequency spectra of a data-driven industrial process parameter model based on selective fusion multi-condition samples and multi-source features. Multi-layer SEN (MLSEN) strategy is used to simulate the domain expert cognitive process. Genetic algorithm and kernel partial least squares are used to construct the inside-layer SEN sub-model based on each mechanical vibration and acoustic frequency spectral feature subset. Branch-and-bound and adaptive weighted fusion algorithms are integrated to select and combine outputs of the inside-layer SEN sub-models. Then, the outside-layer SEN is constructed. Thus, "sub-sampling training examples"-based and "manipulating input features"-based ensemble construction methods are integrated, thereby realizing the selective information fusion process based on multi-condition history samples and multi-source input features. This novel approach is applied to a laboratory-scale ball mill grinding process. A comparison with other methods indicates that the proposed MLSEN approach effectively models mechanical vibration and acoustic signals.

Changes in the structure and wear resistance of the surface layer of copper under treatment by nitrogen ion beams

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

Sergeev, Victor P., E-mail: vserg@mail.tomsknet.ru, E-mail: kmp1980@mail.ru; Kalashnikov, Mark P., E-mail: vserg@mail.tomsknet.ru, E-mail: kmp1980@mail.ru; Rybalko, Evgeniya V., E-mail: evgeniaribka@yandex.com, E-mail: alfred-1972@mail.ru, E-mail: tehnovak@ispms.tsc.ru, E-mail: zhastas@mail.ru

2014-11-14

The structural-phase state of the treated sample surface was investigated by TEM. It was shown by the TEM and VIMS method that the improvement of tribological properties of the copper samples can be associated with an increase of relaxation ability due to a significant increase of the nitrogen concentration in it, which is accompanied by the refinement of fcc-Cu main phase grain structure and the formation of nanopores or gas bubbles in the ion-modified surface layer. A high-dose implantation of nitrogen ions and copper samples increases the wear resistance in 1.5-4.5 times together with a counterbody from the same materialmore » in the argon environment. The microhardness of the copper samples also increases.« less

An extension of command shaping methods for controlling residual vibration using frequency sampling

NASA Technical Reports Server (NTRS)

Singer, Neil C.; Seering, Warren P.

1992-01-01

The authors present an extension to the impulse shaping technique for commanding machines to move with reduced residual vibration. The extension, called frequency sampling, is a method for generating constraints that are used to obtain shaping sequences which minimize residual vibration in systems such as robots whose resonant frequencies change during motion. The authors present a review of impulse shaping methods, a development of the proposed extension, and a comparison of results of tests conducted on a simple model of the space shuttle robot arm. Frequency shaping provides a method for minimizing the impulse sequence duration required to give the desired insensitivity.

Generation of mechanical vibrations in metal samples by the use of the pinch effect

NASA Astrophysics Data System (ADS)

Troitskiy, O. A.; Skvortsov, O. B.; Stashenko, V. I.

2017-07-01

The article presents the recent research in electrodynamic processes for metal samples exposed to current pulses. The pinch effect and the skin effect cause the vibration of the metal rods. The results of these studies show how current and magnetic field interact with material samples of gold, silver and copper. The analysis allowed establishing the dependences of peak acceleration on current density and conductor diameter. The dependencies can be used in metal workings and for nondestructive testing.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Interparticle interaction effects on magnetic behaviors of hematite (α-Fe2O3) nanoparticles

NASA Astrophysics Data System (ADS)

Can, Musa Mutlu; Fırat, Tezer; Özcan, Şadan

2011-07-01

The interparticle magnetic interactions of hematite (α-Fe2O3) nanoparticles were investigated by temperature and magnetic field dependent magnetization curves. The synthesis were done in two steps; milling metallic iron (Fe) powders in pure water (H2O), known as mechanical milling technique, and annealing at 600 °C. The crystal and molecular structure of prepared samples were determined by X-ray powder diffraction (XRD) spectra and Fourier transform infrared (FTIR) spectra results. The average particle sizes and the size distributions were figured out using transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The magnetic behaviors of α-Fe2O3 nanoparticles were analyzed with a vibrating sample magnetometer (VSM). As a result of the analysis, it was observed that the prepared α-Fe2O3 nanoparticles did not perform a sharp Morin transition (the characteristic transition of α-Fe2O3) due to lack of unique particle size distribution. However, the transition can be observed in the wide temperature range as “a continuously transition”. Additionally, the effect of interparticle interaction on magnetic behavior was determined from the magnetization versus applied field (σ(M)) curves for 26±2 nm particles, dispersed in sodium oxalate matrix under ratios of 200:1, 300:1, 500:1 and 1000:1. The interparticle interaction fields, recorded at 5 K to avoid the thermal interactions, were found as ∼1082 Oe for 26±2 nm particles.

The dynamic magnetoviscoelastic properties of biomineralized (Fe3O4) PVP-CMC hydrogel

NASA Astrophysics Data System (ADS)

Ray, Ayan; Saha, Nabanita; Saha, Petr

2017-05-01

The Polyvinylpyrrolidone (PVP) and carboxymethylcellulose (CMC) based polymer matrix was used as a template for the preparation of magnetic hydrogel. This freshly prepared PVP-CMC hydrogel template was successfully mineralized by in situ synthesis of magnetic nanoparticles (Fe3O4) via chemical co-precipitation reaction using liquid diffusion method. The present study emphasizes on the rheological behavior of non-mineralized and mineralized PVP-CMC hydrogels. Scanning Electron Microscopy (SEM), transmission electron microscopy (TEM), X-ray Diffraction (XRD) pattern, Fourier transform infrared spectroscopy (FT-TR), Vibrating sample magnetometer (VSM) and dynamic magneto rheometer were used to study the morphological, physical, chemical and magnetic properties of nanoparticle (Fe3O4) filled PVP-CMC hydrogel respectively in order to monitor how Fe3O4 magnetic nanoparticles affects the mechanical properties of the hydrogel network. The storage (G') and loss (G") moduli with a complex viscosity of the system was measured using a parallel plate rheometer. Frequency and amplitude sweep with temperature variation was performed to determine the frequency and amplitude dependent magneto viscoelastic moduli for both hydrogel samples. A strong shear thinning effect was observed in both (non-mineralized and mineralized) PVP-CMC hydrogels, which confirm that Fe3O4 filled magnetic hydrogels, are pseudoplastic in nature. This Fe3O4 filled PVP-CMC hydrogel can be considered as stimuli-responsive soft matter that may be used as an actuator in medical devices.

Photocatalytic degradation of methylene blue dye and magneto-optical studies of magnetically recyclable spinel NixMn1-xFe2O4 (x = 0.0-1.0) nanoparticles

NASA Astrophysics Data System (ADS)

Mathubala, G.; Manikandan, A.; Arul Antony, S.; Ramar, P.

2016-06-01

Nickel doped spinel manganese ferrite (NixMn1-xFe2O4: x = 0.0-1.0) nanoparticles were prepared successfully by a superficial microwave irradiation technique using urea as the fuel. Powder X-ray diffraction (XRD) analysis was recognized the configuration of single phase spinel structure of NixMn1-xFe2O4. Debye Sherrer's formula was used to calculate the average crystallite size of the samples, which were found in the range of 15-20 nm. High resolution scanning electron microscopy (HR-SEM) was used to analyze the surface morphology of the samples, which showed the particle like-morphology with smaller agglomeration, and it was also confirmed by high resolution transmission electron microscopy (HR-TEM). Energy dispersive X-ray (EDX) analysis confirmed the elemental composition, which also evidence for the formation of single pure phase. Microwave heating method produced well crystalline nature of the products, which was confirmed by selected area electron diffraction (SAED) analysis. UV-Visible diffuse reflectance spectra (DRS) were used to calculate the energy band gap and the observed values are increased slightly from 2.05 eV to 2.44 eV with increasing the Ni-dapant. Magnetic characterization of the samples were analyzed by room temperature vibrating sample magnetometer (VSM) technique and the observed magnetization (Ms) values are decreased with increasing Ni content, due to the different magnetic moments of Mn2+ and Ni2+ cations. Photocatalytic degradation (PCD) of methylene blue dye was carried out by self designed photo-catalytic reactor. It was observed that PCD efficiency is increased with increase in concentration of Ni and the sample Ni0.6Mn0.4Fe2O4 shows better photocatalytic activity (96.73%) than other samples.

Study on the application of Raman spectroscopy on detecting water hardness.

PubMed

Yang, Chang-Hu; Shi, Xiang-Hua; Yuan, Jian-Hui

2014-05-01

Laser Raman spectrum method was used to study the hardness index of four water samples. The ratio of bending vibration peak intensity to stretching vibration peak intensity of these water samples was measured. The results showed that as the total hardness of water decreases, so does the ratio. This offers a possible new approach to water quality analysis that is both simple and effective.

Investigation of C3 S hydration mechanism by transmission electron microscope (TEM) with integrated Super-XTM EDS system.

PubMed

Sakalli, Y; Trettin, R

2017-07-01

Tricalciumsilicate (C 3 S, Alite) is the major component of the Portland cement clinker. Hydration of Alite is decisive in influencing the properties of the resulting material. This is due to its high content in cement. The mechanism of the hydration of C 3 S is very complicated and not yet fully understood. There are different models describing the hydration of C 3 S in various ways. In this work for a better understanding of hydration mechanism, the hydrated C 3 S was investigated by using the transmission electron microscope (TEM) and for the first time, the samples for the investigations were prepared by using of focused ion beam from sintered pellets of C 3 S. Also, an FEI Talos F200x with an integrated Super-X EDS system was used for the investigations. FEI Talos F200X combines outstanding high-resolution S/TEM and TEM imaging with energy dispersive X-ray spectroscopy signal detection, and 3D chemical characterization with compositional mapping. TEM is a very powerful tool for material science. A high energy beam of electrons passes through a very thin sample, and the interactions between the electrons and the atoms can be used to observe the structure of the material and other features in the structure. TEM can be used to study the growth of layers and their composition. TEM produces high-resolution, two-dimensional images and will be used for a wide range of educational, science and industry applications. Chemical analysis can also be performed. The purpose of these investigations was to get the information about the composition of the C-S-H phases and some details of the nanostructure of the C-S-H phases. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Complete Tem-Tomography: 3D Structure of Gems Cluster

NASA Technical Reports Server (NTRS)

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

2015-01-01

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

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.

Analysis of structural transformation in wool fiber resulting from oxygen plasma treatment using vibrational spectroscopy

NASA Astrophysics Data System (ADS)

Barani, Hossein; Haji, Aminoddin

2015-01-01

The aim of this study was to investigate the influence of oxygen plasma procedure at different time treatments on wool fiber using the micro-Raman spectroscopy as a non-destructive vibrational spectroscopic technique and Fourier transform infrared spectroscopy. The amide I and III regions, Csbnd C skeletal vibration region, and Ssbnd S and Csbnd S bonds vibration regions were analyzed with the Raman microscope. The Fourier transform infrared spectroscope analysis was employed to find out the effect of oxygen plasma treatment on the cysteic acid residues content of the wool fiber sample. The results indicated that the α-helix structure was the highest component content of wool fiber. Moreover, the protein secondary structure of wool fibers was transformed from α-helical arrangement to the β-pleated sheet configuration during the oxygen plasma treatment. Also, the disulphide bonds content in the treated wool fiber reduced because they were fractured and oxidized during oxygen plasma treatment. The oxygen plasma treated samples presented higher cysteic acid compared to the untreated wool samples due to produce more cleavage of disulfide linkages.

The Eating Motivation Survey: results from the USA, India and Germany.

PubMed

Sproesser, Gudrun; Ruby, Matthew B; Arbit, Naomi; Rozin, Paul; Schupp, Harald T; Renner, Britta

2018-02-01

Research has shown that there is a large variety of different motives underlying why people eat what they eat, which can be assessed with The Eating Motivation Survey (TEMS). The present study investigates the consistency and measurement invariance of the fifteen basic motives included in TEMS in countries with greatly differing eating environments. The fifteen-factor structure of TEMS (brief version: forty-six items) was tested in confirmatory factor analyses. An online survey was conducted. US-American, Indian and German adults (total N 749) took part. Despite the complexity of the model, fit indices indicated a reasonable model fit (for the total sample: χ 2/df=4·03; standardized root-mean-squared residual (SRMR)=0·063; root-mean-square error of approximation (RMSEA)=0·064 (95 % CI 0·062, 0·066)). Only the comparative fit index (CFI) was below the recommended threshold (for the total sample: CFI=0·84). Altogether, 181 out of 184 item loadings were above the recommended threshold of 0·30. Furthermore, the factorial structure of TEMS was invariant across countries with respect to factor configuration and factor loadings (configural v. metric invariance model: ΔCFI=0·009; ΔRMSEA=0·001; ΔSRMR=0·001). Moreover, forty-three out of forty-six items showed invariant intercepts across countries. The fifteen-factor structure of TEMS was, in general, confirmed across countries despite marked differences in eating environments. Moreover, latent means of fourteen out of fifteen motive factors can be compared across countries in future studies. This is a first step towards determining generalizability of the fifteen basic eating motives of TEMS across eating environments.

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

Cantilever Beam Static and Dynamic Response Comparison with Mid-Point Bending for Thin MDF composite Panels

Treesearch

John F. Hunt; Houjiang Zhang; Zhiren Guo; Feng Fu

2013-01-01

A new cantilever beam apparatus has been developed to measure static and vibrational properties of small and thin samples of wood or composite panels. The apparatus applies a known displacement to a cantilever beam, measures its static load, then releases it into its natural first mode of transverse vibration. Free vibrational tip displacements as a function of time...

Vibrational force alters mRNA expression in osteoblasts

NASA Technical Reports Server (NTRS)

Tjandrawinata, R. R.; Vincent, V. L.; Hughes-Fulford, M.

1997-01-01

Serum-deprived mouse osteoblastic (MC3T3E1) cells were subjected to a vibrational force modeled by NASA to simulate a space shuttle launch (7.83 G rms). The mRNA levels for eight genes were investigated to determine the effect of vibrational force on mRNA expression. The mRNA levels of two growth-related protooncogenes, c-fos and c-myc, were up-regulated significantly within 30 min after vibration, whereas those of osteocalcin as well as transforming growth factor-beta1 were decreased significantly within 3 h after vibration. No changes were detected in the levels of beta-actin, histone H4, or cytoplasmic phospholipase A2 after vibration. No basal levels of cyclooxygenase-2 expression were detected. In addition, the extracellular concentrations of prostaglandin E2 (PGE2), a potent autocrine/paracrine growth factor in bone, were not significantly altered after vibration most likely due to the serum deprivation state of the osteoblasts. In comparison with the gravitational launch profile, vibrational-induced changes in gene expression were greater both in magnitude and number of genes activated. Taken together, these data suggest that the changes in mRNA expression are due to a direct mechanical effect of the vibrational force on the osteoblast cells and not to changes in the local PGE2 concentrations. The finding that launch forces induce gene expression is of utmost importance since many of the biological experiments do not dampen vibrational loads on experimental samples. This lack of dampening of vibrational forces may partially explain why 1-G onboard controls sometimes do not reflect 1-G ground controls. These data may also suggest that scientists use extra ground controls that are exposed to launch forces, have these forces dampened on launched samples, or use facilities such as Biorack that provide an onboard 1-G centrufuge in order to control for space shuttle launch forces.

Transmission of vibration through gloves: effects of material thickness.

PubMed

Md Rezali, Khairil Anas; Griffin, Michael J

2016-08-01

It might be assumed that increasing the thickness of a glove would reduce the vibration transmitted to the hand. Three material samples from an anti-vibration glove were stacked to produce three thicknesses: 6.4, 12.8 and 19.2 mm. The dynamic stiffnesses of all three thicknesses, the apparent mass at the palm and the finger and the transmission of vibration to the palm and finger were measured. At frequencies from 20 to 350 Hz, the material reduced vibration at the palm but increased vibration at the finger. Increased thickness reduced vibration at the palm but increased vibration at the finger. The measured transmissibilities could be predicted from the material dynamic stiffness and the apparent mass of the palm and finger. Reducing the dynamic stiffness of glove material may increase or decrease the transmission of vibration, depending on the material, the frequency of vibration and the location of measurement (palm or finger). Practitioner Summary: Transmission of vibration through gloves depends on the dynamic response of the hand and the dynamic stiffness of glove material, which depends on material thickness. Measuring the transmission of vibration through gloves to the palm of the hand gives a misleading indication of the transmission of vibration to the fingers.

Detecting the magnetic response of iron oxide capped organosilane nanostructures using magnetic sample modulation and atomic force microscopy.

PubMed

Li, Jie-Ren; Lewandowski, Brian R; Xu, Song; Garno, Jayne C

2009-06-15

A new imaging strategy using atomic force microscopy (AFM) is demonstrated for mapping magnetic domains at size regimes below 100 nm. The AFM-based imaging mode is referred to as magnetic sample modulation (MSM), since the flux of an AC-generated electromagnetic field is used to induce physical movement of magnetic nanomaterials on surfaces during imaging. The AFM is operated in contact mode using a soft, nonmagnetic tip to detect the physical motion of the sample. By slowly scanning an AFM probe across a vibrating area of the sample, the frequency and amplitude of vibration induced by the magnetic field is tracked by changes in tip deflection. Thus, the AFM tip serves as a force and motion sensor for mapping the vibrational response of magnetic nanomaterials. Essentially, MSM is a hybrid of contact mode AFM combined with selective modulation of magnetic domains. The positional feedback loop for MSM imaging is the same as that used for force modulation and contact mode AFM; however, the vibration of the sample is analyzed using channels of a lock-in amplifier. The investigations are facilitated by nanofabrication methods combining particle lithography with organic vapor deposition and electroless deposition of iron oxide, to prepare designed test platforms of magnetic materials at nanometer length scales. Custom test platforms furnished suitable surfaces for MSM characterizations at the level of individual metal nanostructures.

Crack identification and evolution law in the vibration failure process of loaded coal

NASA Astrophysics Data System (ADS)

Li, Chengwu; Ai, Dihao; Sun, Xiaoyuan; Xie, Beijing

2017-08-01

To study the characteristics of coal cracks produced in the vibration failure process, we set up a static load and static and dynamic combination load failure test simulation system, prepared with different particle size, formation pressure, and firmness coefficient coal samples. Through static load damage testing of coal samples and then dynamic load (vibration exciter) and static (jack) combination destructive testing, the crack images of coal samples under the load condition were obtained. Combined with digital image processing technology, an algorithm of crack identification with high precision and in real-time is proposed. With the crack features of the coal samples under different load conditions as the research object, we analyzed the distribution of cracks on the surface of the coal samples and the factors influencing crack evolution using the proposed algorithm and a high-resolution industrial camera. Experimental results showed that the major portion of the crack after excitation is located in the rear of the coal sample where the vibration exciter cannot act. Under the same disturbance conditions, crack size and particle size exhibit a positive correlation, while crack size and formation pressure exhibit a negative correlation. Soft coal is more likely to lead to crack evolution than hard coal, and more easily causes instability failure. The experimental results and crack identification algorithm provide a solid basis for the prevention and control of instability and failure of coal and rock mass, and they are helpful in improving the monitoring method of coal and rock dynamic disasters.

Spectroscopic investigation of the spectroscopic signatures of 2,4-DNT and 2,6-DNT: their interactions with sand particles

NASA Astrophysics Data System (ADS)

Blanco, Alejandro; Mina, Nairmen; Castro, Miguel E.; Castillo-Chara, Jairo; Hernandez-Rivera, Samuel P.

2004-09-01

Raman Spectroscopy is a well established tool for vibrational spectroscopy analysis. Interactions of explosives with different substrates can be measured by using quantitative vibrational signal shift information of scattered Raman light associated with these interactions. A vibrational spectroscopic study has been carried out on 2,4-DNT and 2,6-DNT crystals. Raman Microscopy spectrometers equipped with 514 nm and 785 nm laser excitation lines were used. The samples were recrystallized on different solvents (water, methanol and acetonitrile) and allowed to interact with soil samples. The interaction with sand and soil samples doped with the nitroaromatic compounds showed significant shifts in its peaks. The above information was used to detect DNT in soil using Raman Microscopy. These results will make possible the development of highly sensitive sensors for detection of explosives materials.

Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

NASA Astrophysics Data System (ADS)

Lari, L.; Dudkiewicz, A.

2014-06-01

Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility.

Microchemical and Structural Evidence for Space Weathering in Soils from Asteroid Itokawa

NASA Technical Reports Server (NTRS)

Thompson, M. S.; Christoffersen, R.; Zega, T. J.

2013-01-01

The chemistry, microstructure and optical properties of grains on the surfaces of airless bodies are continu-ously modified due to their interactions predominantly with solar energetic ions and micrometeorite impacts. Collectively known as space weathering, this phenomenon results in a discrepancy between remotely sensed spectra from asteroids and those ac-quired directly from meteorites. The return of pristine samples from the asteroid Itokawa provides insight into surface processes on airless bodies and will help in correlating remote sensing data with laboratory analysis of meteorites. Samples and Methods: We examined Itokawa samples RA-QD02-0042-01 and RA-QD-02-0042-02, ultramicrotomed sec-tions of a singular grain prepared by the Hayabusa sample cura-tion team. We analyzed these slices using a 200 keV JEOL 2010F transmission electron microscope (TEM) at Arizona State Uni-versity and a 200 keV JEOL 2500SE TEM at NASA JSC. Both field emission TEMs are equipped with energy-dispersive X-ray spectrometers (EDS) and scanning TEM (STEM) detectors. Results and Discussion: TEM observations reveal that the sectioned grain predominantly consists of a single crystal of low-Ca orthopyroxene, with subsidiary smaller regions of olivine, Fe-Ni sulfide, and Fe-Ni metal. EDS-spectrum imaging and high-resolution TEM (HRTEM) show local, nanocrystalline regions of the outermost 2 to 5 nm of the pyroxene are composed of an Fe-Mg-S-rich and Si- and O-depleted layer that is underlain by a 2- to 5-nm thick amorphous zone enriched in Si. These layers occur in multiple microtome slices and have uniform thicknesses. We also observe localized 'islands' of material on the surface of the pyroxene which HRTEM imaging indicates are amorphous and EDS measurements show are compositionally heterogeneous. A 10- to 60-nm thick partially amorphous zone occurs below the compositionally distinct rim. While this this zone is associated with the compositionally heterogeneous outer layer, it also occurs as a local stand-alone feature on the exterior rim of the grain. Ar-eas of the pyroxene grain rim also exhibit a vesicular texture. The TEM data indicate a complex history of space weather-ing for samples RA-QD02-0042-01 and -02. The outermost layer of nanocrystalline material with varied composition is consistent with previously suggested [3-4] chemical and structural pro-cessing by solar wind ions, with a possible additional role for im-pact vapor deposition [3-4]. The amorphous and compositionally distinct islands on the surface of this grain, similar to lunar glasses, suggest formation through vapor deposition via micrometeor-ite impact events. In comparison, the amorphization and vesicula-tion textures are likely a product of radiation damage from the solar wind. The depth and degree of amorphization, in conjunction with model calculations, will help provide an upper limit on exposure time for these particles.

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.

Atomic-Resolution Transmission Electron Microscopic Movies for Study of Organic Molecules, Assemblies, and Reactions: The First 10 Years of Development.

PubMed

Nakamura, Eiichi

2017-06-20

A molecule is a quantum mechanical entity. "Watching motions and reactions of a molecule with our eyes" has therefore been a dream of chemists for a century. This dream has come true with the aid of the movies of atomic-resolution transmission electron microscopic (AR-TEM) molecular images through real-time observation of dynamic motions of single organic molecules (denoted hereafter as single-molecule atomic-resolution real-time (SMART) TEM imaging). Since 2007, we have reported movies of a variety of single organic molecules, organometallic molecules, and their assemblies, which are rotating, stretching, and reacting. Like movies in the theater, the atomic-resolution molecular movies provide us information on the 3-D structures of the molecules and also their time evolution. The success of the SMART-TEM imaging crucially depends on the development of "chemical fishhooks" with which fish (organic molecules) in solution can be captured on a single-walled carbon nanotube (CNT, serving as a "fishing rod"). The captured molecules are connected to a slowly vibrating CNT, and their motions are displayed on a monitor in real time. A "fishing line" connecting the fish and the rod may be a σ-bond, a van der Waals force, or other weak connections. Here, the molecule/CNT system behaves as a coupled oscillator, where the low-frequency anisotropic vibration of the CNT is transmitted to the molecules via the weak chemical connections that act as an energy filter. Interpretation of the observed motions of the molecules at atomic resolution needs us to consider the quantum mechanical nature of electrons as well as bond rotation, letting us deviate from the conventional statistical world of chemistry. What new horizons can we explore? We have so far carried out conformational studies of individual molecules, assigning anti or gauche conformations to each C-C bond in conformers that we saw. We can also determine the structures of van der Waals assemblies of organic molecules, thereby providing mechanistic insights into crystal formation-phenomena of general significance in science, engineering, and our daily life. Whereas many of the single organic molecules in a vacuum seen by SMART-TEM are sufficiently long-lived for detailed studies, molecules with low ionization potentials (<6 eV) were found to undergo chemical reactions, for example, [60]fullerene and organometallic compounds possibly via a hole catalysis mechanism, where a radical cation of CNT generated under electron irradiation catalyzes the transformation via an electron transfer mechanism. Common organic molecules whose ionization potentials are much higher (>8 eV) than that of CNT (5 eV) remain stable for a time long enough for observation at 60-120 kV acceleration voltage, as they are not oxidized by the CNT radical cation. Alternatively, the reaction may have taken place via an excited state of a molecule produced by energy transfer from CNT possessing excess energy provided by the electron beam. SMART-TEM imaging is a simple approach to the study of the structures and reactions of molecules and their assemblies and will serve as a gateway to the research and education of the science connecting the quantum mechanical world and the real world.

Structural and morphological study of Zn0.9Mn0.05Fe0.05O synthesized by sol-gel wet chemical precipitation route

NASA Astrophysics Data System (ADS)

Jain, S. K.; Dolia, S. N.; Choudhary, B. L.; Prashant, B. L.

2018-04-01

Transition metal substituted Zinc oxide (ZnO) has drawn a great deal of attention due to its excellent properties. Zn0.9Mn0.05Fe0.05O sample synthesized was by Sol-gel wet chemical precipitation route at temperature 350°C. The crystallinity and the structure of Zn0.9Mn0.05Fe0.05O was determined by X-ray diffraction by Cu-Kα radiations operated at 40kV and 35mA in the range of 20° to 80°. The pattern gets indexed in wurtzite (hexagonal) structure with lattice constants a=b=3.2525Å and c=5.2071Å and approves the single phase material with no impurity. The values of particle size assessed by Debye Scherer’s (DS) formula lie in the range of 13nm to 33nm indicating the nano-crystalline nature of the sample. The morphological analysis of the sample was performed by Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM) measurements. The observed size of Zn0.9Mn0.05Fe0.05O nanoparticles by TEM micrograph exhibits the similar trend with the size calculated by Debye-Scherer formula. TEM image show the irregular shape of the nanoparticles and particle size lies in the range of 10-35nm. Similar to SEM image, the slight agglomeration of the nanoparticles have been observed from TEM.

The Morphology of Silver Layers on SU8 polymers prepared by Electroless Deposition

NASA Astrophysics Data System (ADS)

Dutta, Aniruddha; Yuan, Biao; Heinrich, Helge; Grabill, Chris; Williams, Henry; Kuebler, Stephen; Bhattacharya, Aniket

2010-03-01

Silver was deposited onto the functionalized surface of polymeric SU-8 where gold nanoparticles (Au-NPs) act as nucleation sites using electroless metallization chemistry. Here we report on the evolution of the nanoscale morphology of deposited Ag studied by Transmission Electron Microscopy (TEM). In TEM of sample cross sections correlations between the original gold and the silver nanoparticles were obtained while plan-view TEM results showed the distribution of nanoparticles on the surface. Scanning TEM with a high-angle annular dark field detector was used to obtain atomic number contrast. The morphology of the deposited Ag was controlled through the presence and absence of gum Arabic. The thickness and height fluctuations of the Ag layer were determined as a function of time and a statistical analysis of the growth process was conducted for the initial deposition periods.

Iron oxides in human spleen.

PubMed

Kopáni, Martin; Miglierini, Marcel; Lančok, Adriana; Dekan, Július; Čaplovicová, Mária; Jakubovský, Ján; Boča, Roman; Mrazova, Hedviga

2015-10-01

Iron is an essential element for fundamental cell functions and a catalyst for chemical reactions. Three samples extracted from the human spleen were investigated by scanning (SEM) and transmission electron microscopy (TEM), Mössbauer spectrometry (MS), and SQUID magnetometry. The sample with diagnosis of hemosiderosis (H) differs from that referring to hereditary spherocytosis and the reference sample. SEM reveals iron-rich micrometer-sized aggregate of various structures-tiny fibrils in hereditary spherocytosis sample and no fibrils in hemochromatosis. Hematite and magnetite particles from 2 to 6 μm in TEM with diffraction in all samples were shown. The SQUID magnetometry shows different amount of diamagnetic, paramagnetic and ferrimagnetic structures in the tissues. The MS results indicate contribution of ferromagnetically split sextets for all investigated samples. Their occurrence indicates that at least part of the sample is magnetically ordered below the critical temperature. The iron accumulation process is different in hereditary spherocytosis and hemosiderosis. This fact may be the reason of different iron crystallization.

Preparation of Superparamagnetic Zn0.5Mn0.5Fe2O4 Particle by Coprecipitation-Sonochemical Method for Radar Absorbing Material

NASA Astrophysics Data System (ADS)

Taufiq, A.; Bahtiar, S.; Sunaryono; Hidayat, N.; Hidayat, A.; Mufti, N.; Diantoro, M.; Fuad, A.; Munasir; Rahmawati, R.; Adi, W. A.; Pratapa, S.; Darminto

2017-05-01

One of many applications of spinel ferrite nanoparticles is related to their performance as radar absorbing materials. In this work, we report developing synthesis method through combined coprecipitation-sonochemical routes in preparing Zn0.5Mn0.5Fe2O4 nanoparticle from iron sand in Indonesia as a vital raw material. The structure, size, morphology, and elements of the Zn0.5Mn0.5Fe2O4 nanoparticle were investigated via X-Ray diffractometry and Transmission/Scanning Electron Microscopy (TEM/SEM) combining Energy Dispersive Spectroscopy (EDS). The magnetic properties of the Zn0.5Mn0.5Fe2O4 nanoparticle were characterized by using Vibrating Sample Magnetometer (VSM). Furthermore, the reflection loss character of the Zn0.5Mn0.5Fe2O4 nanoparticle was determined via Vector Network Analyzer (VNA). From the qualitative and quantitative analysis of the XRD data, it can be identified that the Zn0.5Mn0.5Fe2O4 particle formed a spinel cubic structure in a single phase with the lattice parameter of approximately 8.401 Å. It is known from the TEM image that the Zn0.5Mn0.5Fe2O4 particle had a size of about 9.7 nm and tended to agglomerate. Furthermore, the data analysis of the M(H) curve presented that the Zn0.5Mn0.5Fe2O4 nanoparticle has a superparamagnetic behavior with the saturation magnetization of approximately 43 emu/g. Finally, the data analysis of the reflection loss as a function of frequency showed that the Zn0.5Mn0.5Fe2O4 nanoparticle performs as a radar absorbing material with the absorption performance of approximately -11.0 dB at the frequency of 10.8 GHz

Chemical synthesis and characterization of hollow dopamine coated, pentagonal and flower shaped magnetic iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Riasat, Rabia; Kaynat, Sumbal

2018-04-01

Iron oxide nanoparticles have gained attention recently in the field of nanoscience and technology due to their unique physicochemical properties. We hereby chemically synthesized novel pentagonal flower shaped iron oxide nanoparticles by thermal decomposition of iron penta-carbonyl in a two way annealing process. Controlled oxidation by acid etching was performed for these nanoparticles. At first 13 nm core shell nanoparticles of iron oxide (Fe/Fe3O4) were synthesized at 120°C annealing temperature that act as template material. The core shell nanoparticles then converted into porous hollow core shell nanoparticles (PH Fe/ Fe3O4) in a two way annealing process of heating, first at 100°C then at 250°C and heating rate of 5°C was kept constant throughout the reaction time. X-Ray diffraction (XRD) was done for the phase confirmation of as synthesized nanoparticles. Transmission electron microscopy (TEM) and higher resolution transmission electron microscopy (HRTEM) clearly shows the flower like nanoparticles that are approx. 16 nm-18 nm in size having the 4-5 nm core of Fe and 1-2 nm of the pores in the shell while the cavity between the shell and core is about 2 nm and the shell is 4-5 nm in diameter according to the TEM micrographs. The as prepared nanoparticles were then surface functionalized by dopamine polymer to make them water dispersible. Fourier transform Infrared spectroscopy confirmed the dopamine coating on the nanoparticles and the magnetic saturation of 38 emu/g of nanoparticles was analyzed by vibrating sample magnetometer (VSM). Magnetic saturation persists in the dopamine coated nanoparticles. These nanoparticles were surface functionalized with dopamine and show dispersity in the aqueous media and can further be exploited in many nano-biotechnological applications including target specific therapeutic applications for several diseases.

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

PubMed

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

2016-08-15

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

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

NASA Astrophysics Data System (ADS)

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

2012-12-01

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

[The combined use of capillaroscopy and skin thermometry in health surveillance of workers exposed to hand-arm vibration].

PubMed

Riolfi, A; Perbellini, L

2010-01-01

The use of nailfold capillaroscopy combined with skin thermometry in the study of microcirculation of the hands in workers exposed to hand-arm vibration is assessed. Fifty-eight subjects were studied; 40 asymptomatic forestry workers exposed to hand-arm vibration, 13 forestry workers exposed to hand-arm vibration with Raynaud-like symptoms confirmed by skin thermometry; 5 controls. Reduction of capillary density was observed in workers exposed to vibrating tools with respect to controls. Tortuosity of capillary loops was significantly more frequent in subjects exposed to vibrating tools than in controls. No statistically significant difference in capillary vessels of the hands was found between asymptomatic exposed subjects and workers affected by Raynaud-like symptoms. In our sample nailfold capillaroscopy shows good sensibilty and specificity in detecting capillary modifications secondary to exposure to hand-vibration. Weaker evidence is instead given in order to actual disturbances of hands circulation in chronic exposure to vibrating tools.

Enhanced antibacterial activity of zinc oxide nanoparticles synthesized using Petroselinum crispum extracts

NASA Astrophysics Data System (ADS)

Stan, Manuela; Popa, Adriana; Toloman, Dana; Silipas, Teofil-Danut; Vodnar, Dan Cristian; Katona, Gabriel

2015-12-01

The present contribution reports the synthesis of zinc oxide nanoparticles (ZnO NPs) using aqueous leaf and root extracts of Petroselinum crispum (parsley) and characterization of as-prepared samples. ZnO NPs are subjected to X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron paramagnetic resonance (EPR) studies. The XRD studies reveal a hexagonal wurtzite structure without supplementary diffraction lines for all ZnO samples. TEM analysis shows that the particle size is influenced by the type of plant extract. The EPR spectra indicate the presence of Mn2+ ions in ZnO sample synthesized using P. crispum leaf extract, while zinc vacancy complexes and oxygen vacancies are evidenced in all analyzed samples. ZnO NPs synthesized using P. crispum extracts exhibit increased (2-16 times) antibacterial activity as compared to chemically synthesized ZnO NPs.

Effects of Vibration Therapy in Pediatric Immunizations.

PubMed

Benjamin, Arika L; Hendrix, Thomas J; Woody, Jacque L

2016-01-01

A randomized clinical trial of 100 children (52 boys, 48 girls) ages 2 months to 7 years was conducted to evaluate the effect of vibration therapy without cold analgesia on pain. A convenience sample was recruited at two sites: a publicly funded, free immunization clinic and a private group pediatric practice. Participants were randomly assigned to receive vibration therapy via a specialized vibrating device or standard care. All children regardless of intervention group were allowed to be distracted and soothed by the parent. Pain was evaluated using the FLACC score, which two nurses assessed at three points in time: prior to, during, and after the injection(s). Data were analyzed using a two-independent samples-paired t-test. Results show that vibration therapy had no effect on pain scores in the younger age groups studied (2 months ≤ 1 year, > 1 year ≤ 4 years). In the oldest age group (> 4 to 7 years of age), a heightened pain reading was found in the period from preinjection to post-injection periods (p = 0.045). These results indicate that the addition of vibration therapy (without cold analgesia) to standard soothing techniques is no more effective in reducing immunization pain than standard soothing techniques alone, and thus, is not indicated for use with immunization pain. Recommendations include further evaluation of interventions.

Infrared extinction and microwave absorption properties of hybrid Fe3O4@SiO2@Ag nanospheres synthesized via a facile seed-mediated growth route.

PubMed

Chen, Yongpeng; Li, Shichuan; Wei, Xuebin; Tang, Runze; Zhou, Zunning

2018-06-21

Fe3O4@SiO2@Ag ternary hybrid nanoparticles were synthesized via a facile seed-mediated growth route. X-ray diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM) measurements were used to characterize the as-prepared product. The results indicated that the nanoparticles exhibited excellent magnetic properties and an extremely dense structure with Ag layer thicknesses of 30 nm, 40 nm, and 50 nm. Furthermore, the microwave shielding effectiveness exceeded 20 dB over almost the entire frequency range (2-18 GHz), and the effectiveness obviously improved as the thickness of the Ag layer increased. In addition, the IR extinction coefficient of the nanoparticles was calculated by a finite-difference time-domain (FDTD) method, which showed that the nanoparticles can inherit the extinction performance of pure silver when the Ag shell thickness was 30 nm. Specifically, after assembling into chains, the peak position of the IR extinction curves displayed a significant redshift and an intensity increase as the number of nanoparticles increased in the chain, which dramatically promoted the IR extinction capability. As a result, the Fe3O4@SiO2@Ag nanoparticles are expected to be used as a new multispectral interference material. © 2018 IOP Publishing Ltd.

Preparation and properties of hybrid monodispersed magnetic α-Fe2O3 based chitosan nanocomposite film for industrial and biomedical applications.

PubMed

Singh, Jay; Srivastava, M; Dutta, Joydeep; Dutta, P K

2011-01-01

In this study, hydrothermally prepared magnetic α-Fe2O3 nanoparticles were dispersed in chitosan (CH) solution to fabricate nanocomposite film. X-ray diffraction (XRD) patterns indicated that the α-Fe2O3 nanoparticles were pure α-Fe2O3 with rhombohedral structures, and the fabrication of CH did not result in a phase change. The scanning electron microscopy (SEM) and transmission electron microscope (TEM) results showed that the hexagonal and spherical monodispersed α-Fe2O3 nanoparticles were encapsulated into the spherical dumb shaped CH-α-Fe2O3 nanocomposite film with a mean diameter of ∼87 and ∼110 nm respectively. The α-Fe2O3 nanoparticles and CH-α-Fe2O3 nanocomposite film were also characterized by Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and vibrating sample magnetometer (VSM). Magnetic measurements revealed that the saturated magnetization (Ms) and remanent magnetization (Mr) of the pure α-Fe2O3 nanoparticles reached 0.573 emu/g and 0.100 emu/g respectively and the nanoparticles showed the characteristics of weak ferromagnetic before and after coating with CH. Copyright © 2010 Elsevier B.V. All rights reserved.

Synthesis and cytotoxicity assessment of superparamagnetic iron-gold core-shell nanoparticles coated with polyglycerol.

PubMed

Jafari, T; Simchi, A; Khakpash, N

2010-05-01

Core-shell iron-gold (Fe@Au) nanoparticles were synthesized by a facile reverse micelle procedure and the effect of water to surfactant molar ratio (w) on the size, size distribution and magnetic properties of the nanoparticles was studied. MTT assay was utilized to evaluate the cell toxicity of the nanoparticles. To functionalize the particles for MRI imaging and targeted drug delivery, the particles were coated by polyglycerol through capping with thiol followed by polymerization of glycidol. The characteristics of the particles were examined by X-ray diffraction (XRD), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), UV-visible spectroscopy, and Fourier transform infrared spectroscopy (FT-IR). It was found that the size and size distribution of the nanoparticles increase by increasing the water to surfactant molar ratio (w). The particles were spherical in shape with a thin layer of gold. Complementary growth of the gold shell on the iron core was noticed. Meanwhile, two types of agglomeration including magnetic beads and magnetic colloidal nanocrystals clusters were observed dependent on the w-value. The magnetic measurement studies revealed the superparamagnetic behavior of the nanoparticles. MTT assay result indicated the synthesized nanoparticles are nontoxic that will be useful for biomedical applications. Copyright 2010 Elsevier Inc. All rights reserved.

Functionalized graphene oxide/Fe3O4 hybrids for cellular magnetic resonance imaging and fluorescence labeling.

PubMed

Zhou, Chaohui; Wu, Hui; Wang, Mingliang; Huang, Chusen; Yang, Dapeng; Jia, Nengqin

2017-09-01

In this work, we developed a T 2 -weighted contrast agent based on graphene oxide (GO)/Fe 3 O 4 hybrids for efficient cellular magnetic resonance imaging (MRI). The GO/Fe 3 O 4 hybrids were obtained by combining with co-precipitation method and pyrolysis method. The structural, surface and magnetic characteristics of the hybrids were systematically characterized by transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), AFM, Raman, FT-IR and XRD. The GO/Fe 3 O 4 hybrids were functionalized by modifying with anionic and cationic polyelectrolyte through layer-by-layer assembling. The fluorescence probe fluorescein isothiocyanate (FITC) was further loaded on the surface of functionalized GO/Fe 3 O 4 hybrids to trace the location of GO/Fe 3 O 4 hybrids in cells. Functionalized GO/Fe 3 O 4 hybrids possess good hydrophilicity, less cytotoxicity, high MRI enhancement with the relaxivity (r 2 ) of 493mM -1 s -1 as well as cellular MRI contrast effect. These obtained results indicated that the functionalized GO/Fe 3 O 4 hybrids could have great potential to be utilized as cellular MRI contrast agents for tumor early diagnosis and monitoring. Copyright © 2017 Elsevier B.V. All rights reserved.

Chondroitin sulfate-capped super-paramagnetic iron oxide nanoparticles as potential carriers of doxorubicin hydrochloride.

PubMed

Mallick, Neha; Anwar, Mohammed; Asfer, Mohammed; Mehdi, Syed Hassan; Rizvi, Mohammed Moshahid Alam; Panda, Amulya Kumar; Talegaonkar, Sushama; Ahmad, Farhan Jalees

2016-10-20

Chondroitin-4-sulfate (CS), a glycosaminoglycan, was used to prepare CS-capped super-paramagnetic iron oxide nanoparticles, which were further employed for loading a water-soluble chemotherapeutic agent (doxorubicin hydrochloride, DOX). CS-capped SPIONs have potential biomedical application in cancer targeting. The optimized formulation had a hydrodynamic size of 91.2±0.8nm (PDI; 0.228±0.004) and zeta potential of -49.1±1.66mV. DOX was loaded onto the formulation up to 2% (w/w) by physical interaction with CS. TEM showed nano-sized particles having a core-shell structure. XRD confirmed crystal phase of iron oxide. FT-IR conceived the interaction of iron oxide with CS as bidentate chelation and also confirmed DOX loading. Vibration sample magnetometry confirmed super-paramagnetic nature of nanoparticles, with saturation magnetization of 0.238emug(-1). In vitro release profile at pH 7.4 showed that 96.67% of DOX was released within 24h (first order kinetics). MTT assay in MCF7 cells showed significantly higher (p<0.0001) cytotoxicity for DOX in SPIONs than DOX solution (IC50 values 6.294±0.4169 and 11.316±0.1102μgmL(-1), respectively). Copyright © 2016 Elsevier Ltd. All rights reserved.

Structural, optical and magnetic properties of gadolinium sesquioxide nanobars synthesized via thermal decomposition of gadolinium oxalate

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

Manigandan, R.; Giribabu, K.; Suresh, R.

2013-10-15

Graphical abstract: - Highlights: • The cubic Gd{sub 2}O{sub 3} nanobars are synthesized by decomposition of C{sub 6}H{sub 20}Gd{sub 2}O{sub 22}. • The nanoparticles are rectangular bar shape with high porous surface. • The combination of magnetic and optical properties within a single particle. • The Gd{sub 2}O{sub 3} nanobars have tailorable nanostructure, wide bandgap and are paramagnetic. - Abstract: Gadolinium oxide nanobars were obtained by thermal decomposition of gadolinium oxalate, which was synthesized by the chemical precipitation method along with glycerol. The functional group analysis and formation of gadolinium oxide from gadolinium oxalate were characterized by the Fourier transformmore » infrared spectroscopy and thermo gravimetric analyzer. The crystal structure, average crystallite size, and lattice parameter were analyzed by X-ray diffraction technique. Moreover, Raman shifts, elemental composition and morphology of the gadolinium oxide was widely investigated by the laser Raman microscope, X-ray photoelectron spectroscopy, FE-SEM-EDAX and HR-TEM, respectively. Furthermore, the optical properties like band gap, absorbance measurement of the gadolinium oxide were extensively examined. In addition, the paramagnetic property of gadolinium oxide nanobars was explored by the vibrating sample magnetometer.« less

Crystal-growth kinetics of magnetite (Fe3O4) nanoparticles with Ostwald Ripening Model approach

NASA Astrophysics Data System (ADS)

Utami, S. P.; Fadli, A.; Sari, E. O.; Addabsi, A. S.

2018-04-01

Magnetite (Fe3O4) nanoparticles is a magnetic nanomaterial that have potential properties to be applied as drug delivery The purpose of this study was to determine the influence of time and temperature synthesis of magnetie characteristics and determine its crystal growth kinetics model with Ostwald ripening model approach. Magnetite nanoparticles synthesized from FeCl3, citrate, urea and polyethylene glycol with hydrothermal method at 180, 200 and 220 °C for 1,3,5,7,9 and 12 hours. Characterization by X-ray Diffraction (XRD) indicated that magnetite formed at temperatures of 200 and 220 °C. Magnetite crystallite diameter obtained was 10-29 nm. Characterization by Transmission Electron Mycroscope (TEM) shows that magnetite nanoparticles have uniform size and non-agglomerated. Core-shell shaped particles formed at 200 °C and 220 °C for 3 hours. Irregular shape obtained at 220 °C for 12 hour synthesis with particle diameter about 120 nm. Characterization using Vibrating Sample Magnetometer (VSM) shown that magnetite has super paramagnetism behaviour with the highest saturation magnetization (Ms) was 70.27 emu/g. magnetite crystal growth data at temperature of 220 °C can be fitted by Ostwald ripening growth model with growth controlled by the dissolution of surface reaction (n≈4) with the percent error of 2.53%.

Preparation and characterization of polymer nanocomposites coated magnetic nanoparticles for drug delivery applications

NASA Astrophysics Data System (ADS)

Prabha, G.; Raj, V.

2016-06-01

In the present research work, the anticancer drug 'curcumin' is loaded with Chitosan (CS)-polyethylene glycol (PEG)-polyvinylpyrrolidone (PVP) (CS-PEG-PVP) polymer nanocomposites coated with superparamagnetic iron oxide (Fe3O4) nanoparticles. The system can be used for targeted and controlled drug delivery of anticancer drugs with reduced side effects and greater efficiency. The prepared nanoparticles were characterized by Fourier transmission infrared spectroscopy (FTIR), vibrating sample magnetometry (VSM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Curcumin drug loaded Fe3O4-CS, Fe3O4-CS-PEG and Fe3O4-CS-PEG-PVP nanoparticles exhibited the mean particle size in the range of 183-390 nm with a zeta potential value of 26-41 mV as measured using Malvern Zetasizer. The encapsulation efficiency, loading capacity and in-vitro drug release behavior of curcumin drug loaded Fe3O4-CS, Fe3O4-CS-PEG and Fe3O4-CS-PEG-PVP nanoparticles were studied using UV spectrophotometer. Besides, the cytotoxicity of the prepared nanoparticles using MTT assay was also studied. The curcumin drug release was examined at different pH medium and it was proved that the drug release depends upon the pH medium in addition to the nature of matrix.

Microwave-assisted synthesis of iron oxide nanoparticles in biocompatible organic environment

NASA Astrophysics Data System (ADS)

Aivazoglou, E.; Metaxa, E.; Hristoforou, E.

2018-04-01

The development of magnetite and maghemite particles in uniform nanometer size has triggered the interest of the research community due to their many interesting properties leading to a wide range of applications, such as catalysis, nanomedicine-nanobiology and other engineering applications. In this study, a simple, time-saving and low energy-consuming, microwave-assisted synthesis of iron oxide nanoparticles, is presented. The nanoparticles were prepared by microwave-assisted synthesis using polyethylene glycol (PEG) or PEG and β-cyclodextrin (β-CD)/water solutions of chloride salts of iron in the presence of ammonia solution. The prepared nano-powders were characterized using X-Ray Diffraction (XRD), Transition Electron Microscopy (TEM), Fourier-transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, Vibrating Sample Magnetometer (VSM), X-Ray Photoelectron Spectroscopy (XPS) and Thermal analysis (TG/DSC). The produced nanoparticles are crystallized mostly in the magnetite and maghemite lattice exhibiting very similar shape and size, with indications of partial PEG coating. Heating time, microwave power and presence of PEG, are the key factors shaping the size properties of nanoparticles. The average size of particles ranges from 10.3 to 19.2 nm. The nanoparticles exhibit a faceted morphology, with zero contamination levels. The magnetic measurements indicate that the powders are soft magnetic materials with negligible coercivity and remanence, illustrating super-paramagnetic behavior.

Adsorbent for p-phenylenediamine adsorption and removal based on graphene oxide functionalized with magnetic cyclodextrin

NASA Astrophysics Data System (ADS)

Wang, Dongxue; Liu, Liangliang; Jiang, Xinyu; Yu, Jingang; Chen, Xiaohong; Chen, Xiaoqing

2015-02-01

Recently, graphene oxide (GO) based magnetic nanocomposites have been widely used in an adsorption-based process for the removal of organic pollutants from the water system. In this study, magnetic β-cyclodextrin-graphene oxide nanocomposites (MCG) were synthesized according to covalent binding of magnetic β-cyclodextrin nanoparticles onto the GO surface and the as-made nanocomposites were successfully applied as adsorbents for the adsorption and removal of p-phenylenediamines (PPD). The composition and morphology of prepared materials were characterized by Fourier infrared spectrometry (FT-IR), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). Effects of pH, temperature, time and reusability on the adsorption of PPD were investigated, as well as the kinetics and isotherms parameters of the adsorbents were determined. The results indicated that the maximum adsorption capacity of MCG was 1102.58 mg/g at 45 °C and pH 8. The adsorption capacity remained at 81% after five cycles. Removal rate could reach 98% after three times of adsorption. The adsorption process with PPD was found that fitted pseudo-second-order kinetics equations and the Langmuir adsorption model. The results showed the MCG had a good adsorption ability to remove organic pollutants in wastewater.

Surface-Enhanced Impulsive Coherent Vibrational Spectroscopy

PubMed Central

Du, Juan; Harra, Juha; Virkki, Matti; Mäkelä, Jyrki M.; Leng, Yuxin; Kauranen, Martti; Kobayashi, Takayoshi

2016-01-01

Surface-enhanced Raman spectroscopy (SERS) has attracted a lot of attention in molecular sensing because of the remarkable ability of plasmonic metal nanostructures to enhance the weak Raman scattering process. On the other hand, coherent vibrational spectroscopy triggered by impulsive excitation using ultrafast laser pulses provides complete information about the temporal evolution of molecular vibrations, allowing dynamical processes in molecular systems to be followed in “real time”. Here, we combine these two concepts and demonstrate surface-enhanced impulsive vibrational spectroscopy. The vibrational modes of the ground and excited states of poly[2-methoxy-5-(2-ethylhexyloxy)−1,4-phenylenevinylene] (MEH-PPV), spin-coated on a substrate covered with monodisperse silver nanoparticles, are impulsively excited with a sub-10 fs pump pulse and characterized with a delayed broad-band probe pulse. The maximum enhancement in the spectrally and temporally resolved vibrational signatures averaged over the whole sample is about 4.6, while the real-time information about the instantaneous vibrational amplitude together with the initial vibrational phase is preserved. The phase is essential to determine the vibrational contributions from the ground and excited states. PMID:27812020

Construction and calibration of a low cost and fully automated vibrating sample magnetometer

NASA Astrophysics Data System (ADS)

El-Alaily, T. M.; El-Nimr, M. K.; Saafan, S. A.; Kamel, M. M.; Meaz, T. M.; Assar, S. T.

2015-07-01

A low cost vibrating sample magnetometer (VSM) has been constructed by using an electromagnet and an audio loud speaker; where both are controlled by a data acquisition device. The constructed VSM records the magnetic hysteresis loop up to 8.3 KG at room temperature. The apparatus has been calibrated and tested by using magnetic hysteresis data of some ferrite samples measured by two scientifically calibrated magnetometers; model (Lake Shore 7410) and model (LDJ Electronics Inc. Troy, MI). Our VSM lab-built new design proved success and reliability.

Nitrate-assisted photocatalytic efficiency of defective Eu-doped Pr(OH)3 nanostructures.

PubMed

Aškrabić, S; Araújo, V D; Passacantando, M; Bernardi, M I B; Tomić, N; Dojčinović, B; Manojlović, D; Čalija, B; Miletić, M; Dohčević-Mitrović, Z D

2017-12-06

Pr(OH) 3 one-dimensional nanostructures are a less studied member of lanthanide hydroxide nanostructures, which recently demonstrated an excellent adsorption capacity for organic pollutant removal from wastewater. In this study, Pr 1-x Eu x (OH) 3 (x = 0, 0.01, 0.03, and 0.05) defective nanostructures were synthesized by a facile and scalable microwave-assisted hydrothermal method using KOH as an alkaline metal precursor. The phase and surface composition, morphology, vibrational, electronic and optical properties of the as-prepared samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma optical emission spectrometry (ICP-OES), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), Raman, infrared (IR), photoluminescence (PL), and diffuse reflectance spectroscopy (DRS). It was deduced that the incorporation of Eu 3+ ions promoted the formation of oxygen vacancies in the already defective Pr(OH) 3 , subsequently changing the Pr(OH) 3 nanorod morphology. The presence of KNO 3 phase was registered in the Eu-doped samples. The oxygen-deficient Eu-doped Pr(OH) 3 nanostructures displayed an improved photocatalytic activity in the removal of reactive orange (RO16) dye under UV-vis light irradiation. An enhanced photocatalytic activity of the Eu-doped Pr(OH) 3 nanostructures was caused by the synergetic effect of oxygen vacancies and Eu 3+ (NO 3 - ) ions present on the Pr(OH) 3 surface, the charge separation efficiency and the formation of the reactive radicals. In addition, the 3% Eu-doped sample exhibited very good adsorptive properties due to different morphology and higher electrostatic attraction with the anionic dye. Pr 1-x Eu x (OH) 3 nanostructures with the possibility of tuning their adsorption/photocatalytic properties present a great potential for wastewater treatment.

Ultrasound assisted extraction of Maxilon Red GRL dye from water samples using cobalt ferrite nanoparticles loaded on activated carbon as sorbent: Optimization and modeling.

PubMed

Mehrabi, Fatemeh; Vafaei, Azam; Ghaedi, Mehrorang; Ghaedi, Abdol Mohammad; Alipanahpour Dil, Ebrahim; Asfaram, Arash

2017-09-01

In this research, a selective, simple and rapid ultrasound assisted dispersive solid-phase micro-microextraction (UA-DSPME) was developed using cobalt ferrite nanoparticles loaded on activated carbon (CoFe 2 O 4 -NPs-AC) as an efficient sorbent for the preconcentration and determination of Maxilon Red GRL (MR-GRL) dye. The properties of sorbent are characterized by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Vibrating sample magnetometers (VSM), Fourier transform infrared spectroscopy (FTIR), Particle size distribution (PSD) and Scanning Electron Microscope (SEM) techniques. The factors affecting on the determination of MR-GRL dye were investigated and optimized by central composite design (CCD) and artificial neural networks based on genetic algorithm (ANN-GA). CCD and ANN-GA were used for optimization. Using ANN-GA, optimum conditions were set at 6.70, 1.2mg, 5.5min and 174μL for pH, sorbent amount, sonication time and volume of eluent, respectively. Under the optimized conditions obtained from ANN-GA, the method exhibited a linear dynamic range of 30-3000ngmL -1 with a detection limit of 5.70ngmL -1 . The preconcentration factor and enrichment factor were 57.47 and 93.54, respectively with relative standard deviations (RSDs) less than 4.0% (N=6). The interference effect of some ions and dyes was also investigated and the results show a good selectivity for this method. Finally, the method was successfully applied to the preconcentration and determination of Maxilon Red GRL in water and wastewater samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis, characterization and magnetic properties of MFe2O4 (M=Co, Mg, Mn, Ni) nanoparticles using ricin oil as capping agent

NASA Astrophysics Data System (ADS)

Gherca, Daniel; Pui, Aurel; Cornei, Nicoleta; Cojocariu, Alina; Nica, Valentin; Caltun, Ovidiu

2012-11-01

We focused on obtaining MFe2O4 nanoparticles using ricin oil solution as surfactant and on their structural characterization and magnetic properties. The annealed samples at 500 °C in air for 6 h were analyzed for the crystal phase identification by powder X-ray diffraction using CuKα radiation. The particle size, the chemical composition and the morphology of the calcinated powders were characterized by scanning electron microscopy. All sintered samples contain only one phase, which has a cubic structure with crystallite sizes of 12-21 nm. From the infrared spectra of all samples were observed two strong bands around 600 and 400 cm-1, which correspond to the intrinsic lattice vibrations of octahedral and tetrahedral sites of the spinel structure, respectively, and characteristic vibration for capping agent. The magnetic properties of fine powders were investigated at room temperature by using a vibrating sample magnetometer. The room temperature M-H hysteresis loops show ferromagnetic behavior of the calcined samples, with specific saturation magnetization (Ms) values ranging between 11 and 53 emu/g.

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.

Fe3O4@p-Naphtholbenzein as a novel nano-sorbent for highly effective removal and recovery of Berberine: Response surface methodology for optimization of ultrasound assisted dispersive magnetic solid phase extraction.

PubMed

Aghaie, Ali B G; Hadjmohammadi, Mohammad Reza

2016-08-15

A hydrophobic surface modified iron oxide magnetic nano-sorbent was successfully synthesized, characterized and utilized for highly effective removal and recovery of Berberine (Brb) by Ultrasound Assisted Dispersive Magnetic Solid Phase Extraction (UADM-SPE). Fabrication of p-Naphtholbenzein-coated magnetic nanoparticles (PNB-MNPs) was certified by characteristic analyses such as: Fourier transform infrared spectroscopy (FT-IR), X-ray Diffraction (XRD), thermogravimetric analysis (TGA), vibrating sample magnetometer (VSM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The characterized PNB-MNPs were utilized to develop a UADM-SPE method for Brb, a well-known isoquinoline alkaloid with a highlighted chemical skeleton for designing selective and powerful bioactive molecules. Affecting parameters on the extraction of Brb were optimized through an orthogonal rotatable central composite design (CCD). The optimum condition is obtained when the variables are set to: pH=4, amount of MNPs=20mg, sample volume=30ml, sonication time=1min at room temperature, and desorbing solvent=500µL of methanol. Under the mentioned condition, an extraction recovery of 98.2%, with relative standard deviation of 3.7%, was obtained via five replicated measurements on a 0.1mgL(-1) Brb standard solution. Finally, the method was successfully applied for determination of Brb in human plasma and urine samples. Regarding the method calibration graphs in plasma and urine matrices, spiked in the range of 0.01-200.00µgL(-1), pre-concentration factors of 134 and 122, method detection limit (MDL) of 0.17 and 0.19µgL(-1), and lower limit of quantification of 0.57 and 0.63µgL(-1) were obtained for plasma and urine samples, respectively. The method exhibits good potentials to be a fast, efficient and reliable method for determination of Brb in human biological samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Gel performance in rheology and profile control under low-frequency vibration: coupling application of physical and chemical EOR techniques.

PubMed

Zheng, Li Ming; Pu, Chun Sheng; Liu, Jing; Ma, Bo; Khan, Nasir

2017-01-01

Flowing gel plugging and low-frequency vibration oil extraction technology have been widely applied in low-permeability formation. High probability of overlapping in action spheres of two technologies might lead to poor operating efficiency during gel injection. Study on flowing gel rheological properties under low-frequency vibration was essential, which was carried out indoor with viscosity measurement. Potential dynamic mechanisms were analyzed for the rheological variation. Under low-frequency vibration, gel rheological properties were found to be obviously influenced, with vibration delaying gel cross-linking in induction period, causing a two-stage gel viscosity change in acceleration period, and decreasing gel strength in stable period. Surface of gel system under vibration presented different fluctuating phenomenon from initial harmonic vibrating to heterogeneous fluctuating (droplet separation might appear) to final harmonic vibrating again. Dynamic displacement in unconsolidated sand pack revealed that low-frequency vibration during gel injection might be a measure to achieve deep profile control, with the gel injection depth increased by 65.8 % compared with the vibration-free sample. At last, suggestions for field test were given in the paper to achieve lower injection friction and better gel plugging efficiency.

[Synthesis and characterization of CO-3(2-) doping nano-hydroxyapatite].

PubMed

Liao, Jian-Guo; Li, Yan-Qun; Duan, Xing-Ze; Liu, Qiong

2014-11-01

CO3(2-) doping is an effective method to increase the biological activity of nano-hydroxyapatite (n-HA). In the present study, calcium nitrate and trisodium phosphate were chosen as raw materials, with a certain amount of Na2CO3 as a source of CO-3(2-) ions, to synthesize nano-carbonate hydroxyapatite (n-CHA) slurry by solution precipitation method. The structure and micro-morphology of n-CHA were characterized by transmission electron microscope (TEM), X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FTIR) and Raman spectroscopy (RS). The results revealed that the synthetic n-HA crystals are acicular in nanometer scale and have a crystal size of 20-30 nm in diameter and 60-80 nm in length, which are similar to natural bone apatite. And the crystallinity of n-CHA crystals decreases to the increment of CO3(2-). Samples with more CO3(2) have composition and structure more similar to the bone apatite. The value of lattice parameters a decreases, value of c increases, and c/a value increases with the increase in the amount of CO3(2-), in accordance with crystal cell parameters change rule of type B replacement. In the AB mixed type (substitution OH- and PO4(3-)) CHA, IR characteristic peak of CO3(2-) out-of-plane bending vibration appears at 872 cm(-1), meanwhile, the asymmetry flexible vibration band is split into band at 1 454 cm(-1) and band at 1 420 cm(-1), while weak CO3(2)-peak appears at 1 540 cm(-1). CO3(2-) Raman peak of symmetric stretching vibration appears at 1 122 cm(-1). CO3(2-) B-type (substitution PO4(3-)) peak appeared at 1 071 cm(-1). Through the calculation of integral area ratio of PO4(3-)/ CO3(2-), OH-/CO3(2-), and PO4(3-)/OH-, low quantity CO3(2-) is B-type and high quantity CO3(2-) is A-type (substitution OH-). The results show that the synthesized apatite crystals are AB hybrid substitued nano-carbonate hydroxyapatite, however B-type replacement is the main substitute mode. Due to similarity inthe shape, size, crystal structure and growth mode, the synthesized apatite crystals can be called a kind of bone-like apatite.

Bacteriophages carrying antibiotic resistance genes in fecal waste from cattle, pigs, and poultry.

PubMed

Colomer-Lluch, Marta; Imamovic, Lejla; Jofre, Juan; Muniesa, Maite

2011-10-01

This study evaluates the occurrence of bacteriophages carrying antibiotic resistance genes in animal environments. bla(TEM), bla(CTX-M) (clusters 1 and 9), and mecA were quantified by quantitative PCR in 71 phage DNA samples from pigs, poultry, and cattle fecal wastes. Densities of 3 to 4 log(10) gene copies (GC) of bla(TEM), 2 to 3 log(10) GC of bla(CTX-M), and 1 to 3 log(10) GC of mecA per milliliter or gram of sample were detected, suggesting that bacteriophages can be environmental vectors for the horizontal transfer of antibiotic resistance genes.

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

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

Wachid, Frischa M., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Perkasa, Adhi Y., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Prasetya, Fandi A., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id

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

Acceleration of a ground-state reaction by selective femtosecond-infrared-laser-pulse excitation

NASA Astrophysics Data System (ADS)

Stensitzki, Till; Yang, Yang; Kozich, Valeri; Ahmed, Ashour A.; Kössl, Florian; Kühn, Oliver; Heyne, Karsten

2018-02-01

Infrared (IR) excitation of vibrations that participate in the reaction coordinate of an otherwise thermally driven chemical reaction are believed to lead to its acceleration. Attempts at the practical realization of this concept have been hampered so far by competing processes leading to sample heating. Here we demonstrate, using femtosecond IR-pump IR-probe experiments, the acceleration of urethane and polyurethane formation due to vibrational excitation of the reactants for 1:1 mixtures of phenylisocyanate and cyclohexanol, and toluene-2,4-diisocyanate and 2,2,2-trichloroethane-1,1-diol, respectively. We measured reaction rate changes upon selective vibrational excitation with negligible heating of the sample and observed an increase of the reaction rate up to 24%. The observation is rationalized using reactant and transition-state structures obtained from quantum chemical calculations. We subsequently used IR-driven reaction acceleration to write a polyurethane square on sample windows using a femtosecond IR pulse.

Quality Factor and Microslipping of Fatigue Cracks in Thin Plates at Resonant Vibration

NASA Technical Reports Server (NTRS)

Wincheski, B.; Namkung, M.; Fulton, J. P.

1993-01-01

Resonant vibrations have been stimulated in thin metal plates using a non-contacting electromagnetic driver. A sinusoidal force was applied in a swept frequency fashion and the resulting surface displacements were monitored through the use of an acoustic microphone. It has been found that the presence of a fatigue crack in the sample causes a broadening of the second resonance peak. The Q factors of the resonance curves were determined and are directly correlated with the presence of fatigue cracks in the samples. The broadening of the curves is explained in terms of a microslipping at the crack face walls which reduces the amplitude of the resonant vibration by increasing the damping of the system. A comparison is made between the resonance characteristics of fatigue damaged and notched samples, where the stiffness of the two systems is nearly constant while the interaction between crack face walls is eliminated in the latter.

Strain mapping in TEM using precession electron diffraction

DOEpatents

Taheri, Mitra Lenore; Leff, Asher Calvin

2017-02-14

A sample material is scanned with a transmission electron microscope (TEM) over multiple steps having a predetermined size at a predetermined angle. Each scan at a predetermined step and angle is compared to a template, wherein the template is generated from parameters of the material and the scanning. The data is then analyzed using local mis-orientation mapping and/or Nye's tensor analysis to provide information about local strain states.

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

Nano-inclusions in diamond: Evidence of diamond genesis

NASA Astrophysics Data System (ADS)

Wirth, R.

2015-12-01

The use of Focused Ion Beam technology (FIB) for TEM sample preparation introduced approximately 15 years ago revolutionized the application of TEM in Geosciences. For the first time, FIB enabled cutting samples for TEM use from exactly the location we are interested in. Applied to diamond investigation, this technique revealed the presence of nanometre-sized inclusions in diamond that have been simply unknown before. Nanoinclusions in diamond from different location and origin such as diamonds from the Lower and Upper Mantle, metamorphic diamonds (Kazakhstan, Erzgebirge, Bohemia), diamonds from ophiolites (Tibet, Mongolia, Xinjiang, Ural Mountains), diamonds from igneous rocks (Hawaii, Kamchatka) and impact diamonds (Popigai Crater, Siberia) have been investigated during the last 15 years. The major conclusion of all these TEM studies is, that the nanoinclusions, their phases and phase composition together with the micro- and nanostructure evidence the origin of diamond and genesis of diamond. We can discriminate Five different mechanisms of diamond genesis in nature are observed: Diamond crystallized from a high-density fluid (Upper mantle and metamorphic diamond). Diamond crystallized from carbonatitic melt (Lower mantle diamond). Diamond precipitates from a metal alloy melt (Diamond from ophiolites). Diamond crystallized by gas phase condensation or chemical vapour condensation (CVD) (Lavas from Kamchatka, xenoliths in Hawaiian lavas). Direct transformation of graphite into diamond.

A method for measuring the local gas pressure within a gas-flow stage in situ in the transmission electron microscope

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

Colby, Robert J.; Alsem, Daan H.; Liyu, Andrey V.

2015-06-01

The development of environmental transmission electron microscopy (TEM) has enabled in situ experiments in a gaseous environment with high resolution imaging and spectroscopy. Addressing scientific challenges in areas such as catalysis, corrosion, and geochemistry can require pressures much higher than the ~20 mbar achievable with a differentially pumped, dedicated environmental TEM. Gas flow stages, in which the environment is contained between two semi-transparent thin membrane windows, have been demonstrated at pressures of several atmospheres. While this constitutes significant progress towards operando measurements, the design of many current gas flow stages is such that the pressure at the sample cannot necessarilymore » be directly inferred from the pressure differential across the system. Small differences in the setup and design of the gas flow stage can lead to very different sample pressures. We demonstrate a method for measuring the gas pressure directly, using a combination of electron energy loss spectroscopy and TEM imaging. This method requires only two energy filtered TEM images, limiting the measurement time to a few seconds and can be performed during an ongoing experiment at the region of interest. This approach provides a means to ensure reproducibility between different experiments, and even between very differently designed gas flow stages.« less

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.

Bacterial diversity in faeces from polar bear (Ursus maritimus) in Arctic Svalbard.

PubMed

Glad, Trine; Bernhardsen, Pål; Nielsen, Kaare M; Brusetti, Lorenzo; Andersen, Magnus; Aars, Jon; Sundset, Monica A

2010-01-14

Polar bears (Ursus maritimus) are major predators in the Arctic marine ecosystem, feeding mainly on seals, and living closely associated with sea ice. Little is known of their gut microbial ecology and the main purpose of this study was to investigate the microbial diversity in faeces of polar bears in Svalbard, Norway (74-81 degrees N, 10-33 degrees E). In addition the level of blaTEM alleles, encoding ampicillin resistance (ampr) were determined. In total, ten samples were collected from ten individual bears, rectum swabs from five individuals in 2004 and faeces samples from five individuals in 2006. A 16S rRNA gene clone library was constructed, and all sequences obtained from 161 clones showed affiliation with the phylum Firmicutes, with 160 sequences identified as Clostridiales and one sequence identified as unclassified Firmicutes. The majority of the sequences (70%) were affiliated with the genus Clostridium. Aerobic heterotrophic cell counts on chocolate agar ranged between 5.0 x 10(4) to 1.6 x 10(6) colony forming units (cfu)/ml for the rectum swabs and 4.0 x 10(3) to 1.0 x 10(5) cfu/g for the faeces samples. The proportion of ampr bacteria ranged from 0% to 44%. All of 144 randomly selected ampr isolates tested positive for enzymatic beta-lactamase activity. Three % of the ampr isolates from the rectal samples yielded positive results when screened for the presence of blaTEM genes by PCR. BlaTEM alleles were also detected by PCR in two out of three total faecal DNA samples from polar bears. The bacterial diversity in faeces from polar bears in their natural environment in Svalbard is low compared to other animal species, with all obtained clones affiliating to Firmicutes. Furthermore, only low levels of blaTEM alleles were detected in contrast to their increasing prevalence in some clinical and commensal bacterial populations.

Bacterial diversity in faeces from polar bear (Ursus maritimus) in Arctic Svalbard

PubMed Central

2010-01-01

Background Polar bears (Ursus maritimus) are major predators in the Arctic marine ecosystem, feeding mainly on seals, and living closely associated with sea ice. Little is known of their gut microbial ecology and the main purpose of this study was to investigate the microbial diversity in faeces of polar bears in Svalbard, Norway (74-81°N, 10-33°E). In addition the level of blaTEM alleles, encoding ampicillin resistance (ampr) were determined. In total, ten samples were collected from ten individual bears, rectum swabs from five individuals in 2004 and faeces samples from five individuals in 2006. Results A 16S rRNA gene clone library was constructed, and all sequences obtained from 161 clones showed affiliation with the phylum Firmicutes, with 160 sequences identified as Clostridiales and one sequence identified as unclassified Firmicutes. The majority of the sequences (70%) were affiliated with the genus Clostridium. Aerobic heterotrophic cell counts on chocolate agar ranged between 5.0 × 104 to 1.6 × 106 colony forming units (cfu)/ml for the rectum swabs and 4.0 × 103 to 1.0 × 105 cfu/g for the faeces samples. The proportion of ampr bacteria ranged from 0% to 44%. All of 144 randomly selected ampr isolates tested positive for enzymatic β-lactamase activity. Three % of the ampr isolates from the rectal samples yielded positive results when screened for the presence of blaTEM genes by PCR. BlaTEM alleles were also detected by PCR in two out of three total faecal DNA samples from polar bears. Conclusion The bacterial diversity in faeces from polar bears in their natural environment in Svalbard is low compared to other animal species, with all obtained clones affiliating to Firmicutes. Furthermore, only low levels of blaTEM alleles were detected in contrast to their increasing prevalence in some clinical and commensal bacterial populations. PMID:20074323

Imaging Organ of Corti Vibration Using Fourier-Domain OCT

NASA Astrophysics Data System (ADS)

Choudhury, Niloy; Chen, Fangyi; Fridberger, Anders; Zha, Dingjun; Jacques, Steven L.; Wang, Ruikang K.; Nuttall, Alfred L.

2011-11-01

Measuring the sound stimulated vibration from various structures in the organ of Corti is important in understanding how the small vibrations are amplified and detected. In this study we examine the feasibility of using phase-sensitive Fourier domain optical coherence tomography (PSFD-OCT) to measure vibration of the cellular structures of the organ of Corti. PSFD-OCT is a low coherence interferrometry system where the interferrogram is detected as a function of wavelength. The phase of the Fourier transformation of the detected spectra contains path deference (between the sample arm and the reference arm) information of the interferometer. In PSFD-OCT this phase is measured as a function of time and thus any time dependent change in the path difference between the sample arm and the reference arm can be detected. In the experiment, we used an in vitro preparation of the guinea pig cochlea and made a surgical opening at the apical end to access the organ of Corti. By applying tones with different frequencies via the intact middle ear, we recorded the structural vibration inside the organ of Corti. Vibration amplitude and phase of different substructures were mapped on a cross-section view of the organ of Corti. Although the measurements were made at the apical turn of the cochlea, it will be possible to make vibration measurement from various turns of the cochlea. The noise floor of the system was 0.3 nm, calibrated using a piezo stack as a calibrator.

Beliefs about women's vibrator use: results from a nationally representative probability survey in the United States.

PubMed

Herbenick, Debra; Reece, Michael; Schick, Vanessa; Jozkowski, Kristen N; Middelstadt, Susan E; Sanders, Stephanie A; Dodge, Brian S; Ghassemi, Annahita; Fortenberry, J Dennis

2011-01-01

Women's vibrator use is common in the United States, although little is known about beliefs about its use. Elicitation surveys and interviews informed the development of a 10-item scale, the Beliefs About Women's Vibrator Use Scale, which was administered to a nationally representative probability sample of adults ages 18 to 60 years. Most women and men held high positive and low negative beliefs about women's vibrator use. Women with positive beliefs reported higher Female Sexual Function Index scores related to arousal, lubrication, orgasm, satisfaction, and pain (indicating less pain).

High-Resolution Characterization of UMo Alloy Microstructure

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

Devaraj, Arun; Kovarik, Libor; Joshi, Vineet V.

2016-11-30

This report highlights the capabilities and procedure for high-resolution characterization of UMo fuels in PNNL. Uranium-molybdenum (UMo) fuel processing steps, from casting to forming final fuel, directly affect the microstructure of the fuel, which in turn dictates the in-reactor performance of the fuel under irradiation. In order to understand the influence of processing on UMo microstructure, microstructure characterization techniques are necessary. Higher-resolution characterization techniques like transmission electron microscopy (TEM) and atom probe tomography (APT) are needed to interrogate the details of the microstructure. The findings from TEM and APT are also directly beneficial for developing predictive multiscale modeling tools thatmore » can predict the microstructure as a function of process parameters. This report provides background on focused-ion-beam–based TEM and APT sample preparation, TEM and APT analysis procedures, and the unique information achievable through such advanced characterization capabilities for UMo fuels, from a fuel fabrication capability viewpoint.« less

Microstructural Characterization of Aluminum-Lithium Alloys 1460 and 2195

NASA Technical Reports Server (NTRS)

Wang, Z. M.; Shenoy, R. N.

1998-01-01

Transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) techniques were employed to characterize the precipitate distributions in lithium-containing aluminum alloys 1460 and 2195 in the T8 condition. TEM examinations revealed delta prime and T1 as the primary strengthening precipitates in alloys 1460 and 2195 respectively. TEM results showed a close similarity of the Russian alloy 1460 to the U.S. alloy 2090, which has a similar composition and heat treatment schedule. DSC analyses also indicate a comparable delta prime volume fraction. TEM study of a fractured tensile sample of alloy 1460 showed that delta prime precipitates are sheared by dislocations during plastic deformation and that intense stress fields arise at grain boundaries due to planar slip. Differences in fracture toughness of alloys 1460 and 2195 are rationalized on the basis of a literature review and observations from the present study.

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.

Infrared and Raman spectroscopic studies of structural variations in minerals from Apollo 11, 12, 14 and 15 samples, volume 3

NASA Technical Reports Server (NTRS)

Estep, P. A.; Kovach, J. J.; Waldstein, P.; Karr, C., Jr.

1972-01-01

Infrared and Raman vibrational spectroscopic data, yielding direct information on molecular structure, were obtained for single grains ( 150 microns) of minerals, basalts, and glasses isolated from Apollo 11, 12, 14, and 15 rock and dust samples, and for grains in Apollo 14 polished butt samples. From the vibrational data, specification substitutions were determined for the predominant silicate minerals of plagioclase, pyroxene, and olivine. Unique spectral variations for grains of K-feldspar, orthopyroxene, pyroxenoid, and ilmenite were observed to exceed the ranges of terrestrial samples, and these variations may be correlatable with formation histories. Alpha-quartz was isolated as pure single grains, in granitic grains composited with sanidine, and in unique grains that were intimately mixed with varying amounts of glass. Accessory minerals of chromite and ulvospinel were isolated as pure grains and structurally characterized from their distinctive infrared spectra. Fundamental vibrations of the SiO4 tetrahedra in silicate minerals were used to classify bulk compositions in dust sieved fractions, basalt grains and glass particles, and to compare modal characteristics for maria, highland and rille samples. No hydrated minerals were found in any of the samples studied, indicating anhydrous formation conditions.

Characterization of extended-spectrum β-lactamase (ESBL)-producing Klebsiella, Enterobacter, and Citrobacter obtained in environmental samples of a Tunisian hospital.

PubMed

Dziri, Raoudha; Klibi, Naouel; Alonso, Carla Andrea; Said, Leila Ben; Bellaaj, Ridha; Slama, Karim Ben; Boudabous, Abdellatif; Torres, Carmen

2016-10-01

The assessment of the hospital environment as a reservoir of ESBL-producing Enterobacteriaceae in Tunisian hospitals is scarcely analyzed, except for Escherichia coli. The aim of this study was to evaluate the presence of ESBL-producing non-E. coli Enterobacteriaceae (ESBL-EbNoEc) in 300 samples of abiotic surfaces and the hands of patients and staff of a Tunisian Hospital, and to characterize the ESBL genes of the recovered isolates. ESBL-EbNoEc were recovered in 28 of 300 (9.3%) analyzed samples and were identified as Klebsiella pneumoniae (n= 11), Enterobacter cloacae (n=11), Citrobacter freundii (n=4) and Klebsiella oxytoca (n=2). The bla genes identified by PCR and sequencing among the strains were as follows: 11 K.pneumoniae strains [blaCTX-M-15+ blaTEM-1+ blaSHV-11 (n=6); blaCTX-M-15+ blaTEM-1+ blaSHV-28 (n=3); blaCTX-M-15+ blaTEM-1+ blaSHV-1 (n=2)], 11 E. cloacae strains [blaCTX-M-15 (n=6); blaCTX-M-15+ blaTEM-1b (n=2); blaCTX-M-15+ blaTEM-1b+ blaOXA-1 (n=1);blaCTX-M-15+ blaOXA-1 (n=1);blaSHV-12 (n=1)], 4 C. freundii strains [blaCTX-M-15] and 2 K. oxytoca strains [blaCTX-M-15 (n=1); blaSHV-12 (n=1)]. The ISEcp1 and orf477 sequences were identified upstream and downstream of the blaCTX-M-15 gene, respectively, in 3 K. pneumoniae and 3 E. cloacae isolates. The PFGE analysis demonstrated three unrelated pulsotypes in K. pneumoniae strains and five pulsotypes in E. cloacae. The uncontrolled dissemination of ESBL-producing bacteria, even in the hospital environment, has become a real problem and new strategies and hygienic rules are needed to stop this bacterial dissemination. Copyright © 2016 Elsevier Inc. All rights reserved.

Micro-Vibration Measurements on Thermally Loaded Multi-Layer Insulation Samples in Vacuum

NASA Technical Reports Server (NTRS)

Deutsch, Georg; Grillenbeck, Anton

2008-01-01

Some scientific missions require to an extreme extent the absence of any on-board microvibration. Recent projects dedicated to measuring the Earth's gravity field and modeling the geoid with extremely high accuracy are examples. Their missions demand for extremely low micro-vibration environment on orbit for: (1) Not disturbing the measurement of earth gravity effects with the installed gradiometer or (2) Even not damaging the very high sensitive instruments. Based on evidence from ongoing missions multi-layer insulation (MLI) type thermal control blankets have been identified as a structural element of spacecrafts which might deform under temperature variations being caused by varying solar irradiation in orbit. Any such deformation exerts tiny forces which may cause small reactions resulting in micro-vibrations, in particular by exciting the spacecraft eigenmodes. The principle of the test set-up for the micro-vibration test was as follows. A real side wall panel of the spacecraft (size about 0.25 m2) was low-frequency suspended in a thermal vacuum chamber. On the one side of this panel, the MLI samples were fixed by using the standard methods. In front of the MLI, an IR-rig was installed which provided actively controlled IR-radiation power of about 6 kW/m2 in order to heat the MLI surface. The cooling was passive using the shroud temperature at a chamber pressure <1E-5mbar. The resulting micro-vibrations due to MLI motion in the heating and the cooling phase were measured via seismic accelerometers which were rigidly mounted to the panel. Video recording was used to correlate micro-vibration events to any visual MLI motion. Different MLI sample types were subjected to various thermal cycles in a temperature range between -60 C to +80 C. In this paper, the experience on these micro-vibration measurements will be presented and the conclusions for future applications will be discussed

Environmental Asbestos Assessment Manual: Superfund Method for the Determination of Asbestos in Ambient Air, Part 1: Method

EPA Science Inventory

This is a sampling and analysis method for the determination of asbestos in air. Samples are analyzed by transmission electron microscopy (TEM). Although a small subset of samples are to be prepared using a direct procedure, the majority of samples analyzed using this method wil...

Spotiton: A prototype for an integrated inkjet dispense and vitrification system for cryo-TEM

PubMed Central

Jain, Tilak; Sheehan, Patrick; Crum, John; Carragher, Bridget; Potter, Clinton S.

2012-01-01

Over the last three decades, Cryo-TEM has developed into a powerful technique for high-resolution imaging of biological macromolecules in their native vitrified state. However, the technique for vitrifying specimens onto EM grids is essentially unchanged – application of ~ 3 µL sample to a grid, followed by blotting and rapid plunge freezing into liquid ethane. Several trials are often required to obtain suitable thin (few hundred nanometers or less) vitrified layers amenable for cryo-TEM imaging, which results in waste of precious sample and resources. While commercially available instruments provide some level of automation to control the vitrification process in an effort to increase quality and reproducibility, obtaining satisfactory vitrified specimens remains a bottleneck in the Cryo-TEM pipeline. We describe here a completely novel method for EM specimen preparation based on small volume (picoliter to nanoliter) dispensing using inkjet technology. A first prototype system (Spotiton v0.5) demonstrates feasibility of this new approach for specimen vitrification. A piezo-electric inkjet dispenser is integrated with optical real-time cameras (100 Hz frame rate) to analyze picoliter to nanoliter droplet profiles in-flight and spreading dynamics on the grid, and thus provides a method to optimize timing of the process. Using TEM imaging and biochemical assays we demonstrate that the piezo-electric inkjet mechanism does not disrupt the structural or functional integrity of macromolecules. These preliminary studies provide insight into the factors and components that will need further development to enable a robust and repeatable technique for specimen vitrification using this novel approach. PMID:22569522

Enhanced antibacterial activity of zinc oxide nanoparticles synthesized using Petroselinum crispum extracts

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

Stan, Manuela, E-mail: manuela.stan@itim-cj.ro; Popa, Adriana; Toloman, Dana

The present contribution reports the synthesis of zinc oxide nanoparticles (ZnO NPs) using aqueous leaf and root extracts of Petroselinum crispum (parsley) and characterization of as-prepared samples. ZnO NPs are subjected to X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron paramagnetic resonance (EPR) studies. The XRD studies reveal a hexagonal wurtzite structure without supplementary diffraction lines for all ZnO samples. TEM analysis shows that the particle size is influenced by the type of plant extract. The EPR spectra indicate the presence of Mn{sup 2+} ions in ZnO sample synthesized using P. crispum leaf extract, while zinc vacancy complexes andmore » oxygen vacancies are evidenced in all analyzed samples. ZnO NPs synthesized using P. crispum extracts exhibit increased (2-16 times) antibacterial activity as compared to chemically synthesized ZnO NPs.« less

An evaluation of potential occupational exposure to asbestiform amphiboles near a former vermiculite mine.

PubMed

Hart, Julie F; Spear, Terry M; Ward, Tony J; Baldwin, Caitlan E; Salo, Marissa N; Elashheb, Mohamed I

2009-01-01

Amphibole asbestos (AA) has been detected on the surface of tree bark in forests neighboring an abandoned vermiculite mine near Libby, Montana. In the present study, simulations were performed to assess potential AA exposure associated with United States Department of Agriculture Forest Service (FS) occupational activities. Bark samples were collected prior, and personal breathing zone (PBZ) and Tyvek clothing wipe samples were collected during and immediately after trials that simulated FS activities. Transmission electron microscopy (TEM) analyses revealed AA bark concentrations up to 15 million structures per square centimeter (s/cm(2)). AA was detected in 25% of the PBZ TEM samples. AA was detected on wipe samples collected from all activities evaluated. This research demonstrates the potential for airborne exposure and transport of AA in the Kootenai National Forest. These findings are especially relevant to those that work in the area and to the general public who may conduct recreational activities.

An Examination of a Music Appreciation Method Incorporating Tactile Sensations from Artificial Vibrations

NASA Astrophysics Data System (ADS)

Ideguchi, Tsuyoshi; Yoshida, Ryujyu; Ooshima, Keita

We examined how test subject impressions of music changed when artificial vibrations were incorporated as constituent elements of a musical composition. In this study, test subjects listened to several music samples in which different types of artificial vibration had been incorporated and then subjectively evaluated any resulting changes to their impressions of the music. The following results were obtained: i) Even if rhythm vibration is added to a silent component of a musical composition, it can effectively enhance musical fitness. This could be readily accomplished when actual sounds that had been synchronized with the vibration components were provided beforehand. ii) The music could be listened to more comfortably by adding not only a natural vibration extracted from percussion instruments but also artificial vibration as tactile stimulation according to intentional timing. Furthermore, it was found that the test subjects' impression of the music was affected by a characteristic of the artificial vibration. iii) Adding vibration to high-frequency areas can offer an effective and practical way of enhancing the appeal of a musical composition. iv) The movement sensations of sound and vibration could be experienced when the strength of the sound and vibration are modified in turn. These results suggest that the intentional application of artificial vibration could result in a sensitivity amplification factor on the part of a listener.

Coupled rotor/airframe vibration analysis program manual. Volume 2: Sample input and output listings

NASA Technical Reports Server (NTRS)

Cassarino, S.; Sopher, R.

1982-01-01

Sample input and output listings obtained with the base program (SIMVIB) of the coupled rotor/airframe vibration analysis and the external programs, G400/F389 and E927 are presented. Results for five of the base program test cases are shown. They represent different applications of the SIMVIB program to study the vibration characteristics of various dynamic configurations. Input and output listings obtained for one cycle of the G400/F389 coupled program are presented. Results from the rotor aeroelastic analysis E927 also appear. A brief description of the check cases is provided. A summary of the check cases for all the external programs interacting with the SIMVIB program is illustrated.

Measurement of correlations between low-frequency vibrational modes and particle rearrangements in quasi-two-dimensional colloidal glasses.

PubMed

Chen, Ke; Manning, M L; Yunker, Peter J; Ellenbroek, Wouter G; Zhang, Zexin; Liu, Andrea J; Yodh, A G

2011-09-02

We investigate correlations between low-frequency vibrational modes and rearrangements in two-dimensional colloidal glasses composed of thermosensitive microgel particles, which readily permit variation of the sample packing fraction. At each packing fraction, the particle displacement covariance matrix is measured and used to extract the vibrational spectrum of the "shadow" colloidal glass (i.e., the particle network with the same geometry and interactions as the sample colloid but absent damping). Rearrangements are induced by successive, small reductions in the packing fraction. The experimental results suggest that low-frequency quasilocalized phonon modes in colloidal glasses, i.e., modes that present low energy barriers for system rearrangements, are spatially correlated with rearrangements in this thermal system.

Nanoparticle formation of deposited Agn-clusters on free-standing graphene

NASA Astrophysics Data System (ADS)

Al-Hada, M.; Peters, S.; Gregoratti, L.; Amati, M.; Sezen, H.; Parisse, P.; Selve, S.; Niermann, T.; Berger, D.; Neeb, M.; Eberhardt, W.

2017-11-01

Size-selected Agn-clusters on unsupported graphene of a commercial Quantifoil sample have been investigated by surface and element-specific techniques such as transmission electron microscopy (TEM), spatially-resolved inner-shell X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). An agglomeration of the highly mobile clusters into nm-sized Ag-nanodots of 2-3 nm is observed. Moreover, crystalline as well as non-periodic fivefold symmetric structures of the Ag-nanoparticles are evident by high-resolution TEM. Using a lognormal size-distribution as revealed by TEM, the measured positive binding energy shift of the air-exposed Ag-nanodots can be explained by the size-dependent dynamical liquid-drop model.

Occupational and genetic risk factors associated with intervertebral disc disease.

PubMed

Virtanen, Iita M; Karppinen, Jaro; Taimela, Simo; Ott, Jürg; Barral, Sandra; Kaikkonen, Kaisu; Heikkilä, Olli; Mutanen, Pertti; Noponen, Noora; Männikkö, Minna; Tervonen, Osmo; Natri, Antero; Ala-Kokko, Leena

2007-05-01

Cross-sectional epidemiologic study. To evaluate the interaction between known genetic risk factors and whole-body vibration for symptomatic intervertebral disc disease (IDD) in an occupational sample. Risk factors of IDD include, among others, whole-body vibration and heredity. In this study, the importance of a set of known genetic risk factors and whole-body vibration was evaluated in an occupational sample of train engineers and sedentary controls. Eleven variations in 8 genes (COL9A2, COL9A3, COL11A2, IL1A, IL1B, IL6, MMP-3, and VDR) were genotyped in 150 male train engineers with an average of 21-year exposure to whole-body vibration and 61 male paper mill workers with no exposure to vibration. Subjects were classified into IDD-phenotype and asymptomatic groups, based on the latent class analysis. The number of individuals belonging to the IDD-phenotype was significantly higher among train engineers (42% of train engineers vs. 17.5% of sedentary workers; P = 0.005). IL1A -889T allele represented a significant risk factor for the IDD-phenotype both in the single marker allelic association test (P = 0.043) and in the logistic regression analysis (P = 0.01). None of the other allele markers was significantly associated with symptoms when analyzed independently. However, for all the SNP markers considered, whole-body vibration represents a nominally significant risk factor. The results suggest that whole-body vibration is a risk factor for symptomatic IDD. Moreover, whole-body vibration had an additive effect with genetic risk factors increasing the likelihood of belonging to the IDD-phenotype group. Of the independent genetic markers, IL1A -889T allele had strongest association with IDD-phenotype.

Harnessing data structure for recovery of randomly missing structural vibration responses time history: Sparse representation versus low-rank structure

NASA Astrophysics Data System (ADS)

Yang, Yongchao; Nagarajaiah, Satish

2016-06-01

Randomly missing data of structural vibration responses time history often occurs in structural dynamics and health monitoring. For example, structural vibration responses are often corrupted by outliers or erroneous measurements due to sensor malfunction; in wireless sensing platforms, data loss during wireless communication is a common issue. Besides, to alleviate the wireless data sampling or communication burden, certain accounts of data are often discarded during sampling or before transmission. In these and other applications, recovery of the randomly missing structural vibration responses from the available, incomplete data, is essential for system identification and structural health monitoring; it is an ill-posed inverse problem, however. This paper explicitly harnesses the data structure itself-of the structural vibration responses-to address this (inverse) problem. What is relevant is an empirical, but often practically true, observation, that is, typically there are only few modes active in the structural vibration responses; hence a sparse representation (in frequency domain) of the single-channel data vector, or, a low-rank structure (by singular value decomposition) of the multi-channel data matrix. Exploiting such prior knowledge of data structure (intra-channel sparse or inter-channel low-rank), the new theories of ℓ1-minimization sparse recovery and nuclear-norm-minimization low-rank matrix completion enable recovery of the randomly missing or corrupted structural vibration response data. The performance of these two alternatives, in terms of recovery accuracy and computational time under different data missing rates, is investigated on a few structural vibration response data sets-the seismic responses of the super high-rise Canton Tower and the structural health monitoring accelerations of a real large-scale cable-stayed bridge. Encouraging results are obtained and the applicability and limitation of the presented methods are discussed.

Carbonyl iron powder surface modification of magnetorheological elastomers for vibration absorbing application

NASA Astrophysics Data System (ADS)

Chen, Dong; Yu, Miao; Zhu, Mi; Qi, Song; Fu, Jie

2016-11-01

With excellent characteristic of magnetic-control stiffness, magnetorheological elastomer (MRE) is well suited as a spring element of vibration absorber. To improve the vibration attenuation performance of MRE vibration absorbers, this paper expects to improve the mechanical strength and reduce the loss factor of MRE by interface modification. The surface of carbonyl iron powder (CIP) was modified with silica coating by a simple and convenient approach. Several MRE samples, with different proportions of modified CIPs were fabricated under a constant magnetic field. The morphology and composition of modified CIP were characterized by scanning electron microscope and Fourier transform infrared spectra. The results indicated that the modified CIPs were coated with uniform and continuous silica, which can make a better combination between particle and matrix. The tensile strength, magnetorheological properties and the damping properties of the MRE samples were tested by material testing machine and rheometer. The experimental results demonstrated that the loss factor of the MRE which incorporated with modified CIPs decreased markedly, and the tensile strength of such material has been much improved, at the same time this kind of MRE kept high MR effect. It is expected that this MRE material will meet the requirements of vibration absorber.

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.

Structure, microstructure, and size dependent catalytic properties of nanostructured ruthenium dioxide

NASA Astrophysics Data System (ADS)

Nowakowski, Pawel; Dallas, Jean-Pierre; Villain, Sylvie; Kopia, Agnieszka; Gavarri, Jean-Raymond

2008-05-01

Nanostructured powders of ruthenium dioxide RuO 2 were synthesized via a sol gel route involving acidic solutions with pH varying between 0.4 and 4.5. The RuO 2 nanopowders were characterized by X-ray diffraction, scanning and transmission electron microscopy (SEM and TEM). Rietveld refinement of mean crystal structure was performed on RuO 2 nanopowders and crystallized standard RuO 2 sample. Crystallite sizes measured from X-ray diffraction profiles and TEM analysis varied in the range of 4-10 nm, with a minimum of crystallite dimension for pH=1.5. A good agreement between crystallite sizes calculated from Williamson Hall approach of X-ray data and from direct TEM observations was obtained. The tetragonal crystal cell parameter (a) and cell volumes of nanostructured samples were characterized by values greater than the values of standard RuO 2 sample. In addition, the [Ru-O 6] oxygen octahedrons of rutile structure also depended on crystal size. Catalytic conversion of methane by these RuO 2 nanostructured catalysts was studied as a function of pH, catalytic interaction time, air methane composition, and catalysis temperature, by the way of Fourier transform infrared (FTIR) spectroscopy coupled to homemade catalytic cell. The catalytic efficiency defined as FTIR absorption band intensities I(CO 2) was maximum for sample prepared at pH=1.5, and mainly correlated to crystallite dimensions. No significant catalytic effect was observed from sintered RuO 2 samples.

Vibration-induced particle formation during yogurt fermentation - Industrial vibration measurements and development of an experimental setup.

PubMed

Körzendörfer, Adrian; Temme, Philipp; Nöbel, Stefan; Schlücker, Eberhard; Hinrichs, Jörg

2016-07-01

The aim of the study was to investigate the effects of vibrations during yogurt fermentation. Machinery such as pumps and switching valves generate vibrations that may disturb the gelation by inducing large particles. Oscillation measurements on an industrial yogurt production line showed that oscillations are transferred from pumps right up to the fermentation tanks. An experimental setup (20L) was developed to study the effect of vibrations systematically. The fermenters were decoupled with air springs to enable reference fermentations under idle conditions. A vibration exciter was used to stimulate the fermenters. Frequency sweeps (25-1005Hz, periodic time 10s) for 20min from pH5.4 induced large particles. The number of visible particles was significantly increased from 35±4 (reference) to 89±9 particles per 100g yogurt. Rheological parameters of the stirred yogurt samples were not influenced by vibrations. Copyright © 2016 Elsevier Ltd. All rights reserved.

The Effect of a Short-Term and Long-Term Whole-Body Vibration in Healthy Men upon the Postural Stability

PubMed Central

Piecha, Magdalena; Juras, Grzegorz; Król, Piotr; Sobota, Grzegorz; Polak, Anna; Bacik, Bogdan

2014-01-01

The study aimed to establish the short-term and long-term effects of whole-body vibration on postural stability. The sample consisted of 28 male subjects randomly allocated to four comparative groups, three of which exercised on a vibration platform with parameters set individually for the groups. The stabilographic signal was recorded before the test commenced, after a single session of whole-body vibration, immediately after the last set of exercises of the 4-week whole-body vibration training, and one week after the training ended. The subjects were exposed to vibrations 3 times a week for 4 weeks. Long-term vibration training significantly shortened the rambling and trembling paths in the frontal plane. The path lengths were significantly reduced in the frontal plane one week after the training end date. Most changes in the values of the center of pressure (COP) path lengths in the sagittal and frontal plane were statistically insignificant. We concluded that long-term vibration training improves the postural stability of young healthy individuals in the frontal plane. PMID:24520362

An effective parameter optimization technique for vibration flow field characterization of PP melts via LS-SVM combined with SALS in an electromagnetism dynamic extruder

NASA Astrophysics Data System (ADS)

Xian, Guangming

2018-03-01

A method for predicting the optimal vibration field parameters by least square support vector machine (LS-SVM) is presented in this paper. One convenient and commonly used technique for characterizing the the vibration flow field of polymer melts films is small angle light scattering (SALS) in a visualized slit die of the electromagnetism dynamic extruder. The optimal value of vibration vibration frequency, vibration amplitude, and the maximum light intensity projection area can be obtained by using LS-SVM for prediction. For illustrating this method and show its validity, the flowing material is used with polypropylene (PP) and fifteen samples are tested at the rotation speed of screw at 36rpm. This paper first describes the apparatus of SALS to perform the experiments, then gives the theoretical basis of this new method, and detail the experimental results for parameter prediction of vibration flow field. It is demonstrated that it is possible to use the method of SALS and obtain detailed information on optimal parameter of vibration flow field of PP melts by LS-SVM.

Characterizing Amorphous Silicates in Extraterrestrial Materials

NASA Astrophysics Data System (ADS)

Fu, X.; Wang, A.; Krawczynski, M. J.

2015-12-01

Amorphous silicates are common in extraterrestrial materials. They are seen in the matrix of carbonaceous chondrites as well as in planetary materials. Tagish Lake is one of the most primitive carbonaceous meteorites in which TEM and XRD analyses found evidence for poorly crystalline phyllosilicate-like species; Raman spectra revealed amorphous silicates with variable degree of polymerization and low crystallinity. On Mars, CheMin discovered amorphous phases in all analyzed samples, and poorly crystalline smectite in mudstone samples. These discoveries pose questions on the crystallinity of phyllosilicates found by remote sensing on Mars, which is directly relevant to aqueous alteration during geologic history of Mars. Our goal is to use spectroscopy to better characterize amorphous silicates. We use three approaches: (1) using silicate glasses synthesized with controlled chemistry to study the effects of silicate polymerization and (2) using phyllosilicates synthesized with controlled hydrothermal treatment to study the effect of crystallinity on vibrational spectroscopy, finally (3) to use the developed correlations in above two steps to study amorphous phases in meteorites, and those found in future missions to Mars. In the 1st step, silicate glasses were synthesized from pure oxides in a range of NBO/T ratios (from 0 to 4). Depending on the targeted NBO/T and composition of mixed oxides, temperatures for each experiment fell in a range from 1260 to 1520 °C, run for ~ 4 hrs. The melt was quenched in liquid N2 or water. Homogeneity of glass was checked under optical microscopy. Raman spectra were taken over 100 spots on small chips free of bubbles and crystals. We have observed that accompanying an increase of NBO/T, there is a strengthening and a position shift of the Raman peak near 1000 cm-1 (Si-Onon-bridging stretching mode), and the weakening of broad Raman peaks near 500 cm-1 (ring breathing mode) and 700cm-1 (Si-Obridging-Si mode). We are building the correlation between peak area ratio, A(500+700)/A1000, and NBO/T. In the 2nd step, we are synthesizing Mg-saponite using a sol-gel method. The crystallinity of sol-gel starting materials will be increased by a controlled hydrothermal treatment. The products will be characterized using XRD/TEM/Raman/NIR. The results will be reported at the conference.

Physics of Radiation Exposure and Characterization for Future Electronic Materials

DTIC Science & Technology

2014-12-01

TEM probe. These visits have included an invited talk at the Annual User’s Meeting at BNL in which the DTRA project was highlighted. • Columbia...at PNNL. • Columbia graduate student Luozhou Li was trained by BNL researchers Dr. Ming Lu on nanofabrication techniques related to the fabrication...Jacob Mower were trained by BNL researcher Kim Kisslinger on diamond membrane fabrication and TEM cross-section sample fabrication. • Columbia

Lights Will Guide You : Sample Preparation and Applications for Integrated Laser and Electron Microscopy

NASA Astrophysics Data System (ADS)

Karreman, M. A.

2013-03-01

Correlative microscopy is the combined use of two different forms of microscopy in the study of a specimen, allowing for the exploitation of the advantages of both imaging tools. The integrated Laser and Electron Microscope (iLEM), developed at Utrecht University, combines a fluorescence microscope (FM) and a transmission electron microscope (TEM) in a single set-up. The region of interest in the specimen is labeled or tagged with a fluorescent probe and can easily be identified within a large field of view with the FM. Next, this same area is retraced in the TEM and can be studied at high resolution. The iLEM demands samples that can be imaged with both FM and TEM. Biological specimen, typically composed of light elements, generate low image contrast in the TEM. Therefore, these samples are often ‘contrasted’ with heavy metal stains. FM, on the other hand, images fluorescent samples. Sample preparation for correlative microscopy, and iLEM in particular, is complicated by the fact that the heavy metals stains employed for TEM quench the fluorescent signal of the probe that is imaged with FM. The first part of this thesis outlines preparation procedures for biological material yielding specimen that can be imaged with the iLEM. Here, approaches for the contrasting of thin sections of cells and tissue are introduced that do not affect the fluorescence signal of the probe that marks the region of interest. Furthermore, two novel procedures, VIS2FIXH and VIS2FIX­FS are described that allow for the chemical fixation of thin sections of cryo-immobilized material. These procedures greatly expedite the sample preparation process, and open up novel possibilities for the immuno-labeling of difficult antigens, eg. proteins and lipids that are challenging to preserve. The second part of this thesis describes applications of iLEM in research in the field of life and material science. The iLEM was employed in the study of UVC induced apoptosis (programmed cell death) of human umbilical vein endothelial cells. A novel, RNA containing body was identified in the nuclei of cells going through the various stages of the apoptotic process. Furthermore, we demonstrated the potential of iLEM in the study of Facio Scapulo Humeral Dystrophy (FSHD), the third most common form of inherited muscular dystrophy. In this study, diseased cells are identified based on the immuno-labeling of proteins associated with FSHD pathology. In the field of heterogeneous catalysis, a structural and functional characterization of Fluid Catalytic Cracking (FCC) particles was performed with iLEM. FCC particles are employed in petrochemical industry, where they catalyze the breakdown of large molecules in crude oil fractions into functional products with lower molecular weight, like gasoline. The catalytic sites in the FCC particles were selectively stained with a fluorescent probe, and next their structure was investigated with TEM. The iLEM allowed for the identification and characterization of catalytically active areas in the FCC particles. Furthermore, a unique study of the deactivation processes taking place in an industrial FCC unit was performed by analyzing a sample derived from a FCC reactor

Anharmonic Vibrational Analyses of Pentapeptide Conformations Explored with Enhanced Sampling Simulations.

PubMed

Otaki, Hiroki; Yagi, Kiyoshi; Ishiuchi, Shun-Ichi; Fujii, Masaaki; Sugita, Yuji

2016-10-06

An accurate theoretical prediction of the vibrational spectrum of polypeptides remains to be a challenge due to (1) their conformational flexibility and (2) non-negligible anharmonic effects. The former makes the search for conformers that contribute to the spectrum difficult, and the latter requires an expensive, quantum mechanical calculation for both electrons and vibrations. Here, we propose a new theoretical approach, which implements an enhanced conformational sampling by the replica-exchange molecular dynamics method, a structural clustering to identify distinct conformations, and a vibrational structure calculation by the second-order vibrational quasi-degenerate perturbation theory (VQDPT2). A systematic mode-selection scheme is developed to reduce the cost of VQDPT2 and the generation of a potential energy surface by the electronic structure calculation. The proposed method is applied to a pentapeptide, SIVSF-NH 2 , for which the infrared spectrum has recently been measured in the gas phase with high resolution in the OH and NH stretching region. The theoretical spectrum of the lowest energy conformer is obtained with a mean absolute deviation of 11.2 cm -1 from the experimental spectrum. Furthermore, the NH stretching frequencies of the five lowest energy conformers are found to be consistent with the literature values measured for small peptides with a similar secondary structure. Therefore, the proposed method is a promising way to analyze the vibrational spectrum of polypeptides.

Whole-body vibration exposure of haul truck drivers at a surface coal mine.

PubMed

Wolfgang, Rebecca; Burgess-Limerick, Robin

2014-11-01

Haul truck drivers at surface mines are exposed to whole-body vibration for extended periods. Thirty-two whole-body vibration measurements were gathered from haul trucks under a range of normal operating conditions. Measurements taken from 30 of the 32 trucks fell within the health guidance caution zone defined by ISO2631-1 for an 8 h daily exposure suggesting, according to ISO2631-1, that "caution with respect to potential health risks is indicated". Maintained roadways were associated with substantially lower vibration amplitudes. Larger trucks were associated with lower vibration levels than small trucks. The descriptive nature of the research, and small sample size, prevents any strong conclusion regarding causal links. Further investigation of the variables associated with elevated vibration levels is justified. The operators of mining equipment such as haul trucks are exposed to whole-body vibration amplitudes which have potential to lead to long term health effects. Systematic whole-body vibration measurements taken at frequent intervals are required to provide an understanding of the causes of elevated vibration levels and hence determine appropriate control measures. Copyright © 2014 Elsevier Ltd and The Ergonomics Society. All rights reserved.

Nuclear Resonance Vibrational Spectra of Five-Coordinate Imidazole-ligated Iron(II) Porphyrinates

PubMed Central

Hu, Chuanjiang; Barabanschikov, Alexander; Ellison, Mary K.; Zhao, Jiyong; Alp, E. Ercan; Sturhahn, Wolfgang; Zgierski, Marek Z.; Sage, J. Timothy; Scheidt, W. Robert

2012-01-01

Nuclear resonance vibrational spectra have been obtained for six five-coordinate imidazole-ligated iron(II) porphyrinates, [Fe(Por)(L)] (Por = tetraphenylporphyrinate, octaethylporphyrinate, tetratolylporphyrinate or protoporphyrinate IX and L = 2-methylimidazole or 1,2-dimethylimidazole). Measurements have been made on both powder and oriented crystal samples. The spectra are dominated by strong signals around 200–300 cm−1. Although the in-plane and out-of-plane vibrations are seriously overlapped, oriented crystal spectra allow their deconvolution. Thus, oriented crystal experimental data, along with DFT calculations, enable the assignment of key vibrations in the spectra. Molecular dynamics are also discussed. The nature of the Fe–NIm vibrations has been elaborated further than was possible from resonance Raman studies. Our study suggests that the Fe motions are coupled with the porphyrin core and peripheral groups motions. Both peripheral groups and their conformations have significant influence on the vibrational spectra (position and shape). PMID:22243131

Analytical design and evaluation of an active control system for helicopter vibration reduction and gust response alleviation

NASA Technical Reports Server (NTRS)

Taylor, R. B.; Zwicke, P. E.; Gold, P.; Miao, W.

1980-01-01

An analytical study was conducted to define the basic configuration of an active control system for helicopter vibration and gust response alleviation. The study culminated in a control system design which has two separate systems: narrow band loop for vibration reduction and wider band loop for gust response alleviation. The narrow band vibration loop utilizes the standard swashplate control configuration to input controller for the vibration loop is based on adaptive optimal control theory and is designed to adapt to any flight condition including maneuvers and transients. The prime characteristics of the vibration control system is its real time capability. The gust alleviation control system studied consists of optimal sampled data feedback gains together with an optimal one-step-ahead prediction. The prediction permits the estimation of the gust disturbance which can then be used to minimize the gust effects on the helicopter.

Biomolecular Imaging with Coherent Nonlinear Vibrational Microscopy

PubMed Central

Chung, Chao-Yu; Boik, John; Potma, Eric O.

2014-01-01

Optical imaging with spectroscopic vibrational contrast is a label-free solution for visualizing, identifying, and quantifying a wide range of biomolecular compounds in biological materials. Both linear and nonlinear vibrational microscopy techniques derive their imaging contrast from infrared active or Raman allowed molecular transitions, which provide a rich palette for interrogating chemical and structural details of the sample. Yet nonlinear optical methods, which include both second-order sum-frequency generation (SFG) and third-order coherent Raman scattering (CRS) techniques, offer several improved imaging capabilities over their linear precursors. Nonlinear vibrational microscopy features unprecedented vibrational imaging speeds, provides strategies for higher spatial resolution, and gives access to additional molecular parameters. These advances have turned vibrational microscopy into a premier tool for chemically dissecting live cells and tissues. This review discusses the molecular contrast of SFG and CRS microscopy and highlights several of the advanced imaging capabilities that have impacted biological and biomedical research. PMID:23245525

A method for the measurement and analysis of ride vibrations of transportation systems

NASA Technical Reports Server (NTRS)

Catherines, J. J.; Clevenson, S. A.; Scholl, H. F.

1972-01-01

The measurement and recording of ride vibrations which affect passenger comfort in transportation systems and the subsequent data-reduction methods necessary for interpreting the data present exceptional instrumentation requirements and necessitate the use of computers for specialized analysis techniques. A method is presented for both measuring and analyzing ride vibrations of the type encountered in ground and air transportation systems. A portable system for measuring and recording low-frequency, low-amplitude accelerations and specialized data-reduction procedures are described. Sample vibration measurements in the form of statistical parameters representative of typical transportation systems are also presented to demonstrate the utility of the techniques.

Microvibration and Centre-of-Gravity Shift Measurements on Thermally Stressed Thermal-Control Blankets

NASA Astrophysics Data System (ADS)

Magg, Manfred; Grillenbeck, Anton, , Dr.

2004-08-01

Several samples of thermal control blankets were subjected to transient thermal loads in a thermal vacuum chamber in order to study their ability to excite micro- vibrations on a carrier structure and to cause tiny centre- of-gravity shifts. The reason for this investigation was driven by the GOCE project in order to minimize micro- vibrations on-board of the spacecraft while on-orbit. The objectives of this investigation were to better understand the mechanism which may produce micro- vibrations induced by the thermal control blankets, and to identify thermal control blanket lay-ups with minimum micro-vibration activity.

Strains on the nano- and microscale in nickel-titanium: An advanced TEM study

NASA Astrophysics Data System (ADS)

Tirry, Wim

2007-12-01

A general introduction to shape memory behavior and the martensitic transformation is given in chapter 1, with speck information concerning the NiTi material. The technique used to study the material is transmission electron microscopy (TEM) of which the basics are explained in chapter 2 as well as information concerning the NiTi material. The main goal was to apply more advanced TEM techniques in order to measure some aspects in a quantitative way rather than qualitative, which is mostly the case in conventional TEM. (1) Quantitative electron diffraction was used to refine the structure of Ni4Ti3 precipitates, this was done by using the MSLS method in combination with density functional theory (DFT) calculations. (2) These Ni4Ti3 precipitates are (semi-)coherent which results in a strain field in the matrix close to the precipitate. High resolution TEM (HRTEM) in combination with image processing techniques was used to measure these strain fields. The obtained results are compared to the Eshelby model for elliptical inclusions, and major difference is an underestimation of the strain magnitude by the model. One of the algorithms used to extract strain information from HRTEM images is the geometric phase method. (3) The Ni4Ti3-Ni4Ti3 and Ni4Ti3-precipitate interface was investigated with HRTEM showing that the Ni4Ti3-precipitate interface might be diffuse over a range of 3nm. (4) In-situ straining experiments were performed on single crystalline and superelastic polycrystalline NiTi samples. It seems that the strain induced martensite planes in the polycrystalline sample show no sign of twinning. This is in contradiction to what is expected and is discussed in the view of the crystallographic theory of martensite, in addition a first model explaining this behavior is proposed. In this dissertation the main attention is divided over the material aspects of NiTi and on how to apply these more advanced TEM techniques.

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

NASA Astrophysics Data System (ADS)

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

2015-01-01

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

Changes in microstructure and physical properties of skutterudites after severe plastic deformation.

PubMed

Rogl, Gerda; Grytsiv, Andriy; Bursik, Jiri; Horky, Jelena; Anbalagan, Ramakrishnan; Bauer, Ernst; Mallik, Ramesh Chandra; Rogl, Peter; Zehetbauer, Michael

2015-02-07

The best p-type skutterudites with ZT > 1.1 so far are didymium (DD) filled, Fe/Co substituted, Sb-based skutterudites. DD0.68Fe3CoSb12 was prepared using an annealing-reacting-melting-quenching technique followed by ball milling and hot pressing. After severe plastic deformation via high-pressure torsion (HPT), no phase changes but particular structural variations were achieved, leading to modified transport properties with higher ZT values. Although after measurement-induced heating some of the HPT induced defects were annealed out, a still attractive ZT-value was preserved. In this paper we focus on explanations for these changes via TEM investigations, Raman spectroscopy and texture measurements. The grain sizes and dislocation densities, evaluated from TEM images, showed that (i) the majority of cracks generated during high-pressure torsion are healed during annealing, leaving only small pores, that (ii) the grains have grown, and that (iii) the dislocation density is decreased. While Raman spectra indicate that after HPT processing and annealing the vibration modes related to the shorter Sb-Sb bonds in the Sb4 rings are more affected than those related to the longer Sb-Sb bonds, almost no visible changes were observed in the pole intensity and/or orientation.

Synthesis and characterization of monosodium urate (MSU) nano particles

NASA Astrophysics Data System (ADS)

Tank, Nirali S.; Rathod, K. R.; Parekh, B. B.; Parikh, K. D.; Joshi, M. J.

2016-05-01

In Gout the deposition of crystals of Monosodium Urate (MSU) in various connective tissues and joints occurs, which is very painful with immflamation. The deposition likely to begin with nano particles form and expected to grow in to micro-paricles and hence it is important to synthesize and characrterize MSU nano-particles. The MSU nano particles were synthesized by wet chemical method using NaOH and uric acid (C5H4N4O3) and then characterized by powder XRD, TEM, FT-IR and thermal analysis. From the powder XRD the triclinic structure was found and 40 nm average particle size was estimated by using Scherrer's formula. From TEM the particle size was found to be in the range of 20 to 60 nm. The FT-IR spectrum for the MSU nano particles confirmed the presence of O-H stretching, N-H stretching, N-H rocking, C = O, C = C Enol or Keto and C = N vibrations. The thermal analysis was carried out from room temperature to 900°C. With comparison to the bulk MSU the thermal stability of MSU nano particles was slightly higher and 1.5 water molecules were found to be associated with MSU nano particles. Present results are compared with the bulk MSU.

Highly Transparent Wafer-Scale Synthesis of Crystalline WS2 Nanoparticle Thin Film for Photodetector and Humidity-Sensing Applications.

PubMed

Pawbake, Amit S; Waykar, Ravindra G; Late, Dattatray J; Jadkar, Sandesh R

2016-02-10

In the present investigation, we report a one-step synthesis method of wafer-scale highly crystalline tungsten disulfide (WS2) nanoparticle thin film by using a modified hot wire chemical vapor deposition (HW-CVD) technique. The average size of WS2 nanoparticle is found to be 25-40 nm over an entire 4 in. wafer of quartz substrate. The low-angle XRD data of WS2 nanoparticle shows the highly crystalline nature of sample along with orientation (002) direction. Furthermore, Raman spectroscopy shows two prominent phonon vibration modes of E(1)2g and A1g at ∼356 and ∼420 cm(-1), respectively, indicating high purity of material. The TEM analysis shows good crystalline quality of sample. The synthesized WS2 nanoparticle thin film based device shows good response to humidity and good photosensitivity along with good long-term stability of the device. It was found that the resistance of the films decreases with increasing relative humidity (RH). The maximum humidity sensitivity of 469% along with response time of ∼12 s and recovery time of ∼13 s were observed for the WS2 thin film humidity sensor device. In the case of photodetection, the response time of ∼51 s and recovery time of ∼88 s were observed with sensitivity ∼137% under white light illumination. Our results open up several avenues to grow other transition metal dichalcogenide nanoparticle thin film for large-area nanoelectronics as well as industrial applications.

Synthesis of hydrophilic superparamagnetic magnetite nanoparticles via thermal decomposition of Fe(acac), in 80 vol% TREG + 20 vol% TREM.

PubMed

Maityt, Dipak; Pradhan, Pallab; Chandrasekharan, Prashant; Kale, S N; Shuter, Borys; Bahadur, Dhirendra; Feng, Si-Shen; Xue, Jun-Min; Ding, Jun

2011-03-01

In this paper, we report single step synthesis of hydrophilic superparamagnetic magnetite nanoparticles by thermolysis of Fe(acac)3 and their characterization of the properties relevant to biomedical applications like hyperthermia and magnetic resonance imaging (MRI). Size and morphology of the particles were determined by Transmission electron microscopy (TEM) while phase purity and structure of the particles were identified by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). Magnetic properties were evaluated using vibrating sample magnetometer (VSM) and superconducting quantum interference device (SQUID) measurements. The as prepared nanoparticles were found to be superparamagnetic with the blocking temperature of 136 K and were easily suspendable in water. Cytotoxicity studies on human cervical (SiHa), mouse melanoma (B16F10) and mouse primary fibroblast cells demonstrated that up to a dose of 0.1 mg/ml, the magnetite nanoparticles were nontoxic to the cells. To evaluate the feasibility of their uses in hyperthermia and MRI applications, specific absorption rate (SAR) and spin-spin relaxation time (T2) were measured respectively. SAR has been calculated to be above 80 Watt/g for samples with the iron concentration of 5-20 mg/ml at 10 kA/m AC magnetic field and 425 kHz frequency. r2 relaxivity value was measured as 358.4 mM(-1)S(-1) which is almost double as compared to that of the Resovist, a commercially available MRI contrast agent. Thus the as-prepared magnetite nanoparticles may be used for hyperthermia and MRI applications due to their promising SAR and r2 values.

Role of reduced precursor and solvolytic reagent molar ratio on preparation and properties of ionogel

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

Gupta, Abhishek Kumar; Verma, Yogendra Lal; Singh, Manish Pratap

In the present study, ionogels have been synthesized by immobilizing IL (1-ethyl-3-methylimidazolium tetrafluoroborate) in silica gel matrices using non-aqueous route. In this process, tetraethyl orho-silane (TEOS) as a precursor to silicon dioxide and formic acid as a solvolytic gelating reagent in reduced molar ratio 1:4 were used. We find that reduced molar concentration of formic acid results the formation of ionogels having less number of closed pores (totally isolated from their neighbours), larger density and stable monolithic form. TEM and SEM measurements are used to visualize the morphology of sample and closed pores present in the sample. N{sub 2}-sorption measurementmore » is used to measure the pore parameters of the silica matrices which shows the mesoporous structure. DSC and TGA results show the change in phase transition temperature and thermal stability of IL upon confinement in silica matrices. Moreover, ionic conductivity of bulk and confined IL is measured using impedance spectroscopy and it has been found that it increases with increasing the temperature as well as concentration of IL in ionogels. Apart from these characterization techniques, ionogels have been characterized using FTIR and fluorescence spectroscopy which exhibit the change in vibrational frequencies and fluorescence behaviour of confined IL. - Highlights: • Synthesis of stable ionogel using non-hydrolytic route with reduced precursor and solvolytic reagent molar ratio. • Ionogels are free from entrapped residual reaction product. • The ionogels synthesized with higher amount of ionic liquids show bulk liquid like electrical behaviour.« less

Ultrasound-assisted fabrication of a biocompatible magnetic hydroxyapatite.

PubMed

Zhou, Gang; Song, Wei; Hou, Yongzhao; Li, Qing; Deng, Xuliang; Fan, Yubo

2014-10-01

This work describes the fabrication and characterization of a biocompatible magnetic hydroxyapatite (HA) using an ultrasound-assisted co-precipitation method. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and transmission electron microscopy (TEM) were used to characterize the structure and chemical composition of the produced samples. The M-H loops of synthesized materials were traced using a vibrating sample magnetometer (VSM) and the biocompatibility was evaluated by cell culture and MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay. Furthermore, in vivo histopathological examinations were used to evaluate the potential toxicological effects of Fe₃O₄-HA composites on kidney of SD rats injected intraperitoneally with Fe₃O₄-HA particles. The results showed that magnetic iron oxide particles first replace OH ions of HA, which are parallel to the c axis, and then enter the HA crystal lattice which produces changes in the crystal surface of HA. Chemical bond interaction was observed between PO₄³⁻ groups of HA and iron ions of Fe₃O₄. The saturation magnetization (MS ) of Fe₃O₄-HA composites was 46.36 emu/g obtained from VSM data. Cell culture and MTT assays indicated that HA could affect the growth and proliferation of HEK-293 cells. This Fe₃O₄-HA composite produced no negative effects on cell morphology, viability, and proliferation and exhibited remarkable biocompatibility. Moreover, no inflammatory cell infiltration was observed in kidney histopathology slices. Therefore, this study succeeds to develop a Fe₃O₄-HA composite as a prospective biomagnetic material for future applications. © 2013 Wiley Periodicals, Inc.

The influence of PEG-4000 and silica on crystal structure and magnetic properties of magnesium ferrite (MgFe{sub 2}O{sub 4}) nanoparticles

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

Puspitarum, Deska Lismawenning; Hermawan, Agung; Suharyadi, Edi, E-mail: esuharyadi@ugm.ac.id

2016-04-19

In this paper, reports the influence of polyethylene glycol (PEG-4000) and silica on crystal structure and magnetic properties of MgFe{sub 2}O{sub 4} nanoparticles which is synthesized by the co-precipitation method. The particle size of before coated MgFe{sub 2}O{sub 4} was around 10.5 nm, and became 5.2 nm after PEG-4000 coating and 18.8 nm after silica coating. After coating, there were appeared new phases, α-Fe{sub 2}O{sub 3} (antiferromagnetic), SiO{sub 2} and γ-FeO(OH) which are paramagnetics. The second phase sample decreased responses to the external field. Transmission Electron Microscopy (TEM) morphology analysis on nanoparticles which was coated with PEG 4000 showed that the particles becomemore » more spherical, more dispersive, and less aglomerated. The magnetic hysteresis loops which was investigated with Vibrating Sample Magnetometer (VSM) indicated that coercivity of MgFe{sub 2}O{sub 4} was 120.7 Oe, and then decreased to 40.9 Oe after coating and 34.7 Oe for coating with PEG-4000 and silica, respectively. At 15 kOe, the magnetization value decreased from 2.69 emu/g to 0.96 emu/g after coating with PEG-4000 and increased 2.82 emu/g after silica coating. The result revealed the coating with both PEG-4000 and silica influence the magnetic properties of MgFe{sub 2}O{sub 4} nanoparticles.« less

Dynamic effect in ultrasonic assisted micro-upsetting

NASA Astrophysics Data System (ADS)

Presz, Wojciech

2018-05-01

The use of ultrasonic assistance in microforming is becoming more and more popular. Mainly due to the beneficial effect of vibrations on the flow of plastic deformation reported already in the 50s of the last century. The influence is of two types: surface and volume. The surface effect is mainly the reduction of friction forces, and volumetric is the impact on the dislocation movement and even on phase transitions. The work focuses on the dynamic aspect of vibration assisted microforming. The use of ultrasonic vibrations at a frequency of 20 kHz and an amplitude of 16 µm, in the micro-upsetting process of an aluminum sample resulted in a high concentration of strain on both ends of the sample - at 14% of the height on both sides. There was observed (in relation to deformations of the sample without vibrations) 150-250% increase and a 50% decrease in strain in the center of the sample. At the same time, the larger deformations occurred from the impact side of the punch. Analyzing the course of forces of the upsetting process in the loading and unloading phase as well as the process of breaking glass samples, the spring deflections of key system elements and their natural frequencies were determined or calculated. Based on the determined or calculated parameters of the test stand, it was shown that during the micro-upsetting process the punch may detach from the sample surface and this is the main reason for the phenomena occurring. Detach of the punch is also the cause of the observed instability of the measurement of force, which should be considered unbelievable in such a situation.

Characterization of Train-Induced Vibration and its Effect on Fecal Corticosterone Metabolites in Mice

PubMed Central

Atanasov, Nicholas A; Sargent, Jennifer L; Parmigiani, John P; Palme, Rupert; Diggs, Helen E

2015-01-01

Excessive environmental vibrations can have deleterious effects on animal health and experimental results, but they remain poorly understood in the animal laboratory setting. The aims of this study were to characterize train-associated vibration in a rodent vivarium and to assess the effects of this vibration on the reproductive success and fecal corticosterone metabolite levels of mice. An instrumented cage, featuring a high-sensitivity microphone and accelerometer, was used to characterize the vibrations and sound in a vivarium that is near an active railroad. The vibrations caused by the passing trains are 3 times larger in amplitude than are the ambient facility vibrations, whereas most of the associated sound was below the audible range for mice. Mice housed in the room closest to the railroad tracks had pregnancy rates that were 50% to 60% lower than those of mice of the same strains but bred in other parts of the facility. To verify the effect of the train vibrations, we used a custom-built electromagnetic shaker to simulate the train-induced vibrations in a controlled environment. Fecal pellets were collected from male and female mice that were exposed to the simulated vibrations and from unexposed control animals. Analysis of the fecal samples revealed that vibrations similar to those produced by a passing train can increase the levels of fecal corticosterone metabolites in female mice. These increases warrant attention to the effects of vibration on mice and, consequently, on reproduction and experimental outcomes. PMID:26632783

Characterization of Train-Induced Vibration and its Effect on Fecal Corticosterone Metabolites in Mice.

PubMed

Atanasov, Nicholas A; Sargent, Jennifer L; Parmigiani, John P; Palme, Rupert; Diggs, Helen E

2015-11-01

Excessive environmental vibrations can have deleterious effects on animal health and experimental results, but they remain poorly understood in the animal laboratory setting. The aims of this study were to characterize train-associated vibration in a rodent vivarium and to assess the effects of this vibration on the reproductive success and fecal corticosterone metabolite levels of mice. An instrumented cage, featuring a high-sensitivity microphone and accelerometer, was used to characterize the vibrations and sound in a vivarium that is near an active railroad. The vibrations caused by the passing trains are 3 times larger in amplitude than are the ambient facility vibrations, whereas most of the associated sound was below the audible range for mice. Mice housed in the room closest to the railroad tracks had pregnancy rates that were 50% to 60% lower than those of mice of the same strains but bred in other parts of the facility. To verify the effect of the train vibrations, we used a custom-built electromagnetic shaker to simulate the train-induced vibrations in a controlled environment. Fecal pellets were collected from male and female mice that were exposed to the simulated vibrations and from unexposed control animals. Analysis of the fecal samples revealed that vibrations similar to those produced by a passing train can increase the levels of fecal corticosterone metabolites in female mice. These increases warrant attention to the effects of vibration on mice and, consequently, on reproduction and experimental outcomes.

A simple way to obtain backscattered electron images in a scanning transmission electron microscope.

PubMed

Tsuruta, Hiroki; Tanaka, Shigeyasu; Tanji, Takayoshi; Morita, Chiaki

2014-08-01

We have fabricated a simple detector for backscattered electrons (BSEs) and incorporated the detector into a scanning transmission electron microscope (STEM) sample holder. Our detector was made from a 4-mm(2) Si chip. The fabrication procedure was easy, and similar to a standard transmission electron microscopy (TEM) sample thinning process based on ion milling. A TEM grid containing particle objects was fixed to the detector with a silver paste. Observations were carried out using samples of Au and latex particles at 75 and 200 kV. Such a detector provides an easy way to obtain BSE images in an STEM. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Three-Dimensional Solution of the Free Vibration Problem for Metal-Ceramic Shells Using the Method of Sampling Surfaces

NASA Astrophysics Data System (ADS)

Kulikov, G. M.; Plotnikova, S. V.

2017-03-01

The possibility of using the method of sampling surfaces (SaS) for solving the free vibration problem of threedimensional elasticity for metal-ceramic shells is studied. According to this method, in the shell body, an arbitrary number of SaS parallel to its middle surface are selected in order to take displacements of these surfaces as unknowns. The SaS pass through the nodes of a Chebyshev polynomial, which improves the convergence of the SaS method significantly. As a result, the SaS method can be used to obtain analytical solutions of the vibration problem for metal-ceramic plates and cylindrical shells that asymptotically approach the exact solutions of elasticity as the number of SaS tends to infinity.

An electron energy loss spectrometer based streak camera for time resolved TEM measurements.

PubMed

Ali, Hasan; Eriksson, Johan; Li, Hu; Jafri, S Hassan M; Kumar, M S Sharath; Ögren, Jim; Ziemann, Volker; Leifer, Klaus

2017-05-01

We propose an experimental setup based on a streak camera approach inside an energy filter to measure time resolved properties of materials in the transmission electron microscope (TEM). In order to put in place the streak camera, a beam sweeper was built inside an energy filter. After exciting the TEM sample, the beam is swept across the CCD camera of the filter. We describe different parts of the setup at the example of a magnetic measurement. This setup is capable to acquire time resolved diffraction patterns, electron energy loss spectra (EELS) and images with total streaking times in the range between 100ns and 10μs. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

High-Resolution AES Mapping and TEM Study of Cu(In,Ga)Se2 Thin Film Growth: Preprint

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

Perkins, C. L.; Yan, Y.; Jones, K.

2001-10-01

Presented at 2001 NCPV Program Review Meeting: TEM and high-resolution AES mapping data on CIGS samples. The chalcopyrite Cu(In,Ga)Se{sub 2} (CIGS) shows promise as an absorber layer in thin polycrystalline solar cells, however, details of the PVD growth of this complicated material remain in a developing stage. Previous workers have postulated the existence of a thin film of liquid Cu{sub x}Se on the growing CIGS film, and that this layer acts as a reservoir of copper as well as a layer in which rapid mass transport is possible. In this paper we present transmission electron microscopy (TEM) and high resolutionmore » Auger electron spectroscopy (AES) mapping data taken on samples that had their growth interrupted at a stage when Cu{sub x}Se was expected to be present. The AES maps show CIGS grains which are highly enriched in copper relative to the rest of the CIGS film, and that these same areas contain almost no indium, results consistent with the presence of CuxSe. Small-area diffraction analysis and energy dispersive spectroscopy (EDS) performed on these same samples independently confirm the presence of Cu{sub x}Se at the surface of growing CIGS films.« less

Whole-body vibration and blood flow and muscle oxygenation: a meta-analysis.

PubMed

Games, Kenneth E; Sefton, JoEllen M; Wilson, Alan E

2015-05-01

The use and popularity of whole-body vibration (WBV) has increased in recent years, but there is a lack of consensus in the literature about the effectiveness of the treatment. To quantitatively examine the effects of WBV on muscle oxygenation and peripheral blood flow in healthy adults. We searched Web of Science and PubMed databases and reference lists from relevant articles using the key terms whole body vibration, whole-body vibration, WBV, blood flow, peripheral blood flow, oxygenation, muscle oxygenation, circulation, circulatory, near infrared spectroscopy, NIRS, and power Doppler. Key terms were searched using single word and combination searches. No date range was specified. Criteria for inclusion were (1) use of a commercially available WBV device, (2) a human research model, (3) a pre-WBV condition and at least 1 WBV experimental condition, and (4) reporting of unstandardized means and standard deviations of muscle oxygenation or peripheral blood flow. Means, standard deviations, and sample sizes were extracted from the text, tables, and figures of included studies. A total of 35 and 90 data points were extracted for the muscle-oxygenation and blood-flow meta-analyses, respectively. Data for each meta-analysis were combined and analyzed using meta-analysis software. Weighted, random-effects meta-analyses using the Hedges g metric were completed for muscle oxygenation and blood flow. We then conducted follow-up analyses using the moderator variables of vibration type, vibration time, vibration frequency, measurement location, and sample type. We found 18 potential articles. Further examination yielded 10 studies meeting the inclusion criteria. Whole-body vibration was shown to positively influence peripheral blood flow. Additionally, the moderators of vibration type and frequency altered the influence of WBV on blood flow. Overall, WBV did not alter muscle oxygenation; however, when the measurement site was considered, muscle oxygenation increased or decreased depending on the location. Acute bouts of WBV increase peripheral blood flow but do not alter skeletal muscle oxygenation. Vibration type appears to be the most important factor influencing both muscle oxygenation and peripheral blood flow.

Whole-Body Vibration and Blood Flow and Muscle Oxygenation: A Meta-Analysis

PubMed Central

Games, Kenneth E.; Sefton, JoEllen M.; Wilson, Alan E.

2015-01-01

Context: The use and popularity of whole-body vibration (WBV) has increased in recent years, but there is a lack of consensus in the literature about the effectiveness of the treatment. Objective: To quantitatively examine the effects of WBV on muscle oxygenation and peripheral blood flow in healthy adults. Data Sources: We searched Web of Science and PubMed databases and reference lists from relevant articles using the key terms whole body vibration, whole-body vibration, WBV, blood flow, peripheral blood flow, oxygenation, muscle oxygenation, circulation, circulatory, near infrared spectroscopy, NIRS, and power Doppler. Key terms were searched using single word and combination searches. No date range was specified. Study Selection: Criteria for inclusion were (1) use of a commercially available WBV device, (2) a human research model, (3) a pre-WBV condition and at least 1 WBV experimental condition, and (4) reporting of unstandardized means and standard deviations of muscle oxygenation or peripheral blood flow. Data Extraction: Means, standard deviations, and sample sizes were extracted from the text, tables, and figures of included studies. A total of 35 and 90 data points were extracted for the muscle-oxygenation and blood-flow meta-analyses, respectively. Data for each meta-analysis were combined and analyzed using meta-analysis software. Weighted, random-effects meta-analyses using the Hedges g metric were completed for muscle oxygenation and blood flow. We then conducted follow-up analyses using the moderator variables of vibration type, vibration time, vibration frequency, measurement location, and sample type. Data Synthesis: We found 18 potential articles. Further examination yielded 10 studies meeting the inclusion criteria. Whole-body vibration was shown to positively influence peripheral blood flow. Additionally, the moderators of vibration type and frequency altered the influence of WBV on blood flow. Overall, WBV did not alter muscle oxygenation; however, when the measurement site was considered, muscle oxygenation increased or decreased depending on the location. Conclusions: Acute bouts of WBV increase peripheral blood flow but do not alter skeletal muscle oxygenation. Vibration type appears to be the most important factor influencing both muscle oxygenation and peripheral blood flow. PMID:25974682

Magnetic solid phase extraction coupled with inductively coupled plasma mass spectrometry for the speciation of mercury in environmental water and human hair samples.

PubMed

Ma, Shishuai; He, Man; Chen, Beibei; Deng, Wenchao; Zheng, Qi; Hu, Bin

2016-01-01

In this work, γ-mercaptopropyltrimethoxysilane (γ-MPTS) modified Fe3O4@SiO2 magnetic nanoparticles (MNPs) was successfully prepared, and characterized by Fourier transform infrared spectrometer (FT-IR), Transmission electron microscope (TEM) and Vibrating sample magnetometer (VSM). The sorption performance of the prepared Fe3O4@SiO2@γ-MPTS MNPs towards methylmercury (CH3Hg(+)) and inorganic mercury (Hg(2+)) was investigated. It was found that CH3Hg(+) and Hg(2+) could be simultaneously retained on the prepared Fe3O4@SiO2@γ-MPTS MNPs, and the quantitative elution of CH3Hg(+) and total mercury (THg) was achieved by using 1.5 mol L(-1) HCl containing 0.01% and 3% thiourea (m/v), respectively. And the levels of Hg(2+) were obtained by subtracting CH3Hg(+) from THg. Based on the above facts, a method of magnetic solid phase extraction (MSPE) combined with inductively coupled plasma mass spectrometry (ICP-MS) was developed for the speciation of CH3Hg(+) and Hg(2+). Various experimental parameters affecting MSPE of CH3Hg(+) and Hg(2+) such as pH, eluent, sample volume, and co-existing ions have been studied. Under the optimized conditions, the limits of detection (LODs) for CH3Hg(+) and THg were 1.6 and 1.9 ng L(-1), respectively. The accuracy of the proposed method was validated by analysis of a Certified Reference Material NRCC DORM-2 dogfish muscle, and the determined values are in good agreement with the certified values. The proposed method has also been successfully applied for the speciation of CH3Hg(+) and Hg(2+) in environmental water and human hair samples. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Use of units of measurement error in anthropometric comparisons.

PubMed

Lucas, Teghan; Henneberg, Maciej

2017-09-01

Anthropometrists attempt to minimise measurement errors, however, errors cannot be eliminated entirely. Currently, measurement errors are simply reported. Measurement errors should be included into analyses of anthropometric data. This study proposes a method which incorporates measurement errors into reported values, replacing metric units with 'units of technical error of measurement (TEM)' by applying these to forensics, industrial anthropometry and biological variation. The USA armed forces anthropometric survey (ANSUR) contains 132 anthropometric dimensions of 3982 individuals. Concepts of duplication and Euclidean distance calculations were applied to the forensic-style identification of individuals in this survey. The National Size and Shape Survey of Australia contains 65 anthropometric measurements of 1265 women. This sample was used to show how a woman's body measurements expressed in TEM could be 'matched' to standard clothing sizes. Euclidean distances show that two sets of repeated anthropometric measurements of the same person cannot be matched (> 0) on measurements expressed in millimetres but can in units of TEM (= 0). Only 81 women can fit into any standard clothing size when matched using centimetres, with units of TEM, 1944 women fit. The proposed method can be applied to all fields that use anthropometry. Units of TEM are considered a more reliable unit of measurement for comparisons.

Solar Flare Track Exposure Ages in Regolith Particles: A Calibration for Transmission Electron Microscope Measurements

NASA Technical Reports Server (NTRS)

Berger, Eve L.; Keller, Lindsay P.

2015-01-01

Mineral grains in lunar and asteroidal regolith samples provide a unique record of their interaction with the space environment. Space weathering effects result from multiple processes including: exposure to the solar wind, which results in ion damage and implantation effects that are preserved in the rims of grains (typically the outermost 100 nm); cosmic ray and solar flare activity, which result in track formation; and impact processes that result in the accumulation of vapor-deposited elements, impact melts and adhering grains on particle surfaces. Determining the rate at which these effects accumulate in the grains during their space exposure is critical to studies of the surface evolution of airless bodies. Solar flare energetic particles (mainly Fe-group nuclei) have a penetration depth of a few millimeters and leave a trail of ionization damage in insulating materials that is readily observable by transmission electron microscope (TEM) imaging. The density of solar flare particle tracks is used to infer the length of time an object was at or near the regolith surface (i.e., its exposure age). Track measurements by TEM methods are routine, yet track production rate calibrations have only been determined using chemical etching techniques [e.g., 1, and references therein]. We used focused ion beam-scanning electron microscope (FIB-SEM) sample preparation techniques combined with TEM imaging to determine the track density/exposure age relations for lunar rock 64455. The 64455 sample was used earlier by [2] to determine a track production rate by chemical etching of tracks in anorthite. Here, we show that combined FIB/TEM techniques provide a more accurate determination of a track production rate and also allow us to extend the calibration to solar flare tracks in olivine.

Statistical prediction of nanoparticle delivery: from culture media to cell

NASA Astrophysics Data System (ADS)

Rowan Brown, M.; Hondow, Nicole; Brydson, Rik; Rees, Paul; Brown, Andrew P.; Summers, Huw D.

2015-04-01

The application of nanoparticles (NPs) within medicine is of great interest; their innate physicochemical characteristics provide the potential to enhance current technology, diagnostics and therapeutics. Recently a number of NP-based diagnostic and therapeutic agents have been developed for treatment of various diseases, where judicious surface functionalization is exploited to increase efficacy of administered therapeutic dose. However, quantification of heterogeneity associated with absolute dose of a nanotherapeutic (NP number), how this is trafficked across biological barriers has proven difficult to achieve. The main issue being the quantitative assessment of NP number at the spatial scale of the individual NP, data which is essential for the continued growth and development of the next generation of nanotherapeutics. Recent advances in sample preparation and the imaging fidelity of transmission electron microscopy (TEM) platforms provide information at the required spatial scale, where individual NPs can be individually identified. High spatial resolution however reduces the sample frequency and as a result dynamic biological features or processes become opaque. However, the combination of TEM data with appropriate probabilistic models provide a means to extract biophysical information that imaging alone cannot. Previously, we demonstrated that limited cell sampling via TEM can be statistically coupled to large population flow cytometry measurements to quantify exact NP dose. Here we extended this concept to link TEM measurements of NP agglomerates in cell culture media to that encapsulated within vesicles in human osteosarcoma cells. By construction and validation of a data-driven transfer function, we are able to investigate the dynamic properties of NP agglomeration through endocytosis. In particular, we statistically predict how NP agglomerates may traverse a biological barrier, detailing inter-agglomerate merging events providing the basis for predictive modelling of nanopharmacology.

Application of FTIR Spectroscopy for Assessment of Green Coffee Beans According to Their Origin

NASA Astrophysics Data System (ADS)

Obeidat, S. M.; Hammoudeh, A. Y.; Alomary, A. A.

2018-01-01

Samples of green coffee beans originating from five different countries were ground and analyzed using FTIR spectra in the region of 600-4000 cm-1. Successful discrimination of each coffee type based on their origin was achieved applying a PCA algorithm on the obtained IR spectra for all samples. PCA loading plots show that the IR bands at 2850, 2920, and 1745 cm-1 corresponding to the symmetric, and antisymmetric vibrations of CH2 and the stretching vibration of C=O bond in ester, respectively, are the most significant peaks in distinguishing the origin of the above coffee samples.

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.

TEM in situ micropillar compression tests of ion irradiated oxide dispersion strengthened alloy

NASA Astrophysics Data System (ADS)

Yano, K. H.; Swenson, M. J.; Wu, Y.; Wharry, J. P.

2017-01-01

The growing role of charged particle irradiation in the evaluation of nuclear reactor candidate materials requires the development of novel methods to assess mechanical properties in near-surface irradiation damage layers just a few micrometers thick. In situ transmission electron microscopic (TEM) mechanical testing is one such promising method. In this work, microcompression pillars are fabricated from a Fe2+ ion irradiated bulk specimen of a model Fe-9%Cr oxide dispersion strengthened (ODS) alloy. Yield strengths measured directly from TEM in situ compression tests are within expected values, and are consistent with predictions based on the irradiated microstructure. Measured elastic modulus values, once adjusted for the amount of deformation and deflection in the base material, are also within the expected range. A pillar size effect is only observed in samples with minimum dimension ≤100 nm due to the low inter-obstacle spacing in the as received and irradiated material. TEM in situ micropillar compression tests hold great promise for quantitatively determining mechanical properties of shallow ion-irradiated layers.

[Study on the vibrational spectra and XRD characters of Huanglong jade from Longling County, Yunnan Province].

PubMed

Pei, Jing-cheng; Fan, Lu-wei; Xie, Hao

2014-12-01

Based on the conventional test methods, the infrared absorption spectrum, Raman spectrum and X-ray diffraction (XRD) were employed to study the characters of the vibration spectrum and mineral composition of Huanglong jade. The testing results show that Huanglong jade shows typical vibrational spectrum characteristics of quartziferous jade. The main infrared absorption bands at 1162, 1076, 800, 779, 691, 530 and 466 cm(-1) were induced by the asymmetric stretching vibration, symmetrical stretching vibration and bending vibration of Si-O-Si separately. Especially the absorption band near 800 cm(-1) is split, which indicates that Huanglong jade has good crystallinity. In Raman spectrum, the main strong vibration bands at 463 and 355 cm(-1) were attributed to bending vibration of Si-O-Si. XRD test confirmed that Quartz is main mineral composition of Huanglong jade and there is a small amount of hematite in red color samples which induced the red color of Huanglong jade. This is the first report on the infrared, Raman and XRD spectra feature of Huanglong jade. It will provide a scientific basis for the identification, naming and other research for huanglong jade.

Feasibility of coded vibration in a vibro-ultrasound system for tissue elasticity measurement.

PubMed

Zhao, Jinxin; Wang, Yuanyuan; Yu, Jinhua; Li, Tianjie; Zheng, Yong-Ping

2016-07-01

The ability of various methods for elasticity measurement and imaging is hampered by the vibration amplitude on biological tissues. Based on the inference that coded excitation will improve the performance of the cross-correlation function of the tissue displacement waves, the idea of exerting encoded external vibration on tested samples for measuring its elasticity is proposed. It was implemented by integrating a programmable vibration generation function into a customized vibro-ultrasound system to generate Barker coded vibration for elasticity measurement. Experiments were conducted on silicone phantoms and porcine muscles. The results showed that coded excitation of the vibration enhanced the accuracy and robustness of the elasticity measurement especially in low signal-to-noise ratio scenarios. In the phantom study, the measured shear modulus values with coded vibration had an R(2 )= 0.993 linear correlation to that of referenced indentation, while for single-cycle pulse the R(2) decreased to 0.987. In porcine muscle study, the coded vibration also obtained a shear modulus value which is more accurate than the single-cycle pulse by 0.16 kPa and 0.33 kPa at two different depths. These results demonstrated the feasibility and potentiality of the coded vibration for enhancing the quality of elasticity measurement and imaging.

Effect of ultrasonic vibration on the retention of adhesively luted intra-radicular posts.

PubMed

Satterthwaite, Julian D; Stokes, Alastair N

2004-09-01

The aim of this study was to determine the effect of prolonged ultrasonic vibration on tensile force necessary to dislodge two different post types luted with an adhesive resin. Extracted human canine teeth were decoronated and root-filled. Either a ceramic or stainless steel intra-radicular post was luted into each root with resin-based cement. Half the samples in each group were randomly assigned to be subjected to ultrasonic vibration of the post (test group), the remaining samples did not receive vibration (control group). The tensile force required to dislodge each post was then determined in a universal testing machine. The mean force required to dislodge the stainless steel posts in the control group was 510.1N (SD 170.6) and in the 'treatment' group it was 539.5N (SD 163.3). For the ceramic posts in the control group the mean force was 447.8N (SD 165.5) and in the 'treatment' group it was 473.9N (SD 137.8). There was no statistical difference between the groups (p = 0.597). Within the limitations of this in-vitro study, the results cast doubt on the ability of application of ultrasonic vibration to displace/loosen intra-radicular posts luted with a resin-based cement.

Simultaneous Measurement of Multiple Mechanical Properties of Single Cells Using AFM by Indentation and Vibration.

PubMed

Zhang, Chuang; Shi, Jialin; Wang, Wenxue; Xi, Ning; Wang, Yuechao; Liu, Lianqing

2017-12-01

The mechanical properties of cells, which are the main characteristics determining their physical performance and physiological functions, have been actively studied in the fields of cytobiology and biomedical engineering and for the development of medicines. In this study, an indentation-vibration-based method is proposed to simultaneously measure the mechanical properties of cells in situ, including cellular mass (m), elasticity (k), and viscosity (c). The proposed measurement method is implemented based on the principle of forced vibration stimulated by simple harmonic force using an atomic force microscope (AFM) system integrated with a piezoelectric transducer as the substrate vibrator. The corresponding theoretical model containing the three mechanical properties is derived and used to perform simulations and calculations. Living and fixed human embryonic kidney 293 (HEK 293) cells were subjected to indentation and vibration to measure and compare their mechanical parameters and verify the proposed approach. The results that the fixed sample cells are more viscous and elastic than the living sample cells and the measured mechanical properties of cell are consistent within, but not outside of the central region of the cell, are in accordance with the previous studies. This work provides an approach to simultaneous measurement of the multiple mechanical properties of single cells using an integrated AFM system based on the principle force vibration and thickness-corrected Hertz model. This study should contribute to progress in biomedical engineering, cytobiology, medicine, early diagnosis, specific therapy and cell-powered robots.

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

Engel, Edgar A., E-mail: eae32@cam.ac.uk; Needs, Richard J.; Monserrat, Bartomeu

Surface energies of hexagonal and cubic water ice are calculated using first-principles quantum mechanical methods, including an accurate description of anharmonic nuclear vibrations. We consider two proton-orderings of the hexagonal and cubic ice basal surfaces and three proton-orderings of hexagonal ice prism surfaces, finding that vibrations reduce the surface energies by more than 10%. We compare our vibrational densities of states to recent sum frequency generation absorption measurements and identify surface proton-orderings of experimental ice samples and the origins of characteristic absorption peaks. We also calculate zero point quantum vibrational corrections to the surface electronic band gaps, which range frommore » −1.2 eV for the cubic ice basal surface up to −1.4 eV for the hexagonal ice prism surface. The vibrational corrections to the surface band gaps are up to 12% smaller than for bulk ice.« less

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.

Detection of antibiotic resistance genes in samples from acute and chronic endodontic infections and after treatment.

PubMed

Rôças, Isabela N; Siqueira, José F

2013-09-01

The purpose of this study was twofold: survey samples from acute and chronic endodontic infections for the presence of genes encoding resistance to beta-lactams, tetracycline and erythromycin, and evaluate the ability of treatment to eliminate these genes from root canals. DNA extracts from samples of abscess aspirates (n=25) and root canals of teeth with asymptomatic apical periodontitis (n=24) were used as template for direct detection of the genes blaTEM, cfxA, tetM, tetQ, tetW, and ermC using real-time polymerase chain reaction (PCR). Bacterial presence was determined using PCR with universal bacterial primers. Root canals of the asymptomatic cases were also sampled and evaluated after chemomechanical procedures using NiTi instruments with 2.5% NaOCl irrigation. All abscess and initial root canal samples were positive for bacteria. At least one of the target resistance genes was found in 36% of the abscess samples and 67% of the asymptomatic cases. The most prevalent genes in abscesses were blaTEM (24%) and ermC (24%), while tetM (42%) and tetW (29%) prevailed in asymptomatic cases. The blaTEM gene was significantly associated with acute cases (p=0.02). Conversely, tetM was significantly more prevalent in asymptomatic cases (p=0.008). Treatment eliminated resistance genes from most cases. Acute and chronic endodontic infections harboured resistance genes for 3 classes of widely used antibiotics. In most cases, treatment was effective in eliminating these genes, but there were a few cases in which they persisted. The implications of persistence are unknown. Direct detection of resistance genes in abscesses may be a potential method for rapid diagnosis and establishment of proactive antimicrobial therapy. Copyright © 2013 Elsevier Ltd. All rights reserved.

Antibiotic Resistance Genes in the Bacteriophage DNA Fraction of Environmental Samples

PubMed Central

Colomer-Lluch, Marta; Jofre, Juan; Muniesa, Maite

2011-01-01

Antibiotic resistance is an increasing global problem resulting from the pressure of antibiotic usage, greater mobility of the population, and industrialization. Many antibiotic resistance genes are believed to have originated in microorganisms in the environment, and to have been transferred to other bacteria through mobile genetic elements. Among others, β-lactam antibiotics show clinical efficacy and low toxicity, and they are thus widely used as antimicrobials. Resistance to β-lactam antibiotics is conferred by β-lactamase genes and penicillin-binding proteins, which are chromosomal- or plasmid-encoded, although there is little information available on the contribution of other mobile genetic elements, such as phages. This study is focused on three genes that confer resistance to β-lactam antibiotics, namely two β-lactamase genes (blaTEM and blaCTX-M9) and one encoding a penicillin-binding protein (mecA) in bacteriophage DNA isolated from environmental water samples. The three genes were quantified in the DNA isolated from bacteriophages collected from 30 urban sewage and river water samples, using quantitative PCR amplification. All three genes were detected in the DNA of phages from all the samples tested, in some cases reaching 104 gene copies (GC) of blaTEM or 102 GC of blaCTX-M and mecA. These values are consistent with the amount of fecal pollution in the sample, except for mecA, which showed a higher number of copies in river water samples than in urban sewage. The bla genes from phage DNA were transferred by electroporation to sensitive host bacteria, which became resistant to ampicillin. blaTEM and blaCTX were detected in the DNA of the resistant clones after transfection. This study indicates that phages are reservoirs of resistance genes in the environment. PMID:21390233

Dose-response relation between exposure to two types of hand-arm vibration and sensorineural perception of vibration.

PubMed

Virokannas, H

1995-05-01

31 railway workers and 32 lumberjacks were examined to compare the dose-response relation between the exposure to two types of hand-arm vibration and the sensory disturbances in peripheral nerves as evaluated by the vibration perception thresholds (VPTs). Clinical examinations were carried out that included measurements of the VPTs, and electroneuromyography (ENMG), and an inquiry to confirm the use of vibrating tools. Diseases of the central nervous system and neuropathies were checked by inquiry and a clinical examination, diabetes was excluded by a blood sample analysis, and the subjects with carpal tunnel syndrome confirmed with ENMG were excluded from the study. Lifetime use of hand held tamping machines (railway workers) and chain saws (lumberjacks) had a significant correlation with the VPTs at frequencies from 32 to 500 Hz. The increase of the VPTs (250 Hz) in relation to use of vibrating tools was 1.8-fold higher on average in the whole group and 2.3-fold higher in the young (< 45) railway workers who had used hand held tamping machines, than in the corresponding groups of lumberjacks, who had used chain saws, whereas the frequency weighted acceleration of vibration in tamping machines was fourfold. There was a significant dose-response relation between the exposure to hand-arm vibration and the VPTs. The VPTs as a function of the frequency weighted acceleration of vibration and the exposure to vibration gave promising results for assessment of the risk of damage to sensory nerves induced by vibration.

Seagulls of the Berlengas natural reserve of Portugal as carriers of fecal Escherichia coli harboring CTX-M and TEM extended-spectrum beta-lactamases.

PubMed

Poeta, Patricia; Radhouani, Hajer; Igrejas, Gilberto; Gonçalves, Alexandre; Carvalho, Carlos; Rodrigues, Jorge; Vinué, Laura; Somalo, Sergio; Torres, Carmen

2008-12-01

Escherichia coli isolates containing the following extended-spectrum beta-lactamases have been detected in 11 of 57 fecal samples (19.3%) in Berlengas Island seagulls: TEM-52 (eight isolates), CTX-M-1 (one isolate), CTX-M-14a (one isolate), and CTX-M-32 (one isolate). Most of the extended-spectrum beta-lactamase-positive isolates harbored class 1 or class 2 integrons, which included different antibiotic resistance gene cassettes.

Seagulls of the Berlengas Natural Reserve of Portugal as Carriers of Fecal Escherichia coli Harboring CTX-M and TEM Extended-Spectrum Beta-Lactamases▿

PubMed Central

Poeta, Patricia; Radhouani, Hajer; Igrejas, Gilberto; Gonçalves, Alexandre; Carvalho, Carlos; Rodrigues, Jorge; Vinué, Laura; Somalo, Sergio; Torres, Carmen

2008-01-01

Escherichia coli isolates containing the following extended-spectrum beta-lactamases have been detected in 11 of 57 fecal samples (19.3%) in Berlengas Island seagulls: TEM-52 (eight isolates), CTX-M-1 (one isolate), CTX-M-14a (one isolate), and CTX-M-32 (one isolate). Most of the extended-spectrum beta-lactamase-positive isolates harbored class 1 or class 2 integrons, which included different antibiotic resistance gene cassettes. PMID:18835997

Effect of Moisture Sorption State on Vibrational Properties of Wood

Treesearch

Jianxiong Lu; Jiali Jiang; Yiqiang Wu; Xianjun Li; Zhiyong Cai

2012-01-01

The purpose of this study was to investigate the vibrational properties and corresponding anisotropicity in wood during different states of moisture sorption. Samples of maple (Acer spp.) and red oak (Quercus rubra Michx.f.) were moisture conditioned by the adsorption process from an ovendried state and by the desorption process...

Possibility for new PolyCO imaging: stroboscopic imaging based on vibrating capillary optics

NASA Astrophysics Data System (ADS)

Liedl, A.; Dabagov, S. B.; Della Ventura, G.; Hampai, D.; Polese, C.

2015-08-01

Polycapillary lenses are well known optical devices for radiation and charged particles. These lenses consist of thousands channels through which the signal is transmitted by total external reflection phenomenon. Their application have made possible technical improvements in different fields such as imaging, fluorescence analysis, channeling studies etc. In particular, the application of this optics coupled with conventional sources such as X-ray tubes has opened a new season for potential applications of desktop instrumentations. For instance, the usage of such lenses has enhanced the spatial coherence and the brilliance over the sample allowing better resolution and contrast for imaging purposes. In addiction, improved focusing power and confocal configuration of other lenses has improved the resolution, from both the energy and the spatial points of view, in fluorescence mapping. A recent work has addressed the behavior of the transmitted radiation through a single capillary in vibrating regime. In this work a test of using a vibrating capillary for stroboscopic imaging is presented. A sample characterized by a known periodic event is studied with a synchronized vibrating capillary.

Low-temperature vibrational dynamics of fused silica and binary silicate glasses

NASA Astrophysics Data System (ADS)

Cai, Ling; Shi, Ying; Hrdina, Ken; Moore, Lisa; Wu, Jingshi; Daemen, Luke L.; Cheng, Yongqiang

2018-02-01

Inelastic neutron scattering was used to study the vibrational dynamics of fused silica and its mixed binary glasses that were doped with either TiO2 or K2O . The energy transfer was measured from zero to 180 meV where the so-called Boson peaks (BP) at low energy and molecular vibrations at high energy are included. Although most of the vibrational spectra at the high energy resemble those reported in earlier literature, a defect-mode-like peak is observed for the doped binary systems near 120 meV . At very low temperature, the BP intensity increases rapidly with temperature and then, at higher temperature, the peak intensity decreases. As a result, a maximum is observed in the temperature dependence of the BP intensity. This maximum was shown in all four samples, but the pure SiO2 sample shows the highest intensity peak and the lowest temperature for peak position. Broadband energy spectra reveal a shift of intensity from BP to the more localized modes at higher energy. Temperature evolution of BP and its relationship with heat conduction and thermal expansion are discussed.

Vibration-based monitoring and diagnostics using compressive sensing

NASA Astrophysics Data System (ADS)

Ganesan, Vaahini; Das, Tuhin; Rahnavard, Nazanin; Kauffman, Jeffrey L.

2017-04-01

Vibration data from mechanical systems carry important information that is useful for characterization and diagnosis. Standard approaches rely on continually streaming data at a fixed sampling frequency. For applications involving continuous monitoring, such as Structural Health Monitoring (SHM), such approaches result in high volume data and rely on sensors being powered for prolonged durations. Furthermore, for spatial resolution, structures are instrumented with a large array of sensors. This paper shows that both volume of data and number of sensors can be reduced significantly by applying Compressive Sensing (CS) in vibration monitoring applications. The reduction is achieved by using random sampling and capitalizing on the sparsity of vibration signals in the frequency domain. Preliminary experimental results validating CS-based frequency recovery are also provided. By exploiting the sparsity of mode shapes, CS can also enable efficient spatial reconstruction using fewer spatially distributed sensors. CS can thereby reduce the cost and power requirement of sensing as well as streamline data storage and processing in monitoring applications. In well-instrumented structures, CS can enable continued monitoring in case of sensor or computational failures.

Effect of sonic vibration of an ultrasonic toothbrush on the removal of Streptococcus mutans biofilm from enamel surface.

PubMed

Hashizume, Lina Naomi; Dariva, Alessandra

2015-12-01

To evaluate in vitro the effect of sonic vibration of an ultrasonic toothbrush in the removal of Streptococcus mutans (S. mutans) biofilm from human enamel. S. mutans dental biofilm was formed in vitro on human enamel blocks coated by salivary pellicle. The blocks were incubated with a suspension of S. mutans at 37°C for 24 or 72 hours. The blocks were divided to one of three conditions according to the different toothbrush action modes: ultrasound plus sonic vibration (U+SV), ultrasound-only (U) and no ultrasound and no sonic vibration (control). Samples were exposed to each mode for 3 minutes with the toothbrush bristles placed 5 mm away from the enamel block surface. The samples were observed by scanning electron microscopy (SEM) and quantification of S. mutans was performed. U+SV showed lower bacterial counts compared to U and control on the 72 hour-biofilm (P < 0.05). The SEM analysis revealed that U+SV and U disrupted the S. mutans chains in the 24- and 72-hour biofilm.

Effect of Vibration on Pain Response to Heel Lance: A Pilot Randomized Control Trial.

PubMed

McGinnis, Kate; Murray, Eileen; Cherven, Brooke; McCracken, Courtney; Travers, Curtis

2016-12-01

Applied mechanical vibration in pediatric and adult populations has been shown to be an effective analgesic for acute and chronic pain, including needle pain. Studies among the neonatal population are lacking. According to the Gate Control Theory, it is expected that applied mechanical vibration will have a summative effect with standard nonpharmacologic pain control strategies, reducing behavioral and physiologic pain responses to heel lancing. To determine the safety and efficacy of mechanical vibration for relief of heel lance pain among neonates. In this parallel design randomized controlled trial, eligible enrolled term or term-corrected neonates (n = 56) in a level IV neonatal intensive care unit were randomized to receive either sucrose and swaddling or sucrose, swaddling, and vibration for heel lance analgesia. Vibration was applied using a handheld battery-powered vibrator (Norco MiniVibrator, Hz = 92) to the lateral aspect of the lower leg along the sural dermatome throughout the heel lance procedure. Neonatal Pain, Agitation, and Sedation Scale (N-PASS) scores, heart rate, and oxygen saturations were collected at defined intervals surrounding heel lancing. Infants in the vibration group (n = 30) had significantly lower N-PASS scores and more stable heart rates during heel stick (P = .006, P = .037) and 2 minutes after heel lance (P = .002, P = .016) than those in the nonvibration group. There were no adverse behavioral or physiologic responses to applied vibration in the sample. Applied mechanical vibration is a safe and effective method for managing heel lance pain. This pilot study suggests that mechanical vibration warrants further exploration as a nonpharmacologic pain management tool among the neonatal population.

A study of the eigenvectors of low frequency vibrational modes in crystalline cytidine via high pressure Raman spectroscopy

NASA Astrophysics Data System (ADS)

Lee, Scott A.

2014-03-01

High-pressure Raman spectroscopy has been used to study the eigenvectors and eigenvalues of the low-frequency vibrational modes of crystalline cytidine at 295 K by evaluating the logarithmic derivative of the vibrational frequency with respect to pressure: 1/ω dω/dP. Crystalline samples of molecular materials such as cytidine have vibrational modes that are localized within a molecular unit (``internal'' modes) as well as modes in which the molecular units vibrate against each other (``external'' modes). The value of the logarithmic derivative is a diagnostic probe of the nature of the eigenvector of the vibrational modes, making high pressure experiments a very useful probe for such studies. Internal stretching modes have low logarithmic derivatives while external as well as internal torsional and bending modes have higher logarithmic derivatives. All of the Raman modes below 200 cm-1 in cytidine are found to have high logarithmic derivatives, consistent with being either external modes or internal torsional or bending modes.

Imaging of fullerene-like structures in CNx thin films by electron microscopy; sample preparation artefacts due to ion-beam milling.

PubMed

Czigány, Zs; Neidhardt, J; Brunell, I F; Hultman, L

2003-04-01

The microstructure of CN(x) thin films, deposited by reactive magnetron sputtering, was investigated by transmission electron microscopy (TEM) at 200kV in plan-view and cross-sectional samples. Imaging artefacts arise in high-resolution TEM due to overlap of nm-sized fullerene-like features for specimen thickness above 5nm. The thinnest and apparently artefact-free areas were obtained at the fracture edges of plan-view specimens floated-off from NaCl substrates. Cross-sectional samples were prepared by ion-beam milling at low energy to minimize sample preparation artefacts. The depth of the ion-bombardment-induced surface amorphization was determined by TEM cross sections of ion-milled fullerene-like CN(x) surfaces. The thickness of the damaged surface layer at 5 degrees grazing incidence was 13 and 10nm at 3 and 0.8keV, respectively, which is approximately three times larger than that observed on Si prepared under the same conditions. The shallowest damage depth, observed for 0.25keV, was less than 1nm. Chemical changes due to N loss and graphitization were also observed by X-ray photoelectron spectroscopy. As a consequence of chemical effects, sputtering rates of CN(x) films were similar to that of Si, which enables relatively fast ion-milling procedure compared to carbon compounds. No electron beam damage of fullerene-like CN(x) was observed at 200kV.

Sample presentation, sources of error and future perspectives on the application of vibrational spectroscopy in the wine industry.

PubMed

Cozzolino, Daniel

2015-03-30

Vibrational spectroscopy encompasses a number of techniques and methods including ultra-violet, visible, Fourier transform infrared or mid infrared, near infrared and Raman spectroscopy. The use and application of spectroscopy generates spectra containing hundreds of variables (absorbances at each wavenumbers or wavelengths), resulting in the production of large data sets representing the chemical and biochemical wine fingerprint. Multivariate data analysis techniques are then required to handle the large amount of data generated in order to interpret the spectra in a meaningful way in order to develop a specific application. This paper focuses on the developments of sample presentation and main sources of error when vibrational spectroscopy methods are applied in wine analysis. Recent and novel applications will be discussed as examples of these developments. © 2014 Society of Chemical Industry.

Synthesis and characterization of Ni doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Tamgadge, Y. S.; Gedam, P. P.; Ganorkar, R. P.; Mahure, M. A.; Pahurkar, V. G.; Muley, G. G.

2018-05-01

In this paper, we present synthesis of L-valine assisted surface modification of Ni doped ZnO nanoparticles (NPs) using chemical precipitation method. Samples were calcined at 500oC for 2h. Uncalcined and calcined samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and ultraviolet-visible (UV-vis) spectroscopy. Ni doped ZnO NPs with average particle size of 8 nm have been successfully obtained using L-valine as surface modifying agent. Increase in the particle size was observed after the calcination. XRD and TEM studies confirmed the purity, surface morphology and hexagonal wurtzite crystal structure of ZnO NPs. UV-vis spectroscopy indicated the blue shift of excitons absorption wavelength and surface modification by L-valine.

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

PubMed

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

2015-06-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Thermoelectric technique to precisely control hyperthermic exposures of human whole blood.

PubMed

DuBose, D A; Langevin, R C; Morehouse, D H

1996-12-01

The need in military research to avoid exposing humans to harsh environments and reduce animal use requires the development of in vitro models for the study of hyperthermic injury. A thermoelectric module (TEM) system was employed to heat human whole blood (HWB) in a manner similar to that experienced by heat-stroked rats. This system precisely and accurately replicated mild, moderate, and extreme heat-stress exposures. Temperature changes could be monitored without the introduction of a test sample thermistor, which reduced contamination problems. HWB with hematocrits of 45 or 50% had similar heating curves, indicating that the system compensated for differences in sample character. The unit's size permitted its containment within a standard carbon dioxide incubator to further control sample environment. These results indicate that the TEM system can precisely control temperature change in this heat stress in vitro model employing HWB. Information obtained from such a model could contribute to military preparedness.

Psycho-vibratory evaluation of timber floors - Towards the determination of design indicators of vibration acceptability and vibration annoyance

NASA Astrophysics Data System (ADS)

Negreira, J.; Trollé, A.; Jarnerö, K.; Sjökvist, L.-G.; Bard, D.

2015-03-01

In timber housing constructions, vibrations can be a nuisance for inhabitants. Notably, the vibrational response of wooden floor systems is an issue in need of being dealt with more adequately in the designing of such buildings. Studies addressing human response to vibrations are needed in order to be able to better estimate what level of vibrations in dwellings can be seen as acceptable. In the present study, measurements on five different wooden floors were performed in a laboratory environment at two locations in Sweden (SP in Växjö and LU in Lund). Acceleration measurements were carried out while a person either was walking on a particular floor or was seated in a chair placed there as the test leader was walking on the floor. These participants filled out a questionnaire regarding their perception and experiencing of the vibrations in question. Independently of the subjective tests, several static and dynamic characteristics of the floors were determined through measurements. The ultimate aim was to develop indicators of human response to floor vibrations, specifically those regarding vibration acceptability and vibration annoyance, their being drawn based on relationships between the questionnaire responses obtained and the parameter values determined on the basis of the measurements carried out. To that end, use was made of multilevel regression. Although the sample of floors tested was small, certain clear trends could be noted. The first eigenfrequency (calculated in accordance with Eurocode 5) and Hu and Chui's criterion (calculated from measured quantities) proved to be the best indicators of vibration annoyance, and the Maximum Transient Vibration Value (computed on the basis of the accelerations experienced by the test subjects) to be the best indicator of vibration acceptability.

Interpreting Quasi-Thermal Effects in Ultrafast Spectroscopy of Hydrogen-Bonded Systems.

PubMed

Stingel, Ashley M; Petersen, Poul B

2018-03-15

Vibrational excitation of molecules in the condensed phase relaxes through vibrational modes of decreasing energy to ultimately generate an equilibrium state in which the energy is distributed among low-frequency modes. In ultrafast vibrational spectroscopy, changes in the vibrational features of hydrogen-bonded NH and OH stretch modes are typically observed to persist long after these high-frequency vibrations have relaxed. Due to the resemblance to the spectral changes caused by heating the sample, these features are typically described as arising from a hot ground state. However, these spectral features appear on ultrafast time scales that are much too fast to result from a true thermal state, and significant differences between the thermal difference spectrum and the induced quasi-thermal changes in ultrafast spectroscopy are often observed. Here, we examine and directly compare the thermal and quasi-thermal responses of the hydrogen-bonded homodimer of 7-azaindole with temperature-dependent FTIR spectroscopy and ultrafast mid-IR continuum spectroscopy. We find that the thermal difference spectra contain contributions from both dissociation of the hydrogen bonds and from frequency shifts due to changes in the thermal population of low-frequency modes. The transient spectra in ultrafast vibrational spectroscopy are also found to contain two contributions: initial frequency shifts over 2.3 ± 0.11 ps associated with equilibration of the initial excitation, and frequency shifts associated with the excitation of several fingerprint modes, which decay over 21.8 ± 0.11 ps, giving rise to a quasi-thermal response caused by a distribution of fingerprint modes being excited within the sample ensemble. This resembles the thermal frequency shifts due to population changes of low-frequency modes, but not the overall thermal spectrum, which is dominated by features caused by dimer dissociation. These findings provide insight into the changes in the vibrational spectrum from different origins and are important for assigning, analyzing, and comparing features in thermal and ultrafast vibrational spectroscopy of hydrogen-bonded complexes.

One pot synthesis of exchange coupled Nd2Fe14B/alpha-Fe by pechini type sol-gel method.

PubMed

Hussain, Abid; Jadhav, Abhijit P; Baek, Yeon Kyung; Choi, Hul Jin; Lee, Jaeho; Kang, Young Soo

2013-11-01

In this work, a combination of nanoparticles of Nd2Fe14B hard magnetic phase and alpha-Fe soft magnetic phase were synthesized by one pot chemical synthesis technique using sol-gel method. A gel of Nd-Fe-B was prepared using NdCl3 x 6H2O, FeCl3 x 6H2O, H3BO3, citric acid, and ethylene glycol by pechini type sol-gel method. The gel was subsequently calcined and annealed to obtain the mixed oxide powders. The produced metal oxide particles were identified with XRD, SEM, TEM to obtain the crystal structure, shape and domain structure of them. The nanoparticles of mixed phase of Nd2Fe14B/alpha-Fe were obtained from these oxides by a process of reduction-diffusion in vacuum by employing CaH2 as reducing agent. During this process it was optimized by controlling temperature, reaction time and concentration of the reducing agent (CaH2). The phase formation of Nd2Fe14B was resulted by the direct diffusion of NdH2, Fe and B. The magnetic property of produced hard and soft phases was successfully identified with vibrating sample magnetometer (VSM). The mixed domains of the hard and soft phases were identified with selected area electron diffraction method (SAED) patterns.

Highly selective and efficient removal of lead with magnetic nano-adsorbent: Multivariate optimization, isotherm and thermodynamic studies.

PubMed

Khani, Rouhollah; Sobhani, Sara; Beyki, Mostafa Hossein

2016-03-15

2-Hydroxyethylammonium sulfonate immobilized on γ-Fe2O3 nanoparticles (γ-Fe2O3-2-HEAS) was synthesized by the reaction of n-butylsulfonated γ-Fe2O3 with ethanolamine. The structure of the resulting product was confirmed by fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD) spectrometry, transmission electron microscopy (TEM), thermogravimetric analysis (TGA), elemental analysis, N2 adsorption-desorption and vibrating sample magnetometer (VSM) techniques. The supported ionic liquid on γ-Fe2O3 was applied as a new and green adsorbent to remove Pb(II) from aqueous solution. The effect of adsorption parameters such as pH, shaking time and amount of the adsorbent were investigated using two level three factor (2(3)) full factorial central composite design with the help of Design-Expert, Stat-Ease Inc. version 9.0 software. The significance of independent variables and their interactions were tested by means of the analysis of variance (ANOVA) with 95% confidence limits (α=0.05). The thermodynamic parameters of the adsorption process are estimated. It is found that the process is exothermic and spontaneous. The Langmuir and Freundlich models have been also applied to evaluate the removal efficiency and the data were correlated well with the Freundlich model. Copyright © 2015 Elsevier Inc. All rights reserved.

Bio-inspired green synthesis of Fe3O4 magnetic nanoparticles using watermelon rinds and their catalytic activity

NASA Astrophysics Data System (ADS)

Prasad, Ch.; Gangadhara, S.; Venkateswarlu, P.

2016-08-01

Novel and bio-inspired magnetic nanoparticles were synthesized using watermelon rinds (WR) which are nontoxic and biodegradable. Watermelon rind extract was used as a solvent and capping and reducing agent in the synthesis. The Fe3o4 MNPs were characterized by using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer techniques (VSM). XRD studies revealed a high degree of crystalline and monophasic Fe nanoparticles of face-centered cubic stricture. FTIR analysis proved that particles are reduced and stabilized in solution by the capping agent that is likely to be proteins secreted by the biomass. The present process in an excellent candidate for the synthesis of iron nanoparticles that is simple, easy to execute, pollutant free and inexpensive. A practical and convenient method for the synthesis of highly stable and small-sized iron nanoparticles with a narrow distribution from 2 to 20 nm is reported. Also, the MNPs present in higher saturation magnetization (Ms) of 14.2 emu/g demonstrate tremendous magnetic response behavior. However, the synthesized iron nanoparticles were used as a catalyst for the preparation of biologically interesting 2-oxo-1,2,3,4-tetrahydropyrimidine derivatives in high yields. These results exhibited that the synthesized Fe3O4 MNPs could be used as a catalyst in organic synthesis.

Biomedical applications of SPION@APTES@PEG-folic acid@carboxylated quercetin nanodrug on various cancer cells

NASA Astrophysics Data System (ADS)

Akal, Z. Ü.; Alpsoy, L.; Baykal, A.

2016-08-01

In this study, carboxylated quercetin (CQ) was conjugated to superparamagnetic iron oxide nanoparticles (SPIONs) which were modified by (3-aminopropyl) triethoxysilane (APTES), Folic acid (FA) and carboxylated Polyethylene glycol (PEG); (SPION@APTES@FA-PEG@CQ), nanodrug has been synthesized via polyol and accompanying by various chemical synthesis routes. The characterization of the final product was done via X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Thermal gravimetric analysis (TGA), Transmission electron spectroscopy (TEM) and Vibrating sample magnetometer (VSM). Its cytotoxic and apoptotic activities on over expressed folic acid receptor (FR +) (MCF-7, HeLa) and none expressed folic acid receptor (FR-) (A549) cancer cell lines were determined by using MTT assay, Real-Time Cell Analysis, TUNEL assay, Annexin assay and RT-PCR analysis for Caspase3/7 respectively. SPION@APTES@FA-PEG@CQ nanodrug showed higher cytotoxicity against HeLa and MCF-7 cell lines as compared with A549 cell line. Moreover, SPION@APTES@FA-PEG@CQ nanodrug also caused higher apoptotic and necrotic effects in 100 μg/mL HeLa and MCF-7 cells than A549 cells. The findings showed that SPION@APTES@FA-PEG@CQ nanodrug has cytotoxic, apoptotic and necrotic effects on HeLa and MCF-7 which are FR over expressed cell lines and can be potentially used for the delivery of quercetin to cervical and breast cancer cells.

Laboratory Studies of Solid Carbon Dioxide in Planetary and Interstellar Ices

NASA Technical Reports Server (NTRS)

White, Douglas; Sandford, Scott A.; Mastrapa, Rachel M.

2012-01-01

Laboratory spectra have shown that CO2. is a powerful diagnostic tool for analyzing infrared data from remote observations, as it has been detected on icy moons in the outer solar system as well as dust grain surfaces in the interstellar medium. IR absorption profiles of CO2 wi thin ice mixtures containing H2O and CH30H change with respect to tem perature and mixture ratios. In this particular study, the CO2 stretch mode around 235O cm (exp -1) (4.3 rricrons) is systematically observ ed in different mixtures with H2O and CH30H in temperature ranges from 15K to 150 K, as well as vibrational modes in the near-IR such as th e combination bands near 3700 cm (exp -1) (2.7 microns) and 5080 (exp -1) (2.0 microns). Additionally, some high?temperature deposits (T > 50 K) of H2O, CH30H, and CO2 ice mixtures were performed to determine the maximum temperatures at which CO2 will deposit on the sample win dow. These data may then be used to interpret spectra obtained from remote IR observations. This research was sponsored by Oak Ridge Associ ated Universities (ORAU) through the NASA Postdoctoral Program (NPP) as well as Ames Research Center and the SETI institute who provided fa cilities and equipment.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Innovative methodology for the synthesis of Ba-M hexaferrite BaFe{sub 12}O{sub 19} nanoparticles

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

Ahmed, M.A., E-mail: moala@47hotmail.com; Helmy, N.; El-Dek, S.I.

2013-09-01

Graphical abstract: Transmission electron microscope images for the BaFe12O19. - Highlights: • BaFe{sub 12}O{sub 19}nanoparticles were prepared in single-phase from organometallic precursors. • BaFe{sub 12}O{sub 19} possesses small size 65 nm, H{sub C} = 3695 Oe and M{sub s} = 58 emu/g. • This method of preparation could be extended in the synthesis of other metal oxide nanoparticles. - Abstract: In this piece of work, high quality and homogeneity, barium hexaferrite (BaM) BaFe{sub 12}O{sub 19} nanoparticles were prepared from organometallic precursors for the 1st time. This method is based on the formation of supramolecular crystal structure of Ba[Fe(H{sub 3}NCH{sub 2}CH{submore » 2}NH{sub 3})]Cl{sub 7}·8H{sub 2}O. The crystal structure, morphology and magnetic properties of BaFe{sub 12}O{sub 19} at two different annealing temperatures namely 1000 °C and 1200 °C were investigated using X-ray diffraction, transmission electron microscope TEM and vibrating sample magnetometry (VSM). The results show that monophasic nanoparticles of hexaferrites were obtained. Nanoparticles of crystallite size 40–50 nm distinguished by narrow distribution and excellent homogeneity were obtained with superior magnetic properties which suggested single-domain particles of Ba-M hexaferrite.« less

Self-assembled mPEG-PCL-g-PEI micelles for multifunctional nanoprobes of doxorubicin delivery and magnetic resonance imaging and optical imaging.

PubMed

Guo, Qingfa; Kuang, Lei; Cao, Hui; Li, Weizhong; Wei, Jing

2015-12-01

In this paper, a novel bifunctional nanoprobe based on polyethylene glycol(MPEG)-poly(ϵ-caprolactone)(ϵ-CL)-polyethylenimine(PEI) labeled with FITC (MPEG-PCL-PEI-FITC, PCIF) were prepared to provide tumor therapy and simultaneous diagnostic information via magnetic resonance imaging (MRI) and optical imaging. Superparamagnetic iron oxide (SPIO) and doxorubicin (DOX) loaded PCIF (PCIF/SPIO/DOX) nanoprobes were prepared by self-assembling into micelles, which had uniformly distributed particle size of 130 ± 5 nm and a zeta potential of +35 ± 2 mV. Transmission electronic microscopy(TEM) showed that SPIO NPs were loaded into PCIF micelles. The PCIF/SPIO/DOX nanoprobes were superparamagnetic at 300 K with saturated magnetization of 20.5 emu/g Fe by vibrating-sample-magnetomete (VSM). Studies on cellular uptake of PCIF/SPIO/DOX nanoprobes demonstrated that SPIO NPs, DOX and FITC labeled MPEG-PCL-PEI were simultaneously taken up by the breast cancer (4T1) cells. After intravenous injection of PCIF/SPIO/DOX nanoprobes in 4T1 tumor-bearing mice, SPIO NPs, DOX and FITC labeled MPEG-PCL-PEI micelles were simultaneously delivered into tumor tissue by histochemisty. This work is important for the applications to multimodal diagnostic and theragnosis as nanomedicine. Copyright © 2015 Elsevier B.V. All rights reserved.

Shape- and Size-Controlled Synthesis of Silver Nanoparticles Using Aloe vera Plant Extract and Their Antimicrobial Activity

NASA Astrophysics Data System (ADS)

Logaranjan, Kaliyaperumal; Raiza, Anasdass Jaculin; Gopinath, Subash C. B.; Chen, Yeng; Pandian, Kannaiyan

2016-11-01

Biogenic synthesis of silver nanoparticles (AgNP) was performed at room temperature using Aloe vera plant extract in the presence of ammoniacal silver nitrate as a metal salt precursor. The formation of AgNP was monitored by UV-visible spectroscopy at different time intervals. The shape and size of the synthesized particle were visualized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations. These results were confirmed by X-ray powder diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) analyses and further supported by surface-enhanced Raman spectroscopy/Raman scattering (SERS) study. UV-visible spectrum has shown a sharp peak at 420 nm and further evidenced by FTIR peak profile (at 1587.6, 1386.4, and 1076 cm-1 with corresponding compounds). The main band position with SERS was noticed at 1594 cm-1 (C-C stretching vibration). When samples were heated under microwave radiation, AgNP with octahedron shapes with 5-50 nm were found and this method can be one of the easier ways to synthesis anisotropic AgNP, in which the plant extract plays a vital role to regulate the size and shape of the nanoparticles. Enhanced antibacterial effects (two- to fourfold) were observed in the case of Aloe vera plant protected AgNP than the routinely synthesized antibiotic drugs.

Design and synthesis of pH-sensitive polyamino-ester magneto-dendrimers: Surface functional groups effect on viability of human prostate carcinoma cell lines DU145.

PubMed

Dayyani, Nahid; Khoee, Sepideh; Ramazani, Ali

2015-06-15

Novel pH-sensitive, biocompatible and biodegradable magneto-dendrimers with OH and/or NH2 functional groups based on poly amino-ester were synthesized for delivery of anti-cancer drugs. Magnetite nanoparticles (MNPs) were synthesized by the co-precipitation method and their surfaces were modified by 3-aminopropyl triethoxysilane. The first and second generations of the magneto-dendrimer with hydroxyl end groups were produced by sequential acrylation and Michael addition reactions using the required amounts of acryloyl chloride and diethanolamine, respectively. The dendrimer containing amino functional surface groups up to second generation was synthesized by the same method using the necessary amounts of acryloyl chloride and ethylenediamine. These dendrimers were fully characterized by the Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), dynamic light scattering (DLS) and zeta potential analysis, vibrating-sample magnetometer (VSM), scanning electron microscope (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). In-vitro release profiles of the drug-loaded magnetic nanoparticles and their cytotoxicity assay were investigated at two pHs (7.4 and 5.8). The hydrolytic degradation behavior of magneto-dendrimers was evaluated in PBS buffer. Our research suggests that magneto-dendrimers having amine or hydroxyl functional groups could be considered as the suitable nanocarriers for therapy applications. Copyright © 2015 Elsevier Masson SAS. All rights reserved.

Dynamic balancing of dual-rotor system with very little rotating speed difference.

PubMed

Yang, Jian; He, Shi-zheng; Wang, Le-qin

2003-01-01

Unbalanced vibration in dual-rotor rotating machinery was studied with numerical simulations and experiments. A new method is proposed to separate vibration signals of inner and outer rotors for a system with very little difference in rotating speeds. Magnitudes and phase values of unbalance defects can be obtained directly by sampling the vibration signal synchronized with reference signal. The balancing process is completed by the reciprocity influence coefficients of inner and outer rotors method. Results showed the advantage of such method for a dual-rotor system as compared with conventional balancing.

Perovskite-Type Oxides. I. Structural, Magnetic, and Morphological Properties of LaMn 1- xCu xO 3 and LaCo 1- xCu xO 3 Solid Solutions with Large Surface Area

NASA Astrophysics Data System (ADS)

Porta, Piero; De Rossi, Sergio; Faticanti, Marco; Minelli, Giuliano; Pettiti, Ida; Lisi, Luciana; Turco, Maria

1999-09-01

Perovskite-type compounds of general formula LaMn1-xCuxO3 and LaCo1-xCuxO3 (x=0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared by calcining the citrate gel precursors at 823, 923, and 1073 K. The decomposition of the precursors was followed by thermal analysis and the oxides were investigated by means of elemental analysis (atomic absorption and redox titration), X-ray powder diffraction, BET surface area, X-ray absorption (EXAFS and XANES), electron microscopy (SEM and TEM), and magnetic susceptibility. LaMn1-xCuxO3 samples are perovskite-like single phases up to x=0.6. At x=0.8 CuO and La2CuO4 phases are present in addition to perovskite. For x=1.0 the material is formed by CuO and La2CuO4. Mn(IV) was found by redox titration in all Mn-based perovskite samples, its fraction increasing with the increase in copper content. EXAFS and XANES analyses confirmed the presence of Mn(IV). Cation vacancies in equal amounts in the 12-coordinated A and octahedral B sites are suggested in the samples with x=0.0 and x=0.2, while for x=0.6 anionic vacancies are present. Materials with sufficiently high surface area (22-36 m2 g-1 for samples fired at 923 K and 14-22 m2 g-1 for those fired at 1073 K) were obtained. Crystallite sizes in the ranges 390-500 and 590-940 Å for samples calcined at 923 and 1073 K, respectively, were determined from the FWHM of the (102) X-ray diffraction peak. TEM patterns of LaMnO3 showed almost regular hexagonal prismatic crystals with sizes of the same order of magnitude (800 Å) of those drawn from X-ray diffraction, while no evidence of defect clustering was drawn out from TEM and electron diffraction images. For the sample with x=0.6, TEM and electron diffraction patterns revealed perturbation of the structure. Magnetic susceptibility studies show a ferromagnetic behavior that decreases with increase in x. LaCo1-xCuxO3 samples are perovskite-like single phases up to x=0.2. For x=0.4 a small amount of La2CuO4, in addition to perovskite, is detected. For x≥0.6 massive formation of La2CuO4 and CuO is observed. Only trivalent cobalt is found by redox titration. Magnetic susceptibility studies have shown that trivalent cobalt is present in all samples as a mixture of paramagnetic Co3+ and diamagnetic CoIII ions, the Co3+ fraction being, at least up to x=0.4, equal to ≈0.34. Antiferromagnetic behavior, which increases with increase in x, is observed in all LaCo1-xCuxO3 samples. LaCoO3 is a stoichiometric perovskite. The substitution of cobalt by Cu2+ leads to a positive charge defectivity which is compensated by oxygen vacancies. EXAFS and XANES analyses confirmed the presence of trivalent cobalt. Materials with fairly high surface area (in the ranges 19-27 and 13-21 m2 g-1 for samples calcined at 923 and 1073 K, respectively) were obtained. Crystallite sizes of ≈400 and ≈1000 Å for samples calcined at 923 and 1073 K, respectively, were determined from the FWHM of the (102) X-ray diffraction peak. Materials with not very clear morphology and crystals with definite structure are distinguishable by SEM for samples calcined at 1073 and at 1273 K, respectively. TEM patterns, for samples calcined at 1073 K, evidence almost regular hexagonal prismatic crystals connected to form "linked structures" and some "spotty crystals," suggesting short-range ordered local defects. For copper-containing samples, calcined at 1273 K, a higher degree of defectivity (probably associated with the interaction of anion vacancies) and the occurrence of "planar faults" are shown by TEM.

Ion-Neutron Irradiated BOR60 Sample Preparation and Characterization: Nuclear Science User Facility 2017 Milestone Report

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

Linton, Kory D.; Parish, Chad M.; Smith, Quinlan B.

2017-09-01

This document outlines the results obtained by Oak Ridge National Laboratory (ORNL) in collaboration with the University of Michigan-led Consolidated Innovative Nuclear Research project, “Feasibility of combined ion-neutron irradiation for accessing high dose levels.” In this reporting period, neutron irradiated were prepared and shipped to the University of Michigan for subsequent ion irradiation. The specimens were returned to ORNL’s Low Activation Materials Development and Analysis facility, prepared via focused ion beam for examination using scanning/transmission electron microscopy (S/TEM), and then examined using S/TEM to measure the as-irradiated microstructure. This report briefly summarizes the S/TEM results obtained at ORNL’s Low Activationmore » Materials Development and Analysis facility.« less

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.

Perspectives on in situ electron microscopy

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

Zheng, Haimei; Zhu, Yimei

In situ transmission electron microscopy (TEM) with the ability to reveal materials dynamic processes with high spatial and temporal resolution has attracted significant interest. The recent advances in in situ methods, including liquid and gas sample environment, pump-probe ultrafast microscopy, nanomechanics and ferroelectric domain switching the aberration corrected electron optics as well as fast electron detector has opened new opportunities to extend the impact of in situ TEM in broad areas of research ranging from materials science to chemistry, physics and biology. Here in this paper, we highlight the development of liquid environment electron microscopy and its applications in themore » study of colloidal nanoparticle growth, electrochemical processes and others; in situ study of topological vortices in ferroelectric and ferromagnetic materials. At the end, perspectives of future in situ TEM are provided.« less

Perspectives on in situ electron microscopy

DOE PAGES

Zheng, Haimei; Zhu, Yimei

2017-03-29

In situ transmission electron microscopy (TEM) with the ability to reveal materials dynamic processes with high spatial and temporal resolution has attracted significant interest. The recent advances in in situ methods, including liquid and gas sample environment, pump-probe ultrafast microscopy, nanomechanics and ferroelectric domain switching the aberration corrected electron optics as well as fast electron detector has opened new opportunities to extend the impact of in situ TEM in broad areas of research ranging from materials science to chemistry, physics and biology. Here in this paper, we highlight the development of liquid environment electron microscopy and its applications in themore » study of colloidal nanoparticle growth, electrochemical processes and others; in situ study of topological vortices in ferroelectric and ferromagnetic materials. At the end, perspectives of future in situ TEM are provided.« less

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

The effect of PVP on morphology, optical properties and electron paramagnetic resonance of Zn0.5Co0.5Fe2-xPrxO4 nanoparticles

NASA Astrophysics Data System (ADS)

Bitar, Z.; El-Said Bakeer, D.; Awad, R.

2017-07-01

Zinc Cobalt nano ferrite doped with Praseodymium, Zn0.5Co0.5Fe2-xPrxO4 (0 ≤ x ≤ 0.2), were prepared by co-precipitation method from an aqueous solution containing metal chlorides and two concentrations of poly(vinylpyrrolidone) (PVP) 0 and 30g/L as capping agent. The samples were characterized using X-ray powder diffraction (XRD), Transmission Electron Microscope (TEM), UV-visible optical spectroscopy, Fourier transform infrared (FTIR) and Electron Paramagnetic Resonance (EPR). XRD results display the formation of cubic spinel structure with space group Fd3m and the lattice parameter (a) is slightly decreased for PVP capping samples. The particle size that determined by TEM, decreases for PVP capping samples. The optical band energy Eg increases for PVP capping samples, confirming the variation of energy gap with the particle size. The FTIR results indicate that the metal oxide bands were shifted for the PVP capping samples. EPR data shows that the PVP addition increases the magnetic resonance field and hence decreases the g-factor.

Stability of an aluminum salt-adjuvanted protein D-conjugated pneumococcal vaccine after exposure to subzero temperatures

PubMed Central

Fortpied, Juliette; Wauters, Florence; Rochart, Christelle; Hermand, Philippe; Hoet, Bernard; Moniotte, Nicolas; Vojtek, Ivo

2018-01-01

ABSTRACT Accidental exposure of a vaccine containing an aluminum-salt adjuvant to temperatures below 0°C in the cold chain can lead to freeze damage. Our study evaluated the potential for freeze damage in a licensed aluminum-salt-containing protein-D-conjugated pneumococcal vaccine (PHiD-CV; Synflorix, GSK) in conditions that included static storage, single subzero-temperature excursions, and simulated air-freight transportation. Several parameters were assessed including freezing at subzero temperatures, aluminum-salt-particle size, antigen integrity and immunogenicity in the mouse. The suitability of the WHO's shake test for identifying freeze-damaged vaccines was also assessed. During subzero-temperature excursions, the mean temperatures at which PHiD-CV froze (−16.7°C to −18.1°C) appeared unaffected by the type of vaccine container (two-dose or four-dose vial, or single-dose syringe), vaccine batch, rotational agitation, or the rate of temperature decline (−0.5 to −10°C/hour). At constant subzero temperature and in simulated air-freight transportation, the freezing of PHiD-CV appeared to be promoted by vibration. At −5°C, no PHiD-CV sample froze in static storage (>1 month), whereas when subjected to vibration, a minority of samples froze (7/21, 33%) within 18 hours. At −8°C with vibration, nearly all (5/6, 83%) samples froze. In these vibration regimes, the shake test identified most samples that froze (10/12, 93%) except two in the −5°C regime. Nevertheless, PHiD-CV-antigen integrity appeared unaffected by freezing up to −20°C or by vibration. And although aluminum-salt-particle size was increased only by freezing at −20°C, PHiD-CV immunogenicity appeared only marginally affected by freezing at −20°C. Therefore, our study supports the use of the shake test to exclude freeze-damaged PHiD-CV in the field. PMID:29337646

Effects of high power ultrasonic vibration on the cold compaction of titanium.

PubMed

Fartashvand, Vahid; Abdullah, Amir; Ali Sadough Vanini, Seyed

2017-05-01

Titanium has widely been used in chemical and aerospace industries. In order to overcome the drawbacks of cold compaction of titanium, the process was assisted by an ultrasonic vibration system. For this purpose, a uniaxial ultrasonic assisted cold powder compaction system was designed and fabricated. The process variables were powder size, compaction pressure and initial powder compact thickness. Density, friction force, ejection force and spring back of the fabricated samples were measured and studied. The density was observed to improve under the action of ultrasonic vibration. Fine size powders showed better results of consolidation while using ultrasonic vibration. Under the ultrasonic action, it is thought that the friction forces between the die walls and the particles and those friction forces among the powder particles are reduced. Spring back and ejection force didn't considerably change when using ultrasonic vibration. Copyright © 2016 Elsevier B.V. All rights reserved.

Construction of Two-Axis Acceleration Sensor Using a Cross-Coupled Vibrator

NASA Astrophysics Data System (ADS)

Terada, Jiro; Uetsuji, Yasutomo; Sugawara, Sumio

2012-10-01

We describe an acceleration sensor composed of four vibration bars, with a detection mechanism in which the resonant frequencies of the four bars are brought close together. The bars are connected mechanically at the center, and a cross-shaped layout is used such that for any load direction, the sizes of the loads on the vibration bars mutually oppose each other. Using this structure, acceleration can be easily calculated by differential detection of the oscillation amplitude signals of each of the four vibration bars. The body of the sensor is made of stainless steel (SUS304). The volume of the experimental sample is about 76 ×76 ×8 mm3, and the resonance frequency and quality factor are about 1041 Hz and 87, respectively. The sensor characteristics are measured using the gravitational field, and the acceleration is changed by rotating the sensor around the axis along the length of the vibrator.

Vibration and acoustic noise emitted by dry-type air-core reactors under PWM voltage excitation

NASA Astrophysics Data System (ADS)

Li, Jingsong; Wang, Shanming; Hong, Jianfeng; Yang, Zhanlu; Jiang, Shengqian; Xia, Shichong

2018-05-01

According to coupling way between the magnetic field and the structural order, structure mode is discussed by engaging finite element (FE) method and both natural frequency and modal shape for a dry-type air-core reactor (DAR) are obtained in this paper. On the basis of harmonic response analysis, electromagnetic force under PWM (Pulse Width Modulation) voltage excitation is mapped with the structure mesh, the vibration spectrum is gained and the consequences represents that the whole structure vibration predominates in the radial direction, with less axial vibration. Referring to the test standard of reactor noise, the rules of emitted noise of the DAR are measured and analyzed at chosen switching frequency matches the sample resonant frequency and the methods of active vibration and noise reduction are put forward. Finally, the low acoustic noise emission of a prototype DAR is verified by measurement.

Towards identifying the dynamics of sliding by acoustic emission and vibration

NASA Astrophysics Data System (ADS)

Korchuganov, M. A.; Filippov, A. V.; Tarasov, S. Yu.; Podgornyh, O. A.; Shamarin, N. N.; Filippova, E. O.

2016-11-01

The results of experiments with high load and sliding speed sliding conditions on tribologically mated pairs such as steel 1045/steel 1045 (test 1), steel 1045/basalt (test 2) and Hadfield steel/basalt (test 3) have been carried out in order to identify their response in terms of the acoustic emission and vibration signals. The steel to rock and rock to steel transfer has been revealed by examining the worn surfaces of both steel and rock samples with the use of laser scanning microscopy. The AE signal characteristics have been determined for the tribological pairs studied. The dynamics of sliding has been evaluated by measuring the vibration accelerations. Relationship between wear mode and either acoustic emission signal or vibration signal has been established. The minimal vibration oscillations amplitude and acoustic emission signal energy have been found out in sliding Hadfield steel/basalt pair.

Young's modulus and internal friction of the SiC/Si biomorphic composite based on the sapele wood precursor

NASA Astrophysics Data System (ADS)

Kardashev, B. K.; Orlova, T. S.; Smirnov, B. I.; de Arellano-Lopez, A. R.; Martinez-Fernandez, J.

2009-04-01

The effect of the vibrational strain amplitude on the Young’s modulus and ultrasound absorption (internal friction) of a SiC/Si biomorphic composite prepared by pyrolysis of sapele wood followed by infiltration of silicon were investigated. The studies were conducted in air and in vacuum by the acoustic resonance method with the use of a composite vibrator in longitudinal vibrations at frequencies of about 100 kHz. Measurements performed on sapele wood-based bio-SiC/Si samples revealed a substantial effect of adsorption-desorption of molecules contained in air on the effective elasticity modulus and elastic vibration decrement. Microplastic characteristics of the SiC/Si composites prepared from wood of different tree species were compared.

Elasticity and inelasticity of biomorphic carbon, silicon carbide, and SiC/Si composite produced on the basis of medium density fiberboard

NASA Astrophysics Data System (ADS)

Kardashev, B. K.; Orlova, T. S.; Smirnov, B. I.; de Arellano-Lopez, A. R.; Martinez-Fernandez, J.

2010-10-01

The amplitude and temperature dependences of the Young’s modulus and the internal friction (ultrasonic absorption) of biomorphic carbon, silicon carbide, and SiC/Si composite produced from medium density fiberboard (MDF) by pyrolysis (carbonization), followed by infiltration of molten silicon into the prepared carbon preform have been studied in the temperature range 100-293 K in air and under vacuum. The measurements have been performed by the acoustic resonance method with the use of a composite vibrator for longitudinal vibrations at frequencies of approximately 100 kHz. The data obtained by acoustic measurements of the amplitude dependences of the elastic modulus have been used for evaluating the microplastic properties of samples under study. It has been shown that the Young’s modulus, the decrement of elastic vibrations, and the conventional microyield strength of the MDF samples differ from the corresponding data for previously studied similar materials produced from natural eucalyptus, beech, sapele, and pine woods. In particular, the desorption of environmental molecules at small amplitudes of vibrations, which is typical of biomorphic materials based on natural wood, is almost absent for the MDF samples. The results obtained have been explained by different structures and the influence of pores and other defects, which, to a large extent, determine the mechanical characteristics of the biomaterials under investigation.

Evaluating degradation of silk's fibroin by attenuated total reflectance infrared spectroscopy: Case study of ancient banners from Polish collections

NASA Astrophysics Data System (ADS)

Koperska, M. A.; Łojewski, T.; Łojewska, J.

2015-01-01

In this study a part of research where artificially aged model samples were used as a guideline to the mechanism of degradation is presented. In previous work Bombyx Mori silk samples were exposed to various environments such as different oxygen, water vapour and volatile organic products content, all at the temperature of 150 °C [11]. Based on those results gathered with by Attenuated Total Reflectance/Fourier Transform Infrared Spectroscopy (ATR-FTIR) the degradation estimators were proposed and classified as follows: Primary functional groups estimators EAmideI/II - intensity ratios of Amide I Cdbnd O stretching vibration to Amide II Nsbnd H in-plane bending and Csbnd N stretching vibrations A1620/A1514. ECOOH - band 1318 cm-1 integral to band integral of CH3 bending vibration band located at 1442 cm-1P1318/P1442. Secondary conformational estimators EcCdbndO2 - intensity ratios within Amide I Cdbnd O stretching vibration of parallel β-sheet to antiparallel β-sheet A1620/A1699. In this work estimators were verified against estimators calculated from spectra of silk samples from 8 museum objects: 3 from 19th, 2 from 18th, 1 from 17th and 2 from 16th century including 3 banners from the storage resources of the Wawel Royal Castle in Cracow, Poland.

Effects of Short-Period Whole-Body Vibration of 20 Hz on Selected Blood Biomarkers in Wistar Rats.

PubMed

Monteiro, Milena de Oliveira Bravo; de Sá-Caputo, Danúbia da Cunha; Carmo, Fernanda Santos do; Bernardo, Raquel Mattos; Pacheco, Raphaelle; Arnóbio, Adriano; Guimarães, Carlos Alberto Sampaio; Bernardo, Luciana Camargo; Santos-Filho, Sebastião David; Asad, Nasser Ribeiro; Unger, Marianne; Marin, Pedro Jesus; Bernardo-Filho, Mario

2015-08-31

There is a growing interest in the use of vibration generated by oscillating/vibratory platforms - also known as whole-body vibration (WBV) - for achieving therapeutic, preventative and/or physical performance goals. This study investigated the effects of vibration generated by an oscillating platform on the concentration of blood biomarkers in rats. Wistar rats (n = 8) were divided in 2 groups, sedated and individually positioned on an oscillating platform. The experimental group (EG) was subjected to vibrations of 20 Hz for one min per day for one week while the control group (CG) experienced no vibration. Samples of heparinized whole blood were drawn by cardiac puncture for biochemical analysis. Concentrations of total cholesterol, triglycerides, HDL, LDL, VLDL, glucose, CK, albumin, alkaline phosphates, TGP, TGO, γGT, lipase, amylase, urea and creatinine were determined. White blood cell count and a platelet hemogram were also performed. Following seven sessions of exposure to the vibration, a significant (P < 0.05) reduction in γGT, VLDL and leukocytes was found. A weekly 1-min/day exposure of 20 Hz vibration can was shown to alter the concentrations of selected blood biomarkers in rats. The action mechanism associated with these effects seems highly complex, but the findings might contribute to the understanding of these mechanisms related to the exposure to 20 Hz vibration.

Dose-response relation between exposure to two types of hand-arm vibration and sensorineural perception of vibration.

PubMed Central

Virokannas, H

1995-01-01

OBJECTIVES--31 railway workers and 32 lumberjacks were examined to compare the dose-response relation between the exposure to two types of hand-arm vibration and the sensory disturbances in peripheral nerves as evaluated by the vibration perception thresholds (VPTs). METHODS--Clinical examinations were carried out that included measurements of the VPTs, and electroneuromyography (ENMG), and an inquiry to confirm the use of vibrating tools. Diseases of the central nervous system and neuropathies were checked by inquiry and a clinical examination, diabetes was excluded by a blood sample analysis, and the subjects with carpal tunnel syndrome confirmed with ENMG were excluded from the study. RESULTS--Lifetime use of hand held tamping machines (railway workers) and chain saws (lumberjacks) had a significant correlation with the VPTs at frequencies from 32 to 500 Hz. The increase of the VPTs (250 Hz) in relation to use of vibrating tools was 1.8-fold higher on average in the whole group and 2.3-fold higher in the young (< 45) railway workers who had used hand held tamping machines, than in the corresponding groups of lumberjacks, who had used chain saws, whereas the frequency weighted acceleration of vibration in tamping machines was fourfold. CONCLUSION--There was a significant dose-response relation between the exposure to hand-arm vibration and the VPTs. The VPTs as a function of the frequency weighted acceleration of vibration and the exposure to vibration gave promising results for assessment of the risk of damage to sensory nerves induced by vibration. PMID:7795756

Effects of seated posture on erector spinae EMG activity during whole body vibration.

PubMed

Zimmermann, C L; Cook, T M; Goel, V K

1993-06-01

The purpose of this study was to evaluate the electromyographic (EMG) response of the erector spinae to whole body vibration in three different unsupported seated postures: neutral upright, forward lean, and posterior lean. Subjects were 11 healthy college-age men. EMG was collected using bipolar surface electrodes placed bilaterally over the erector spinae at the L4 level. A modified chair with attached accelerometer was affixed to an induction type vibrator. Subjects were vibrated vertically at 4.5 Hz and 6.21 m.s-2 RMS. Data were collected in each of the three postures for 30 s pre- and post-vibration and for 2 min during vibration. Mean EMG values were determined for each sampling period and compared using ANOVA. The mean value for anterior lean was significantly larger (p < 0.05) than that for posterior lean and neutral. EMG data analysed by triggered averaging showed a phase-dependent response to the vibratory cycle for the forward leaning and neutral upright postures. The results of this study indicate that the magnitude of the vibration synchronous response of the erector spinae musculature is dependent upon body posture. This response may be an important factor in the onset of muscular fatigue and the increased incidence of back disorders among individuals exposed to whole body vibration.

Effects of whole body vibration on muscle spasticity for people with central nervous system disorders: a systematic review.

PubMed

Huang, Meizhen; Liao, Lin-Rong; Pang, Marco Yc

2017-01-01

To examine the effects of whole-body vibration on spasticity among people with central nervous system disorders. Electronic searches were conducted using CINAHL, Cochrane Library, MEDLINE, Physiotherapy Evidence Database, PubMed, PsycINFO, SPORTDiscus and Scopus to identify randomized controlled trials that investigated the effect of whole-body vibration on spasticity among people with central nervous system disorders (last search in August 2015). The methodological quality and level of evidence were rated using the PEDro scale and guidelines set by the Oxford Centre for Evidence-Based Medicine. Nine trials with totally 266 subjects (three in cerebral palsy, one in multiple sclerosis, one in spinocerebellar ataxia, and four in stroke) fulfilled all selection criteria. One study was level 1b (PEDro⩾6 and sample size>50) and eight were level 2b (PEDro<6 or sample size ⩽50). All three cerebral palsy trials (level 2b) reported some beneficial effects of whole-body vibration on reducing leg muscle spasticity. Otherwise, the results revealed no consistent benefits on spasticity in other neurological conditions studied. There is little evidence that change in spasticity was related to change in functional performance. The optimal protocol could not be identified. Many reviewed studies were limited by weak methodological and reporting quality. Adverse events were minor and rare. Whole-body vibration may be useful in reducing leg muscle spasticity in cerebral palsy but this needs to be verified by future high quality trials. There is insufficient evidence to support or refute the notion that whole-body vibration can reduce spasticity in stroke, spinocerebellar ataxia or multiple sclerosis.

The effect of whole-body resonance vibration in a porcine model of spinal cord injury.

PubMed

Streijger, Femke; Lee, Jae H T; Chak, Jason; Dressler, Dan; Manouchehri, Neda; Okon, Elena B; Anderson, Lisa M; Melnyk, Angela D; Cripton, Peter A; Kwon, Brian K

2015-06-15

Whole-body vibration has been identified as a potential stressor to spinal cord injury (SCI) patients during pre-hospital transportation. However, the effect that such vibration has on the acutely injured spinal cord is largely unknown, particularly in the frequency domain of 5 Hz in which resonance of the spine occurs. The objective of the study was to investigate the consequences of resonance vibration on the injured spinal cord. Using our previously characterized porcine model of SCI, we subjected animals to resonance vibration (5.7±0.46 Hz) or no vibration for a period of 1.5 or 3.0 h. Locomotor function was assessed weekly and cerebrospinal fluid (CSF) samples were collected to assess different inflammatory and injury severity markers. Spinal cords were evaluated histologically to quantify preserved white and gray matter. No significant differences were found between groups for CSF levels of monocyte chemotactic protein-1, interleukin 6 (IL-6) and lL-8. Glial fibrillary acidic protein levels were lower in the resonance vibration group, compared with the non-vibrated control group. Spared white matter tissue was increased within the vibrated group at 7 d post-injury but this difference was not apparent at the 12-week time-point. No significant difference was observed in locomotor recovery following resonance vibration of the spine. Here, we demonstrate that exposure to resonance vibration for 1.5 or 3 h following SCI in our porcine model is not detrimental to the functional or histological outcomes. Our observation that a 3.0-h period of vibration at resonance frequency induces modest histological improvement at one week post-injury warrants further study.

Characteristics of vibrator use by gay and bisexually identified men in the United States.

PubMed

Reece, Michael; Rosenberger, Joshua G; Schick, Vanessa; Herbenick, Debby; Dodge, Brian; Novak, David S

2010-10-01

Recent reports indicate that vibrator use during solo and partnered sexual activities is common among heterosexual men and women in the United States. However, little research has comprehensively assessed vibrator use among gay and bisexually identified men. This study sought to document the extent to which gay and bisexually identified men report using vibrators, the sexual and relational situations within which they use them, and how men use vibrators on their own and their partners' bodies. Data were collected from 25,294 gay and bisexually identified men from 50 U.S. states and from the District of Columbia via an internet-based survey. Measures included sociodemographics, health-related indicators, sexual behaviors, and those related to recent and past use of vibrators during solo and partnered sexual interactions with other men. Approximately half (49.8%) of gay and bisexually identified men reported having used vibrators. Most men who had used a vibrator in the past reported use during masturbation (86.2%). When used during partnered interactions, vibrators were incorporated into foreplay (65.9%) and intercourse (59.4%). Men reported frequent insertion of vibrators into the anus or rectum when using them during masturbation (87.3%), which was also common during partnered interactions (∼60%), but varied slightly for casual and relationship sex partners. For both masturbation and partnered interactions, men overwhelmingly endorsed the extent to which vibrator use contributed to sexual arousal, orgasm, and pleasure. Vibrator use during both solo and partnered sexual acts was common among the gay and bisexually identified men in this sample and was described by men as adding to the quality of their sexual experiences. © 2010 International Society for Sexual Medicine.

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.

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

PubMed

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

2017-09-12

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

Focused ion beam (FIB)/scanning electron microscopy (SEM) in tissue structural research.

PubMed

Leser, Vladka; Milani, Marziale; Tatti, Francesco; Tkalec, Ziva Pipan; Strus, Jasna; Drobne, Damjana

2010-10-01

The focused ion beam (FIB) and scanning electron microscope (SEM) are commonly used in material sciences for imaging and analysis of materials. Over the last decade, the combined FIB/SEM system has proven to be also applicable in the life sciences. We have examined the potential of the focused ion beam/scanning electron microscope system for the investigation of biological tissues of the model organism Porcellio scaber (Crustacea: Isopoda). Tissue from digestive glands was prepared as for conventional SEM or as for transmission electron microscopy (TEM). The samples were transferred into FIB/SEM for FIB milling and an imaging operation. FIB-milled regions were secondary electron imaged, back-scattered electron imaged, or energy dispersive X-ray (EDX) analyzed. Our results demonstrated that FIB/SEM enables simultaneous investigation of sample gross morphology, cell surface characteristics, and subsurface structures. The same FIB-exposed regions were analyzed by EDX to provide basic compositional data. When samples were prepared as for TEM, the information obtained with FIB/SEM is comparable, though at limited magnification, to that obtained from TEM. A combination of imaging, micro-manipulation, and compositional analysis appears of particular interest in the investigation of epithelial tissues, which are subjected to various endogenous and exogenous conditions affecting their structure and function. The FIB/SEM is a promising tool for an overall examination of epithelial tissue under normal, stressed, or pathological conditions.

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

PubMed

Drobne, Damjana

2013-01-01

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

Carbon Nanotube and Nanofiber Exposure Assessments: An Analysis of 14 Site Visits.

PubMed

Dahm, Matthew M; Schubauer-Berigan, Mary K; Evans, Douglas E; Birch, M Eileen; Fernback, Joseph E; Deddens, James A

2015-07-01

Recent evidence has suggested the potential for wide-ranging health effects that could result from exposure to carbon nanotubes (CNT) and carbon nanofibers (CNF). In response, the National Institute for Occupational Safety and Health (NIOSH) set a recommended exposure limit (REL) for CNT and CNF: 1 µg m(-3) as an 8-h time weighted average (TWA) of elemental carbon (EC) for the respirable size fraction. The purpose of this study was to conduct an industrywide exposure assessment among US CNT and CNF manufacturers and users. Fourteen total sites were visited to assess exposures to CNT (13 sites) and CNF (1 site). Personal breathing zone (PBZ) and area samples were collected for both the inhalable and respirable mass concentration of EC, using NIOSH Method 5040. Inhalable PBZ samples were collected at nine sites while at the remaining five sites both respirable and inhalable PBZ samples were collected side-by-side. Transmission electron microscopy (TEM) PBZ and area samples were also collected at the inhalable size fraction and analyzed to quantify and size CNT and CNF agglomerate and fibrous exposures. Respirable EC PBZ concentrations ranged from 0.02 to 2.94 µg m(-3) with a geometric mean (GM) of 0.34 µg m(-3) and an 8-h TWA of 0.16 µg m(-3). PBZ samples at the inhalable size fraction for EC ranged from 0.01 to 79.57 µg m(-3) with a GM of 1.21 µg m(-3). PBZ samples analyzed by TEM showed concentrations ranging from 0.0001 to 1.613 CNT or CNF-structures per cm(3) with a GM of 0.008 and an 8-h TWA concentration of 0.003. The most common CNT structure sizes were found to be larger agglomerates in the 2-5 µm range as well as agglomerates >5 µm. A statistically significant correlation was observed between the inhalable samples for the mass of EC and structure counts by TEM (Spearman ρ = 0.39, P < 0.0001). Overall, EC PBZ and area TWA samples were below the NIOSH REL (96% were <1 μg m(-3) at the respirable size fraction), while 30% of the inhalable PBZ EC samples were found to be >1 μg m(-3). Until more information is known about health effects associated with larger agglomerates, it seems prudent to assess worker exposure to airborne CNT and CNF materials by monitoring EC at both the respirable and inhalable size fractions. Concurrent TEM samples should be collected to confirm the presence of CNT and CNF. Published by Oxford University Press on behalf of the British Occupational Hygiene Society 2015.

Sensitization of a stray-field NMR to vibrations: a potential for MR elastometry with a portable NMR sensor.

PubMed

Mastikhin, Igor; Barnhill, Marie

2014-11-01

An NMR signal from a sample in a constant stray field of a portable NMR sensor is sensitized to vibrations. The CPMG sequence is synchronized to vibrations so that the constant gradient becomes an "effective" square-wave gradient, leading to the vibration-induced phase accumulation. The integrating nature of the spot measurement, combined with the phase distribution due to a non-uniform gradient and/or a wave field, leads to a destructive interference, the drop in the signal intensity and changes in the echo train shape. Vibrations with amplitudes as small as 140 nm were reliably detected with the permanent gradient of 12.4 T/m. The signal intensity depends on the phase offset between the vibrations and the pulse sequence. This approach opens the way for performing elastometry and micro-rheology measurements with portable NMR devices beyond the walls of a laboratory. Even without synchronization, if a vibration frequency is comparable to 1/2TE of the CPMG sequence, the signal can be severely affected, making it important for potential industrial applications of stray-field NMR. Copyright © 2014 Elsevier Inc. All rights reserved.

Statistical analysis of low frequency vibrations in variable speed wind turbines

NASA Astrophysics Data System (ADS)

Escaler, X.; Mebarki, T.

2013-12-01

The spectral content of the low frequency vibrations in the band from 0 to 10 Hz measured in full scale wind turbines has been statistically analyzed as a function of the whole range of steady operating conditions. Attention has been given to the amplitudes of the vibration peaks and their dependency on rotating speed and power output. Two different wind turbine models of 800 and 2000 kW have been compared. For each model, a sample of units located in the same wind farm and operating during a representative period of time have been considered. A condition monitoring system installed in each wind turbine has been used to register the axial acceleration on the gearbox casing between the intermediate and the high speed shafts. The average frequency spectrum has permitted to identify the vibration signature and the position of the first tower natural frequency in both models. The evolution of the vibration amplitudes at the rotor rotating frequency and its multiples has shown that the tower response is amplified by resonance conditions in one of the models. So, it is concluded that a continuous measurement and control of low frequency vibrations is required to protect the turbines against harmful vibrations of this nature.

Polarization Sensitive Coherent Anti-Stokes Raman Spectroscopy of DCVJ in Doped Polymer

NASA Astrophysics Data System (ADS)

Ujj, Laszlo

2014-05-01

Coherent Raman Microscopy is an emerging technic and method to image biological samples such as living cells by recording vibrational fingerprints of molecules with high spatial resolution. The race is on to record the entire image during the shortest time possible in order to increase the time resolution of the recorded cellular events. The electronically enhanced polarization sensitive version of Coherent anti-Stokes Raman scattering is one of the method which can shorten the recording time and increase the sharpness of an image by enhancing the signal level of special molecular vibrational modes. In order to show the effectiveness of the method a model system, a highly fluorescence sample, DCVJ in a polymer matrix is investigated. Polarization sensitive resonance CARS spectra are recorded and analyzed. Vibrational signatures are extracted with model independent methods. Details of the measurements and data analysis will be presented. The author gratefully acknowledge the UWF for financial support.

Stability of athlete blood passport parameters during air freight.

PubMed

Ashenden, M; Sharpe, K; Plowman, J; Allbon, G; Lobigs, L; Baron, A; Gore, C J

2014-10-01

Fluctuations in ambient temperature and pressure, as well as physical jostling, may affect the stability of whole blood samples transported by air freight. The aim of this study was to characterize the stability of key blood variables during air freight and to investigate whether vibration or reduced pressure alone affected results. Over a 72-h interval, we evaluated the stability of full blood count indices (plus reticulocytes) in tubes that were air-freighted a total of 2, 10 and 28 h. We also examined the impact of 24 h of reduced atmospheric pressure (750 hpa or approximately 2500 m.a.s.l) and vibration (5 Hz). Samples were measured on a Sysmex XT-2000i instrument. The two key variables in the context of antidoping (haemoglobin concentration, reticulocytes) remained stable over a 72-h period regardless of the duration of air freight. Atmospheric pressure and vibration had no discernible effect. Whole blood samples stored in NanoCool devices can be relied upon to remain stable for at least 72 h despite interim air freight. © 2013 John Wiley & Sons Ltd.

Spectroscopic characterization of rare hydrated ammonium borate mineral larderellite

NASA Astrophysics Data System (ADS)

Korybska-Sadło, Iwona; Sitarz, Maciej; Król, Magdalena; Bartz, Wojciech; Prell, Marta; Gunia, Piotr

2018-05-01

Two samples of larderellite (NH4)B5O7(OH)2·H2O from Monte Rotonda (Italy) have been studied. Spectroscopic methods, like infrared and Raman spectroscopy, were used in combination with thermal analysis and X-ray diffraction. The main objective was vibrational characteristic of research mineral and, based on the obtained results, test how the long storage of minerals affect their structure. Raman and infrared spectroscopy confirm the presence of tetrahedral and trigonal boron structural units in the investigated samples. The most intensive Raman band is located at 149 cm-1 and is assigned to lattice vibration. The most intensive infrared bands, located at 1209 and 1273 cm-1, are ascribed as in-plane modes (δ) of Bsbnd Osbnd H. Bands associated with water bending mode (ν2) and stretching vibration (ν1) are observed at 1668 cm-1 (IR) and in the 3000-3500 cm-1 region (both Raman and IR spectrum). Thermal analysis showed differences between two research samples of larderellite connected with presence of adsorption water, that can indicate influence of conditions of minerals storage on properties of mineral.

Methods for Determining Particle Size Distributions from Nuclear Detonations.

DTIC Science & Technology

1987-03-01

Debris . . . 30 IV. Summary of Sample Preparation Method . . . . 35 V. Set Parameters for PCS ... ........... 39 VI. Analysis by Vendors...54 XV. Results From Brookhaven Analysis Using The Method of Cumulants ... ........... . 54 XVI. Results From Brookhaven Analysis of Sample...R-3 Using Histogram Method ......... .55 XVII. Results From Brookhaven Analysis of Sample R-8 Using Histogram Method ........... 56 XVIII.TEM Particle

Facile combustion synthesis of ZnO nanoparticles using Cajanus cajan (L.) and its multidisciplinary applications

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

Manjunath, K.; Ravishankar, T.N.; Kumar, Dhanith

Graphical abstract: Facile combustion synthesis of ZnO nanoparticles using Cajanuscajan (L.) and its multidisciplinary applications.Zinc oxide nanoparticles were successfully synthesized by solution combustion method (SCM) using pigeon pea as a combustible fuel for the first time. The as-prepared product shows good photocatalytic, dielectric, antibacterial, electrochemical properties. - Highlights: • ZnO Nps were synthesized via combustion method using pigeon pea as a fuel. • The structure of the product was confirmed by XRD technique. • The morphology was confirmed by SEM and TEM images. • The as-prepared product shown good photocatalytic activity, dielectric property. • It has also shown good antibacterialmore » and electrochemical properties. - Abstract: Zinc oxide nanoparticles (ZnO Nps) were successfully synthesized by solution combustion method (SCM) using pigeon pea as a fuel for the first time. X-Ray diffraction pattern reveals that the product belongs to hexagonal system. FTIR spectrum of ZnO Nps shows the band at 420 cm{sup −1} associated with the characteristic vibration of Zn–O. TEM images show that the nanoparticles are found to be ∼40–80 nm. Furthermore, the as-prepared ZnO Nps exhibits good photocatalytic activity for the photodegradation of methylene blue (MB), indicating that they are indeed a promising photocatalytic semiconductor. The antibacterial properties of ZnO nanopowders were investigated by their bactericidal activity against four bacterial strains.« less

FTIR and Raman spectroscopic studies of selenium nanoparticles synthesised by the bacterium Azospirillum thiophilum

NASA Astrophysics Data System (ADS)

Tugarova, Anna V.; Mamchenkova, Polina V.; Dyatlova, Yulia A.; Kamnev, Alexander A.

2018-03-01

Vibrational (Fourier transform infrared (FTIR) and Raman) spectroscopic techniques can provide unique molecular-level information on the structural and compositional characteristics of complicated biological objects. Thus, their applications in microbiology and related fields are steadily increasing. In this communication, biogenic selenium nanoparticles (Se NPs) were obtained via selenite (SeO32-) reduction by the bacterium Azospirillum thiophilum (strain VKM B-2513) for the first time, using an original methodology for obtaining extracellular NPs. Dynamic light scattering (DLS) and transmission electron microscopy (TEM) showed the Se NPs to have average diameters within 160-250 nm; their zeta potential was measured to be minus 18.5 mV. Transmission FTIR spectra of the Se NPs separated from bacterial cells showed typical proteinacious, polysaccharide and lipid-related bands, in line with TEM data showing a thin layer covering the Se NPs surface. Raman spectra of dried Se NPs layer in the low-frequency region (under 500 cm-1 down to 150 cm-1) showed a single very strong band with a maximum at 250 cm-1 which, in line with its increased width (ca. 30 cm-1 at half intensity), can be attributed to amorphous elementary Se. Thus, a combination of FTIR and Raman spectroscopic approaches is highly informative in non-destructive analysis of structural and compositional properties of biogenic Se NPs.

Bio-synthesis and antimicrobial activity of silver nanoparticles using anaerobically digested parthenium slurry.

PubMed

Adur, Alaknanda J; Nandini, N; Shilpashree Mayachar, K; Ramya, R; Srinatha, N

2018-06-01

Silver nanoparticles were prepared through eco-friendly, cost effective, bio-mediated technique using anaerobically digested Parthenium hysterophorous digested slurry (PDS) for the first time. The synthesized nanoparticles were characterized through different techniques such as UV-Vis spectrophotometer for optical properties; X-ray diffractometer (XRD), high resolution transmission electron spectroscopy (HR-TEM) and Fourier Transform Infra Red (FTIR) Spectroscopy for structural property investigations. It was observed that the prepared silver nanoparticles were crystallized in face centered cubic crystal structure with an average particle size of 19 nm as confirmed from XRD. Also HR-TEM studies reveal the formation of nano-sized silver particles with face centered cubic nano structure. In addition, absorption spectra exhibit Surface Plasmon Resonance (SPR) which suggests the formation of silver nanoparticles. FTIR results show the presence of different characteristic functional groups and their stretching / bending vibrations in turn responsible for the bioreduction of silver ions in Parthenium digested slurry. Further investigations on antimicrobial activity were done by subjecting the synthesized silver nanoparticles on E-coli and Pseudomonas as marker organisms for the group of gram negative bacteria by well plate method on enrichment media. The result obtained shows a clear zone of inhibition confirming the antibacterial activity. Overall, the investigated results confirm the biosynthesized silver nanoparticles are potential candidates for antimicrobial activity applications. Copyright © 2018 Elsevier B.V. All rights reserved.

Whole blood coagulation assays ROTEM and T-TAS to monitor dabigatran treatment.

PubMed

Taune, Viktor; Wallén, Håkan; Ågren, Anna; Gryfelt, Gunilla; Sjövik, Carolina; Wintler, Anna M; Malmström, Rickard E; Wikman, Agneta; Skeppholm, Mika

2017-05-01

A rapid and reliable assessment of the dabigatran effect is desirable in dabigatran treated patients with uncontrolled bleeding or before acute surgery. To evaluate how the viscoelastic point-of-care test Rotational thromboelastometry (ROTEM) and Total Thrombus-formation system (T-TAS), which studies thrombus formation under flowing conditions, correlate with dabigatran concentrations in patients with atrial fibrillation (AF). ROTEM using the reagents In-tem, Ex-tem, Fib-tem or low tissue factor concentration (TF), and T-TAS with the AR-chip (shear rate 600s -1 , representing flow in large arteries) were investigated in whole blood samples. Plasma concentrations were determined by mass spectrometry (LC-MS/MS) at trough and post-dose in 30 patients on dabigatran 150mg BID. Median plasma dabigatran concentrations at trough were 86ng/mL (29-150) and post-dose (2.8h after ingestion) 175ng/mL (67-490). The ROTEM clotting time (CT) correlated strongly with dabigatran concentrations when activated with the reagents Ex-tem (r=0.92, p<0.01) and Fib-tem (r=0.93, p<0.01), while with In-tem and low TF the correlation was weaker (r=0.72 and r=0.36, p<0.01). There were significant but weaker correlations also between dabigatran concentrations and T-TAS variables (r-values 0.39-0.41, p<0.01), aPTT (r=0.70, p<0.01) and PT-INR (r=0.43, p<0.01) respectively. ROTEM Ex-tem and Fib-tem CT shows a strong correlation with dabigatran concentrations in real-life AF-patients, and results are obtained within minutes. This could make ROTEM useful in acute situations. T-TAS detect differences in hemostasis caused by dabigatran, but the relationships to plasma concentrations of dabigatran are weaker than for ROTEM CT with the settings used in this study. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fabrication of Fe{sub 3}O{sub 4}@CuO core-shell from MOF based materials and its antibacterial activity

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

Rajabi, S.K.; Sohrabnezhad, Sh., E-mail: sohrabnezhad@guilan.ac.ir; Ghafourian, S.

Magnetic Fe{sub 3}O{sub 4}@CuO nanocomposite with a core/shell structure was successfully synthesized via direct calcinations of magnetic Fe{sub 3}O{sub 4}@HKUST-1 in air atmosphere. The morphology, structure, magnetic and porous properties of the as-synthesized nano composites were characterized by using scanning electron microscope (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (PXRD), and vibration sample magnetometer (VSM). The results showed that the nanocomposite material included a Fe{sub 3}O{sub 4} core and a CuO shell. The Fe{sub 3}O{sub 4}@CuO core-shell can be separated easily from the medium by a small magnet. The antibacterial activity of Fe{sub 3}O{sub 4}-CuO core-shell was investigated againstmore » gram-positive and gram-negative bacteria. A new mechanism was proposed for inactivation of bacteria over the prepared sample. It was demonstrated that the core-shell exhibit recyclable antibacterial activity, acting as an ideal long-acting antibacterial agent. - Graphical abstract: Fe{sub 3}O{sub 4}@CuO core-shell release of copper ions. These Cu{sup 2+} ions were responsible for the exhibited antibacterial activity. - Highlights: • The Fe{sub 3}O{sub 4}@CuO core-shell was prepared by MOF method. • This is the first study of antibacterial activity of core-shell consist of CuO and Fe{sub 3}O{sub 4}. • The core-shell can be reused effectively. • Core-shell was separated from the reaction solution by external magnetic field.« less

Structural, optical and magnetic studies of CuFe2O4, MgFe2O4 and ZnFe2O4 nanoparticles prepared by hydrothermal/solvothermal method

NASA Astrophysics Data System (ADS)

Kurian, Jessyamma; Mathew, M. Jacob

2018-04-01

In this paper we report the structural, optical and magnetic studies of three spinel ferrites namely CuFe2O4, MgFe2O4 and ZnFe2O4 prepared in an autoclave under the same physical conditions but with two different liquid medium and different surfactant. We use water as the medium and trisodium citrate as the surfactant for one method (Hydrothermal method) and ethylene glycol as the medium and poly ethylene glycol as the surfactant for the second method (solvothermal method). The phase identification and structural characterization are done using XRD and morphological studies are carried out by TEM. Cubical and porous spherical morphologies are obtained for hydrothermal and solvothermal process respectively without any impurity phase. The optical studies are carried out using FTIR and UV-Vis reflectance spectra. In order to elucidate the nonlinear optical behaviour of the prepared nanomaterial, open aperture z-scan technique is used. From the fitted z-scan curves nonlinear absorption coefficient and the saturation intensity are determined. The magnetic characterization of the samples is performed at room temperature using vibrating sample magnetometer measurements. The M-H curves obtained are fitted using theoretical equation and the different components of magnetization are determined. Nanoparticles with high saturation magnetization are obtained for MgFe2O4 and ZnFe2O4 prepared under solvothermal reaction. The magnetic hyperfine parameters and the cation distribution of the prepared materials are determined using room temperature Mössbauer spectroscopy. The fitted spectra reveal the difference in the magnetic hyperfine parameters owing to the change in size and morphology.

Click Synthesis of Hydrophilic Maltose-Functionalized Iron Oxide Magnetic Nanoparticles Based on Dopamine Anchors for Highly Selective Enrichment of Glycopeptides.

PubMed

Bi, Changfen; Zhao, Yingran; Shen, Lijin; Zhang, Kai; He, Xiwen; Chen, Langxing; Zhang, Yukui

2015-11-11

The development of methods to isolate and enrich low-abundance glycopeptides from biological samples is crucial to glycoproteomics. Herein, we present an easy and one-step surface modification strategy to prepare hydrophilic maltose functionalized Fe3O4 nanoparticles (NPs). First, based on the chelation of the catechol ligand with iron atoms, azido-terminated dopamine (DA) derivative was assembled on the surface of magnetic Fe3O4 nanoparticles by sonication. Second, the hydrophilic maltose-functionalized Fe3O4 (Fe3O4-DA-Maltose) NPs were obtained via copper(I)-catalyzed azide-alkyne cycloaddition (click chemistry). The morphology, structure, and composition of Fe3O4-DA-Maltose NPs were investigated by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), X-ray photoelectron spectrometer (XPS), and vibrating sample magnetometer (VSM). Meanwhile, hydrophilicity of the obtained NPs was evaluated by water contact angle measurement. The hydrophilic Fe3O4-DA-Maltose NPs were applied in isolation and enrichment of glycopeptides from horseradish peroxidase (HRP), immunoglobulin (IgG) digests. The MALDI-TOF mass spectrometric analysis indicated that the novel NPs exhibited high detection sensitivity in enrichment from HRP digests at concentration as low as 0.05 ng μL(-1), a large binding capacity up to 43 mg g(-1), and good recovery for glycopeptides enrichment (85-110%). Moreover, the Fe3O4-DA-Maltose NPs were applied to enrich glycopeptides from human renal mesangial cells (HRMC) for identification of N-glycosylation sites. Finally, we identified 115 different N-linked glycopeptides, representing 93 gene products and 124 glycosylation sites in HRMC.

Growth of transparent Zn1 - xSrxO (0.0 ≤ x ≤ 0.08) films by facile wet chemical method: Effect of Sr doping on the structural, optical and sensing properties

NASA Astrophysics Data System (ADS)

Rana, Amit Kumar; Das, Rajasree; Kumar, Yogendra; Sen, Somaditya; Shirage, Parasharam M.

2016-08-01

Zn1 - xSrxO (0.0 ≤ x ≤ 0.08) nano-rods thin films are prepared using simple wet chemical technique on transparent flexible substrate. Effect of Sr-doping on structural and optical properties of ZnO is systematically investigated. SEM and TEM confirm the nano-rods like morphology with single crystalline nature of all the samples. Rietveld refinement of XRD shows the samples belongs to P63mc space group, furthermore, a gradual increment in lattice parameters and change in Zn/oxygen occupancy ratio is observed with Sr doping. SIMS and XPS confirm the doping of Sr in the ZnO nanostructures. XPS measurements shows that increase in Sr doping creates more oxygen associated defects, which is further supported by the photoluminescence spectra indicating the gradual change in Zn vacancy (Vzn) and oxygen interstitial (Oin) point defect intensities in the films. Near band edge emission peak shows to shift toward higher wavelength in the doped films. Pure ZnO film shows Raman peaks around 99 (E2low), 333 (E2high - E2low) , 382 (A1 (TO)), 438 (E2high) and 582 (A1 (LO) +E1 (TO)) cm-1, whereas two additional defect driven vibrational modes (at 277 and 663 cm-1) are appeared in the Sr-doped films. The sensing property of the ZnO is enhanced by Sr doping and replicates as a promising material for future toxic and flammable gas sensor applications as well as for opto-electronic devices.

A novel dianionic amino acid ionic liquid-coated PEG 4000 modified Fe3O4 nanocomposite for the magnetic solid-phase extraction of trypsin.

PubMed

Yang, Qin; Wang, Yuzhi; Zhang, Hongmei; Xu, Kaijia; Wei, Xiaoxiao; Xu, Panli; Zhou, Yigang

2017-11-01

A novel magnetic extractant, PEG 4000 modified Fe 3 O 4 nanomaterial that coated with dianionic amino acid ionic liquid (Fe 3 O 4 @PEG@DAAAIL), was successfully synthesized and characterized. X-ray diffraction (XRD), transmission electron microscope (TEM), vibrating sample magnetometer (VSM), fourier transform infrared spectrometry (FT-IR), thermal gravimetric analysis (TGA) and zeta potentials were used to confirm that the novel nanocomposite was successfully synthesized. Subsequently, the prepared Fe 3 O 4 @PEG@DAAAIL nanocomposite was used as the extractant for trypsin coupled with magnetic solid-phase extraction (MSPE). The concentrations of trypsin in the supernatant were detected by UV-vis spectrophotometer at 278nm. The extraction ability turned out to be better than the other four kinds of extractants prepared in this work. Furthermore, the influence of a series of factors, such as extraction time and temperature, initial trypsin concentration, the value of pH and ionic strength, was systematically investigated. Under the optimal extraction condition, the extraction capacity for trypsin could reach up to 718.73mg/g, absolutely higher than that of other adsorbents reported. This satisfactory extraction capacity could be maintained unchangeable after at least eight days, and kept over 90% of initial extraction capacity after eight recycles. What's more, the activity of trypsin after extraction retained 92.29% of initial activity, verifying the biocompatibility of the prepared extractant. Finally, the developed Fe 3 O 4 @PEG@DAAAIL-MSPE method was successfully applied to the real sample analysis with satisfactory results. All of above proves the potential value of Fe 3 O 4 @PEG@DAAAIL-MSPE in the analysis of biomass. Copyright © 2017 Elsevier B.V. All rights reserved.

Measuring helium nano-bubble formation in tungsten with grazing-incidence small angle X-ray scattering

NASA Astrophysics Data System (ADS)

Thompson, Matt A. T.

The behaviour of helium in tungsten is an important concern for the fusion materials community. Under helium plasma exposure, small nano-scale bubbles form beneath the material surface as helium precipitates from the tungsten matrix. Under certain conditions this can lead to the subsequent formation of a surface "nano-fuzz", though the mechanisms of this process are not presently understood. For sub-surface nano-bubble formation transmission electron microscopy (TEM) has been the most widely used technique. While certainly a powerful technique, TEM suffers from a number of significant drawbacks: sample preparation is difficult and destructive, and there are sampling limitations as nano-structures must be located and characterised individually. This makes quantitative characterisation of nano-scale modification in tungsten challenging, which in turn makes it difficult to perform systematic studies on the effects of factors such as temperature and plasma composition on nano-scale modification. Here, Grazing Incidence Small Angle X-ray Scattering (GISAXS) is presented as a powerful addition to the field of fusion materials. With GISAXS, one can measure the X-ray scattering from nano-scale features throughout a relatively large volume, allowing information about full nano-bubble size distributions to be obtained from a simple, non-destructive measurement. Where it typically takes days or weeks to prepare a sample and study it under TEM, GISAXS measurements can be performed in a matter of minutes, and the data analysis performed autonomously by a computer in hours. This thesis describes the work establishing GISAXS as a viable technique for fusion materials. A GISAXS pattern fitting model was first developed, and then validated via comparison between GISAXS and TEM measurements of helium induced nano-bubble formation in tungsten exposed to a helium discharge in the large helical device. Under these conditions, nano-bubbles were found to follow an approximately exponential diameter distribution, with a mean nano-bubble diameters mu=0.596+/-0.001 nm and mu=0.68+/-0.04 nm computed for GISAXS and TEM, respectively. Depth distributions were also approximately exponential, with average bubble depths estimated at tau=9.1+/-0.4 nm and tau=8.4+/-0.5 for GISAXS and TEM, respectively. GISAXS was then applied to study the effects of plasma fluence, sample temperature and large transient heat and particle loads on nano-bubble formation. Nano-bubble sizes were found to saturate with increasing fluence at fluences less than 2.7x10. 24 He/m. 2 at 473 K. At higher temperatures larger nano-bubblesare able to form, suggesting a shift in the growth mechanisms, possibly from vacancy capture to bubble coalescence. Evidence is also presented which indicates that nano-bubble size distributions are qualitatively different for tungsten exposed to transient heat and particle loads due edge localised modes (ELMs) in the DIII-D tokamak, with a relatively large population of smaller (0.5-1 nm) nano-bubbles forming in this case. This is posited to be a consequence of rapid precipitation due to either extremely high helium concentrations during the ELM, or rapid cooling after it. Finally, synergistic effects between plasma composition and sample temperature are explored to determine which factors are most relevant for hydrogen and helium retention. Here, evidence has been found that helium ions from the plasma require a minimum energy of 9.0+/-1.4 eV in order to be implanted into tungsten. This was the dominant factor governing helium retention in this experiment. On the other hand, sample temperature is the dominant factor for hydrogen retention.

Performance of low-voltage STEM/TEM with delta corrector and cold field emission gun.

PubMed

Sasaki, Takeo; Sawada, Hidetaka; Hosokawa, Fumio; Kohno, Yuji; Tomita, Takeshi; Kaneyama, Toshikatsu; Kondo, Yukihito; Kimoto, Koji; Sato, Yuta; Suenaga, Kazu

2010-08-01

To reduce radiation damage caused by the electron beam and to obtain high-contrast images of specimens, we have developed a highly stabilized transmission electron microscope equipped with a cold field emission gun and spherical aberration correctors for image- and probe-forming systems, which operates at lower acceleration voltages than conventional transmission electron microscopes. A delta-type aberration corrector is designed to simultaneously compensate for third-order spherical aberration and fifth-order 6-fold astigmatism. Both were successfully compensated in both scanning transmission electron microscopy (STEM) and transmission electron microscopy (TEM) modes in the range 30-60 kV. The Fourier transforms of raw high-angle annular dark field (HAADF) images of a Si[110] sample revealed spots corresponding to lattice spacings of 111 and 96 pm at 30 and 60 kV, respectively, and those of raw TEM images of an amorphous Ge film with gold particles showed spots corresponding to spacings of 91 and 79 pm at 30 and 60 kV, respectively. Er@C(82)-doped single-walled carbon nanotubes, which are carbon-based samples, were successfully observed by HAADF-STEM imaging with an atomic-level resolution.

Microstructural analysis of 800H steel exposed at test operation in HTHL by using FIB-SEM and HRTEM techniques

NASA Astrophysics Data System (ADS)

Marušáková, Daniela; Bublíková, Petra; Berka, Jan; Vávrovcová, Zuzana; Burda, Jaroslav

2017-09-01

To understand the degradation process of metal materials which are used in power engineering, appropriate evaluation procedure is necessary to ensure. In that order, the degradation of alloy 800H during the first period of test operation in High Temperature Helium Loop (HTHL) was tested. Experiment was carried out in atmosphere of pure technical helium with purity 4.6 containing only residual concentration of moisture up to 300 vppm. Parameters during the operation test were not constant, process was interrupted several times. The maximum temperature on specimens during this period was 750 °C, average temperature was 460 °C, gas pressure ranged from 3 to 6 MPa and gas flow from 3 to 9 gs-1. Total duration of the test was 264 h. After the exposure the degradation of specimens was investigated by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). Using the technique of Focused Ion Beam (FIB) integrated within SEM the transparent samples with quality surface parameters were obtained for TEM analysis. FIB technique in combination with High Resolution TEM ensured the guaranteed methodology of exposed sample preparation and precise description of changes in this kind of material.

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

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.

Comparison of soil sampling and analytical methods for asbestos at the Sumas Mountain Asbestos Site-Working towards a toolbox for better assessment.

PubMed

Wroble, Julie; Frederick, Timothy; Frame, Alicia; Vallero, Daniel

2017-01-01

Established soil sampling methods for asbestos are inadequate to support risk assessment and risk-based decision making at Superfund sites due to difficulties in detecting asbestos at low concentrations and difficulty in extrapolating soil concentrations to air concentrations. Environmental Protection Agency (EPA)'s Office of Land and Emergency Management (OLEM) currently recommends the rigorous process of Activity Based Sampling (ABS) to characterize site exposures. The purpose of this study was to compare three soil analytical methods and two soil sampling methods to determine whether one method, or combination of methods, would yield more reliable soil asbestos data than other methods. Samples were collected using both traditional discrete ("grab") samples and incremental sampling methodology (ISM). Analyses were conducted using polarized light microscopy (PLM), transmission electron microscopy (TEM) methods or a combination of these two methods. Data show that the fluidized bed asbestos segregator (FBAS) followed by TEM analysis could detect asbestos at locations that were not detected using other analytical methods; however, this method exhibited high relative standard deviations, indicating the results may be more variable than other soil asbestos methods. The comparison of samples collected using ISM versus discrete techniques for asbestos resulted in no clear conclusions regarding preferred sampling method. However, analytical results for metals clearly showed that measured concentrations in ISM samples were less variable than discrete samples.

Comparison of soil sampling and analytical methods for asbestos at the Sumas Mountain Asbestos Site—Working towards a toolbox for better assessment

PubMed Central

2017-01-01

Established soil sampling methods for asbestos are inadequate to support risk assessment and risk-based decision making at Superfund sites due to difficulties in detecting asbestos at low concentrations and difficulty in extrapolating soil concentrations to air concentrations. Environmental Protection Agency (EPA)’s Office of Land and Emergency Management (OLEM) currently recommends the rigorous process of Activity Based Sampling (ABS) to characterize site exposures. The purpose of this study was to compare three soil analytical methods and two soil sampling methods to determine whether one method, or combination of methods, would yield more reliable soil asbestos data than other methods. Samples were collected using both traditional discrete (“grab”) samples and incremental sampling methodology (ISM). Analyses were conducted using polarized light microscopy (PLM), transmission electron microscopy (TEM) methods or a combination of these two methods. Data show that the fluidized bed asbestos segregator (FBAS) followed by TEM analysis could detect asbestos at locations that were not detected using other analytical methods; however, this method exhibited high relative standard deviations, indicating the results may be more variable than other soil asbestos methods. The comparison of samples collected using ISM versus discrete techniques for asbestos resulted in no clear conclusions regarding preferred sampling method. However, analytical results for metals clearly showed that measured concentrations in ISM samples were less variable than discrete samples. PMID:28759607

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.

EFFECT OF A SHORT PERIOD WHOLE BODY VIBRATION WITH 10 HZ ON BLOOD BIOMARKERS IN WISTAR RATS.

PubMed

Monteiro, Milena de Oliveira Bravo; de Sá-Caputo, Danúbia da Cunha; Moreira-Marconi, Eloá; Frederico, Éric Heleno Freire Ferreira; de Sousa-Gonçalves, Cintia Renata; Bernardo, Luciana Camargo; Guimarães, Carlos Alberto Sampaio; Bernardo-Filho, Mario

2017-01-01

Exposure to whole body vibration exercises (WBVE), besides some biological effects, causes alterations in the concentration of some blood biomarkers. The aim of this study is to evaluate the action of vibration (10 Hz) of WBVE on the concentration of blood biomarkers in Wistar rats. Wistar rats were divided in 2 groups. The experimental group (EG) was subjected to vibrations of 10Hz (one min per day, one week, total time of seven min), while the control group (CG) has not experienced vibration. Samples of whole blood were drawn for biochemical analysis of the concentration of total cholesterol, triglycerides, HDL, LDL, VLDL, glucose, CPK, albumin, alkaline phosphates, TGP, TGO, γGT, lipase, amylase, urea and creatinine. White blood cell count and a platelet-hemogram were also performed. Significant (p<0.05) increase in TGP, TGO and white blood cells and decrease in LDL concentration was found after exposure of 10Hz mechanical vibration. Although these findings were obtained with rats, they might contribute to try to understand better these mechanisms that occur following exposure to a frequency of 10Hz.

Concorde noise-induced building vibrations for Sully Plantation, Chantilly, Virginia

NASA Technical Reports Server (NTRS)

Mayes, W. H.; Scholl, H. F.; Stephens, D. G.; Holliday, B. G.; Deloach, R.; Holmes, H. K.; Lewis, R. B.; Lynch, J. W.

1976-01-01

A study to assess the noise-induced building vibrations associated with Concorde operations is presented. The approach is to record the levels of induced vibrations and associated indoor/outdoor noise levels in selected homes, historic and other buildings near Dulles and Kennedy International Airports. Presented is a small, representative sample of data recorded at Sully Plantation, Chantilly, Virginia during the period of May 20 through May 28, 1976. Recorded data provide relationships between the vibration levels of walls, floors, windows, and the noise associated with Concorde operations (2 landings and 3 takeoffs), other aircraft, nonaircraft sources, and normal household activities. Results suggest that building vibrations resulting from aircraft operations were proportional to the overall sound pressure levels and relatively insensitive to spectral differences associated with the different types of aircraft. Furthermore, the maximum levels of vibratory response resulting from Concorde operations were higher than those associated with conventional aircraft. The vibrations of nonaircraft events were observed in some cases to exceed the levels resulting from aircraft operations. These nonaircraft events are currently being analyzed in greater detail.

The vibrational spectrum and giant tunnelling effect of hydrogen dissolved in α-Mn

NASA Astrophysics Data System (ADS)

Kolesnikov, A. I.; Antonov, V. E.; Bennington, S. M.; Dorner, B.; Fedotov, V. K.; Grosse, G.; Li, J. C.; Parker, S. F.; Wagner, F. E.

1999-03-01

Vibrational spectra of α-MnH 0.07 and α-MnD 0.05 were studied by inelastic neutron scattering at temperatures from 1.7 to 200 K over a wide range of energy and momentum transfers. Together with the high-energy bands of the optical vibrations, pronounced peaks at 6.3 and 1.6 meV were observed in the spectra of the samples loaded with H and D, respectively. The study of the temperature, momentum-transfer and isotope dependence of the spectra demonstrated the tunnelling origin of these peaks.

Effects of diagnostic ionizing radiation on pregnancy via TEM

NASA Astrophysics Data System (ADS)

Mohammed, W. H.; Artoli, A. M.

2008-08-01

In Sudan, X-rays are routinely used at least once for measurements of pelvis during the gestation period, though this is highly prohibited worldwide, except for a few life threatening cases. To demonstrate the effect of diagnostic ionizing radiation on uterus, fetus and neighboring tissues to the ovaries, two independent experiments on pregnant rabbits were conducted. The first experiment was a proof of concept that diagnostic ionizing radiation is hazardous throughout the gestation period. The second experiment was done through Transmission Electron Microscopy (TEM) to elucidate the morphological changes in the ultra structure of samples taken from irradiated pregnant rabbits. This study uses TEM to test the effect of diagnostic radiation of less than 0.6 Gray on the cellular level. Morphological changes have been captured and the images were analyzed to quantify these effects.